Copyright by Brook Colleen Daun Riley 2004

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Copyright by Brook Colleen Daun Riley 2004

Transcript of Copyright by Brook Colleen Daun Riley 2004

Page 1: Copyright by Brook Colleen Daun Riley 2004

Copyright

by

Brook Colleen Daun Riley

2004

Page 2: Copyright by Brook Colleen Daun Riley 2004

The Dissertation Committee for Brook Colleen Daun Riley Certifies that this is the

approved version of the following dissertation:

LARAMIDE EXHUMATION AND HEATING IN SOUTHEASTERN ARIZONA:

LOW-TEMPERATURE THERMAL HISTORY AND IMPLICATIONS FOR ZIRCON FISSION-TRACK

SYSTEMATICS

Committee:

Mark Cloos, Supervisor

John I. Garver

Earle F. McBride

Randall Marrett

Raymond V. Ingersoll

George H. Davis

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LARAMIDE EXHUMATION AND HEATING IN SOUTHEASTERN ARIZONA:

LOW-TEMPERATURE THERMAL HISTORY AND IMPLICATIONS FOR ZIRCON FISSION-TRACK

SYSTEMATICS

by

Brook Colleen Daun Riley, B.S.

Dissertation

Presented to the Faculty of the Graduate School of

The University of Texas at Austin

in Partial Fulfillment

of the Requirements

for the Degree of

Doctor of Philosophy

The University of Texas at Austin

May, 2004

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Dedication

This dissertation is dedicated to Robert K. Goldhammer…he wouldn’t let me quit.

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Acknowledgements

“…exhumin’ things that’s better left alone.”

—Randy Travis, Storms of Life, 1986

That’s what this dissertation and this degree have been about: bringing up questions

that don’t have ready answers, figuring out the best way (or at least one way) to answer them,

and continually expanding one’s horizons in order to do that. But of course this did not happen

in a vacuum.

Geologic expertise and considerable financial assistance were contributed by Mark

Cloos. I am continually impressed by the extent of Mark’s knowledge of geology, and his

support of projects and ideas outside the general realm of tectonics, structure, and petrology.

When I first came to UT, and confessed that I had this idea about the Laramide of SE Arizona

that I wished to pursue, I was floored by Mark’s response: it was something along the lines of

“It’s your Ph.D….you should make it what you want.” I hadn’t ever experienced such open-

minded willingness to let me pursue what a friend once called the “last best chance to do what

you really want to do.” Mark always supported my research, both financially and in spirit. He

also recognized my ability to self-direct, and I was given my head very early in my course of

study.

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Of course that kind of freedom opened me up to a whole new world (and trouble!), some

of which I was ill-prepared to realize. Enter John Garver. I’ll bet that when he met me over a

beer in Lorne, Australia, he never would have realized the fundamental (‘crucial’ he might call it)

role he would play in this work. Simply put, there is no way that this dissertation would be what it

is without John, and it likely would not even have been possible in it’s current form without his

tremendous effort and patience. John is a talented mind, capable of seeing the best in

everything, and picking up on the thread that links seemingly disparate observations. This goes

a long way in your third year when you’re just about ready to throw in the towel should things not

begin to go your way. Perhaps the best thing about an advisor like John is having someone who

you can call, whenever, and they’re always ready to talk, about whatever. I always liked picking

up the phone in our office and hearing “Dude, John Garver here…this plot is cool!” I think one of

my acquaintances put it best after she met John at a GSA meeting recently: she gave him a hug

and said “Man, I wish you were my advisor!”

I must also thank my committee, each of whom was carefully selected for their expertise

in sedimentary petrology and diagenesis, brittle deformation, ‘the Laramide’ of southeastern

Arizona, and tectonics and sandstone petrology. Profs. Earle McBride, Randy Marrett, George

Davis, and Ray Ingersoll always proved available when needed, never blinked when my papers

didn’t come out on schedule, and were understanding as things took a turn for the unknown. I

could not have crafted a better committee.

Technical assistance was provided willingly and cheerfully by many people. Raman

spectroscopy proved to be one of the turning points in my work, and without the direction and

encouragement of Dr. Lutz Nasdala (University of Mäinz), breakthroughs might never have been

made. The road to crystallization ages and REE chemistries for The Holy Sample was paved by

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John Lansdown, Jim Connelly, and Kathy Manser, all from the University of Texas. Kitty

Milliken, also of UT, provided assistance with the SEM and CL, which laid the groundwork for the

Raman spectroscopy and laser analyses. Finally, Eric James always provided a ready ear for

some off-the-wall sedimentologist’s idea on recycling of Sierran arc-derived zircons or what Ce

anomalies really mean…subjects far outside my normal frame of reference.

Without the efforts of Philip Guerrero, Debra Sue Trinque, and Bill Woods, I wouldn’t

have been able to register, defend, graduate, pay my bills, or get anything administrative done.

A Ph.D. is a time-consuming, selfish, expensive, and strange thing to do, albeit

rewarding in the end. And many of us forget while we’re here that it is a choice: we choose this

path, whereas most people would turn tail when they realized what it was all about. And so I

must thank the following people for putting up with me while I did this to myself: Matthias Bernet,

Donna Cathro, Kara Dotter, Rob Forkner, Tim Gibbons, Kristin Goddard, Fabienne Grellet-

Tinner, Chris Hare, Dan Harrington, Jeff Harrison, Kim High, Brian Knight, Cori Lambert,

Graham Moss, J. Terrill Paterson, Barbara Tillotson, Keith Woodburne, and Richard Weiland. In

particular, when I was probably at my worst, Jason Poe saw me as ‘the best.’

Most deserving of thanks are Bill and Dianne Riley, who provided field assistance, home

base, encouragement, food, and who listened intently as I explained how a mass spec works

(sorry, Ma!).

Some of the most important people in my life while I’ve been at UT have been my

students. While in theory they have no choice but to pay attention to the person in front of them

and what that person tells them how to do, the truth is that learning and engaging are always a

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choice. It was often my refuge to enter the classroom or go into the field and discuss plunging

folds, cross-cutting relationships, and trough cross-strata, and always my pleasure to be a part of

that process. I thank each student with whom I had contact for that opportunity.

In parallel with this are the people for whom I taught. I learned more than I can express

about teaching field geology, mapping, structure, sedimentology, and field logistics from Mark

Helper, Earle McBride, Randy Marrett, Jim Connelly, and Bob Goldhammer. I very much

appreciate the opportunity to learn from and teach with these consummate professionals.

Projects like mine, which seed in the blurry head of an undergrad at the U of A, typically

are not funded by large NSF-style grants, and rely on many smaller contributions to complete

field work and analyses, in addition to the daily routine of eating and paying rent. Funding was

provided by the following entities: Department of Geological Sciences; Chevron Merit Fellowship

Program; Getty Oil Company Centennial Chair/Mark Cloos; Laura Thomson Barrow Graduate

Fellowship/Dr. Thomas D. Barrow; Gulf Coast Association of Geological Societies; Atlantic-

Richfield Company (ARCO); Society of Independent Professional Earth Scientists; Department

of Energy Reactor Use Sharing Program (DOE-RUS)/Steve Binney; BP-Amoco; Austin

Geological Society; Bowman Endowed Presidential Scholarship/Mr. John B. Payne; Geological

Society of America; University of Texas at Austin Continuing Fellowship Program; Wendler

Professional Development Fund.

Access was provided by the following: Fort Huachuca Army Intelligence Base, Fort

Huachuca, Arizona; KG Ranch, Canelo Hills, Arizona; Tom Hunt, Foreman, Rail X Ranch,

Patagonia, Arizona.

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LARAMIDE EXHUMATION AND HEATING IN SOUTHEASTERN ARIZONA:

LOW-TEMPERATURE THERMAL HISTORY AND IMPLICATIONS FOR ZIRCON FISSION-TRACK

SYSTEMATICS

Publication No._____________

Brook Colleen Daun Riley, Ph.D.

The University of Texas at Austin, 2004

Supervisor: Mark Cloos

Fission-track (FT) ages of zircon from Mesozoic sandstones were analyzed to address

provenance and post-depositional thermal history of Laramide synorogenic strata. Upper

Cretaceous samples show a complex provenance, with significant recycling from underlying

rocks. FT peak ages from 14 Jura-Cretaceous sandstones include populations of 570-165, 140-

82, and 68-42 Ma. Older single-grain ages (1000-600 Ma) indicate long-term sub-annealing

temperatures (<180°C, up to 260°C, depending on single-grain response to heating) for portions

of the source area. Older FT ages present in all sampled units indicate little burial of the Jura-

Cretaceous rocks prior to recycling into the Upper Cretaceous; record little variation in the

thermal signature of recycled crustal detritus; and show that the older Jurassic and Cretaceous

rocks likely provided an important source for the Fort Crittenden Formation. The uniformity of FT

ages necessitates that source rocks all record essentially the same thermal signatures.

Accordingly, the relative abundance of rock units in the source terrane was rather uniform, and

there was no preferential exhumation of one source area over another.

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Some zircons show evidence for significant post-depositional thermal annealing; these

strata reached temperatures sufficient to anneal fission tracks in some grains (c. 180°C-260°C).

Thicknesses of overlying units was likely less than 2 km; as such, the FT age structure is not

purely the result of burial. Regionally, samples with Paleocene-Eocene reset peak ages

coincide with proximity to magmatic bodies (75-40 Ma). Besides conductive heating, a

hydrothermal system may have locally modified these rocks, causing preferential resetting of

certain zircons. This setting provides an opportunity to investigate controls on single-grain

thermal response. Geochemical and crystallinity data indicate a correlation between old

crystallization ages, high U+Th concentrations, elevated alpha-damage, and young reset FT

ages. Resetting occurred in grains with higher radiation damage, and less damaged grains have

a higher temperature of track retention and therefore retain a primary detrital signature. Zircon

color is related in part to increasing radiation damage, and can be used for identifying different

thermal events in both the pre- and post-depositional history of individual zircons. In this study,

honey and colorless grains essentially behave as one population in all data sets. Based on

these data, this study establishes criteria for identifying reset grains in detrital populations, and

suggests revisions in the current methodology.

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Table of Contents

List of Tables .................................................................................................................... xiv

List of Figures.................................................................................................................... xv

List of Figures.................................................................................................................... xv

Chapter 1—Laramide exhumation and heating in southeastern Arizona: Low- temperature thermal history and provenance............................................................1

Abstract......................................................................................................................1

Introduction................................................................................................................3

Background/Methods/Sampling ................................................................................7

Early Laramide Sedimentation—Existing Age Constraints .............................7

Santa Rita Mountains/Canelo Hills ........................................................8

Huachuca Mountains ...........................................................................15

Sample Suite .................................................................................................16

Fission-track Analysis ....................................................................................17

Vitrinite Reflectance.......................................................................................19

Data/Observations...................................................................................................26

Fission-track Data..........................................................................................26

Young Reset Peak Ages......................................................................26

Provenance Ages.................................................................................29

Pb-Pb Geochronology ...................................................................................31

Mineralogic Provenance ................................................................................32

Diagenetic Overprint ......................................................................................33

Discussion ...............................................................................................................34

Age Data—Young Reset Peak Ages.............................................................34

Age Data—Static Peaks ................................................................................35

Pb-Pb Ages....................................................................................................38

Provenance of FT Samples, Prior Work ........................................................40

Diagenesis of Fort Crittenden Formation Samples, and Prior Work .............42

Regional versus Local Heating......................................................................42

Implications for Provenance of Fort Crittenden Formation and Changes in Thermal Structure through Time..........................................................47

Provenance..........................................................................................48

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Structural Constraints ..........................................................................49

Conclusions .............................................................................................................55

Chapter 2—Controls on the low-temperature thermal response of single detrital zircons: Temperature, crystallinity, and chemistry .................................................57

Abstract....................................................................................................................57

Introduction..............................................................................................................59

Methods...................................................................................................................62

Field Setting...................................................................................................62

Fission-track Analysis ....................................................................................64

Cathodoluminescence ...................................................................................65

Crystallinity.....................................................................................................69

Rare-Earth-Element Geochemistry and Pb-Pb Ages ....................................69

Data/Observations...................................................................................................71

Fission-track Data..........................................................................................71

Vitrinite-Reflectance Data ..............................................................................82

Pb-Pb Data from Color/Morphology Fractions...............................................85

Raman Microscopy Data ...............................................................................88

Effective Dose/Effective Dose Factor ..................................................96

FT Ages versus Minimum Damage Storage Ages.............................101

REE Data.....................................................................................................108

Discussion .............................................................................................................113

FT Age Data ................................................................................................113

Raman Crystallinity Data .............................................................................114

Overlapping Behavior: Honey vs. Colorless Zircons ..................................116

Activation Energy for Damage Annealing....................................................117

Criteria for Recognizing Reset Grains .........................................................118

Conclusions ...........................................................................................................123

Appendix 1—Age data for Upper Cretaceous and key post-Upper Cretaceous igneous rocks in southeastern Arizona ...............................................................127

Appendix 2—Sample suite field descriptions for fission-track work, Santa Rita and Huachuca Mountains, southeastern Arizona.........................................................131

Appendix 3—Description of techniques used in this study .............................................149

Fission-track Thermochronology ...........................................................................149

Cathodoluminescence...........................................................................................153

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Raman Microscopy................................................................................................154

U-Th-Pb and Rare-earth-element Analysis ...........................................................156

Appendix 4—Complete fission-track data for Jura-Cretaceous sandstone samples, Santa Rita and Huachuca Mountains, southeastern Arizona................................159

Appendix 5—Compositional data for Upper Cretaceous Fort Crittenden Formation sandstones, Santa Rita and Huachuca Mountains, southeastern Arizona ...........208

Appendix 6—Electron-microprobe analyses of 57 zircons from Station 23, Huachuca Mountains ..............................................................................................................209

References ......................................................................................................................213

Vita.…..............................................................................................................................222

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List of Tables

Table 1-1. Binomial fitted and χ2 fission-track peak ages for Mesozoic sandstone

samples from the Santa Rita and Huachuca Mountains, southeastern

Arizona. ......................................................................................................22

Table 2-1. Zircon color and morphology fractions, Station 23, Huachuca Mountains. ....66

Table 2-2. Single-grain fission-track ages (FTGA), Pb-Pb ages, effective uranium

concentrations (eU), and Raman crystallinity data (bandwidth and position)

for color fraction zircons from Station 23, Huachuca Mountains................67

Table 2-3. Fission-track peak ages from Station 23, Huachuca Mountains. ...................78

Table 2-4. Radiation damage dose data for color fraction zircons from Station 23,

Huachuca Mountains..................................................................................98

Table 2-5. Rare earth element concentration data (ppm) for color fraction zircons from

Station 23, Huachuca Mountains. ............................................................109

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List of Figures

Figure 1-1. Regional geologic map of southeastern Arizona (after Reynolds, 1988),

showing study areas in the Santa Rita and Huachuca Mountains)..............5

Figure 1-2. Generalized time-stratigraphic column for the Middle Jurassic-Paleogene

section, southeastern Arizona (column and lithologies after Hayes, 1970a,

1970b; Inman, 1982; Hayes, 1986, 1987; Inman, 1987; Dickinson and

others, 1989; Bassett and Busby, 1996). .....................................................6

Figure 1-3. Geologic map of the Huachuca Mountains (generalized after Hayes and

Raup, 1968) showing sample locations as part of the regional study..........9

Figure 1-4. Geologic map of the eastern flank of the Santa Rita Mountains,

southeastern Arizona (after Drewes, 1971a). ............................................10

Figure 1-5. Geologic map of the northern part of the Canelo Hills, southeastern

Arizona (after Drewes, 1980; Kluth, 1982; Reynolds, 1988). .....................13

Figure 1-6a. Qm-P-K, Qm-F-Lt, and Qp-Lv-Ls ternary plots from Inman (1987) for 10

Fort Crittenden Formation samples (shale member) from the Adobe

Canyon area, eastern Santa Rita Mountains. ............................................20

Figure 1-6b. Qm-P-K, Qm-F-Lt, and Qp-Lv-Ls ternary plots from Hayes (1987).............20

Figure 1-6c. Qm-P-K, Qm-F-Lt, and Qp-Lv-Ls ternary plots for 10 Fort Crittenden

Formation samples from the Huachuca and Santa Rita mountains from

this study. ...................................................................................................20

Figure 1-7. Pb-Pb age versus fission-track grain age (FTGA) for the same zircon

grains from Station 23, Huachuca Mountains. ...........................................25

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Figure 1-8. Huachuca and Santa Rita Mountains geologic maps (after Hayes and

Raup, 1968; Drewes, 1971) showing zircon fission-track peak ages (χ2

ages as noted; binomial fitted ages elsewhere) for sample sites included

in this study.................................................................................................28

Figure 1-9. Compositional ternary diagram for conglomerates in the Fort Crittenden

Formation (N = 27 clast counts; from Hayes, 1987)...................................51

Figure 1-10a. Idealized structural-sedimentologic scenario for the Fort Crittenden

Formation depositional period. ...................................................................53

Figure 1-10b. Evolution of 200°C isotherm during post-depositional magmatic activity

and subsequent burial by uppermost Cretaceous and younger volcanic

and sedimentary rocks. ..............................................................................53

Figure 2-1a. Generalized time-stratigraphic column for the Upper Jurassic-Upper

Cretaceous section, Huachuca Mountains, showing approximate

stratigraphic position of sample from Station 23 (column and lithologies

after Hayes, 1970a; Hayes, 1970b; Palmer, 1983; Hayes, 1986; Hayes,

1987; Dickinson and others, 1989).............................................................63

Figure 2-1b. Huachuca Mountains geologic map (generalized after Hayes and Raup,

1968) showing location of Station 23, sample locations as part of the

regional study. ............................................................................................63

Figure 2-2. Cumulative probability density (PD) plot and fitted for bulk zircon from

Station 23, Huachuca Mountains; peak ages fitted after Brandon (1996). 72

Figure 2-3. Cumulative probability density (PD) curves for zircon fractions from Station

23, Huachuca Mountains............................................................................73

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Figure 2-4. Cumulative probability distribution (PD) plot and fitted peaks for all counted

grains (bulk plus color fractions), Station 23, Huachuca Mountains; peak

ages fitted after Brandon (1996).................................................................74

Figure 2-5. Huachuca Mountains geologic map (generalized after Hayes and Raup,

1968) showing representative zircon fission-track peak ages from the

regional study. ............................................................................................77

Figure 2-6. Pb-Pb age versus fission-track age (FTGA) for the same zircon grains

from Station 23, Huachuca Mountains. ......................................................86

Figure 2-7. Full-width at half maximum (FWHM) versus Raman wave number for

color fractions from Station 23, Huachuca Mountains................................90

Figure 2-8. Full-width at half maximum (FWHM) versus U+Th concentration (effective

uranium, or eU (= U+Th in ppm)) for color fractions from Station 23,

Huachuca Mountains..................................................................................93

Figure 2-9. Full-width at half maximum (FWHM) versus fission-track grain age (FTGA)

for color fractions from Station 23, Huachuca Mountains. .........................95

Figure 2-10a. Comparison of color fractions from Station 23, Huachuca Mountains

with 'complete storage' line and analyses of 33 zircons considered to

have remained at sub-annealing temperatures since crystallization

(Nasdala and others, 2001)........................................................................97

Figure 2-10b. Comparison of effective dose factor with eU from color fraction zircons

from Station 23. ..........................................................................................97

Figure 2-10c. Effective dose factor compared to fission-track age of color fraction

zircons from Station 23...............................................................................97

Figure 2-10d. Effective dose compared to eU concentration for color fraction zircons

from Station 23. ..........................................................................................97

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Figure 2-10e. Comparison of effective dose to FT age for color fraction zircons from

Station 23. ..................................................................................................97

Figure 2-11a. Comparison of effective doses using those calculated from the fission-

track ages, and those calculated based on present crystallinities (from

Raman microprobe data, FWHM). ...........................................................102

Figure 2-11b. Comparison of minimum damage storage ages (based on Raman

microprobe data, FWHM) with fission-track ages. ...................................102

Figure 2-12. Normalized rare-earth-element data for color fraction zircons from

Station 23, Huachuca Mountains. ............................................................111

Figure 2-13. Qualitative relationship between time, alpha-damage, and effective

uranium (eU) concentration......................................................................119

Figure 2-14. Inferred relationship between annealing of fission tracks, annealing

temperature, and accumulated alpha-damage. .......................................124

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Chapter 1—Laramide exhumation and heating in southeastern Arizona: Low-temperature thermal history and provenance

ABSTRACT

Disagreement regarding patterns of Laramide deformation and basin development in SE

Arizona underlies the lack of a clear picture of exhumation and sediment recycling for

syntectonic basins in this area. Fission-track (FT) ages of zircon from Mesozoic sandstones

were analyzed to address the provenance and post-depositional thermal history of the

synorogenic strata. Samples from strike-normal transects across the Laramide basin boundary

within the Upper Jurassic-Upper Cretaceous section show a complex provenance, with

significant recycling from the underlying rocks. FT peak ages from 14 Jura-Cretaceous

sandstones include populations of 570-165, 140-82, and 68-42 Ma. Numerous older single-

grain ages (1000-600 Ma) are also present, indicating long-term sub-annealing temperatures

(less than perhaps 180°C, up to 260°C, depending on single-grain response to heating) for

portions of the source area. While most samples show a range of provenance ages, a small

fraction of grains shows evidence for significant post-depositional thermal annealing. Burial

depths were highly variable, but the cumulative thicknesses of units overlying the Jura-

Cretaceous section was likely less than 2 km. Accordingly, the zircon FT age structure present

in sandstone samples included in this study is not just the result of burial. Regionally, samples

with Paleocene-Eocene reset peak ages coincide with proximity to magmatic bodies ranging

from 75-40 Ma in age. Besides conductive heating, a hydrothermal system may have locally

modified these rocks, and caused preferential resetting of certain zircons. Older grain ages

present in all sampled units indicate little burial of the older Jurassic and Cretaceous rocks prior

to recycling into the Fort Crittenden Formation (Upper Cretaceous); record little variation in the

thermal signature of the recycled crustal detritus; and show that the older Jurassic and

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Cretaceous rocks likely provided an important sediment source for the Fort Crittenden

Formation. Prior work on the provenance of early Laramide sedimentary rocks in this area

documented the presence of primarily volcanic and granitic source rocks. The uniformity of FT

ages necessitates that source rocks, no matter their composition or age of

deposition/crystallization, all record essentially the same thermal signatures. Accordingly, during

the perhaps 10 m.y. of deposition of the Fort Crittenden Formation, the relative abundance of

different rock units in the source terrane was rather uniform, and it is likely that there was no

preferential exhumation of one source area over another.

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INTRODUCTION

Structural development and basin formation in the Laramide orogen in southeastern

Arizona present a longstanding problem in the regional geology of the southwestern U.S.

(Eardley, 1963; Coney, 1976; Krantz, 1989). Uncertain structural, kinematic, and sedimentologic

ties between the southern Laramide province and the classic Laramide province in Colorado and

Wyoming have led to contradictory tectonic models, as discussed in detail by Coney (1976) and

Krantz (1989). Two fundamental questions are basin-formation mechanisms and source-rock

exhumation histories. Additionally, confusion arises simply from terminology. Some workers

use the term ‘Laramide’ as a time descriptor (e.g. Coney, 1972; Davis, 1979), as a region (e.g.

Coney, 1972; Dickinson and Snyder, 1978), or as a structural style (e.g. Drewes, 1978, 1981,

1988a, 1988b; Dickinson and Snyder, 1978; Dickinson and others, 1988). In addition, the

spatially and temporally transgressive nature of deformation from west to east across western

North America, and across southern Arizona in particular, as well as different basement

anisotropies from place to place, should have caused variations in the style of Laramide

deformation. Consequently, no one style adequately describes structures in all areas (Dickinson

and Snyder, 1978).

In the context of this work, the term Laramide is broadly defined as the structural

development associated with ‘shallow-slab’ subduction beneath western North America

(Dickinson and Snyder, 1978). In concert with subduction-driven shortening, laterally restricted

foreland basins developed adjacent to locally uplifted and exhumed blocks along high- and low-

angle reverse faults. Deformation and magmatic activity associated with the progressive

decrease in the dip of the subducting slab were both temporally and spatially transgressive

(Dickinson and Snyder, 1978). However, as the area included in this study is relatively small,

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the time-transgressive nature of Laramide deformation is limited. Nonetheless, the superposition

of structures, and dating of these features, remains a problem.

Understanding basin formation and attendant processes must be based on knowledge

of relationships among fault activation and movement, exhumation of adjacent source areas, and

basin initiation and evolution. Modification of Laramide strata by subsequent deformation and

magmatism has complicated the picture, and seeing through that deformation proves difficult,

particularly where the major Laramide structures also have a younger history of movement (e.g.,

Sawmill Canyon fault zone, Santa Rita Mountains; Drewes, 1981). In general, these

relationships are more clearly defined for basins and associated source rocks in the classic

Laramide province (i.e. Chapin and Cather, 1983; Dickinson and others, 1988; Yin and Ingersoll,

1997), and in portions of the New Mexico segment of the belt (Seager and Mack, 1986; Mack

and Clemons, 1988). Understanding of these problems in southeastern Arizona is fragmentary,

and few studies within the southern Laramide province are linked regionally.

To better address thermal evolution and basin development in southeastern Arizona

during early Laramide sedimentation and subsequent magmatism, this study presents new

thermal and timing information obtained from zircon fission-track (FT) analysis with new and

existing provenance data for the Santa Rita and Huachuca mountains (Figure 1-1). Sample

suites from sandstones of Middle Jurassic through Late Cretaceous age (Figure 1-2) provide

new thermochronologic data, and traditional provenance analysis complements the

geochronology. Key factors in understanding Laramide thermal, tectonic, and basin

development in southeastern Arizona include the age of initial sedimentation; the timing of basin

subsidence; and the thermochronology of detrital grains which record the exhumation history of

the source areas.

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cks

U. C

reta

ce

ou

s-L

. E

oce

ne

gra

nito

ids

(me

talu

min

ou

s g

ran

ite

to

dio

rite

, su

b-

vo

lca

nic

po

rph

yritic r

ocks)

U. C

reta

ce

ou

s v

olc

an

ic r

ocks (

rhyo

litic

to a

nd

esitic

vo

lca

nic

ro

cks, lo

ca

lly

asso

cia

ted

su

bvo

lca

nic

in

tru

sio

ns,

se

dim

en

tary

ro

cks)

U. Ju

rassic

-Cre

tace

ou

s s

ed

ime

nta

ry

rocks, in

terc

ala

ted

vo

lca

nic

ro

cks

Ju

rassic

se

dim

en

tary

, vo

lca

nic

ro

cks

Ju

rassic

gra

nito

id r

ocks (

gra

nite

to

dio

rite

, lo

ca

l a

lka

line

ro

cks)

Pa

leo

zo

ic s

ed

ime

nta

ry r

ocks,

un

diffe

ren

tia

ted

Pe

nn

sylv

an

ian

-Pe

rmia

n s

ed

ime

nta

ry

rocks

Ca

mb

ria

n-M

issis

sip

pia

n s

ed

ime

nta

ry

rocks

M. P

rote

rozo

ic g

ran

ito

id r

ocks (

~1

40

0

Ma

)

L. P

rote

rozo

ic m

eta

se

dim

en

tary

ro

cks,

un

diffe

ren

tia

ted

me

tam

orp

hic

ro

cks

Jg

Tsn

Tsp

Tv Ti

KT

g

Kv

JK

s

Jsv

Pzu

IPP

Yg

Xm

s

CM

CM

JK

s

Fig

ure

1-1

. R

eg

ion

al g

eo

log

ic m

ap

of so

uth

ea

ste

rn A

rizo

na

(a

fte

r R

eyn

old

s, 1

98

8),

sh

ow

ing

stu

dy a

rea

s in

th

e S

an

ta

S A N T A R I T A M O U N T A I N S

C A N

E L O

H I

L L S

H U A

C H

U C

A

M O

U N

T A

I N S

Rita a

nd H

uachuca M

ounta

ins. F

ield

are

a for

this

stu

dy inclu

des e

xposure

s o

f th

e J

ura

-

Cre

tace

ou

s s

ectio

n (

port

ion

s o

f Jsv,

JK

s).

5

PATAGONIA

MOUNTAINS

Page 24: Copyright by Brook Colleen Daun Riley 2004

Sa

nta

Rit

a

Mo

un

tain

s

W E S T

E A S T

Hu

ac

hu

ca

Mo

un

tain

s

Apache C

anyon

Form

ation (

~250 m

)

Will

ow

Ca

nyo

nF

orm

ation (

~1300 m

)

Fort

Crittenden

Form

ation (

~1500 m

)

Sa

lero

Fm

.

vo

lca

nic

s

Turn

ey R

anch

Form

ation (

~1500 m

)

? ?

Sh

elle

nb

erg

er

Ca

nyo

nF

orm

ation (

~1000 m

)

Gla

nce

Co

ng

lom

era

te (

0-2

00

0 m

)

?

Te

mp

ora

l/B

ath

tub

Fo

rma

tio

ns

?

Helv

etia s

tocks/q

uart

z latite

plu

gs

Gre

ate

rvill

e p

lugs/q

uart

z latite

porp

hyry

Re

dM

ounta

inco

mp

lex

Grin

go

Gu

lch

plu

ton

/vo

lca

nic

s

Pa

tag

on

ia

Mo

un

tain

s

Ca

ne

lo

Hills

ce

ntr

al S

an

ta R

ita

hyd

roth

erm

al a

lte

ratio

n

Ele

ph

an

t H

ea

d/M

ad

era

Ca

nyo

n/

Jo

se

ph

ine

Ca

nyo

n in

tru

siv

es

Coro

na s

tock/q

uart

z d

iorite

E o

f M

t.F

agan R

anch

vo

lca

nic

s o

fD

ove

Ca

nyo

n/

tra

ch

ya

nd

esite

of M

ea

do

wV

alle

y

Cin

tura

Form

ation

(Bis

bee G

roup)

Fort

Crittenden

Form

ation

(~1200 m

)

?? ?

vo

lca

nic

s o

f

Jo

ne

s M

esa

Ju

rassic

vo

lca

nic

s o

f

Jo

ne

s M

esa

?

Cin

tura

Form

ation

(~2

90

m)

Fort

Crittenden

Form

ation (

~660 m

)

Mu

ral F

orm

atio

n(~

210 m

)

Gla

nce

co

ng

lom

era

te,

an

de

site

(0-6

30 m

)

?? ?

Morita

Form

ation

(~1270 m

)

Ca

ne

lo H

ills

vo

lca

nic

s

qu

art

z m

on

zo

nite

,ce

ntr

al H

ua

ch

uca

s??

50 M

a

60 M

a

70 M

a

80 M

a

90 M

a

110 M

a

120 M

a

130 M

a

163 M

a

150 M

a

140 M

a

100 M

a

APTIANALBIANCENOMANIAN

TU

RO

NIA

N

CO

NIA

CIA

N

SA

NT

ON

IAN

CAMPANIANMAASTRICHTIAN

LATE EARLY

CRETACEOUSE

AR

LY

LA

TE

EA

RLY

EOCENE PALEOCENE

PALEOGENETERTIARY

NEOCOMIAN

JURASSIC

LATE

Co

rra

l C

an

yo

nvo

lca

nic

s

?

Fig

ure

1-2

. G

enera

lized tim

e-s

tratigra

phic

colu

mn for

the M

iddle

Jura

ssic

-Pale

ogene s

ection,

south

easte

rn A

rizona

up

pe

r co

ng

lom

era

te

su

bu

nit

low

er

co

ng

lom

era

te

su

bu

nit

sh

ale

me

mb

er

tuff/u

pp

er

red

co

ng

lom

era

te m

em

be

r

low

er

red

co

ng

lom

era

te m

em

be

r

bro

wn

co

ng

lom

era

te m

em

be

r

sh

ale

me

mb

er

(colu

mn a

nd litholo

gie

s a

fter

Hayes, 1970a, 1970b; In

man, 1982; H

ayes, 1986, 1987; In

man, 1987;

Dic

kin

son a

nd o

thers

, 1989; B

assett a

nd B

usby,

1996).

T

imescale

of

Palm

er

(1983).

N

ote

that

these

are

com

posite c

olu

mns for

the e

ntire

are

a, and that all

form

ation a

nd intr

a-f

orm

ational boundaries a

re

tim

e-t

ransgre

ssiv

e in d

eta

il.

6

Bis

bee G

roup

Bis

be

e G

rou

p

Page 25: Copyright by Brook Colleen Daun Riley 2004

7

Most crucial is to define the source area for Laramide basin sediments, in terms of both

the thermal signature (low-temperature cooling histories of source terranes), as well as the

petrologic provenance. The focus of this study is the Upper Cretaceous Fort Crittenden

Formation (Figure 1-2), as it records the onset of Laramide sedimentation in this area (Dickinson

and others, 1989). It will be shown that the thermal signature and the provenance of sandstones

in the Fort Crittenden Formation can be related to that of the Jurassic and Lower Cretaceous

section.

BACKGROUND/METHODS/SAMPLING

Early Laramide Sedimentation—Existing Age Constraints

The depositional age of the Fort Crittenden Formation in the study area is 85-75 Ma

based on limited terrestrial faunal records and K-Ar dating of volcanic rocks stratigraphically

above and below the formation (Drewes, 1968; Hayes, 1970a; Hayes, 1970b; Inman, 1982;

Hayes, 1986; Dickinson and others, 1989). Based on measured sections and regional mapping

in the Santa Rita and Huachuca Mountains, early Laramide sedimentation is thought to have

ceased by the time of deposition of the Salero Formation volcanic rocks (Dickinson and others,

1989), dated at about 75 Ma (± 4 m.y.; K-Ar on biotite from multiple members of the formation,

detailed in Appendix 1; Drewes, 1968; Inman, 1982; Keith and Wilt, 1986).

Previous work on the regional depositional and stratigraphic relationships of the Fort

Crittenden Formation includes that of Inman (1982, 1987) and Hayes (1986, 1987). At the

regional scale in the Fort Crittenden Formation, Hayes’ work (1986) suggests the presence of

two separate depositional systems: one in the Santa Rita Mountains and Canelo Hills, which is

distinct from other Fort Crittenden Formation deposits in the Huachuca Mountains (Figure 1-1).

Lithologies in most sections define overall fining-upward sequences, which Hayes (1986)

Page 26: Copyright by Brook Colleen Daun Riley 2004

8

attributed to the destruction of tectonic relief. According to Hayes (1986), depositional

environments in the Santa Rita Mountains and Canelo Hills include middle alluvial fans, with

deposition by streamflood, sheet flood, and debris flow processes. In contrast, depositional

elements in the Huachuca Mountains section, best expressed at Brushy Canyon in the north-

central part of the range (Figure 1-3), show an evolution from alluvial fans to coarse braidplains,

capped at the top by marginal lacustrine mudflat deposits.

Santa Rita Mountains/Canelo Hills

The Fort Crittenden Formation (Upper Cretaceous) in the Santa Rita Mountains includes

five members defined by Drewes (1968). From oldest to youngest, these include the shale,

lower red conglomerate, brown conglomerate, upper red conglomerate, and tuff members

(Figure 1-2). The uppermost Cretaceous section unconformably overlies the Lower Cretaceous

Bisbee Group in the Santa Rita Mountains, but in many exposures, the formation is faulted

against Lower Cretaceous sedimentary and volcanic, Triassic-Jurassic igneous, Paleozoic

sedimentary, and Precambrian granitic rocks (Drewes, 1971a; Kluth, 1982). In the Adobe

Canyon area on the east flank of the range (Figure 1-4), there is a disconformity between the

Turney Ranch Formation (uppermost Bisbee Group) and the basal Fort Crittenden Formation

shale member (Inman, 1982; Hayes, 1986; Inman, 1987). According to Inman’s work (1982,

1987), the contact lacks the structural discordance suggested in previous studies (i.e. Drewes,

1971a, 1971b). In the Santa Rita Mountains, the Fort Crittenden Formation is locally

conformably overlain by the Maastrichtian Salero Formation (Drewes, 1971a, 1971b), composed

predominantly of dacitic volcanic and associated sedimentary rocks. The igneous rocks are

considered by most to reflect the encroachment of arc activity into southeastern Arizona during

the eastward sweep of magmatism associated with slab flattening (Hayes, 1970b; Coney,

Page 27: Copyright by Brook Colleen Daun Riley 2004

Kfc

Kc

Kc

Kg

aJh

?

Km

oK

ga

Kc

23

Kfc

Kc

Km

o

Km

u

Kc

Km

o

Km

o

Km

o

Km

u

Kg

Kg

Kg

aP

zu

Pzu

Kga

Kg

eK

ga

Pzu

e

Pzu

Pzu

Jh

Km

o

Kg

Pzu

Km

o

Kg

Kga

Kg

Km

oK

g

Km

u

Kc

Kfc

TQ

uK

b?

TQ

u

Km

o?

Tg

Tg

TQ

u

TQ

u

TQ

u

TQ

uTi

Ti

Km

o

pC

g

Tg

TQ

u

KfcTi

Pzu

eQg

Tg

Qal

TQ

u

Km

o

Km

u

Kc

Kg

a

Kg

Kb

pC

g

Jh

TJc

Te

rtia

ry a

nd

Qu

ate

rna

ry g

rave

ls,

allu

viu

m

Tert

iary

intr

usiv

es (

quart

z

mo

nzo

nite

, a

laskite

, g

ran

o-

dio

rite

, a

lka

li d

iorite

); in

tern

al

ag

e r

ela

tio

nsh

ips u

nce

rta

in

Up

pe

r C

reta

ce

ou

s F

ort

Critt

en

de

n

Fo

rma

tio

n (

ea

rly L

ara

mid

e b

asin

fill

)

Lo

we

r C

reta

ce

ou

s B

isb

ee

Gro

up

Ju

rassic

Ca

ne

lo H

ills

Vo

lca

nic

s a

nd

asso

cia

ted

rocks

Pa

leo

zo

ic s

ed

ime

nta

ry

rocks, e

xo

tic b

locks o

f

Pa

leo

zo

ic w

ith

in o

the

r u

nits

Pre

ca

mb

ria

n g

ran

ite

01

kilo

me

ters

mile

s0

1

fissio

n tra

ck s

am

ple

; S

tation 2

3 d

enote

d

vitrin

ite

sa

mp

le

Ro =

3.0

0%

(N

= 4

4)

Tm

ax 2

25

-30

0°C

Ro =

2.0

3%

(N

= 5

0)

Tm

ax 1

50

-25

0°C

fau

lt;

da

sh

ed

wh

ere

in

ferr

ed

an

ticlin

al tr

ace

; d

ash

ed

wh

ere

in

ferr

ed

,

plu

ng

ing

wh

ere

in

dic

ate

d

syn

clin

al tr

ace

; d

ash

ed

wh

ere

in

ferr

ed

,

plu

ng

ing

an

d/o

r o

ve

rtu

rne

d w

he

re in

dic

ate

d

co

nta

ct;

da

sh

ed

wh

ere

in

ferr

ed

Map

Un

its

Map

Sym

bo

ls

pC

g

pC

g

pC

g

pC

g

pC

g

Fig

ure

1-3

. G

eo

log

ic m

ap

of th

e H

ua

ch

uca

Mo

un

tain

s (

ge

ne

raliz

ed

aft

er

Ha

ye

s a

nd

Ra

up

, 1

96

8)

sh

ow

ing

sa

mp

le

Bru

sh

y C

an

yo

n

are

a

9

locations a

s p

art

of th

e r

egio

nal stu

dy.

V

itrinite-r

eflecta

nce d

ata

show

n a

dja

cent

to s

am

ple

loca

tio

ns (

Tm

ax e

stim

ate

s b

ased o

n v

itrinite-r

eflecta

nce d

ata

fro

m F

ort

Critt

enden F

orm

ation

silt

sto

ne

/sh

ale

sa

mp

les, in

terp

rete

d a

fte

r H

éro

ux a

nd

oth

ers

, 1

97

9; S

tap

lin, 1

98

2; B

urn

ha

m

an

d S

we

en

ey,

19

89

; B

ark

er

an

d P

aw

lew

icz, 1

99

4).

TJh

TJc?

TJc?

TJc

TJc

TJh

TJc

TJh

TJh

TJc

TJh

TJh

11

113°

112

°111°

110

°3

36

°

35

°

34

°

33

°

32

°114°

113

°

112

°

111°

110°

37

°

36

°

35°

34

°

33

°

32

°

Page 28: Copyright by Brook Colleen Daun Riley 2004

pCg

Kbw

KbaTQg

Ti

Kba

Kbt

Kbw

Kbg

Pzu

pCg

Kfs

Kflr

Kfb

Kfur

Kft

Jbu

Jbm

Jbl

Jtu

Jtm

Jtl

Js

Tp

Tg

Tw

Tqd

Tg

Kiu

Jtlm

Kbt

Pzu

Kfb

Tg

Tw

Tw

Tqd

TQg

Jtu

Jtu

Jbl

Jbm Jbu

Tp

Js

Tp

Jtm

Jtlm

Jtl

Jbl

Ti Tg

Jtm

Kbt

Kflr

Kfur

KbtKflr

KfbTertiary-Quaternary gravel and conglomerate,

undifferentiated

Paleocene? Gringo Gulch Volcanics

Tertiary intrusive rocks (associated with Gringo

Gulch Volcanics, Oligocene Grosvenor Hills

Volcanics)

uppermost Cretaceous intrusive rocks

(associated with Elephant Head Quartz Monzonite)

Upper Cretaceous

Fort Crittenden

Formation (early

Laramide basin

fill)

Lower Cretaceous

Bisbee Group

Middle Jurassic

Bathtub Formation

Middle Jurassic

Temporal Formation

Triassic? Mount Wrightson Formation

Jurassic Squaw Gulch Granite (Lower Jurassic?)

Triassic? quartz diorite

Triassic? Piper Gulch Monzonite

Triassic? Gardner Canyon Formation

Paleozoic sedimentary rocks, undifferentiated

Precambrian granite

0 1

kilometers

miles0 1

Ti

upper red conglomerate member/

tuff member

brown conglomerate member

lower red conglomerate member

shale member

TQg

Figure 1-4. Geologic map of the eastern flank of the southern Santa Rita Mountains, south-

fission track sample

vitrinite sample

fault; dashed where inferred

anticlinal trace; dashed where inferred,

plunging where indicated

synclinal trace; dashed where inferred,

plunging and/or overturned where indicated

contact; dashed where inferredMap Symbols

quartz vein

Map Units

mine location

eastern Arizona (after Drewes, 1971a). Vitrinite-reflectance (VR) datashown adjacent to sample locations (Tmax estimates based on vitrinite-

reflectance data from Fort Crittenden Formation siltstone/shale samples,

interpreted after Héroux and others, 1979; Staplin, 1982; Burnham and

Sweeney, 1989; Barker and Pawlewicz, 1994).

10

Adobe

Canyon

area

Sa

wm

ill

Ro = 2.26% (N = 50)

Tmax 200-250°C

Ro = 0.77% (N = 7)

Tmax 85-135°C

Fa

ult

Ca

nyo

nZ

on

e

114° 113° 112° 111° 110°37°

36°

35°

34°

33°

32°114°

113°

112°

111° 110°

37°

36°

35°

34°

33°

32°

xx x

x

x x

x

x

x

xxx

x

x

xx

xx

x

Page 29: Copyright by Brook Colleen Daun Riley 2004

11

1978; Dickinson and others, 1978). In most locations, however, Tertiary and Quaternary gravels

rest in angular unconformity atop the Fort Crittenden Formation.

The shale member represents deposition in a lacustrine setting, with gradual

progradation of fan deltas into the lacustrine basin (Inman, 1982). The lowermost 55 meters of

the shale member is a volcaniclastic pebble to boulder conglomerate (referred to as the basal

conglomerate by Inman (1982)), reflecting availability of volcanic detritus early in the depositional

history of the Fort Crittenden Formation. The abundance of recycled volcanic material contrasts

with the upper portions of the Bisbee Group that record a source with significant monocrystalline

quartz, and increasing but minor recycled volcanic detritus upsection (Inman, 1987). The

remaining ~180 meters of the shale member are interbedded channel sandstone, and

interdistributary and lacustrine mudstone and shale. A lack of structural discordance (Inman,

1982) has led some workers to suggest that the hiatus between the Bisbee Group and the Fort

Crittenden Formation lasted at most 10-15 m.y. (Inman, 1987; Dickinson and others, 1989).

The contact between the shale member and the lower red conglomerate member (~485

meters thick; Hayes, 1986) is gradational, where lacustrine deposits grade vertically into alluvial-

fan facies deposited as the basin filled (Inman, 1982; Hayes, 1986). The brown conglomerate

(~660 meters thick; Hayes, 1986) intertongues with both the lower red conglomerate member

and the upper red conglomerate member (Drewes, 1968). Both the brown and lower red

conglomerates have similar composition, texture, sedimentary structures, and scales and styles

of interbedding (Hayes, 1986), although the brown conglomerate is coarser toward the top than

the lower red conglomerate, and is overall finer grained throughout the rest of the section.

Page 30: Copyright by Brook Colleen Daun Riley 2004

12

Additionally, both conglomerates show an increase in recycled sedimentary detritus, as well as

intercalated volcanic tuff, toward the top of the respective sections.

The brown and upper red conglomerate members (minimum 355 m; Hayes, 1986)

intertongue along the eastern flank of the Santa Rita Mountains. The upper red conglomerate is

composed almost entirely of recycled sedimentary material, including clasts of muddy to pebbly

sandstone, sandy mudstone, and pebble to cobble conglomerate (Hayes, 1986, 1987); the

interpreted source for this recycled sedimentary material is the Lower Cretaceous Bisbee Group.

Hayes (1986) also stated that the upper red conglomerate coarsens upward, and appears to

display upward-thickening and coarsening trends low in the section. Hayes (1986) considered

facies of all the conglomerate members to be similar, and inferred that the upper portions of the

brown conglomerate member, and entirety of the upper red conglomerate member tapped

mainly sedimentary sources. Intercalated tuffs (<5 meters thick) are increasingly common

upsection into the upper tuff member. Both Drewes (1971b) and Hayes (1986) observed that

tuffs within the section thicken to the west, suggesting that these locations were closer to the

source.

In the Canelo Hills (Figure 1-5), the Fort Crittenden section is more faulted and very

limited in exposure (Kluth, 1982; Hayes, 1986), leading to difficulty in correlation of adjacent

sections along the flanks of the range and with sections in the Santa Rita and Huachuca

Mountains. Individual members, as defined in the Santa Rita or Huachuca Mountains sections

(Figure 1-2), have not been identified here. Mapping by Kluth (1982) indicates that limited

exposures of the Fort Crittenden Formation crop out in two separate major fault blocks, along the

northeastern and northwestern flanks of the range (Figure 1-5). The formation rests in

disconformity atop the Lower Cretaceous Cintura Formation (part of Kbu on Figure 1-5) in the

Page 31: Copyright by Brook Colleen Daun Riley 2004

Kr?

TQu

Pzu

TJu

TJu

Kr?

Kbu

Ka

Klvs TJu

Klvs?Ks

Pzu

TQu

KTi

TJu

TJu

TJu

TQu KTi

Pzu

Pzu

Pzu

Pzu

Pzu

Pzu

Pzu

Kbu

TQuPzu

Ks

KTi

Pzu

TQu

Ka

Kbu

Tertiary and Quaternary gravels and

alluvium, undifferentiated

Cretaceous-Tertiary volcanic and

intrusive rocks (rhyolite, andesite flows;

intercalated pyroclastic/epiclastic

rocks; associated quartz monzonite and

granodiorite stocks, latite porphyries)

Upper Cretaceous Fort Crittenden

Formation (early Laramide basin fill)

Lower Cretaceous Bisbee Group,

undifferentiated

Triassic and Jurassic volcanic and

clastic rocks; includes portions of the

Canelo Hills Volcanics

Paleozoic sedimentary

rocks, undivided

fault; dashed where inferred

anticlinal trace; dashed where

inferred

synclinal trace; dashed where

inferred

contact; dashed where inferred

Map Units

Map Symbols

TJu

Kr

andesitic volcanic rocks; includes

portions of Salero Formation

rhyodacite, welded tuff; includes

portions of Salero Formation

TQuTQu

Kbu

Ks

TQu

Lower Cretaceous andesitic to rhyolitic

volcanic rocks, conglomerate,

sandstone

Klvs

0 1kilometers

miles0 1

TQu

TQu

Ks

Ks

Figure 1-5. Geologic map of the northern part of the Canelo Hills, southeastern Arizona (after

Drewes, 1980; Kluth, 1982; Reynolds, 1988).

13

114° 113° 112° 111° 110°37°

36°

35°

34°

33°

32°114°

113°

112°

111° 110°

37°

36°

35°

34°

33°

32°

Page 32: Copyright by Brook Colleen Daun Riley 2004

14

O’Donnell Canyon area (east side of range; Figure 1-5). The Fort Crittenden Formation

conformably overlies the Corral Canyon andesite (part of Klvs on Figure 1-5; 75 Ma; K-Ar on

biotite; Hayes, 1987; all cited ages from sources prior to 1976 have been corrected after

Dalrymple (1979; refer to Appendix 1)) along the west flank of the range, and is interbedded

with volcanic and volcaniclastic rocks at the base of this section (Hayes, 1987). Hayes (1987)

pointed out that the Corral Canyon section is very similar in composition and depositional style to

the lower red conglomerate member of the Fort Crittenden Formation in the Santa Rita

Mountains. Volcanic activity is also indicated toward the end of, and immediately following, the

Fort Crittenden depositional period in the Canelo Hills, similar to the relationships documented in

the Huachuca Mountains. In the area of Jones Mesa, a unit informally termed the Jones Mesa

volcanics (Hayes, 1970b; part of Kr, Ks on Figure 1-5) overlies the Fort Crittenden Formation and

has been dated at 72 Ma (K-Ar on biotite; Hayes, 1970b). Additional evidence for volcanism

during the same period includes the Dove Canyon volcanics (73 Ma; K-Ar on biotite; Marvin and

others, 1973; Marvin and others, 1978) and the Meadow Valley trachyandesite (74 Ma; K-Ar on

biotite; Marvin and others, 1973; Marvin and others, 1978). Outside the Jones Mesa area, the

exposed top of the section is a fault contact with Jurassic Canelo Hills volcanics, or is overlain by

Tertiary and Quaternary gravels (Figure 1-5). The ages of overlying and underlying volcanic

rocks suggest that deposition of the Fort Crittenden Formation may have been short-lived in the

Canelo Hills. It is also possible that this is the case elsewhere, as there are no radiometric ages

other than those in the Canelo Hills section that constrain the age of the base of the formation

more accurately than post-Albian (the cited age for Bisbee Group sediments younger than the

Mural Formation; Figure 2; Hayes (1986), Dickinson and others (1989)). Because of the lack of

complete sections, and highly faulted nature of Canelo Hills sections and exposures, Fort

Crittenden Formation samples are not included in this discussion. The preceding discussion

Page 33: Copyright by Brook Colleen Daun Riley 2004

15

serves to provide a more complete picture for the Fort Crittenden Formation in the central part of

the field area.

Huachuca Mountains

Partial sections of the Fort Crittenden Formation are exposed along the western flank of

the Huachuca Mountains (Figure 1-3); the most complete section lies along Brushy Canyon, in

the north-central part of the range, where the section is 675 meters thick (Hayes, 1986). Two

informal members were assigned to the Fort Crittenden section in this area by Hayes (1970a);

these include the basal conglomerate (divided into a lower and upper conglomerate) and shale

members. The basal contact is locally an angular unconformity with the Lower Cretaceous

Cintura Formation, and regionally a poorly exposed disconformity. The lower subunit of the

basal conglomerate member is present only in the northwestern Huachuca Mountains and, along

with the upper red conglomerate in the Santa Rita Mountains, is the only part of the section rich

in recycled sedimentary detritus (Hayes, 1986, 1987). The upper part of the basal conglomerate

is similar in character to the lower conglomerate subunit, but tends to display better rounding and

sorting, suggestive of increasing textural maturity up-section. The upper conglomerate subunit

contains approximately equal portions of recycled sedimentary, volcanic, and granitic clasts.

The contact between the basal member and the shale member is gradational.

As discussed above, the Fort Crittenden Formation marks the onset of sedimentation

associated with Laramide deformation. In general, the textural and sedimentologic

characteristics of the Fort Crittenden Formation are in marked contrast to older synorogenic

rocks such as the Lower Cretaceous Glance conglomerate (Bilodeau, 1978; Vedder, 1984), the

Upper Jurassic Temporal and Bathtub formations (Drewes, 1968, 1971b; Bassett and Busby,

1996), and the Upper Jurassic red bed deposits of the Canelo Hills volcanics (Davis and others,

Page 34: Copyright by Brook Colleen Daun Riley 2004

16

1979). The Fort Crittenden Formation is texturally and compositionally more mature than the

older Cretaceous and Jurassic synorogenic basin fill (Bilodeau, 1978; Davis and others, 1979;

Inman, 1982; Hayes, 1986). Additionally, there is no evidence for direct fault control on

sedimentation in terms of clast size, composition, or mechanism of derivation, as present in the

Glance conglomerate, the Temporal and Bathtub formations, and the Canelo Hills volcanics

(Bilodeau, 1978; Davis and others, 1979; Bassett and Busby, 1996). The finer and more mature

nature of the Fort Crittenden Formation requires that new approaches be taken to understand its

provenance.

Sample Suite

Samples from the Middle Jurassic Temporal and Bathtub formations, the Lower

Cretaceous Bisbee Group, and the Upper Cretaceous Fort Crittenden Formation (Figure 1-2)

comprise the basis for the geochronology, provenance, and vitrinite-reflectance data sets

included in this study (Appendix 2). Most samples are composed of approximately 10 kg of

sandstone with little to no pebble content; rarely, samples contained a granule to pebble fraction

up to 20% of the total volume where this is representative of the sample interval. Key sampling

areas are adjacent to the fault zones along the western flank of the Huachuca Mountains, and

the Sawmill Canyon fault zone along the eastern flank of the Santa Rita Mountains (Figure 1-3;

Figure 1-4), in addition to other control points throughout the region. Where possible, a

complete Middle Jurassic through Cretaceous section was sampled along a strike-normal

transect.

The Jura-Cretaceous section in this part of southeastern Arizona records the

progression from arc volcanism associated with Sevier deformation through backarc region

extension associated with deposition of the Bisbee Group, through segmentation of the Sevier

Page 35: Copyright by Brook Colleen Daun Riley 2004

17

foreland and development of smaller basins associated with Laramide contraction (Dickinson

and others, 1989). These transitions in tectonic setting are demonstrated within the

clastic/volcaniclastic and minor carbonate rocks in the form of changes in sedimentation

style/volume, depositional environment, and provenance, both mineralogic and thermal. The

Jura-Cretaceous section was deformed and intruded during the Laramide (Figure 1-3 and 1-4).

The area chosen for this study is the best possible for determining the thermal state of the crust

prior to exhumation and recycling of the upper crust and accumulation of Laramide basin fill.

Laramide basin-fill rocks are relatively well-exposed here, and fairly complete Jura-Cretaceous

sections are present (c.f. Inman, 1982; Hayes, 1986). These two factors enable the petrologic

and thermal character of the Fort Crittenden Formation to be thoroughly evaluated and

compared to potential source terranes. Additionally, the study area lies within the uplift/basin-

bounding fault zone recognized by Davis (1979), thus providing the most direct record of the

evolution of these sediment-source couples. It was discovered that some samples show

evidence for post-depositional heating such that a few zircons were reset by annealing.

Consequently, a derivative study was undertaken to document fission-track response of zircons

to post-depositional heating (Chapter 2).

Fission-track Analysis

Thermal and temporal information, critical to the understanding of source area

exhumation and recycling and central to the understanding of subsequent thermal events, is

provided by fission-track analysis. The closure temperature for the FT chronometer in zircon has

been proposed to be 235°C ± 25°C (Brandon and Vance, 1992), but as shown in Chapter 2, may

be as low as ~180°C or so, depending on single-grain response to heating due primarily to

radiation damage. The temporal information obtained from the FT data at temperatures between

180°C-260°C is unique to this system. In concert with FT samples from the Laramide basin fill

Page 36: Copyright by Brook Colleen Daun Riley 2004

18

(Fort Crittenden Formation), traditional mineralogic provenance from these sandstones was used

to evaluate the nature of source rocks. Point counts (300 counts per section) were made on thin

sections impregnated with blue epoxy and stained for potassium feldspar for each of the Fort

Crittenden Formation samples (Figure 1-3, 1-4), and ternary plots of these data appear in Figure

1-6.

Each sandstone sample (~10 kg of material) was crushed and milled, then separated

using a Wilfley table, heavy liquids, and a Frantz magnetic separator. The zircon separate was

obtained from the methylene iodide sinks, 1.7 A non-magnetic fraction. A small portion of this

material was prepared for fission-track dating, with approximately 2000-3000 grains per mount in

two Teflon mounts. All zircon fractions were mounted and etched according to the procedures in

Garver and others (2000). Mounts were etched in a KOH:NaOH eutectic at 228°C for between 5

and 17 hours to adequately represent the widest possible spectrum of grain types, ages, and U

contents (i.e. Naeser and others, 1987). All zircon mounts were irradiated at the Oregon State

University Reactor Facility, with a requested thermal neutron fluence of 2 x 1015 n/cm2.

According to methods described in Naeser (1976) and Garver and Brandon (1994), pre-

annealed mica sheets were attached to grain mounts prior to irradiation, and were removed and

etched to reveal induced fission tracks following irradiation. All mounts were counted at 1250x

using a dry 100x objective (10x oculars, 1.25x tube factor) on a Zeiss Axioskop microscope fitted

with an automated stage/digitizing tablet. Refer to Appendix 3 for further procedure and data

reduction information. Zircon FT peak ages and 95% confidence intervals for data from 30-60

dated zircon grains per sample appear in Table 1-1. Peak ages were fitted using the binomial

fitting method of Brandon (1996).

Page 37: Copyright by Brook Colleen Daun Riley 2004

19

For the Station 23, Huachuca Mountains sample (Figure 1-3), a small portion of the zircon

separate was prepared for traditional fission-track dating as described above, with approximately

2000-3000 grains in each of two Teflon mounts (bulk sample). The remaining zircons were then

hand-picked into three distinct color fractions. Fractions include light to dark pink and purple

zircons (fraction p; ~5% of total yield), colorless zircons (fraction c; ~20% of total yield), and

honey zircons (fraction h; ~75% of total yield); refer to Chapter 2, Table 1-1 for further detail.

Zircon fractions from this sample, as well as the original bulk zircon material, were mounted and

etched as described above. The original bulk mounts were etched for 17 hours (long etch) and

12 hours (short etch); the pink/purple fraction was etched under the conditions described above

for 5 hours. The colorless and honey fraction yield was high enough to allow two mounts each,

for which the long etch was 10 hours, and the short etch was 5 hours. All suitable grains in each

of the color mounts were counted, yielding a total of 57 single-grain FT ages for color mounts,

combined with the 60 single-grain ages from the unpicked bulk sample. For the zircon color

grain mounts, other analyses shed light on single-grain response to modest heating (150°C-

225°C), and the control of accumulated α-damage on the FT closure temperature (Chapter 2).

Pertinent to the present discussion are Pb-Pb ages from these FT-dated zircons, which appear

plotted versus corresponding FT grain ages in Figure 1-7. This detailed study is described

here only to the extent that these data bear on the exhumation and recycling histories for these

rocks.

Vitrinite Reflectance

To independently estimate the maximum temperatures reached by these sandstones,

interbedded Fort Crittenden Formation mudrocks were sampled where possible for analysis of

vitrinite reflectance (VR; analyses made by D. O’Connor at Baseline DGSI, The Woodlands,

Page 38: Copyright by Brook Colleen Daun Riley 2004

craton interiortransitional continental

quartzose recycled

mixed

transitional recycled

lithic recycled

undissected arctransitional arc

basement uplift

dissected arc

Qm

F Lt

Qm

LtF

Figure 1-6a. Qm-P-K, Qm-F-Lt, and Qp-Lv-Ls ternary plots from Inman (1987) for 10 Fort

a.

b.

Qm

F Lt

Qm

P K

Qp

LsLv

c.

Santa Rita Mountains samples Huachuca Mountains samples

Qp

Lv Ls

Qm

P K

Inman (1987)

n = 10

Hayes (1987)

n = 70

this study

n = 10

Crittenden Formation samples (shale member) from the Adobe Canyon area,

eastern Santa Rita Mountains. Qm = monocrystalline quartz; P =

plagioclase; K = potassium feldspar; F = plagioclase + potassium feldspar;

Lt = total lithic fragments; Qp = polycrystalline quartz (excluding micro-

crystalline quartz); Lv = volcanic lithic fragments; Ls = sedimentary lithic

Figure 1-6b. Qm-P-K, Qm-F-Lt, and Qp-Lv-Ls ternary plots from Hayes (1987). Compositional

ranges for Fort Crittenden Formation samples from the Huachuca

Mountains Brushy Canyon section (n = 24) and Santa Rita Mountains

(n = 46) are plotted.

samples from the Huachuca and Santa Rita mountains from this study.

fragments. Key from Dickinson and others (1983).

Figure 1-6c. Qm-P-K, Qm-F-Lt, and Qp-Lv-Ls ternary plots for 10 Fort Crittenden Formation

20

Map locations on Figures 1-3, 1-4.

0 10 20 30 40 50 60 70 80 90 100

0

10

20

30

40

50

60

70

80

90

100

K

Qm

P

0

10

20

30

40

50

60

70

80

90

100

0 10 20 30 40 50 60 70 80 90 100

0

10

20

30

40

50

60

70

80

90

100

Ls

Qp

Lv

0

10

20

30

40

50

60

70

80

90

100

0 10 20 30 40 50 60 70 80 90 100

0

10

20

30

40

50

60

70

80

90

100

Lt

Qm

F

0

10

20

30

40

50

60

70

80

90

100

Page 39: Copyright by Brook Colleen Daun Riley 2004

21

Texas). As temperature increases, the reflectance of vitrinite fragments also increases, and the

Ro value, or mean reflectance, rises; the relationship between maximum temperature (Tmax) and

Ro is linear or nearly so (Price, 1983). Average Ro values, based on 20-50 measurements

per sample, were used to define maximum temperature bounds for interbedded mudrocks;

these average values are shown adjacent to sample locations in Figures 1-3 and 1-4.

In the northern and central Huachuca Mountains, mudrocks in the lower part of the Upper

Cretaceous Fort Crittenden Formation were sampled at three separate locations adjacent to FT

sampling stations. Unfortunately, siltstone and shale near Station 23 are highly oxidized, and

accordingly a maximum temperature estimate for these rocks was not obtained. Shales and

siltstones farther north at a similar stratigraphic interval contain un-oxidized vitrinite. The

average Ro values for these sites are 3.00% and 2.03%, and correspond to peak temperature

estimates of 225-300°C and 150-250°C, respectively (interpreted after Héroux and others, 1979;

Staplin, 1982; Burnham and Sweeney, 1989; Barker and Pawlewicz, 1994). Because the

estimate of peak temperature from Ro values varies somewhat, a range of peak temperature

values associated with a given Ro measurement is reported here. In the eastern Santa Rita

Mountains, Tmax for interbedded siltstones are available from two sites within the Fort Crittenden

Formation. Station 43, within interbedded siltstone of the brown conglomerate member of the

Fort Crittenden Formation has an Ro value of 2.33%, corresponding to a peak temperature

estimate of 200-250°C. A sample from Station 66 (Fort Crittenden Formation shale member)

yielded only 7 un-oxidized vitrinite fragments, which record an Ro value of 0.77%, corresponding

to a Tmax of 85-135°C.

These estimates provide an independent measure of the maximum paleotemperature,

Page 40: Copyright by Brook Colleen Daun Riley 2004

Tab

le 1

. B

inom

ial fitt

ed a

nd χ

2 f

issio

n t

rack p

eak a

ges f

or

Mesozoic

sandsto

ne s

am

ple

s f

rom

the S

anta

Rita a

nd H

uachuca M

ounta

ins,

south

easte

rn A

rizona.

P1

P2

P3

P4

P5

P6

2 a

ge

(M

a)

SA

NT

A R

ITA

MO

UN

TA

INS

Mid

dle

Ju

ras

sic

Te

mp

ora

l F

orm

atio

n

Sta

tio

n 3

3p

ea

k a

ge

(M

a)

55

—8

21

23

——

—n

= 2

7 (

27

)9

5%

c.i.

(+/-

; m

.y.)

6/5

8/7

10

/10

% o

f g

rain

s2

0.4

37

.44

2.2

Lo

we

r C

reta

ce

ou

s T

urn

ey R

an

ch

Fo

rma

tio

n S

tatio

n 3

8p

ea

k a

ge

(M

a)

——

11

21

75

56

6—

—n

= 4

4 (

14

/30

)9

5%

c.i.

(+/-

; m

.y.)

14

/12

32

/27

18

9/1

43

% o

f g

rain

s4

8.6

43

.48

.0

Up

pe

r C

reta

ce

ou

s F

ort

Cri

tte

nd

en

Fo

rma

tio

n,

up

pe

r re

d c

on

glo

me

rate

me

mb

er

Sta

tio

n 4

2p

ea

k a

ge

(M

a)

52

—1

11

—2

76

——

n =

60

(3

0/3

0)

95

% c

.i.

(+/-

; m

.y.)

23/16

9/9

39

/34

% o

f g

rain

s1.8

65

.53

2.7

Mid

dle

Ju

ras

sic

Ba

thtu

b F

orm

atio

n

Sta

tio

n 4

4p

ea

k a

ge

(M

a)

52

—9

91

67

——

—n

= 5

1 (

30

/21

)9

5%

c.i.

(+/-

; m

.y.)

5/4

12

/11

29

/25

% o

f g

rain

s2

7.2

47

.22

5.6

Up

pe

r C

reta

ce

ou

s F

ort

Cri

tte

nd

en

Fo

rma

tio

n s

ha

le m

em

be

r S

tatio

n 5

2p

ea

k a

ge

(M

a)

——

——

——

15

7

n =

13

(1

3)

95

% c

.i.

(+/-

; m

.y.)

18

/16

% o

f g

rain

s5

4

HU

AC

HU

CA

MO

UN

TA

INS

Up

pe

r C

reta

ce

ou

s F

ort

Cri

tte

nd

en

Fo

rma

tio

n S

tatio

n 9

pe

ak a

ge

(M

a)

42

68

10

7—

——

—n

= 2

9 (

12

/17

)9

5%

c.i.

(+/-

; m

.y.)

12

/98

/71

7/1

5

% o

f g

rain

s7

.26

5.2

27

.6

χ

22

Page 41: Copyright by Brook Colleen Daun Riley 2004

χ

HU

AC

HU

CA

MO

UN

TA

INS

, co

ntin

ue

d

P1

P2

P3

P4

P5

P6

2 a

ge

(M

a)

up

pe

rmo

st

Ju

ras

sic

-Lo

we

r

Cre

tac

eo

us

Gla

nce

co

ng

lom

era

te

Sta

tio

n 1

1p

ea

k a

ge

(M

a)

——

92

12

1317

——

n =

42

(3

0/1

2)

95

% c

.i.

(+/-

; m

.y.)

9/8

13

/12

70/58

% o

f g

rain

s5

1.5

43

.84.8

Up

pe

r C

reta

ce

ou

s F

ort

Cri

tte

nd

en

Fo

rma

tio

n S

tatio

n 1

3p

ea

k a

ge

(M

a)

—6

0—

13

8—

——

n =

31

(2

4/7

)9

5%

c.i.

(+/-

; m

.y.)

6/6

17

/15

% o

f g

rain

s5

6.7

43

.3

Lo

we

r C

reta

ce

ou

s C

intu

ra F

orm

atio

n

Sta

tio

n 1

4p

ea

k a

ge

(M

a)

——

10

6—

23

68

03

—n

= 3

3 (

11

/3/5

/14

)9

5%

c.i.

(+/-

; m

.y.)

13

/12

22

/20

20

1/1

63

% o

f g

rain

s2

0.9

60

.91

8.2

Up

pe

r C

reta

ce

ou

s F

ort

Cri

tte

nd

en

Fo

rma

tio

n S

tatio

n 2

3

bu

lk s

am

ple

pe

ak a

ge

(M

a)

—6

09

11

39

——

—n

= 6

0 (

30

/30

)9

5%

c.i.

(+/-

; m

.y.)

8/7

10

/91

8/1

6

% o

f g

rain

s1

7.3

48

.62

9.1

fra

cti

on

pp

ea

k a

ge

(M

a)

—6

3—

17

5—

——

n =

14

95

% c

.i.

(+/-

; m

.y.)

9/8

19

/17

% o

f g

rain

s2

7.3

72

.7

fra

cti

on

cp

ea

k a

ge

(M

a)

——

78

12

0—

——

n =

30

(1

9/1

1)

95

% c

.i.

(+/-

; m

.y.)

7/7

11

/10

% o

f g

rain

s4

5.6

51

.1

fra

cti

on

hp

ea

k a

ge

(M

a)

—7

0—

11

8—

——

n =

22

(1

6/6

)9

5%

c.i.

(+/-

; m

.y.)

6/5

12

/11

% o

f g

rain

s5

8.8

41

.2

bu

lk +

fra

cti

on

sp

ea

k a

ge

(M

a)

—5

98

01

28

——

—n

= 1

27

95

% c

.i.

(+/-

; m

.y.)

7/6

7/7

10

/9

% o

f g

rain

s1

1.4

37

.24

6.6

23

Page 42: Copyright by Brook Colleen Daun Riley 2004

χ

HU

AC

HU

CA

MO

UN

TA

INS

, co

ntin

ue

d

P1

P2

P3

P4

P5

P6

2 a

ge

(M

a)

Up

pe

r C

reta

ce

ou

s F

ort

Cri

tte

nd

en

Fo

rma

tio

n lo

we

r co

ng

lom

era

te s

ub

un

it

Sta

tio

n 4

5p

ea

k a

ge

(M

a)

——

10

41

71

353

——

n =

26

(6

/3/1

3/4

)9

5%

c.i.

(+/-

; m

.y.)

9/8

17

/16

115/87

% o

f g

rain

s5

0.0

42

.47.6

Up

pe

r C

reta

ce

ou

s F

ort

Cri

tte

nd

en

Fo

rma

tio

n u

pp

er

co

ng

lom

era

te s

ub

un

it

Sta

tio

n 4

6p

ea

k a

ge

(M

a)

——

—1

37

——

—n

= 1

8 (

4/1

3/1

)9

5%

c.i.

(+/-

; m

.y.)

11

/10

% o

f g

rain

s1

00

Up

pe

r C

reta

ce

ou

s F

ort

Cri

tte

nd

en

Fo

rma

tio

n s

ha

le m

em

be

r S

tatio

n 4

7p

ea

k a

ge

(M

a)

——

——

——

19

0

n =

59

5%

c.i.

(+/-

; m

.y.)

32

/27

% o

f g

rain

s8

0

Up

pe

r C

reta

ce

ou

s F

ort

Cri

tte

nd

en

Fo

rma

tio

n S

tatio

n 4

9p

ea

k a

ge

(M

a)

——

——

——

10

9

n =

5 (

1/4

)9

5%

c.i.

(+/-

; m

.y.)

17

/14

% o

f g

rain

s8

0

No

tes:

Bin

om

ial fitt

ed

an

d χ

2 f

issio

n t

rack p

ea

k a

ge

s a

nd

95

% c

on

fid

en

ce

in

terv

als

fo

r zir

co

n f

rom

14

sa

nd

sto

ne

sa

mp

les in

th

e S

an

ta R

ita

an

d H

ua

ch

uca

Mo

un

tain

s.

n =

nu

mb

er

of

gra

ins

co

un

ted

(w

he

re m

ore

th

an

on

e n

um

be

r is

cite

d,

firs

t is

to

tal n

um

be

r co

un

ted

; su

bse

qu

en

t n

um

be

rs a

re n

um

be

rs o

f g

rain

s c

ou

nte

d f

rom

su

cce

ssiv

ely

sh

ort

er

etc

he

s).

Bin

om

ial p

ea

k f

ittin

g m

eth

od

(B

ran

do

n,

19

96

); P

1 =

fitte

d p

ea

k 1

; P

2 =

fitte

d p

ea

k 2

, e

tc.

24

Page 43: Copyright by Brook Colleen Daun Riley 2004

Pb-Pb age vs. Fission-track grain age

100

200

300

400

500

600

700

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200

Pb-Pb age (Ma)

FT

GA

(M

a)

pink/purple (N = 14 grains)

colorless (N = 22 grains)

honey (N = 20 grains)

Figure 1-7. Pb-Pb age versus fission track grain age (FTGA) for the same zircon grains from

depositional

age of sample

Station 23, Huachuca Mountains. Cited uncertainties for Pb-Pb ages are 1

standard deviation, and 95% confidence intervals for FT ages.

25

Page 44: Copyright by Brook Colleen Daun Riley 2004

26

and indicate that peak temperatures in the northern Huachuca Mountains were higher than

suspected during sampling for FT work (up to ~225°C vs. <120°C). Rock characteristics as seen

in the field did not suggest that these sandstones and conglomerates were thermally altered.

Most samples from this area are only moderately indurated and have almost no quartz cement.

Another notable feature, considering the presence of nearby Tertiary plutons is a lack of veining.

Most importantly, the locations with elevated peak temperature values generally correspond well

with locations of sandstone samples containing young reset FT peak ages and/or reset single-

grain ages throughout the northwestern and west-central parts of the Huachuca Mountains.

Similar relationships occur in the Santa Rita Mountains.

DATA/OBSERVATIONS

Fission-track Data

As discussed in previous sections, the sample suite for this regional study includes

Middle Jurassic through Upper Cretaceous clastic and volcaniclastic rocks (Table 1-1; Appendix

2). The most important feature of these data is that despite the 100 m.y. range in depositional

age or varying location of the studied units, all samples have a similar suite of fission-track peak

ages (Figure 1-8). The following observations are pertinent to this discussion.

Young Reset Peak Ages

Given the range of depositional ages in the study area, FT ages younger than the

depositional age of the sample must be due to annealing and resetting of the fission-track

grain ages (FTGA). In many samples, regardless of depositional age, FT ages younger than

the age of the Fort Crittenden Formation (85-75 Ma; Drewes, 1968; Hayes, 1970a, 1970b;

Inman, 1987; Hayes, 1987; Dickinson and others, 1989) are also common (Figure 1-8). As

discussed in previous sections, partially reset samples in some cases occur in proximity to

Page 45: Copyright by Brook Colleen Daun Riley 2004

27

exposed igneous bodies (e.g. Station 23, Huachuca Mountains; Figure 1-8), but there is no

obvious spatial variation in FTGA with respect to the distribution of exposed Laramide igneous

rocks.

Very young reset peak ages (42-55 Ma) are present in most samples from Santa Rita

Mountains, whereas peaks this young are present in only one sample from the

northern Huachuca Mountains (Fort Crittenden Formation). This younger reset peak age is

composed by as much as 2% to 27% of counted grains in a given sample. An intermediate

young peak age of approximately 65 Ma is common in Huachuca Mountains samples, but not in

samples farther to the west.

Young intermediate peak ages between 85-75 Ma are present in a sample from the

Middle Jurassic Temporal Formation, Santa Rita Mountains and in a sample from the Upper

Cretaceous Fort Crittenden Formation, Huachuca Mountains (Figure 1-8; Table 1-1). In the case

of the Jurassic volcaniclastic sample, this population represents either full resetting of some

zircon FT ages around 82 Ma, or partial resetting of older FTGA associated with heating at ~60

Ma. A peak of this age could be related to any of the following: exhumation at the beginning of

the Laramide; thermal resetting associated with magmatism slightly older than the Fort

Crittenden Formation (i.e. Corral Canyon volcanics, Canelo Hills; 75 Ma, K-Ar on biotite; Hayes,

1987; Appendix 1); or partial resetting of an older FT age by either of the two previously

mentioned mechanisms.

In the case of the Fort Crittenden Formation sample with the 80 Ma peak age, discussed

in greater detail in Chapter 2, there are two possibilities for the significance of this peak age: (1)

a volcanogenic source transitional in age between the Bisbee Group and the Fort Crittenden

Page 46: Copyright by Brook Colleen Daun Riley 2004

pCg

Kbw

Kba

Kbt

Pzu

Kfb

Tg

Tw

Tw

Tqd

QTg

Jtu

Jtu

Jbl

Jbm Jbu

Tp

Js

Tp

Jtm

Jtlm

Jtl

Jbl

Ti Tg

Jtm

KfsKbt

Kflr

Kfur

KbtKflr

Kfb

0 1

kilometers

miles0 1

TiQTg

#942 Ma 68 Ma

107 MaN = 29

#2359 Ma80 Ma

128 MaN = 127

#1192 Ma121 Ma

N = 42

#1360 Ma138 MaN = 31

#49χ2 age:

109 MaN = 5

#46137 Ma

N = 18

#45104 Ma171 Ma

N = 26

#14106 Ma236 Ma803 Ma

N = 33

#47χ2 age:

190 MaN = 5

#38 112 Ma175 Ma566 Ma

N = 44

#40 no countable

grains

#42 111 Ma276 Ma

N = 60

#51 no countable

grains

#61 no countable

grains

#44 52 Ma 99 Ma167 Ma

N = 51

#33 55 Ma 82 Ma 123 Ma

N = 27

#36 no countable

grains

#52χ2 age:

157 MaN = 13

Kfc

Kc

KcKga

Jh?

KmoKga

Kc

Kfc

Kc

Kmo

Kmu

Kc

Kmo

Kmo

Kmo

Kmu

Kg

Kg

Kga Pzu

Pzu

Kga

Kg

eKga

Pzu

Kmo

Kg

KmoKg

Kmu

Kc

Kfc

TQu Kb?

TQu

Tg

Tg

TQu

TQu

TQu

Ti

Ti Kmo

pCg

JTh?

JTc

JTc

JTh

JTh

JTc

JTc?

JTc?

0 1

kilometers

miles0 1

pCg

pCg

pCg

Figure 1-8. Huachuca and Santa Rita Mountains geologic maps (after Hayes and Raup, 1968;

reset FTGA

reset FTGA

Drewes, 1971) showing zircon fission-track peak ages (χ2 ages as noted;

binomial fitted ages elsewhere) for sample sites included in this study.

Statistical peak ages are based on approximately 30-60 dated grains per

sample, except where χ2 age is given. Boxes around sample locations

indicate evidence for resetting in sample. Refer to Appendix 4 for further

28

detail on peak ages, uncertainties, and single-grain age data.

x

xx

xx

x

xxx

x

x

xx

x

xx

xx

Page 47: Copyright by Brook Colleen Daun Riley 2004

29

Formation; and/or (2) partially to fully reset older FT ages. Based on constraints from the Pb-Pb

data for this sample, which indicate that all crystallization ages from the FT-dated zircons are

>170 Ma (Figure 1-7), these grains are not first-cycle volcanic zircons associated with early

Laramide volcanism (i.e. units such as the Corral Canyon volcanics, Canelo Hills; Appendix 1).

Pb-Pb ages of the FT-dated grains instead favor the interpretation that this peak is composed of

partially to fully reset older FT ages, probably associated with burial and heating related to

eastward migration of the arc across southern Arizona during the early Laramide (Coney, 1978;

Dickinson and Snyder, 1978; Keith, 1978). Refer to the next section of this chapter and

Chapter 2 for a complete discussion of this sample.

Provenance Ages

There is clear evidence for Paleogene heating and associated annealing in some

samples (Figure 1-8; Appendix 1, 4). Cooling to sub-annealing temperatures (<180°C) occurred

during the Paleocene and Eocene. As such, there is potential for partial resetting in any of the

samples. Accordingly, peak ages older than the depositional age of the sample are termed

minimum provenance ages, or minimum ages for cooling in the source terrane. As discussed in

detail in Chapter 2, grains with varying levels of radiation damage, and thus different effective

closure temperatures, are present in different populations of zircon from a single sample. This

effect makes certain zircons more susceptible to resetting, allowing for partial resetting of an

older component. However, it is doubtful that these older FT ages have been completely reset.

If older FTGA were dominated by resetting, it is unlikely that these older peak ages would be so

similar throughout all samples, and that older ages would represent such a large proportion of

the total grains counted.

Page 48: Copyright by Brook Colleen Daun Riley 2004

30

Zircon FT ages that comprise these older pre-depositional peaks, as well as very old

single-grain FT ages, generally constitute between 30 and 100% of the total number of grains

counted (Appendix 4). Peaks defined by the older FT ages show a fairly narrow dispersion of

ages among the different samples, all of which are consistent with derivation from similar

sources supplying detritus to the Bisbee basin (i.e. related to arc magmatism, or related to

exhumation associated with formation of the Bisbee basin). Finally, peaks with these older ages,

and older widely varying single-grain FT ages, are present in every sample in the study. In the

case of partially resetting an older age component, as discussed in greater detail in Chapter 2,

one might expect the following: (1) a smaller percentage of grains would have the reset peak

age(s); and (2) a wider spread of partially reset ages within the field area and a lack of

consistency of peak ages among samples (depending on the location and timing of heating, and

the susceptibility of a zircon to resetting; Chapter 2). One would not expect a partially reset FT

peak age to be so consistent and ubiquitous throughout the sample suite and field area. Rather,

partially reset FT peak ages would vary spatially depending on the mechanism of resetting (for

example, resetting by local magmatism/hydrothermal activity, or by burial). The key observation

is that rocks that have remained relatively cool (those without any obvious evidence for resetting,

likely remaining at temperatures <180°C) have similar ages for the pre-depositional peaks as

those rocks with clear evidence for Paleogene resetting. As such it is likely that a significant

amount of provenance information has remained unaffected.

Older peak ages, in the range 90-175 Ma, are common to all samples in varying

abundances, and generally represent most of all grains counted, no matter the depositional age

of the sample (Table 1-1; Figure 1-8). Scattered older peak ages are present in a few samples

(for example, in the Turney Ranch Formation and in the upper red conglomerate member of the

Fort Crittenden Formation in the Santa Rita Mountains; Table 1-1). It is also noteworthy that

Page 49: Copyright by Brook Colleen Daun Riley 2004

31

nearly every sample retains grains with very old FT ages, even those samples that also contain

a young reset peak age (e.g. Stations 13, 38, 44, 45, 46; Table 1-1; Appendix 4). These older

peak ages and older single-grain ages indicate that some portion of the source area for Middle

Jurassic-Cretaceous rocks in this area remained below temperatures of 180-260°C, depending

on single-grain response to heating.

Pb-Pb Geochronology

One of the key questions is whether syn-depositional volcanic zircons are present in the

samples. A lack of such zircons is indicated by the FT ages of samples from Stations 9, 13, 42,

47, 49, 46, and 45. These samples have peak ages that are generally 25-200 m.y. older than

the depositional age of the Fort Crittenden Formation (Table 1-1). Pb-Pb ages for FT-dated

grains from Station 23 in the Huachuca Mountains (Figure 1-3) assist in defining the source of

zircons with a given cooling age, but confirm a lack of syn-depositional volcanic zircon.

Zircons with 90-170 Ma FT ages could be arc-derived first- or second-cycle grains,

having been derived from either the arc or recycled from the Bisbee Group or older Jurassic

volcanogenic strata. Alternatively, if these grains have older crystallization ages their FT ages

could have been reset during arc-related magmatism and/or exhumation and block faulting

associated with formation of the Bisbee basin (Hayes, 1970b; Bilodeau, 1978, 1979; Dickinson

and others, 1986; Klute, 1987). Additionally, crystallization ages help determine the age of

granitic source terranes that supplied detritus to the Fort Crittenden Formation (Inman, 1982;

Hayes, 1986). Precambrian granite or Mesozoic granite are possible sources, in terms of both

exhumation and provenance. This possibility feeds back into the question of understanding what

part of the crust was being exhumed and recycled, and when these sediments were shed into

the basin.

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32

Two main groups of Pb-Pb ages occur in FT-dated zircons in the Station 23 sample: the

pink/purple suite is dominantly Proterozoic, ranging from 1200 to 2000 Ma, whereas colorless

and honey-colored zircons from the same sample have a variety of Pb-Pb ages, the majority of

which range from 160 to 720 Ma (Figure 1-7). An older group of both honey and colorless

zircons is also present, with six ages from 1300 to 1800 Ma overlapping with the pink/purple

series. A key discovery from the Pb-Pb data is that syndepositional, probably volcanogenic,

zircons are not present in this particular sample.

Mineralogic Provenance

Sandstones in the Fort Crittenden Formation are typically lithic-rich (Figure 1-6; Inman,

1982; Hayes, 1986). Compositional data for ten Fort Crittenden Formation sandstones from the

current study are compared with compositions of sandstones from the work of Inman (1987) in

the Santa Rita Mountains (shale member, Fort Crittenden Formation), and with sandstone

compositions from Hayes (1987) in the Santa Rita and Huachuca Mountains (including all

members and subunits of the formation in both ranges) (Figure 1-6).

Most Fort Crittenden Formation samples are lithic rich (Figure 1-6; Inman, 1982; Hayes,

1986). Lithic framework components include plutonic rock fragments (PRF), dominant volcanic

rock fragments (VRF), with many unidentified rock fragments (URF) also present. The latter are

problematic in that such grains could be highly altered VRF, sedimentary rock fragments (SRF),

or feldspar. Samples were stained for potassium feldspar, but due to alteration of feldspars to

clays, accurate identification of grain type sometimes proved difficult.

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33

Petrographic observations from this study are generally in keeping with those of Hayes

(1986, 1987) and Inman (1982, 1987) (Figure 1-6). However, due to sample size (10 Fort

Crittenden Formation samples included in this study), data presented here vary somewhat from

that of larger sample suites such as those of Inman (1982) and Hayes (1986). Most sandstone

samples are lithic rich, particularly VRF and quartzose PRF, with subordinate to subequal

populations of SRF. Carbonate rock fragments (CRF) are rare. Monocrystalline quartz has

multiple potential sources. Vein quartz, plutonic quartz, and metamorphic quartz were identified,

based on grain properties (extinction character, presence or absence of inclusions).

Polycrystalline quartz likely also has both metamorphic and plutonic provenance.

Microcrystalline quartz is sparse to rare, and where present, relict ghost textures commonly

suggest volcanogenic provenance. Both VRF and PRF are abundant in samples included in this

study, but unaltered plagioclase is rare, and generally subordinate to potassium feldspar (Figure

1-6).

Diagenetic Overprint

Each of the sampled Fort Crittenden Formation units clearly has an extensive, and in

some cases complicated, diagenetic history, also noted in Hayes (1986). The description

included herein is not intended to review burial histories in exhaustive detail, but rather to

highlight those points pertinent to the thermal history of the samples, which is critical to

interpreting the FT data.

The most clear common thread among the FT-dated samples is abundant evidence for

relatively early compaction. This is indicated by a lack of cementation, and by quartz grains and

other competent framework grains indenting less competent grains, such as potassium feldspar,

lithic fragments, plagioclase, and in some cases, other quartz grains. Further evidence exists in

Page 52: Copyright by Brook Colleen Daun Riley 2004

34

samples such as that from sandstone of the lower red conglomerate member in the Santa Rita

Mountains (Figure 1-4), where mudclasts were deformed into pseudomatrix around more

competent framework types. Compaction in the majority of these samples occurred early, prior

to cementation, and generally limited the opportunity for cementing fluids to later infiltrate

remaining primary or secondary pore space. As such, carbonate and quartz cements are poorly

developed, and primary pore space is nearly obliterated. Secondary pore space is generally

limited to dissolution of feldspars. Dissolution of framework, pseudomatrix, and cement on the

whole is uncommon throughout the suite, and porosities are low (on the order of 1-2%).

The most commonly altered framework types are VRFs, PRFs with high feldspar

content, and feldspar grains. Alteration within VRFs includes chloritization, minor dissolution,

and replacement by patchy, fine-grained carbonate cement (calcite ± dolomite). Alteration of

PRFs is generally restricted to the feldspathic portion of the grain, and typically involves

conversion to clays; replacement by calcite along grain rims and cleavage planes, followed by

patchy replacement by calcite within grain interiors; and dissolution. Where replacement by

calcite is more extensive (on the order of 2-5% of total thin section), quartz within PRFs is locally

replaced. Alteration of single-grain feldspars is similar to that demonstrated by feldspar within

PRFs.

DISCUSSION

Age Data—Young Reset Peak Ages

Younger reset peak ages (42-55 Ma; Figure 1-8; Table 1-1) are common in the Santa

Rita Mountains, but are lacking in most of the Huachuca Mountains samples. These peak ages

could document different ages of magmatic activity in the two ranges. However, this cannot be

properly addressed because Tertiary igneous rocks in the Huachuca Mountains are undated.

Page 53: Copyright by Brook Colleen Daun Riley 2004

35

Most importantly, as discussed more completely in Chapter 2, it is possible that there are varying

responses to modest heating (150°-225°C or so), depending on the character of zircons in the

sample. For example, single-grain differences in the amount of accumulated α-damage can

allow certain grains to respond differently to heating. Alternatively, the presence of the younger

reset peak ages in the Santa Rita Mountains could signify contrasting cooling regimes: if one

area cooled more rapidly than the other, or remained at elevated temperatures longer than the

other, this could produce differences in the ages of reset zircons. However, this case is unlikely

as the FT data indicate that thermal annealing and subsequent Paleocene-Eocene cooling of

some portion of most samples was widespread through the study area, and thus that elevated

temperatures of at least 150°C were probably a regional feature (Figure 1-8; Appendix 4).

As a corollary to the preceding discussion, intermediate young reset peak ages of

approximately 65 Ma are present in Huachuca Mountains samples, but not in Santa Rita

Mountains samples (Figure 1-8; Table 1-1). Again, this poses several questions: (1) did the

Santa Rita Mountains samples cool more slowly, thereby producing younger FT peak ages?; (2)

did the Santa Rita Mountains experience higher peak temperatures? (3) does the difference in

FT peak ages indicate different episodes of magmatic activity in the two ranges?; or (4) were

zircons in the Santa Rita Mountains samples more susceptible to resetting? Chapter 2 presents

some methods for determining the answers to questions such as these, specific to the Huachuca

Mountains.

Age Data—Static Peaks

Older peak ages throughout the study area are similar (Table 1-1), ranging from 99 to

175 Ma in the Santa Rita Mountains, and 91-171 Ma in the Huachuca Mountains samples. The

presence of these peak ages throughout the Middle Jurassic-Upper Cretaceous section

Page 54: Copyright by Brook Colleen Daun Riley 2004

36

suggests that an important source of sediment for the Fort Crittenden Formation was the

underlying Middle Jurassic through Lower Cretaceous section, and/or recycling of components

with similar cooling ages from other units. These older peak ages are herein termed static peaks

(Brandon and Vance, 1992), as these are persistent age components in all samples.

There are several likely sources for grains with cooling ages in the 90-120 Ma range in

the Fort Crittenden Formation: (1) recycling of first-cycle volcanogenic detritus shed into the

Bisbee basin during deposition (i.e., magmatic-arc activity associated with basin extension); (2)

recycling of older rocks affected by heating associated with this igneous activity, or exhumed arc

rocks; and/or (3) zircons from rocks exhumed during extensional block faulting associated with

formation of the Bisbee basin. Radiometric ages within the 90-120 Ma range are common in

dated granitoid suites in the Sierra Nevada of California (Chen and Moore, 1982). Similar older

peak ages (90-115 Ma and 120-175 Ma) are present in all sandstones sampled for this study

(Table 1-1), confirming recycling of the older Jura-Cretaceous rocks as a potential source for

these peak ages in the Fort Crittenden Formation. Additionally, previous workers found local

and regional petrologic evidence for recycling of the Bisbee Group and intermediate volcanic

rocks into the Fort Crittenden Formation (Inman, 1982, 1987; Hayes, 1986, 1987; Lindberg,

1987; Mann, 1995). An equally viable source of grains with these FT ages are rocks exhumed

and cooled during normal faulting associated with Late Jurassic-Early Cretaceous formation of

the Bisbee basin (Hayes, 1970b; Bilodeau, 1978, 1979; Klute, 1987; Dickinson and others,

1986); these grains could subsequently have been recycled into the Laramide basin fill. In the

older Lower Cretaceous and Jurassic rocks that contain peak ages in the range 90-115 Ma and

120-175 Ma, the processes mentioned above would generate FT ages such as these in situ.

Alternatively, grains with FT ages in the older portion of this age range might have been recycled

from older rocks into the Bisbee Group sampled for this work.

Page 55: Copyright by Brook Colleen Daun Riley 2004

37

Minimum provenance ages around 170 Ma likely represent a cooling age associated

with Jurassic volcanism, expressed throughout southeastern Arizona (i.e. Jurassic Canelo Hills

volcanics, Late Jurassic ‘rocks of Mount Hughes,’ Juniper Flat granite near Bisbee, and

equivalents; Creasey and Kistler, 1962; Kluth, 1982; Kluth and others, 1982; Vedder, 1984).

Another probable source of similar ages includes rhyolitic-dome deposits and associated

volcaniclastic rocks of the Middle Jurassic Temporal and Bathtub formations. These rocks have

been dated at 182-172 Ma (U-Pb on zircon; Riggs and others, 1993; Bassett and Busby, 1996),

and have a gradational contact with the basal Glance conglomerate in the Santa Rita Mountains.

These strata mark the transition between widespread volcanism and Bisbee basin

sedimentation, and were deposited in trans-tensional basins possibly associated with movement

along the Mojave-Sonora megashear (Bassett and Busby, 1996). Accordingly, grains with FT

ages around 170 Ma may have been derived directly from these Jurassic volcanic and igneous

rocks, from older rocks affected by that thermal event, or from Bisbee Group lithologies which

sourced these Jurassic and older rocks. These observations support a relatively local source for

at least some of the c. 170 Ma provenance ages.

The source for 140 Ma ages might also have been relatively local. Intercalated within

the basal Bisbee Group in the Huachuca Mountains are intermediate volcanic rocks referred to

as the Glance andesite (Hayes and Raup, 1968; Figure 1-3); these rocks remain undated by

radiometric means. However, based on the age of the Canelo Hills Volcanics (185-165 Ma;

Vedder, 1984) and the rocks of Mount Hughes (intercalated tuffs within the basal portion of the

Glance Conglomerate in the Canelo Hills, 150 Ma; Kluth and others, 1982), and their relationship

with the basal Bisbee Group section, these andesites might be 150 Ma or younger. These

Jurassic and Cretaceous rocks might then have been recycled into the Upper Cretaceous

Page 56: Copyright by Brook Colleen Daun Riley 2004

38

synorogenic fill, yielding a similar age component within the Fort Crittenden Formation. It is also

possible that grains with these cooling ages reflect heating associated with the magmatic source

of these andesites, thus yielding similar cooling ages from rocks with older depositional ages.

The Glance andesite may thus provide a source for cooling ages of c. 140 Ma.

Much older peak ages are present throughout the study area, including those from the

upper red conglomerate member of the Fort Crittenden Formation (276 Ma) and the Turney

Ranch Formation (566 Ma) in the Santa Rita Mountains; and the Cintura Formation (236 Ma and

803 Ma) and the basal conglomerate subunit of the Fort Crittenden Formation (353 Ma) in the

Huachuca Mountains (Table 1-1). The presence of these older peak ages and older single-grain

FTGA in most samples brings up the issue of peak temperatures attained for all units in this

study. Clearly in certain zircons, there is tremendous potential for recording and retaining very

old cooling ages, depending on the thermal history of the grain following closure to the FT

system. Because of this dependence on thermal history, as well as other single-grain

characteristics (Chapter 2), the observation of this very old component in the FT data indicates

that portions of the source area remained at sub-annealing temperatures (perhaps 180-260°C,

depending on single-grain response to heating; Chapter 2) through the myriad of tectonic and

thermal events which have affected southeastern Arizona, in some cases since the Proterozoic

(Appendix 4).

Pb-Pb Ages

Pb-Pb ages for Station 23 in the Huachuca Mountains (Figure 1-3) provide further

constraints on sources of zircon in the basal subunit of the Fort Crittenden Formation. Three

observations about this unit are critical (Hayes, 1986, 1987): (1) the basal conglomerate is only

present in the northwestern Huachuca Mountains; (2) this unit is characterized by poor clast

Page 57: Copyright by Brook Colleen Daun Riley 2004

39

sorting and rounding; and (3) there is an up-section change in conglomerate clast composition

within the unit, from approximately equal components of limestone (proposed by Hayes (1986,

1987) to be derived from the Mural Formation, Bisbee Group; Figure 1-2) and intermediate

volcanics, to almost solely volcanic clasts similar in composition to the Glance andesite.

Pb-Pb ages of detrital zircons from Station 23 in the Huachuca Mountains (Figure 1-7)

indicate a lack of input of Mesozoic volcanic detritus at the base of the Laramide sedimentary

section at this location, because greater than 90% of the crystallization ages in FT-dated zircons

are Paleozoic or older (Figure 1-7). Hayes (1986) suggested the following as sources for the

dominantly volcaniclastic sandstones throughout the section, and volcanic-rich conglomerates in

every Upper Cretaceous sedimentary unit except for the upper red conglomerate in the Santa

Rita Mountains: Triassic-Jurassic volcanic rocks in the Santa Rita Mountains, the Jurassic

Canelo Hills Volcanics, the Glance andesite in the Huachuca Mountains, and early Laramide

volcanic rocks in the Canelo Hills and Santa Rita Mountains. For detrital zircons in the basal

part of the section, however, crystallization ages are dominantly Proterozoic and Paleozoic. As

such, if these zircons represent the volcanogenic component of the sandstone, a more likely

source for this detritus in this portion of the basin is older volcanic rocks. In the present

configuration, the nearest Proterozoic volcanic rocks lie in the northern Dos Cabezas Mountains

(Anderson, 1989); additionally, volcanic, volcaniclastic, and metavolcanic rocks of Proterozoic

age exist throughout central and northwestern Arizona (Anderson, 1989). A small fraction of

these zircons, if derived from the volcanic fraction of the sandstone, could also have been

derived from Mesozoic volcanic and volcaniclastic units, given their Pb-Pb ages; source units

might include the Jurassic Canelo Hills volcanics (Figure 1-3; Figure 1-2). Though older volcanic

and/or plutonic rocks may be the ultimate source of most grains with these crystallization ages, a

multi-cycle origin is quite likely.

Page 58: Copyright by Brook Colleen Daun Riley 2004

40

Another issue to consider is that zircons from Station 23 may not be derived from the

volcanic component of the sandstone, suggested by Hayes (1986) to reflect recycling of the

Glance andesite into the basal conglomerate subunit of the Fort Crittenden Formation. Despite

a significant proportion of VRF in the sampled interval at Station 23 (19% total lithics (Lt), 6%

volcanic lithics (Lv); Appendix 5), detrital zircons in this sample are also likely derived from other

component compositions within the framework, and thus not fully represent the source ages of

the recycled volcanics in the lower part of this section. Additionally, because of the constituent

grain size, many VRF and possible VRF (included in URF) might have a negligible contribution

to the dated fraction. As such, the Station 23 sample is probably dominated by zircon derived

from granitic and recycled sedimentary sources.

Provenance of FT Samples, Prior Work

Provenance work for the Fort Crittenden Formation FT samples indicates that source

areas for most samples included both granitic and volcanic rocks, with subordinate recycling of

sedimentary rocks (Figure 1-6). Given that almost the entire Paleozoic section is composed of

carbonates, the overall lack of CRF and chert indicates a paucity of Paleozoic source rocks,

and/or that rock fragments derived from the Paleozoic carbonates were unstable during transport

and diagenesis, and thus make up some portion of the URF.

Prior work by Hayes (1986, 1987) similarly indicates variable mineralogy and textural

maturity among analyzed sandstones. Most samples show evidence for textural and

compositional immaturity, with Huachuca Mountains samples being the most mature of those

studied (lithic arkose, low-quartz feldspathic litharenite), and samples from the Santa Rita

Mountains being somewhat less mature (dominantly lithic arkoses) than sandstones from the

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41

Huachuca Mountains. Important observations made by Hayes (1986) include the following: (1)

plutonic quartz is dominant over vein and metamorphic quartz; (2) sodic plagioclase, microcline,

and perthite are the most common feldspar compositions; (3) VRFs are abundant, and document

contribution of andesitic detritus (whereas the composition of the Jurassic Canelo Hills volcanics

tend to be more rhyolitic); and (4) SRFs tend to be mostly shale and siltstone, with subordinate

sandstone, limestone, and chert. Metamorphic rock fragments are rare, but detrital chlorite is

common. Important accessory minerals include muscovite, biotite, iron oxides, and epidote.

Petrographic observations on samples from this work agree on all above points, although this

study documents a greater contribution of SRF, feldspar, and MRF in certain samples.

Ten sandstone samples from the shale member of the Fort Crittenden Formation

described by Inman (1982) reflect an enrichment of volcanic rock fragments relative to

sedimentary and plutonic components, and a relative enrichment in plagioclase over potassium

feldspar. Sandstones interbedded with the basal conglomerate of the shale member plot in the

transitional-arc region on a Qm-F-Lt diagram (where Qm is monocrystalline quartz, F is feldspar,

and Lt is total aphanitic lithic content). Sandstones in the remainder of the shale member plot in

the transitional-recycled regions on a Qm-F-Lt diagram (Figure 1-6; Inman, 1987). These

features suggest a dominantly volcanic source for sandstones in the lower Fort Crittenden

Formation in the Santa Rita Mountains, though the lack of potassium feldspar may also be

reflective of diagenetic modification (Inman, 1982). This is a similar provenance signature to the

upper portion of the Turney Ranch Formation (upper transitional unit of Inman, 1982), which

changes from a dominantly sedimentary source to a mixed volcanic and sedimentary

provenance, and finally to a dominantly volcanic source at the top of the formation.

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42

Diagenesis of Fort Crittenden Formation Samples, and Prior Work

Hayes (1986) found evidence for extensive burial diagenetic modification in Fort

Crittenden samples from both the Santa Rita and Huachuca Mountains, including possible

selective replacement/alteration of potassium feldspar; chloritization of biotite; and extensive pre-

cement compaction. This work suggested “rapid, deep burial and/or a high geothermal gradient”

(Hayes, 1986, p. 67) to achieve the diagenetic alteration present, though Hayes (1986) did not

cite a burial depth or maximum peak temperature, and no attempt to constrain these parameters

was made. Evidence for early, extensive compaction and subordinate cementation was also

found in the present study in all FT-dated Fort Crittenden Formation samples. However, without

a more extensive petrographic study, including further X-ray diffraction work on mixed-layer

clays in some samples, the diagenetic character of FT-dated samples remains a qualitative

guide for interpretation of burial temperatures, and hence, inferred depths. Better estimates for

maximum depth of burial are made using the thicknesses of overlying sediments and the FT age

signatures (refer to next section).

Regional versus Local Heating

The question of local versus regional heating is of critical importance to this discussion.

The FT data for the entire study area and sparse vitrinite-reflectance data suggest that, on the

whole, these rocks probably did not exceed 200-225°C (Figure 1-1). In the case of other

samples within the remainder of the study area (Santa Rita Mountains, Fort Crittenden

Formation shale member), vitrinite-reflectance data record temperatures on the order of 150-

250°C, somewhat lower than maximum temperatures recorded elsewhere (this peak

temperature is based on 7 vitrinite measurements). Notably, peak temperature determinations

do not show a clear correlation with proximity to exposed lower Tertiary intrusive rocks, although

the VR data are sparse. Additionally, the presence of reset FT peak ages and/or single-grain

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43

reset FT ages does not always coincide with proximity to exposed intrusive rocks (e.g. Station

13, 14; Table 1-1, Appendix 4).

Trends within the FT data suggest that, with the exception of two locations, most

samples experienced sufficient Paleogene heating to reset the FT ages of certain grains

(Appendix 4; Figure 1-8). This observation includes those samples near Tertiary intrusions and

dikes (i.e. Station 9, 23), but also some samples not near any mapped intrusive rocks (e.g.

Station 13). Additionally, there is little consistent spatial variation in peak ages among dated

samples, which indicates that resetting had little if any resetting effect on most grains. These

observations suggest both local and regional controls on peak temperatures. Locally elevated

temperatures are likely related to plutons associated with a deeper-seated magmatic and

hydrothermal system that changed the regional geothermal gradient. Magmatic activity at depth

would provide a regional heat source for thermal reset at the present level of erosion, with locally

higher paleotemperatures directly adjacent to intrusive bodies. Given the magmatic setting

established in this area during the Laramide, local variations in peak temperatures are possible,

if not likely (Titley and Anthony, 1989). The observations fit well with the eastward migration of

arc-related magmatic activity through southeastern Arizona associated with shallowing of the

subducting slab during this time (Snyder and others, 1976; Coney, 1978; Dickinson and Snyder,

1978; Keith and Wilt, 1986).

Additionally, it is possible that the basin-bounding fault zone in the Huachuca Mountains

and farther northwest along the Sawmill Canyon fault zone in the Santa Rita Mountains aided in

the channelization of fluid flow and heat. Fission-track ages from rocks well outside this zone

would be needed to test this idea. There is clear evidence for focused fluid migration along

mapped fractures and fault zones; Pb-Zn-Ag mineralization is scattered throughout the eastern

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44

Santa Rita Mountains along the western portions of the Sawmill Canyon fault zone (mines

located with X on Figure 1-4; Drewes, 1971a, 1976; Titley and Anthony, 1989). This

mineralization is associated with nearby calc-alkaline intrusions ranging in age from 75 to 55 Ma

(Appendix 1); locations of established mining activity in the district adjacent to or within

Laramide-associated intrusions are shown in Figures 4 and 8.

The effect of thermal resetting of FT ages by enhanced fluid flow along fault zones, and

movement of hydrothermal fluids within basin strata, has been documented in the Late Triassic-

Early Jurassic Newark basin, New Jersey (Steckler and others, 1993). The Newark basin study

documents the importance of low-temperature (100-250°C) hydrothermal systems active in

sedimentary basins and the effect of heat transport during fluid flow on FT ages in zircon. Along

the border fault of this rift basin, zircon and apatite FT ages are older than reset FT ages from

rocks at the same time-stratigraphic level deposited within the basin, indicating that rocks along

the border fault remained cooler. As there is no evidence for differential subsidence or

intrabasinal exhumation relative to the border fault region, lower temperatures along the fault are

attributed to downwelling of cooler water at the basin bounding fault zone, likely resulting from

the high topography along the flank of the basin combined with an active hydrothermal system.

This hypothesis is corroborated by fluid-inclusion work and authigenic clay mineralogy. To

determine the applicability of this scenario to the current study area, new FT ages both inside

and outside the fault zones would be needed, in addition to other thermal indicators, such as

fluid-inclusion work and information on zeolitic and clay cement development (following the

methods of Steckler and others, 1993).

Lateral migration of fluids far outboard of an advancing deformation front can also occur.

Lateral movement of formation and metamorphic fluids as much as 100-200 km outboard of the

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45

contractional deformation front in the Alberta basin has been documented by Machel and Cavell

(1999) and Machel and others (2000). Sr isotopic signatures of cements from Devonian

carbonates and shales indicate lateral migration of extra-basinal fluids associated with burial and

loading during with Laramide deformation (Machel and Cavell, 1999). Additionally, Machel and

others (1999) suggest that subvertical faults played an important role by localizing vertical

movement of fluids through the deeper parts of the section, with subsequent migration into

accumulating sediments of the foreland basin. Such mechanisms could also have played a role

in the development of the hydrothermal system in the Laramide basin in the present study.

Migration of hot fluids along fault zones and lateral movement of fluids through basinal

sediments could have enabled metamorphic and/or magmatic fluids associated with intrusions to

affect strata well outboard of the deformation front.

Another consideration in the present study is the depth of burial of the Jura-Cretaceous

section. Regional map relationships between the Fort Crittenden Formation and older rocks

indicate that the contact is generally a disconformity, or a slight angular unconformity with little

change in dip across the contact (typically <20°; Hayes and Raup, 1968; Drewes, 1971a). As

such, where the section is relatively undeformed, it was likely a nearly horizontal section that

was buried. Where the Jura-Cretaceous section is deformed (i.e. within the Sawmill Canyon

fault zone, Figure 1-4; or along the west flank of the Huachuca Mountains, Figure 1-3), folds are

typically km- to sub-km scale, with meso-scale folding at the outcrop level. Absent overturning

on these larger-scale folds, which is generally not the norm in this area, the Jura-Cretaceous

section was not overturned during burial.

Younger rocks and sediments stratigraphically above the Jura-Cretaceous section

include uppermost Cretaceous and Paleogene volcanic and sedimentary rocks, Tertiary

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46

conglomerate and sandstone, and Quaternary conglomerate, sandstone, and unconsolidated

gravels. The maximum preserved thickness of these units is estimated to be 4200 m

(Scarborough, 1989). The distribution of these rocks is highly variable throughout southern

Arizona, and it is unlikely that a 4-km-thick section existed within the field area. The thickness of

strata deposited atop the section of interest is highly variable, resulting from local interaction

between sedimentation and structural development during the Cenozoic (Scarborough, 1989).

Thus, there is no reason to believe that the thickness of units overlying the Upper Cretaceous

Fort Crittenden Formation exceeded 4200 m, and is likely much less, perhaps on the order of

2000 meters within the field area (un-decompacted thicknesses). Assuming an average

continental geothermal gradient of 30°C/km, burial temperatures for the Upper Cretaceous rocks

probably would not have exceeded 125°C.

Accordingly, there is insufficient overlying strata to bury the section deep enough to heat

zircons to partial annealing zone (PAZ) conditions and anneal tracks. Additionally, if the

resetting of FT ages in zircon were purely the result of burial, one would expect to see a

systematic change in FT ages upward through the section. In other words, the Jurassic rocks

should have been buried to the greatest depths, and the Fort Crittenden Formation buried the

least, and the annealing should reflect this difference in maximum temperature. In this case, the

Middle Jurassic rocks from the Santa Rita Mountains would then have a larger proportion of

zircons with reset FT ages, and these ages would be younger overall than FT ages from strata

upsection. Likewise, the Fort Crittenden Formation would have the fewest reset FT ages, as it

would have been buried the least, and these cooling ages would be somewhat older than cooling

ages present in the older Jurassic rocks, depending on exhumation rate and geothermal

gradient. This pattern of FT ages with respect to depositional age is not seen in the FT data

from this study area (Table 1-1; Figure 1-8). Additionally, if the thermal signature of samples in

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47

this area were purely the result of burial heating, it would be a major coincidence that reset

samples throughout the section would contain similar Paleocene-Eocene reset peak ages (Table

1-1).

Implications for Provenance of Fort Crittenden Formation and Changes in Thermal Structure through Time

Very similar FT age distributions occur throughout the sample suite (Table 1-1). All

samples contain FT peak ages of 90-170 Ma and older single-grain ages, which in some cases

are sufficient in number to define an older peak age. Many samples also contain a young reset

peak, 68-42 Ma, and single reset FT ages (Appendix 4). For the unreset ages, two important

factors are revealed about the thermal structure of the crust recycled into the Laramide basin:

(1) there was potentially direct recycling of Middle Jurassic and Lower Cretaceous strata into the

Fort Crittenden Formation, or at least erosion of some rocks with a similar thermal signature as

the Middle Jurassic-Lower Cretaceous; and (2) the Jura-Cretaceous section was probably not

ever buried very deeply.

It is clear from prior work on the sedimentology and provenance of the Fort Crittenden

Formation that clastic sediments were derived from the Middle Jurassic through Lower

Cretaceous strata, as well as other units, including granitic sources (Inman, 1982; Hayes, 1986).

However, given the FT data, the age distribution of the source area for the Fort Crittenden

Formation is the same as the signature present in the older Jura-Cretaceous lithologies, and that

signature must also have been present in other units being eroded into the basin. This

observation suggests that at least at the beginning of the Laramide, during basin formation, there

was no preferential uplift of one source area relative to another: granites sourced by the Fort

Crittenden Formation were at the same thermal level as the remainder of the section.

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48

Provenance

Certain aspects of prior work on the sedimentology and provenance of the Fort

Crittenden Formation are pertinent to the current discussion of derivation of Laramide basin fill.

Hayes (1986) documented a distinct transition in conglomerate clast compositions in the basal

and upper conglomerate subunits in the Huachuca Mountains. The basal conglomerate subunit

is present only in the northwestern Huachuca Mountains, and is one of the only units for which

Bisbee Group recycling is required by the provenance data (also required in the case of the

upper red conglomerate, Santa Rita Mountains; Hayes, 1986). The basal conglomerate subunit

is characterized by poor size sorting and angular clasts, suggesting textural immaturity,

particularly with respect to the upper conglomerate subunit. Specific to the basal conglomerate

subunit, Hayes (1987) also noted a change in clast composition upsection, from approximately

equal components of limestone and intermediate volcanics to solely volcanic compositions

(clasts similar to composition of Glance andesite; Figure 1-2). This observation may indicate

erosion through the upper part of the Lower Cretaceous section (i.e. limestone component)

through to Glance conglomerate and interbedded Glance andesite. In the upper conglomerate

subunit, clasts are well rounded and well size sorted, indicating greater textural maturity

upsection. Compositions of conglomerates throughout the upper conglomerate subunit are

equal portions of recycled sedimentary, volcanic, and granitic clasts. This pattern suggests

continuing erosion through the Lower Cretaceous section into Jurassic volcanic rocks and

Jurassic intrusions.

Hayes (1986) suggested several different sources for conglomerates in the Upper

Cretaceous section. Compositional fields for Fort Crittenden Formation conglomerates in the

Huachuca and Santa Rita Mountains are shown in Figure 1-9. Most conglomerates in the

section are dominated by volcanic and granitic clasts, with less evidence for recycling of

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49

sedimentary rocks. For granite clasts and detritus, sources may include both Precambrian and

Triassic-Jurassic granites. Where conglomerates sourced volcanic rocks, Hayes (1986) cited

essentially every volcanic rock in the pre-Upper Cretaceous section as a potential source:

Triassic-Jurassic volcanics, Mount Wrightson Formation, Canelo Hills volcanics; Glance

andesite; and early Laramide volcanics. Siliciclastic sedimentary detritus may have been

derived from the Lower Cretaceous Bisbee Group, or from the Cambrian Bolsa quartzite. Some

variation in clast composition is noted through the section: the lower red and brown

conglomerate members contain subequal granitic and volcanic clast compositions; the upper red

conglomerate member sourced dominantly sedimentary rocks.

The evolution of clast compositions of conglomerates in the Huachuca Mountains,

including volcanic clasts in all cases, have been discussed above. Based on Hayes’ (1986)

conglomerate clast compositions (Figure 1-9), source areas for Fort Crittenden sediments may

have evolved in either or both of the following ways: (1) recycling into the basin and sourcing in

the conglomerates works through granites and volcanic cover to uncover sedimentary sources;

and/or (2) tapping of different sources in different areas through time. In the northern Huachuca

Mountains in particular, Hayes (1986) suggests that with progressive alluvial fan development,

there is an evolution of recycling first the Lower Cretaceous section (Bisbee Group), and then

continuing down into underlying Mesozoic volcanic rocks and granitic rocks.

Structural Constraints

Most faults that juxtapose the Fort Crittenden Formation with older rocks dip at relatively high

angles to the attitude of the offset strata (Hayes and Raup, 1968; Drewes, 1971a). Drewes

(1981, 1988) suggested multiple periods of movement along the Sawmill Canyon fault zone,

and that this was a major structure reactivated during Laramide contraction. Davis (1979) noted

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50

the presence of the Sawmill Canyon fault zone and its along-strike parallel relationship with the

west-flank fault zone in the Huachuca Mountains (Figure 1-1), and suggested that these

structures may have formed the bounding fault zone which separated the Laramide structural

uplift from the adjacent basin. These faults generally have steep dips (>45°) relative to the dip of

bedding in Laramide synorogenic strata.

Given the preceding argument, and considering the suggestion that Jura-Cretaceous

strata were buried as a straight section, Figure 1-10a shows the interpreted configuration for the

sediment-source couple that satisfies critical relationships present in the FT and provenance

data, and Figure 1-10b provides one possibility for post-depositional heating of the section:

(1) This scenario provides a straight stratigraphic section that allows for the unroofing

sequence documented in conglomerate and sandstone compositions by Hayes (1986).

(2) Significant recycling of the Jurassic-Cretaceous section occurs in this configuration,

and granitic material is derived from either Precambrian or Mesozoic granitic rocks that

underlie the Lower Cretaceous Bisbee Group (LK in Figure 1-10; documented by

Bilodeau, 1979), via recycling of granite-clast conglomerates abundant in the Glance

conglomerate (detailed in Bilodeau, 1979), or by tapping Precambrian source rocks as

shown in Figure 1-10a. Granite sourcing in this case does not necessitate preferential

uplift of granitic rocks at basin-bounding faults: trunk streams and tributaries feeding

alluvial fans need only incise into the basal Bisbee Group, or into granitic rocks in

nonconformity with the Bisbee Group. However, the configuration presented in Figure 1-

10a agrees with the present relationship of Precambrian granites to the Phanerozoic

section, and presents the possibility for sourcing of granite by exhumation along reverse

faults. Note that because of the thermal signature in units determined in this study,

juxtaposition of Precambrian and Phanerozoic rocks is not associated with significant

Page 69: Copyright by Brook Colleen Daun Riley 2004

granitic

volcanic sedimentary

Figure 1-9. Compositional ternary diagram for conglomerates in the Fort Crittenden Formation

Santa Rita Mountains samples

Huachuca Mountains samples

(N = 27 clast counts from the Santa Rita and Huachuca mountains; from

51

Hayes, 1987).

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52

uplift during the early Laramide.

(3) Volcanic detritus is readily available from at least two sources: the Jurassic Canelo

Hills volcanics, and the Glance andesite (portions of J and LK on Figure 1-10a; Figure 1-

2).

(4) There is a distinct lack of recycling of Paleozoic carbonate units into the Fort

Crittenden Formation samples in this study (Figure 1-6). While Hayes (1986)

documented somewhat greater recycling of sedimentary rocks than found in the current

study, the recycled sedimentary component, including Paleozoic carbonate lithologies, is

overall subordinate to the input of volcanic and granitic detritus. This indicates that the

Paleozoic carbonate section was stripped prior to deposition of the Fort Crittenden

Formation, that Paleozoic carbonate clasts did not survive transport, or that Paleozoic

carbonates were covered and unavailable to the basin during Laramide sedimentation.

(5) Because the FT thermal signature of the underlying section is so similar to that of

the Fort Crittenden Formation, there is no significant differential in the exhumation level

of one source terrane over another.

(6) Because of the similarity of peak ages within the Fort Crittenden Formation,

variations in the thermal signature of the source are minimized by the presence of the

same units along strike, which probably contain similar thermal signatures.

(7) Post-depositional heating of the section is proposed to be a combination of thermal

input from magmatic activity (Drewes, 1976) and limited burial of the section by

uppermost Cretaceous and Cenozoic volcanic and sedimentary rocks (Figure 1-10b).

The maximum thickness of post-Fort Crittenden Formation rocks is 4200 meters

(Scarborough, 1989), but due to local variations in thickness, values on the order of 2

km are present. In combination with deeper-seated magmatic activity, as shown in

Page 71: Copyright by Brook Colleen Daun Riley 2004

SW

NE

4 k

m

?

LK

J

4 k

m

Pz

UK

Pz

J?

20

0°C

/

~65 M

a

20

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~55 M

a

20

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53

ind

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Page 72: Copyright by Brook Colleen Daun Riley 2004

54

Figure 1-10b, the geothermal gradient was elevated and the evolution of the 200°C

isotherm following intrusion at ~65 Ma is shown. This combination allows for the

appropriate scale and timing of heating to achieve the post-depositional annealing found

in the FT data. The scale and relationship of intrusive bodies with the surrounding wall

rocks are in keeping with mapped surficial relationships (i.e. Hayes and Raup, 1968;

Drewes, 1971a), and the scale of thermal effects (as shown by the evolution of the

200°C isotherm) is supported by thermal modeling of Barton and Hanson (1989) and

Hanson (1996).

In terms of direct fault control on sedimentation, the structural and sedimentologic

scenario for the Laramide basin presented in Figure 1-10 is in contrast with sedimentary tectonic

models proposed for older basins in this part of southeastern Arizona. One example of this

contrast is the work of Davis and others (1979), that suggests that extensional faults exerted

marked control on deposition of Permian exotic blocks in Jurassic red-bed deposits in the

Canelo Hills (Figure 1-5). These exotic blocks of Permian carbonates measure up to 400 meters

in thickness, are up to 2 km along strike, and are intercalated with the Jurassic Canelo Hills

volcanics (Figure 1-2) in both the Sawmill Canyon Fault Zone as well as the west-flank fault zone

in the Huachuca Mountains (Davis and others, 1979; Figures 1-4, 1-3). Bedding-parallel faults,

slickenlines, clastic dikes, and breccias near the contact of these blocks are interpreted to have

formed during block emplacement, as the blocks gravitationally glided into unlithified red-bed

sediments. In many cases, emplacement of blocks is related to activity on high-angle north-

northeast- to northeast-striking faults (Davis and others, 1979).

The sedimentologic character of the Fort Crittenden Formation is significantly different

than that of the exotic-block facies of the Canelo Hills volcanics: deposits of the Fort Crittenden

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55

Formation are texturally and mineralogically more mature, finer-grained, and less proximal than

the exotic block/red-bed facies described by Davis and others (1979). Additionally, all exotic

blocks intercalated with the Canelo Hills volcanics are Paleozoic, whereas the Fort Crittenden

Formation appears to have either not sourced the Paleozoic at all, or that Paleozoic-derived rock

fragments and clasts did not survive transport within the basin. Based on mapping and

kinematic analysis, Davis and others (1979) concluded that deposition of these exotic Paleozoic

blocks is the result of gravitational gliding associated with normal faulting. Fault control on facies

and emplacement of large exotic blocks in this manner is not documented for the Fort Crittenden

Formation, and this example thus serves to document the relative lack of direct fault control on

derivation of the Fort Crittenden Formation. The relative uniformity of source rocks for the

Laramide basin indicates that unlike in older synorogenic basins in the same area, the deformed

nature of source rocks and the distribution of these older rocks does not exert significant control

on the FT signature of the Laramide basin fill.

CONCLUSIONS

Based primarily on zircon FT data complemented by petrography and existing

provenance studies, the following conclusions may be made:

(1) Young FT ages (Paleocene-Eocene) in many samples indicate that widespread

thermal activity reset some zircons preferentially, whereas a significant fraction has

much older ages. Because of the thickness of the overlying section and the distribution

of young reset FT peak ages in almost every Jurassic-Cretaceous unit sampled, the FT

age structure present in these samples could not have been produced purely by burial

heating.

(2) Samples with young FT ages do not always coincide with the outcrop distribution of

plutons, and the distribution of these samples widespread throughout the data set, with

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56

similar peak ages from place to place regardless of depositional ages. As such,

Paleogene heating was regional, potentially related to conductive heating and

hydrothermal circulation associated with magmatic activity at depth.

(3) Older FT grain ages provide minimum provenance ages for Fort Crittenden

Formation sediments. These peak ages show that there has been little burial of the

older Jura-Cretaceous section prior to recycling into the Laramide basin, document little

variation in the thermal signature of the crust being recycled, and suggest that the Jura-

Cretaceous section provided an important sediment source for the Fort Crittenden

Formation. The presence of older peaks of similar ages in the Jurassic, Lower

Cretaceous, and Upper Cretaceous sediments, in combination with petrographic

evidence for recycling, demonstrates that there was probably little exhumation of one

source terrane preferentially to others prior to and during deposition of the Fort

Crittenden Formation. It is likely that some fraction of zircon in a given sample is also

derived from granites (Triassic-Jurassic or Precambrian). Although there clearly was

granite exhumed and recycled into the Fort Crittenden Formation (Hayes, 1986), these

units must have been relatively high in the crustal stack, and cooling ages of zircons

derived from these granites are the result of annealing prior to the Laramide. Granite

sources in this case could be either Precambrian or Mesozoic, or both.

(4) Jura-Cretaceous rocks included in this study likely did not exceed temperatures

greater than 200°C-225°C, depending on single-grain annealing characteristics. Units

that do not display any obvious resetting of the FTGA have probably remained at

temperatures <180°C, but have similar age distributions for older FT ages as rocks with

clear evidence for Paleogene resetting. This observation documents the criticality of

single-grain characteristics as controls on the closure temperature of zircon, the focus of

Chapter 2.

Page 75: Copyright by Brook Colleen Daun Riley 2004

57

Chapter 2—Controls on the low-temperature thermal response of single detrital zircons: Temperature, crystallinity, and chemistry

ABSTRACT

Fission-track (FT) ages of zircon from Mesozoic sandstones were analyzed to address

the provenance and post-depositional thermal history of Laramide synorogenic strata in

southeastern Arizona. Samples from strike-normal transects across the Laramide basin

boundary show a complex provenance, with significant recycling from underlying strata.

Fourteen Jura-Cretaceous sandstones have FT populations with peaks between 570-165, 140-

82, and 68-42 Ma. Numerous older single-grain ages (1000-600 Ma) are also present, indicating

long-term cool conditions (temperatures less than perhaps 180°C, up to 260°C, depending on

single-grain response to heating) for portions of the source area. While most samples show a

range of provenance ages, a small fraction have been affected by post-depositional thermal

annealing. The distribution of samples with reset ages coincides in some locations with

proximity to magmatic bodies 75-40 Ma in age. This setting provides an opportunity to

investigate controls on single-grain response to thermal perturbations. The young component of

reset ages falls between 68 and 42 Ma, and is younger than the depositional age of the Jurassic-

Upper Cretaceous strata in which these ages occur. As such, these strata reached

temperatures sufficient to anneal fission tracks in some grains (c. 180°C-260°C). U-Th-Pb, REE,

and Raman microprobe analyses from these samples indicate a correlation among old

crystallization ages, high U+Th (eU, or effective uranium) concentrations, elevated alpha-

damage dose, and young reset FT ages. Resetting occurred in grains with higher radiation

damage, as determined by FT and Raman microprobe analyses, and total and effective alpha-

dose calculations. Less-damaged grains have a higher temperature of track retention, and

therefore retain a primary detrital signature. Zircon color is related, in part, to increasing

Page 76: Copyright by Brook Colleen Daun Riley 2004

58

radiation damage, and can be used for identifying different thermal events in both the pre- and

post-depositional history of individual zircons. In this study, honey and colorless grains

essentially behave as one population in all data sets.

This study establishes some criteria for identifying reset grains in detrital populations:

(1) the pink/purple color series provides the greatest potential for having the combination of old

crystallization ages and/or high α-damage; (2) honey and colorless grains which have high eU,

i.e. greater than 650 ppm, might also be suspected as being preferentially reset, depending on

thermal history and retention time; and (3) zircons in rocks that attained paleotemperatures of

180°C-260°C may provide information on low-temperature thermal effects. The following

revision of methods is necessary to avoid difficulties in interpreting multi-component detrital-

zircon data sets: (1) separate zircons into color populations, and evaluate FTGA accordingly; (2)

evaluate etch behavior, as fission tracks will etch more rapidly in grains with higher accumulated

alpha damage; (3) evaluate FTGA with respect to eU, as high eU is sometimes correlated with

reset FT ages in honey and colorless zircons; and (4) utilize vitrinite-reflectance data where

possible to constrain maximum paleotemperature.

Page 77: Copyright by Brook Colleen Daun Riley 2004

59

INTRODUCTION

Determining the thermal history of sedimentary strata during diagenesis and burial,

specifically in the temperature range 150-300°C, is critical to the understanding of basin

evolution, and provides important constraints on thermal and tectonic processes that affect

strata. The zircon fission-track system, with closure temperatures in the range of 235°C ± 25°C

(Brandon and Vance, 1992), is a proven means of determining the thermal history of upper-

crustal lithologies as these rocks are eroded and deposited into flanking sedimentary basins.

However, this thermal signature is just one aspect of the picture provided by the zircon FT

system. Where sedimentary strata have reached peak temperatures less than about 200°C,

zircon fission-track data primarily provide information on sediment provenance (i.e. Garver and

others, 1999). Where temperatures were higher, and samples are collected in stratigraphic and

structural context, thermal history and processes involved in basin formation and subsequent

deformation are further elucidated.

This study makes the first quantitative link between cooling age and crystallization age

of single grains. New constraints on the low-temperature response of zircons based on

variations in single-grain radiation damage and crystal chemistry are provided. Developing

relationships among these parameters strengthens our understanding of the low-temperature

behavior of zircons, and yields information critical to source-area evolution and pre- and post-

depositional thermal events for clastic rocks. The most important part of this issue centers on

the potential for radiation damage, specifically α-damage, to decrease the stability of fission

tracks in zircon, thus lowering the effective closure temperature of the system (Kasuya and

Naeser, 1988). This preferential annealing of radiation-damaged zircons, which has also been

noted in two recent studies (Kunlun Mountains of northeast Tibet, and Hudson Valley, New York;

Garver and others, 2002), allows dating of both provenance and post-depositional thermal

Page 78: Copyright by Brook Colleen Daun Riley 2004

60

activity using the same sample if the factors controlling zircon behavior can be identified.

Recognizing and quantifying resetting of α-damaged zircons will more clearly reveal the closure

temperature range, and thus, the conditions under which resetting occurs in damaged zircons.

Finally, recognition of post-depositional thermal events is necessary to prevent the

misinterpretation of young (reset) fission-track ages in synorogenic sandstones, because such

ages can be mistakenly interpreted as indicators of synorogenic magmatic activity.

Radiation damage affects zircon (ZrSiO4) in several ways. Color in zircon changes over

geologic timescales, and is related to accumulation of α-damage and crystal chemistry (e.g.

Gastil and others, 1967). The presence of different color populations in zircon from a sandstone

allows optical separation into populations presumably related to differences in source-rock

histories. Many studies have attributed zircon color and/or morphology to: (a) crystallization age

or fission-track age (e.g. Vitanage, 1957; Gastil and others, 1967; Malcuit and Heimlich, 1972;

Garver and Kamp, 2002; and references therein); (b) source (e.g. Vitanage, 1957; Malcuit and

Heimlich, 1972; Gehrels and others, 2000; Riley and others, 2000); (c) chemical composition of

host rocks (e.g. Turniak, 1997); (d) granite genesis (e.g. Poldervaart, 1956; Forbes, 1969; Arps,

1970; Pupin, 1980); and (e) correlation of lithologies (e.g. Poldervaart, 1956; Vitanage, 1957). In

light of this literature, it is clear that the origin of color in zircon is complex. Though the

relationship among heating, color loss (i.e. annealing of α-damage), and resetting of the FT

system has been discussed (Garver and Kamp, 2002), the effects of accumulated radiation

damage and the single-grain response to heating have not been fully explored. Early

observations noted the general relationship of depth of color to crystallization age (e.g. Gastil

and others, 1967; Nerurkar and others, 1979). It is suspected that accumulated α-damage

results in decreased crystallinity and progressive color change (Garver and Kamp, 2002; Rahn

and others, in press). However, with the exception of a study in the Southern Alps of New

Page 79: Copyright by Brook Colleen Daun Riley 2004

61

Zealand (Garver and Kamp, 2002), there is little information as to how color is altered by heating

at low temperatures (<300°C). It seems clear that a fundamental attribute of color is trace-

element impurities in zircon, but this aspect of color generation is also little studied. Work by

Fielding (1970) on hyacinth (pink/purple/red) series zircons suggests that the development of

“color centers” is related to uranium (U) content, rare-earth-element (REE) chemistry, and the

oxidation state and concentration of niobium (Nb). In a study of detrital-zircon populations in the

Potsdam sandstone (New York State), Gaudette and others (1981) suggested a link between

brown color in grains and positive europium (Eu) anomalies.

Prior to the development of laser ablation enhancement of inductively coupled plasma

mass spectrometry (LA-ICP-MS), it was very difficult to determine crystallization age and FT age

on the same grain. In the few cases where this has been attempted, zircons have been

separated into two fractions, one for U-Pb analysis, and one for FT age determination (i.e.

Hoisch and others, 1997; Carter and Moss, 1999). Likewise, single-crystal geochemistry

involved dissolution and/or ion-microprobe work on yet another separate fraction. In these

cases, the major problem is that the interrelation of attributes is unknown because analysis was

done on separate fractions. Such a cumbersome method obviates key information regarding the

relationship of single-grain provenance ages and thermal history, and the complex and

potentially useful link to the color of zircons.

This study investigates the relations among color, Pb-Pb crystallization age, fission-track

age, crystallinity and radiation damage, and trace-element chemistry of single detrital zircons

from a sample from a Laramide basin in southeastern Arizona. Making these measurements on

single detrital zircons provides new and unique insights into the provenance, thermal history, and

composition of these grains, thus providing a clearer picture of the regional evolution of source

Page 80: Copyright by Brook Colleen Daun Riley 2004

62

and thermal history of rocks in this study. The multi-analysis approach employed here also

provides a basis for other workers to use observations and criteria from these data to better

understand what occurs to zircons at temperatures of 150°C to 250°C. To that end, zircons with

different color and morphology were chosen from a specific sample from a group of thirty-four

samples that are part of a larger study in southeastern Arizona (Chapter 1). This sample was

chosen because the FT data revealed a surprising finding: a small fraction of the grains had

been annealed and the FT ages reset, so the sample contains thermal information for the

sandstone as well as provenance information about the source(s).

Acquisition of Pb-Pb and FT ages on the same grains defines both the age of

crystallization and subsequent cooling to ~235°C of source rocks, providing crucial provenance

information. Working from this finding, important information regarding both provenance and

post-depositional heating should be obtainable from multiple analyses of single grains.

Specifically, understanding how the relationship between radiation damage and thermal

response controls the resetting of fission-track ages helps better define factors that control the

lower end of the fission-track system closure temperature (180°C-235°C) and annealing of

different types of radiation damage. Following on the observations made about this particular

sample, this study provides a basis for future workers by presenting criteria for identification of

reset fission-track grain ages (FTGA) in multi-component populations.

METHODS

Field Setting

The sample selected was 5 kg of coarse-grained lithic arkose from the base of the

Upper Cretaceous Fort Crittenden Formation in the Huachuca Mountains of southeastern

Page 81: Copyright by Brook Colleen Daun Riley 2004

Kfc

Kc

Kc

Kga

Jh

?

Km

oK

ga

Kc

Sta

tio

n 2

3K

fc

Kc

Km

o

Km

u

Kc

Km

o

Km

o

Km

o

Km

u

Kg

Kg

Kg

aP

zu

Pzu

Kga

Kg

eK

ga

Pzu

e

Pzu

Pzu

Jh

Km

o

Kg

Pzu

Km

o

Kg

Kga

Kg

Km

oK

g

Km

u

Kc

Kfc

TQ

uK

b?

TQ

u

Km

o?

Tg

Tg

TQ

u

TQ

u

TQ

u

TQ

uTi

Ti

Km

o

pC

g

Tg

TQ

u

KfcTi

Pzu

e

Qal

Tg

TQ

u

Qg

Km

o

Km

u

Kc

Kga

Kg

Kb

pC

g

Jh

JTc

JT

h

JT

h?

JTc

JTc

JT

h

JT

h

JT

h JTc

JT

h

JTc

JTc?

JTc?

Te

rtia

ry a

nd

Qu

ate

rna

ry g

rave

ls,

allu

viu

m

Tert

iary

intr

usiv

es (

quart

z

mo

nzo

nite

, a

laskite

, g

ran

o-

dio

rite

, a

lka

li d

iorite

); in

tern

al

ag

e r

ela

tio

nsh

ips u

nce

rta

in

Up

pe

r C

reta

ce

ou

s F

ort

Critt

en

de

n

Fo

rma

tio

n (

ea

rly L

ara

mid

e b

asin

fill

)

Lo

we

r C

reta

ce

ou

s

Bis

be

e G

rou

p

Ju

rassic

Ca

ne

lo H

ills

Vo

lca

nic

s a

nd

asso

cia

ted

rocks

Pa

leo

zo

ic s

ed

ime

nta

ry

rocks, exotic b

locks o

f

Pa

leo

zo

ic w

ith

in o

the

r u

nits

Pre

ca

mb

ria

n g

ran

ite

01

kilo

me

ters

mile

s0

1

fissio

n tra

ck s

am

ple

; S

tation 2

3 d

enote

d

vitrin

ite

sa

mp

le

Ro =

3.0

0%

(N

= 4

4)

Tm

ax 2

25

-30

0°C

Ro =

2.0

3%

(N

= 5

0)

Tm

ax 1

50

-25

0°C

fau

lt; d

ash

ed

wh

ere

in

ferr

ed

an

ticlin

al tr

ace

; d

ash

ed

wh

ere

in

ferr

ed

,

plu

ng

ing

wh

ere

in

dic

ate

d

syn

clin

al tr

ace

; d

ash

ed

wh

ere

in

ferr

ed

,

plu

ng

ing

an

d/o

r o

ve

rtu

rne

d w

he

re in

dic

ate

d

co

nta

ct;

da

sh

ed

wh

ere

in

ferr

ed

Map

Un

its

Map

Sym

bo

ls

pC

g

pC

g

pC

g

pC

g

pC

g

a.

b.

Bis

be

e G

rou

p, u

nd

iffe

ren

tia

ted

Cin

tura

Fo

rma

tio

n

Mu

ral F

orm

atio

n

Morita

Form

ation

Gla

nce

an

de

site

Gla

nce

co

ng

lom

era

te

63

Hu

ach

uca

Mo

un

tain

s

Cin

tura

Fo

rma

tio

n

(~2

90

m)

Fo

rt C

ritt

en

de

n

Fo

rma

tio

n (

~6

60

m)

Mu

ral F

orm

atio

n

(~2

10

m)

Gla

nce

Co

ng

lom

era

te

(0-6

30

m)

??

Mo

rita

Fo

rma

tio

n

(~1

27

0 m

)

Ca

ne

lo H

ills

volc

anic

s

qu

art

z m

on

zo

nite

,

ce

ntr

al H

ua

ch

uca

s??

50

Ma

60

Ma

70

Ma

80

Ma

90

Ma

110 M

a

12

0 M

a

13

0 M

a

163 M

a

15

0 M

a

14

0 M

a

10

0 M

a

APTIANALBIANCENOMANIAN

TU

RO

NIA

N

CO

NIA

CIA

N

SA

NT

ON

IAN

CAMPANIANMAASTRICHTIAN

LATE EARLY

CRETACEOUS

EA

RLY

LA

TE

EA

RLY

EOCENE PALEOCENE

PALEOGENETERTIARY

NEOCOMIAN

JURASSIC

LATE

? ?? ??

Sta

tio

n 2

3

sa

mp

ling

in

terv

al

114°

11

112

°111°

11

37

°

36

°

35

°

34

°

33

°

32

°11

11

112°

111°

110

°

37

°

36

°

35

°

34°

33

°

32

°

Page 82: Copyright by Brook Colleen Daun Riley 2004

Figure 2-1a. Generalized time-stratigraphic column for the Upper Jurassic-Upper Cretaceous section, Huachuca Mountains, showing approximate stratigraphic position of sample from Station 23 (column and lithologies after Hayes, 1970a; Hayes, 1970b; Palmer, 1983; Hayes, 1986; Hayes, 1987; Dickinson and others, 1989). Timescale of Palmer, 1983. Note that this is a composite column for the entire range, and that all formation and intraformational boundaries are time-transgressive in detail (shown schematically).

Figure 2-1b. Huachuca Mountains geologic map (generalized after Hayes and Raup, 1968) showing location of Station 23, sample locations as part of the regional study. Vitrinite-reflectance data shown adjacent to sample locations (Tmax estimates based on vitrinite-reflectance data from Fort Crittenden Formation siltstone/shale samples, interpreted after Héroux and others, 1979; Staplin, 1982; Burnham and Sweeney, 1989; Barker and Pawlewicz, 1994).

Page 83: Copyright by Brook Colleen Daun Riley 2004

64

Arizona (Figure 2-1). The Cretaceous sequence is locally intruded by a quartz-monzonite

pluton emplaced sub-parallel to bedding within strata of the Lower Cretaceous Bisbee Group

(Figure 2-1). The sample site is 1 km from the intrusion (map distance). Cross-cutting relations

indicate a Tertiary age for the intrusion, and regional considerations imply that it is related to

other intrusions throughout the study area dated at c. 75-55 Ma (Hayes and Raup, 1968;

Drewes, 1972, 1976). Local structural relationships along the west flank of the range indicate

that this and similar smaller dikes and sills in Cretaceous strata are folded, and thus were

emplaced prior to major Laramide deformation (Hayes and Raup, 1968). Accordingly, this phase

of magmatism would have provided a source of heat for the area around this sample location

approximately 10-15 m.y. after deposition.

The sampled interval is the lowest portion of the Fort Crittenden Formation, just above a

disconformable contact with the Lower Cretaceous Cintura Formation. Strata include medium-

to coarse-grained, subangular to subrounded litharenites, deposited in an alluvial-fan setting

(Hayes, 1986, 1987). Framework grains include plutonic and metamorphic rock fragments (RF),

altered K-feldspar, sand-rich clastic RF, carbonate RF, and volcanic and/or microcrystalline to

mud-sized sedimentary RF, as well as common and vein quartz. The rock is partially cemented

by calcite, but cementation is overall subordinate to extensive compaction (contact index

average value of 6; very little cement is present (<1%), indicating thorough early compaction).

Fission-track Analysis

Zircons were separated with standard techniques using a Wilfley table, heavy liquids,

and a Frantz magnetic separator. A fraction of this material was prepared for traditional fission-

track age dating. From another fraction, zircon was then hand-picked into three distinct color

fractions (Table 2-1). The most appropriate division of the remaining sample was by color rather

Page 84: Copyright by Brook Colleen Daun Riley 2004

65

than by grain morphology. Color is difficult to distinguish once mounted in Teflon, but grain

shape is still readily identified. Color fractions include: (1) light to dark pink and purple

(hyacinth) zircons (fraction p; ~5% of total yield); (2) colorless zircons (fraction c; ~20% of total

yield); and (3) honey-colored zircons (fraction h; ~75% of total yield). Each of the color fractions

includes at least two, and as many as seven, individual morphology groups, as shown in Table

2-1.

All hand-picked zircon fractions, as well as the original bulk zircon, were mounted and

etched for FT analysis (i.e. Garver and others, 2000). Each fraction comprised two mounts

containing approximately 1000 grains in each of two Teflon mounts. Mounts were polished and

then etched in a KOH:NaOH eutectic at 228°C for 17 hours (long etch), 12 hours (short etch), 10

hours (fractions c and h long etch), 8 hours (fractions c and h short etch), and 5 hours (fraction

p). All mounts were irradiated at the Oregon State University Reactor Facility, with a thermal

neutron fluence of 2 x 1015 n/cm2, and etched fission tracks were counted at 1250x magnification

(dry). Grains were analyzed using the external-detector method calibrated to zircons from Fish

Canyon Tuff and Buluk tuff zircons (refer to Table 2-2 for details, and Appendix 3 for a brief

discussion of FT systematics).

Cathodoluminescence

Following preparation and analysis for fission tracks (including irradiation and counting),

the color FT mounts were carbon-coated and cathodoluminescence (CL) images of each dated

grain were taken at the University of Texas using an Oxford Instruments photomultiplier-based

CL detector mounted on a JEOL T330A scanning electron microscope (SEM); accelerating

voltages range from 10-15 kV, as described in Milliken (1994). SEM-CL images assist in

delineating zonation and degree of heterogeneity within individual grains for the region counted

Page 85: Copyright by Brook Colleen Daun Riley 2004

Tab

le 2

-1.

Zircon c

olo

r and m

orp

holo

gy f

ractions,

Sta

tion 2

3,

Huachuca M

ounta

ins.

rela

tive

ab

un

da

nce

co

lor

form

ha

bit/r

ou

nd

ing

cla

rity

inclu

sio

ns

siz

e

fra

cti

on

p

(pin

k/p

urp

le)

ab

un

da

nt

ve

ry lig

ht

pin

k t

o v

ery

lig

ht

pu

rple

elo

ng

ate

(~

2:1

to

4:1

)ro

un

de

d t

o w

ell

rou

nd

ed

cle

ar

rare

to

no

ne

larg

e t

o m

ed

ium

co

mm

on

me

diu

m t

o d

ark

pin

k t

o

pu

rple

eq

ua

nt

we

ll r

ou

nd

ed

cle

ar

rare

larg

e t

o m

ed

ium

co

mm

on

me

diu

m p

ink t

o p

urp

lee

qu

an

tw

ell r

ou

nd

ed

cle

ar

rare

larg

e t

o m

ed

ium

rare

me

diu

m p

ink t

o p

urp

leslig

htly t

o m

od

era

tely

elo

ng

ate

(2:1

to

3:1

)

eu

he

dra

l to

su

bh

ed

ral

cle

ar

rare

me

diu

m

rare

da

rk p

urp

le t

o b

lack

eq

ua

nt

su

bh

ed

ral to

ro

un

de

dfr

actu

red

/clo

ud

yu

nkn

ow

n d

ue

to

da

rk c

olo

r/fr

actu

ring

larg

e

rare

lig

ht

pu

rple

elo

ng

ate

(~

2:1

to

5:1

)e

uh

ed

ral

cle

ar

rare

to

no

ne

larg

e

fra

cti

on

c

(co

lorl

es

s)

ab

un

da

nt

co

lorl

ess

eq

ua

nt

we

ll r

ou

nd

ed

cle

ar

rare

larg

e

sp

ars

eco

lorl

ess

ve

ry e

lon

ga

te (

3:1

an

d g

rea

ter)

to s

lig

htly e

lon

ga

te (

2:1

)

eu

he

dra

lcle

ar

sp

ars

e t

o

co

mm

on

me

diu

m

fra

cti

on

h

(ho

ne

y)

ab

un

da

nt

lig

ht

ho

ne

ye

qu

an

t to

slig

htly e

lon

ga

te (

2:1

)su

bh

ed

ral to

an

he

dra

lcle

ar

sp

ars

em

ed

ium

to

la

rge

co

mm

on

ve

ry lig

ht

to lig

ht

ho

ne

yslig

htly t

o v

ery

elo

ng

ate

(2

:1 t

o

4:1

an

d g

rea

ter)

eu

he

dra

lcle

ar

sp

ars

em

ed

ium

to

la

rge

co

mm

on

lig

ht

am

be

r~

eq

ua

nt

an

he

dra

l to

ro

un

de

dslig

htly t

o h

igh

ly f

ractu

red

un

kn

ow

n d

ue

to

fra

ctu

rin

g

me

diu

m

sp

ars

eve

ry lig

ht

ho

ne

y t

o v

ery

lig

ht

am

be

r

eq

ua

nt

we

ll r

ou

nd

ed

cle

ar

rare

me

diu

m t

o la

rge

sp

ars

em

ed

ium

to

da

rk h

on

ey;

co

mm

on

Fe

oxid

e s

tain

eq

ua

nt

to s

lig

htly e

lon

ga

te t

o

mo

de

rate

l y e

lon

ga

te (

3:1

eu

he

dra

lcle

ar

un

kn

ow

n d

ue

to

co

lor

me

diu

m

sp

ars

elig

ht

ho

ne

y t

o d

ark

am

be

re

qu

an

te

uh

ed

ral to

su

bh

ed

ral

fra

ctu

red

un

kn

ow

n d

ue

to

fra

ctu

rin

g

me

diu

m t

o la

rge

rare

da

rk b

row

n t

o r

ed

~e

qu

an

ta

nh

ed

ral to

ro

un

de

dslig

htly t

o h

igh

ly

fra

ctu

red

/clo

ud

y

un

kn

ow

n d

ue

to

co

lor/

fra

ctu

rin

g

me

diu

m t

o la

rge

No

tes:

ab

un

da

nt

= 2

6-9

9%

; co

mm

on

= 6

-25

%;

sp

ars

e =

2-5

%;

rare

= >

0-1

%;

larg

e =

>1

00

µ m

lo

ng

est

exp

ose

d d

ime

nsio

n;

me

diu

m =

50

-10

0 µ

m lo

ng

est

exp

ose

d d

ime

nsio

n;

sm

all =

<5

0 µ

m lo

ng

est

exp

ose

d

dim

en

sio

n.

Zir

co

ns w

ere

se

pa

rate

d u

sin

g s

tan

da

rd t

ech

niq

ue

s (

Wilfle

y t

ab

le,

he

avy liq

uid

s,

an

d m

ag

ne

tic s

ep

ara

tio

n),

an

d h

an

d p

icke

d in

to c

olo

r a

nd

mo

rph

olo

gy f

ractio

ns u

sin

g a

bin

ocu

lar

mic

rosco

pe

.

66

Page 86: Copyright by Brook Colleen Daun Riley 2004

Tab

le 2

-2.

Sin

gle

-gra

in f

issio

n t

rack a

ges (

FT

GA

), P

b-P

b a

ges,

eff

ective u

raniu

m c

oncentr

ations (

eU

), a

nd R

am

an c

rysta

llinity d

ata

(band

wid

th a

nd

positio

n)

for

colo

r fr

action z

ircons f

rom

Sta

tion 2

3,

Huachuca M

ounta

ins.

gra

in #

FT

GA

(M

a)

err

or

(+/-

; m

.y.)

Pb

-Pb

ag

e (

Ma

)e

rro

r (1

SD

; m

.y.)

eU

(p

pm

)e

rro

r (1

SD

; p

pm

)F

WH

M c

orr

. (c

m-1

)e

rro

r (c

m -1

)s

hif

t (c

m-1

)e

rro

r (c

m -1

)

pin

k/p

urp

le

d1

65

59

11

/91

84

61

59

69

45

78

.60

.86

10

03

.70

.50

d1

61

65

18

/14

13

70

14

01

22

22

02

11

.81

.18

10

03

.40

.50

d0

70

74

27

/20

17

92

98

87

92

04

10

.61

.06

10

03

.30

.50

d1

27

13

43

7/2

91

53

21

50

53

93

68

.40

.84

10

04

.10

.50

d0

05

13

84

9/3

51

77

11

19

70

11

89

7.8

0.7

81

00

3.9

0.5

0

d1

44

14

15

2/3

71

54

11

08

41

93

96

.30

.63

10

04

.70

.50

L0

49

14

36

6/4

31

32

41

50

58

82

87

.90

.79

10

06

.10

.50

d1

95

14

35

8/4

01

72

07

35

28

21

6.1

0.6

11

00

5.1

0.5

0

L0

62

14

94

2/3

31

89

22

17

55

13

66

.10

.61

10

06

.20

.50

d1

31

15

47

1/4

71

94

12

48

57

03

77

.20

.72

10

04

.90

.50

L3

04

18

94

6/3

71

20

74

04

81

52

6.9

0.6

91

00

5.4

0.5

0

d0

12

20

76

2/4

81

74

81

16

37

14

66

.50

.65

10

04

.60

.50

d0

13

31

01

16

/80

19

81

14

93

64

13

8.7

0.8

71

00

4.2

0.5

0

L3

30

50

83

85

/19

81

92

61

60

26

42

46

.80

.68

10

05

.00

.50

co

lorl

ess

c2

_0

31

53

15

/12

44

81

27

10

53

13

54

.10

.50

10

06

.40

.50

c1

_3

00

75

19

/15

33

06

09

06

80

3.8

0.5

01

00

7.1

0.5

0

c2

_2

85

75

31

/22

60

34

51

36

71

42

5.5

0.5

51

00

6.4

0.5

0

c2

_2

50

77

15

/13

54

15

11

06

21

33

4.5

0.5

01

00

6.3

0.5

0

c2

_2

97

78

20

/16

31

33

41

05

21

02

4.4

0.5

01

00

6.7

0.5

0

c1

_7

72

84

25

/19

56

55

21

16

88

34

.90

.50

10

05

.40

.50

c1

_2

16

88

28

/21

58

01

40

97

78

24

.70

.50

10

05

.60

.50

c2

_2

22

90

28

/21

68

51

64

92

15

93

.90

.50

10

06

.50

.50

c2

_0

64

92

31

/23

41

14

37

19

57

3.6

0.5

01

00

7.0

0.5

0

c1

_0

82

10

53

1/2

41

74

23

91

21

02

4.8

0.5

01

00

5.7

0.5

0

c2

_6

95

10

52

9/2

33

23

37

77

32

84

.30

.50

10

06

.70

.50

c2

_0

65

10

73

3/2

55

87

11

46

19

14

3.7

0.5

01

00

6.9

0.5

0

c2

_5

28

10

72

8/2

24

58

57

95

98

34

.30

.50

10

06

.40

.50

c1

_7

28

11

13

5/2

76

72

73

82

18

04

.20

.50

10

06

.10

.50

c1

_3

76

11

32

6/2

12

88

20

97

05

85

.30

.53

10

05

.40

.50

c2

_5

44

11

63

8/2

94

81

44

76

65

95

.10

.51

10

06

.20

.50

c1

_2

23

12

83

4/2

73

72

15

28

54

17

44

.60

.50

10

06

.90

.50

c1

_5

98

13

24

1/3

23

06

26

12

58

15

84

.70

.50

10

04

.80

.50

c1

_4

37

13

32

4/2

04

53

28

83

34

04

.70

.50

10

06

.10

.50

c1

_1

10

14

84

5/3

51

78

21

05

33

71

56

.00

.60

10

06

.20

.50

c2

_0

44

18

78

0/5

31

51

91

05

34

21

86

.50

.65

10

05

.40

.50

c1

_2

91

52

01

68

/12

81

32

81

07

23

52

34

.60

.50

10

06

.70

.50

67

Page 87: Copyright by Brook Colleen Daun Riley 2004

Ta

ble

2-2

, co

ntin

ue

d

gra

in #

FT

GA

(M

a)

err

or

(+/-

; m

.y.)

Pb

-Pb

ag

e (

Ma

)e

rro

r (1

SD

; m

.y.)

eU

(p

pm

)e

rro

r (1

SD

; p

pm

)F

WH

M c

orr

. (c

m-1

)e

rro

r (c

m -1

)s

hif

t (c

m-1

)e

rro

r (c

m -1

)

ho

ne

y

h1

_1

09

57

13

/11

31

38

91

17

54

34

.40

.50

10

06

.10

.50

h2

_3

74

58

15

/12

24

84

91

16

82

83

.50

.50

10

07

.30

.50

h2

_2

40

61

17

/13

36

23

61

22

91

69

4.6

0.5

01

00

6.9

0.5

0

h2

_1

19

62

17

/13

46

64

41

13

86

14

.50

.50

10

05

.90

.50

h2

_2

49

64

20

/15

71

61

01

93

72

46

4.5

0.5

01

00

6.3

0.5

0

h2

_2

48

70

17

/14

19

81

91

08

06

94

.50

.50

10

06

.20

.50

h2

_2

92

71

15

/13

56

86

58

08

64

4.3

0.5

01

00

7.4

0.5

0

h2

_2

76

73

17

/14

24

12

28

87

39

3.7

0.5

01

00

6.6

0.5

0

h1

_4

82

74

17

/14

48

71

05

14

54

57

4.6

0.5

01

00

5.9

0.5

0

h2

_0

31

80

18

/15

33

84

18

83

25

5.4

0.5

41

00

6.1

0.5

0

h1

_1

80

85

21

/17

16

81

61

27

14

15

.90

.59

10

06

.70

.50

h2

_3

90

86

24

/19

39

72

18

77

59

4.8

0.5

01

00

6.8

0.5

0

h1

_2

24

10

32

4/2

04

63

34

10

17

50

4.5

0.5

01

00

6.7

0.5

0

h2

_3

58

10

42

6/2

16

09

53

96

19

45

.70

.57

10

06

.40

.50

h2

_1

89

10

83

2/2

41

48

43

04

92

67

24

.70

.50

10

06

.80

.50

h1

_1

01

10

95

0/3

32

50

37

10

11

13

46

.40

.64

10

05

.40

.50

h2

_5

11

11

63

0/2

41

31

13

29

68

63

36

.80

.68

10

06

.10

.50

h1

_3

00

11

83

4/2

63

47

40

15

04

75

4.7

0.5

01

00

7.0

0.5

0

h2

_0

95

13

43

4/2

75

92

92

11

26

64

4.6

0.5

01

00

7.0

0.5

0

h2

_2

21

15

66

6/4

41

68

72

40

50

05

64

.90

.50

10

06

.40

.50

No

tes:

Fis

sio

n t

rack a

ge

s (

± 2

σ u

nce

rta

inty

) w

ere

de

term

ine

d u

sin

g t

he

Ze

ta m

eth

od

, a

nd

ag

es w

ere

ca

lcu

late

d u

sin

g t

he

co

mp

ute

r p

rog

ram

an

d e

qu

atio

ns in

Bra

nd

on

(1

99

2).

F

or

zir

co

n,

a Z

eta

fa

cto

r o

f 3

52

.74

±

8.0

9 (

± 1

se

) is

ba

se

d o

n d

ete

rmin

atio

ns f

rom

bo

th t

he

Fis

h C

an

yo

n T

uff

an

d t

he

Bu

luk T

uff

. G

lass m

on

ito

rs (

CN

5 f

or

zir

co

n),

pla

ce

d a

t th

e t

op

an

d b

ott

om

of

the

irr

ad

iatio

n p

acka

ge

, w

ere

use

d t

o d

ete

rmin

e

the

flu

en

ce

gra

die

nt.

A

ll s

am

ple

s w

ere

co

un

ted

at

12

50

x u

sin

g a

dry

10

0x o

bje

ctive

(1

0x o

cu

lars

an

d 1

.25

x t

ub

e f

acto

r) o

n a

Ze

iss A

xio

sko

p m

icro

sco

pe

fitte

d w

ith

an

au

tom

ate

d s

tag

e a

nd

a d

igitiz

ing

ta

ble

t.

Etc

hin

g o

f sta

nd

ard

s f

ollo

we

d G

arv

er

an

d o

the

rs (

20

00

).

Pb

-Pb

ag

es (

± 1

σ u

nce

rta

inty

) a

re b

ase

d o

n L

A-I

CP

-MS

da

ta u

sin

g c

ou

nts

pe

r se

co

nd

of

bo

th 2

07P

b a

nd

206P

b,

an

d c

alib

rate

d u

sin

g t

he

UT

-01

zir

co

n

sta

nd

ard

; re

fer

to A

pp

en

dix

1 f

or

furt

he

r d

eta

ils.

Eff

ective

ura

niu

m (

± 1

σ u

nce

rta

inty

) co

nce

ntr

atio

ns a

re c

alc

ula

ted

ba

se

d o

n U

co

nce

ntr

atio

ns f

rom

th

e F

T w

ork

, a

nd

Th

co

nce

ntr

atio

ns a

re c

alc

ula

ted

ba

se

d o

n

a c

om

pa

riso

n o

f L

A-I

CP

-MS

U a

nd

Th

me

asu

rem

en

ts a

nd

FT

U m

ea

su

rem

en

ts,

as d

escri

be

d in

th

e t

ext.

R

am

an

ba

nd

wid

ths a

nd

ba

nd

wid

th s

hifts

we

re m

ea

su

red

with

in t

he

FT

-co

un

ted

are

a a

t th

e U

niv

ers

ity o

f

Ma

inz,

usin

g a

Jo

bin

Yvo

n L

ab

Ra

m-H

R e

qu

ipp

ed

with

an

Oly

mp

us o

ptica

l m

icro

sco

pe

(1

00

x o

bje

ctive

, n

um

eri

ca

l a

pe

rtu

re 0

.9).

S

pe

ctr

a w

ere

excite

d u

sin

g t

he

He

-Ne

63

2.8

nm

lin

e (

3 m

W a

t th

e s

am

ple

su

rfa

ce

),

with

wa

ve

nu

mb

er

accu

racie

s o

f ± 0

.5 c

m-1

, a

nd

sp

ectr

al re

so

lutio

n o

f a

pp

roxim

ate

ly 0

.5 c

m-1

(se

e m

eth

od

s in

Na

sd

ala

an

d o

the

rs,

20

01

).

Cite

d e

rro

rs f

or

Ra

ma

n b

an

dw

idth

(F

WH

M)

an

d p

ositio

n (

sh

ift)

qu

an

tifie

d a

s d

escri

be

d in

Na

sd

ala

an

d o

the

rs (

20

01

).

68

Page 88: Copyright by Brook Colleen Daun Riley 2004

69

for FT analysis. The magnitude of CL response within zircon is the result of the degree of

metamictization (Chuanyi and others, 1992; Nasdala and others, 2002), trace-element

composition (Hanchar and Rudnick, 1995), and other factors. As such, the use of CL remains a

qualitative guide for other quantitative portions of this work.

Crystallinity

In this study, at least one representative Raman measurement was made for the FT-

dated region of each grain. Measurements were also made to capture zonation detected in the

CL images, and in general included 2-6 measurements per grain. Raman microscopy measures

short-range order, or crystallinity, in the areas analyzed (volume resolution = 5 µm3), and the

selection of specific areas avoids the time-consuming process of making full Raman crystallinity

maps for each grain (e.g. Nasdala and others, 2001). Raman measurements were made at the

University of Mäinz (Germany) using a Jobin Yvon LabRam-HR equipped with an Olympus

optical microscope (100x objective, numerical aperture 0.9). Spectra were excited using the He-

Ne 632.8 nm line (3 mW at the sample surface), yielding wave number accuracies of ± 0.5 cm-1,

with spectral resolution of approximately 0.5 cm-1 (see methods in Nasdala and others, 2001).

Rare-Earth-Element Geochemistry and Pb-Pb Ages

Each FT-dated zircon was analyzed for Pb, U, Th, and REE in the FT-counted area

using laser-ablation inductively coupled mass spectrometry (LA-ICP-MS). These destructive

measurements were made using a LA-ICP-MS system (Platform quadrapole ICP-MS) at the

University of Texas at Austin. This system utilizes a LUV 213 Nd:YAG laser, which generates a

200 mJ beam at 1064 nm. The laser beam is polarized and passes through a series of harmonic

resonators, resulting in a final laser beam of up to 5 mJ of 213 nm ultraviolet light. Based on

grain behavior and machine response, the laser was used at 40-50% maximum power with 30-

Page 89: Copyright by Brook Colleen Daun Riley 2004

70

40 µm actual spot sizes. In general, this area is well within the FT-counted area. Ablated

material is injected into the plasma, extracted to the Hexapole cell, ionized, and passed through

the quadrapole mass analyzer to a single Daly-cup detector. For each grain, 78 scans of each

mass were made for 28Si, 91Zr, 96Zr, all REE, 176Hf, 179Hf, 206Pb, 207Pb, 208Pb, 232Th, and 238U.

For calculation of Pb-Pb ages, a ratio of the number of counts per second of 206Pb and

207Pb was made for multiple sequential analyses (up to 78 scans) of each grain during the

sample run. The total number of scans for each grain was divided into three groups, and the

blank-subtracted averages of these groups were used to calculate the concentration ages for the

majority of grains for which FT, crystallinity measurements, and REE compositions were

determined. Precision estimates for the ages were determined by finding the standard deviation

of the three counts-per-second averages over the course of the 78 runs; the standard deviation

of these values was then used as an estimate of the error (one standard deviation shown in

Table 2-2).

232Th, 238U, 235U, and REE concentrations were calculated based on counts-per-second

measurements from the LA-ICP-MS. Reduction of these data for the unknown zircons involves

comparison of counts per second for a given element over the run time with solution-

concentration data for a standard zircon (zircon UT-01, from the University of Texas at Austin

Vargas Mineral Collection; dissolved and analyzed by J. Lansdown, University of Texas, January

2003), and with concentrations of Zr from electron-microprobe analysis of the unknown zircons

(analyzed at Rensselaer Polytechnic Institute, Troy, NY, by K. Becker; JEOL-733; Appendix 6).

The data-reduction procedure for calculation of the concentrations appears in Appendix 3.

Page 90: Copyright by Brook Colleen Daun Riley 2004

71

DATA/OBSERVATIONS

Fission-track Data

As expected, the detrital zircon grains have a wide range of FT ages. These ages can

be resolved into fission-track-component populations or “peak ages” and 95% confidence

intervals, using a binomial peak-fitting routine (Brandon, 1996). Peak ages and confidence

intervals for the bulk sample appear in the first part of Table 2-3. From the sixty grains counted

(thirty from the long etch, thirty from the short etch), three well-defined peaks occur at 60, 91,

and 139 Ma (Figure 2-2). Older single-grain ages are also present in the bulk sample, ranging

from 250 Ma to 800 Ma. Sixty-seven grains were counted from the three color fractions (Table

2-1; Figure 2-3). Fitted peak ages and 95% confidence intervals for the p, c, and h fractions are

listed in Table 2-3. Within the bulk data as well as the color fraction data, there are several

single older ages. Fitted peak ages for the bulk sample plus color fractions do not differ much

from those fitted to the bulk data alone (Figure 2-2 and Figure 2-4). These data show statistical

peaks at 59, 80, and 128 Ma, and older single-grain ages range between 200 Ma and 800 Ma.

Given the 85-75 Ma depositional age of the Fort Crittenden Formation in this area

(Hayes, 1970a, 1970b; Hayes, 1987; Inman, 1987; Dickinson and others, 1989), the ~60 Ma

peak age in both the bulk and the composite sample is younger than deposition, and records

cooling following post-depositional heating. This young reset peak (Paleocene) is present in

varying abundance within many samples in the regional study, regardless of the depositional age

(Middle Jurassic-Upper Cretaceous; Chapter 1). Burial depths may have been on the order of 2

km (refer to Chapter 1), so that heating into the range of annealing probably is due to local

magmatic activity.

Page 91: Copyright by Brook Colleen Daun Riley 2004

Fort Crittenden Formation (Upper Cretaceous)

Huachuca Mountains Station 23

bulk data n = 60 grains

FT grain age (Ma)30 50 300 500 70010 1000

Pro

ba

bili

ty d

en

sity (

%/∆

z=

0.1

)

0

1

2

3

4

5

6

7

8

9

10

11

60 M M

a

139

Ma

depositional age

85-75 Ma

Figure 2-2. Cumulative probability density (PD) plot and fitted peaks for bulk zircon from

Station 23, Huachuca Mountains; peak ages fitted after Brandon (1996).

Heavy line is cumulative PD; histogram of grain ages shown behind curves;

data from 60 counted grains (30 from the 17 h etch, 30 from the 12 h etch).

72

Page 92: Copyright by Brook Colleen Daun Riley 2004

FT grain age (Ma)30 50 70 300 500 70010 100 1000

Pro

ba

bili

ty d

en

sity (

%/∆

z=

0.1

)

Fort Crittenden Formation (Upper Cretaceous)

Huachuca Mountains Station 23

color fraction data30 50 70 300 500 70010 100 1000

depositional age

85-75 Ma

colorless (N = 30 grains)

honey (N = 22 grains)

pink/purple (N = 15 grains)

Figure 2-3. Cumulative probability density (PD) curves for zircon fractions from Station 23,

1

2

3

4

5

1

2

3

4

1

2

3

4

5

6

7

73

Huachuca Mountains. Heavy line is cumulative PD; histogram of grain

ages shown behind curves.

Page 93: Copyright by Brook Colleen Daun Riley 2004

FT grain age (Ma)30 50 300 500 70010 1000

0

2

4

6

8

10

12

14

16

18

Pro

ba

bili

ty d

en

sity (

%/∆

z=

0.1

)Fort Crittenden Formation (Upper Cretaceous)

Huachuca Mountains Station 23

composite data

128

Ma

depositional age

85-75 Ma

n = 127 grains

Figure 2-4. Cumulative probability density (PD) plot and fitted peaks for all counted grains

a

59

(bulk plus color fractions), Station 23, Huachuca Mountains; peak ages fitted

after Brandon (1996). Heavy line is cumulative PD; histogram of grain ages

shown behind curves; data from 127 counted grains (60 from bulk sample,

67 from color fractions).

74

Page 94: Copyright by Brook Colleen Daun Riley 2004

75

The Paleocene-Eocene reset peak age is well defined in the bulk sample from Station

23, which contains abundant and varying proportions of each color population. The reset FT

ages are present in the pink/purple suite, but a relatively large percentage of grains in the honey

fraction also record similar young ages (Figure 2-3). The young reset peak age present in zircon

from Station 23 is probably related to the presence of the Tertiary quartz-monzonite body (Figure

2-1). However, as Paleocene-Eocene reset peak ages and/or single-grain reset FT ages occur

within most samples, whether adjacent to an exposed intrusion or not, resetting may also have

been related to regional heating and establishment of a higher geothermal gradient within the

field area, in addition to local intrusive bodies (Chapter 1).

In sandstones with poor depositional age control, detecting the presence of post-

depositional thermal annealing presents a challenge in the interpretation of multi-component

data. In the absence of other data, such as FT ages from older Jurassic and Cretaceous

sandstones or crystallinity measurements, these ages might have been interpreted incorrectly as

representing volcanic input to the basin during deposition; in this case, the depositional age

would have been inferred to have been younger. Additionally, overlooking the post-depositional

thermal event would have potentially significant implications for the understanding of subsequent

thermal and deformation history during the later Laramide orogeny. Resetting is now discussed

below in terms of grain-specific factors such as peak temperature, crystallization age, crystallinity

and radiation damage, and trace-element geochemistry.

Because deposition occurred at c. 85-75 Ma (Hayes, 1970a, 1970b; Hayes, 1987;

Inman, 1987; Dickinson and others, 1989), all FT ages in this range and older must reflect, in

part, source-rock cooling ages. However, based on FT ages alone, partial annealing of these

grains cannot be ruled out. In other words, it cannot be ruled out that some but not all of the

Page 95: Copyright by Brook Colleen Daun Riley 2004

76

accumulated fossil fission tracks in a grain are shortened or fully annealed. As such, these ages

must represent a minimum age for source-rock cooling. This cooling is either related to: (a)

slow cooling during exhumation of rock from depth; or (b) rapid cooling following high-level

magmatic activity. Grains with these FT ages could have been derived from older rocks

exhumed and cooled during extension associated with formation of the Bisbee basin and

deposition of the Bisbee Group (Hayes, 1970b; Bilodeau, 1978, 1979; Dickinson and others,

1986; Klute, 1987). These grains could have then been recycled into the Fort Crittenden

Formation. Older rocks could have included Precambrian granitoids/metasediments, Paleozoic

sandstones, and Triassic-Jurassic granitoids and volcanic and sedimentary rocks, as rocks of all

these ages were exhumed and shed into the Bisbee basin (Bilodeau, 1978). Alternatively, these

older grains could have been recycled from either volcanogenic detritus shed into the Bisbee

basin during deposition (i.e. magmatic arc activity coeval with extension of the basin), or

recycled from older rocks heated during this time by related magmatic activity. Similar older

peak ages (125-140 Ma) are present in all sandstones sampled from the Bisbee Group and the

older Jurassic volcaniclastic section in the Santa Rita Mountains, Canelo Hills, and Huachuca

Mountains (Chapter 1; Figure 2-5), making this a likely source for grains of these ages.

Additionally, there is ample local and regional petrologic evidence for recycling of both the

Bisbee Group as well as intermediate volcanic rocks into the Fort Crittenden Formation (Inman,

1982, 1987; Hayes, 1986, 1987; Lindberg, 1987; Mann, 1995).

The intermediate peak age (P2) in the bulk sample is 91 Ma, whereas for the composite

sample, the intermediate age is 80 Ma (Table 2-3). Given the depositional age of the Fort

Crittenden Formation (85-75 Ma), and the fact that P2 in both the bulk and composite sample is

close to the depositional age, there are two possibilities for the source of grains that comprise

Page 96: Copyright by Brook Colleen Daun Riley 2004

Kfc

Kc

Kc

Kg

aJh

?

Km

oK

ga

Kc

Sta

tion 2

3

Kfc

Kc

Km

o

Km

u

Kc

Km

o

Km

o

Km

o

Km

u

Kg

Kg

Kga

Pzu

Pzu

Kg

a

Kg

eK

ga

Pzu

e

Pzu

Pzu

Jh

Km

o

Kg

Pzu

Km

o

Kg

Kg

a

Kg

Km

oK

g

Km

u

Kc

Kfc

TQ

uK

b?

TQ

u

Km

o?

Tg

Tg

TQ

u

TQ

u

TQ

u

TQ

uTi

Ti

Km

o

pC

g

Tg

TQ

u

KfcTi

Pzu

e

Qa

l

Tg

TQ

u

Qg

Km

o

Km

u

Kc

Kga

Kg

Kb

pC

g

Jh

JTc

JT

h

JT

h?

JTc

JTc

JT

h

JT

h

JT

h JTc

JT

h

JTc

JTc?

JTc?

Te

rtia

ry a

nd

Qu

ate

rna

ry g

rave

ls,

allu

viu

m

Tert

iary

intr

usiv

es (

quart

z

mo

nzo

nite

, a

laskite

, g

ran

o-

dio

rite

, a

lka

li d

iorite

); in

tern

al

ag

e r

ela

tio

nsh

ips u

nce

rta

in

Up

pe

r C

reta

ce

ou

s F

ort

Critt

en

de

n

Fo

rma

tio

n (

ea

rly L

ara

mid

e b

asin

fill

)

Low

er

Cre

taceous B

isbee

Gro

up

Ju

rassic

Ca

ne

lo H

ills

Vo

lca

nic

s a

nd

asso

cia

ted

rocks

Pa

leo

zo

ic s

ed

ime

nta

ry

rocks, exotic b

locks o

f

Pa

leo

zo

ic w

ith

in o

the

r u

nits

Pre

ca

mb

ria

n g

ran

ite

01

kilo

me

ters

mile

s0

1

fissio

n tra

ck s

am

ple

; S

tation 2

3 d

enote

d

vitrin

ite

sa

mp

le

fau

lt;

da

sh

ed

wh

ere

in

ferr

ed

an

ticlin

al tr

ace

; d

ash

ed

wh

ere

in

ferr

ed

,

plu

ng

ing

wh

ere

in

dic

ate

d

syn

clin

al tr

ace

; d

ash

ed

wh

ere

in

ferr

ed

,

plu

ng

ing

an

d/o

r o

ve

rtu

rne

d w

he

re in

dic

ate

d

co

nta

ct;

da

sh

ed

wh

ere

in

ferr

ed

Map

Un

its

Map

Sym

bo

ls

pC

g

pC

g

pC

g

pC

g

pC

g

Fig

ure

2-5

. H

ua

ch

uca

Mo

un

tain

s g

eo

log

ic m

ap

(g

en

era

lize

d a

fte

r H

aye

s a

nd

Ra

up

, 1

96

8)

sh

ow

ing

re

pre

se

nta

tive

zirco

n fis

sio

n-t

rack

reset F

TG

A

pe

ak a

ge

s f

rom

th

e r

eg

ion

al stu

dy.

S

tatistica

l p

ea

k a

ge

s a

re b

ase

d o

n 3

0-6

0 d

ate

d g

rain

s p

er

sa

mp

le, e

xce

pt a

s

no

ted

. R

efe

r to

Ch

ap

ter

1 a

nd

Ap

pe

nd

ix 4

fo

r fu

rth

er

de

tail

on

pe

ak a

ge

s, u

nce

rta

intie

s, sin

gle

-gra

in a

ge

da

ta.

77

42

Ma

68

Ma

10

7 M

aN

= 2

9

59 M

a

80

Ma

12

8 M

aN

= 1

27

92

Ma

12

1 M

aN

= 4

2

60 M

a

13

8 M

aN

= 3

1

13

7 M

aN

= 1

8

10

4 M

a

17

1 M

aN

= 2

6

10

6 M

a

23

6 M

a

80

3 M

aN

= 3

3

χ2

age:

19

0 M

aN

= 5

χ2

age:

10

9 M

aN

= 5

114

°113

°11

111°

110°

37

°

36

°

35

°

34

°

33

°

32

°114°

113°

11

111

°110

°

37

°

36

°

35

°

34°

33

°

32

°

Page 97: Copyright by Brook Colleen Daun Riley 2004

Tab

le 2

-3.

Fis

sio

n t

rack p

eak a

ges f

rom

Sta

tion 2

3,

Huachuca M

ounta

ins.

P1

P2

P3

bu

lk s

am

ple

pe

ak a

ge

(M

a)

60

91

13

9

n =

60

(3

0/3

0)

95

% c

.i.

(+/-

; m

.y.)

8/7

10

/91

8/1

6

% o

f g

rain

s1

7.3

48

.62

9.1

pin

k/p

urp

le (

fra

cti

on

p)

pe

ak a

ge

(M

a)

63

—1

75

n =

14

95

% c

.i.

(+/-

; m

.y.)

9/8

19

/17

% o

f g

rain

s2

7.3

72

.7

co

lorl

es

s (

fra

cti

on

c)

pe

ak a

ge

(M

a)

—7

81

20

n =

30

(1

9/1

1)

95

% c

.i.

(+/-

; m

.y.)

7/7

11

/10

% o

f g

rain

s4

5.6

51

.1

ho

ne

y

(fr

ac

tio

n h

)p

ea

k a

ge

(M

a)

70

—1

18

n =

22

(1

6/6

)9

5%

c.i.

(+/-

; m

.y.)

6/5

12

/11

% o

f g

rain

s5

8.8

41

.2

bu

lk +

fra

cti

on

sp

ea

k a

ge

(M

a)

59

80

12

8

n =

12

79

5%

c.i.

(+/-

; m

.y.)

7/6

7/7

10

/9

% o

f g

rain

s1

1.4

37

.24

6.6

No

tes:

FT

pe

ak a

ge

s (

± 2

σ u

nce

rta

inty

) fo

r b

ulk

zir

co

n,

fra

ctio

ns,

bu

lk +

fra

ctio

ns f

rom

Sta

tio

n 2

3 w

ere

de

term

ine

d u

sin

g t

he

Ze

ta m

eth

od

, a

nd

ag

es w

ere

ca

lcu

late

d u

sin

g t

he

co

mp

ute

r p

rog

ram

an

d e

qu

atio

ns

in B

ran

do

n (

19

92

).

n =

nu

mb

er

of

gra

ins c

ou

nte

d (

wh

ere

th

ree

nu

mb

ers

are

cite

d,

firs

t is

to

tal n

um

be

r o

f g

rain

s,

se

co

nd

is n

um

be

r fr

om

lo

ng

etc

h,

thir

d is n

um

be

r fr

om

sh

ort

etc

h).

P

1 =

fitte

d p

ea

k 1

; P

2 =

fitte

d p

ea

k 2

; P

3 =

fitt

ed

pe

ak t

hre

e.

Fo

r zir

co

n,

a Z

eta

fa

cto

r o

f 3

52

.74

± 8

.09

(± 1

se

) is

ba

se

d o

n d

ete

rmin

atio

ns f

rom

bo

th t

he

Fis

h C

an

yo

n T

uff

an

d t

he

Bu

luk T

uff

. G

lass m

on

ito

rs (

CN

5 f

or

zir

co

n),

pla

ce

d a

t th

e t

op

an

d b

ott

om

of

the

irra

dia

tio

n p

acka

ge

, w

ere

use

d t

o d

ete

rmin

e t

he

flu

en

ce

gra

die

nt.

A

ll s

am

ple

s w

ere

co

un

ted

at

12

50

x u

sin

g a

dry

10

0x o

bje

ctive

(1

0x o

cu

lars

an

d 1

.25

x t

ub

e f

acto

r) o

n a

Ze

iss A

xio

sko

p m

icro

sco

pe

fitte

d w

ith

an

au

tom

ate

d

sta

ge

an

d a

dig

itiz

ing

ta

ble

t.

Etc

hin

g o

f sta

nd

ard

s f

ollo

we

d G

arv

er

an

d o

the

rs (

20

00

).

78

Page 98: Copyright by Brook Colleen Daun Riley 2004

79

these peak ages. If these grains were derived from rapid exhumation of source rock, there

remain approximately 5-15 m.y. in the case of the 91 Ma peak age to move these zircons from

the partial annealing zone (PAZ, at 8-10 km given an average geothermal gradient of 25°C/km)

to the surface (based on the proposed depositional age of the Fort Crittenden Formation and the

peak age). These estimates suggest exhumation rates of approximately 0.5-1.5 km/m.y.

Although this is fairly rapid, it is in keeping with exhumation related to normal faulting in an

extending backarc tectonic environment.

However, the P2 age in the composite sample, 80 Ma, presents a problem in

considering that these grains were derived by exhumation, because exhumation would have to

have been almost instantaneous to generate a peak age of 80 Ma. Thus, there are two

possibilities for the source of the 80 Ma peak: (a) these grains may have a volcanogenic source

transitional in age between deposition of the Bisbee Group and the Fort Crittenden Formation; or

(b) this peak may represent partially or fully reset ages. This resetting may have occurred at ~80

Ma (full reset in the source), or may have occurred in the basin strata during the thermal event

that produced the 59 Ma peak age (i.e. partial reset for these grains).

If zircons that comprise the 80 Ma P2 age are first-cycle volcanic, this would indicate at

least two distinct provenances for zircon in the Fort Crittenden Formation in this area,

considering both the bulk and composite sample: a synorogenic volcanic component, and an

exhumed source (Lower Cretaceous and older; 91 Ma P2 age). Regionally, volcanic activity is

indicated toward the end of and immediately following Fort Crittenden deposition in the nearby

Santa Rita Mountains (Fort Crittenden Formation, upper tuff member (Drewes, 1968, 1971);

Salero Formation, 79-73 Ma, K-Ar and Ar-Ar on biotite (Drewes, 1968; Keith and Wilt, 1986;

Hayes, 1987); all cited ages from sources prior to 1976 have been corrected after Dalrymple,

Page 99: Copyright by Brook Colleen Daun Riley 2004

80

1979; refer to Appendix 1), and in the Canelo Hills (Jones Mesa volcanics, 72 Ma, K-Ar on biotite

(Hayes, 1970b); Appendix 1). Volcanic activity also occurred at this time in the southern Canelo

Hills as well, although the stratigraphic relationship with the Upper Cretaceous section is

indeterminate (Dove Canyon volcanics, 73 Ma, K-Ar on biotite (Marvin and others, 1973; Marvin

and others, 1978); Meadow Valley trachyandesite, 74 Ma, K-Ar on biotite (Marvin and others,

1973; Marvin and others, 1978); Appendix 1). In the Huachuca Mountains, the upper contact of

the Fort Crittenden Formation is either erosional, with Tertiary gravels resting in angular

unconformity atop the Upper Cretaceous, or is a fault (Hayes and Raup, 1968; Hayes, 1986). As

such, it is difficult to discern whether or not this volcanic activity extended to the east. The only

documented occurrence of Cretaceous volcanic rocks directly underlying the Fort Crittenden

Formation are the Corral Canyon volcanics in the Canelo Hills (75 Ma; K-Ar on biotite; (Hayes,

1987); Appendix 1), which are conformably overlain by Fort Crittenden clastic rocks. If these

rocks were more extensive during deposition, and were subsequently eroded, this might have

provided a nearby source for ~80 Ma FT ages. However, as is shown below, Pb-Pb

crystallization ages demonstrate no synorogenic volcanic source for this particular sample.

In both the bulk sample and the color fractions, there is a population of young grain ages

(comprising P1, 59 Ma in the bulk sample; 60 Ma in the composite sample; Table 2-3) that is 15-

25 m.y. younger than the depositional age of 85-75 Ma. This age coincides with widespread

plutonism in the region (Drewes, 1972). Given the presence of this 60-59 Ma peak age, it is

possible that all older peak ages represent a partially reset older component that is a minimum

cooling age for the source. In other words, the original provenance cooling age may have been

compromised. However, this alternative is considered unlikely based on the following

observations. Single-grain ages which comprise both the 91 Ma and the 80 Ma peaks are

abundant in these data (Table 2-3; 29 of 60 counted grains in the bulk sample (49%), and 47 of

Page 100: Copyright by Brook Colleen Daun Riley 2004

81

127 grains counted in the composite sample (37%)). Peaks in the 91/80 Ma age range are

present in all samples throughout the study area, including heated and annealed Upper Jurassic

volcaniclastic sandstones, as well as Lower Cretaceous Bisbee Group sandstones and Upper

Cretaceous synorogenic rocks (Figure 2-5). Older peak ages (detrital; 110-100 Ma, 125 Ma, and

older ages) are also present in all samples from the larger exhumation study (Chapter 1). These

older ages are characteristic of Mesozoic sandstones within this basin, and the spread of these

ages is relatively narrow (Figure 2-5). In the case of resetting an older age component via post-

depositional thermal disturbance, one might expect the following: an overall smaller percentage

of the total grains would have the reset age (depending on the susceptibility of a grain to being

reset); a wider spread of reset peak ages from one locality to the next, depending on the locus,

duration, and areal extent of thermal disturbance; and a distinct lack of consistency of peak ages

among samples throughout the area (depending on the age of thermal resetting in different

locations). These features are not observed in the older peaks (91/80 Ma and older peaks) in

Station 23, and similar peak ages throughout the study area.

The two older statistical peak ages and older single-grain ages could be interpreted as

reflecting exhumation associated with Bisbee basin formation, and heating associated with

intrusion ± volcanism prior to subsidence of the Laramide basin. This hypothesis allows for the

possibility that the 80 and 91 Ma FT peak ages are either volcanic, or related to thermal resetting

during the transition from Bisbee basin deposition to deposition in the Laramide basin. While a

volcanic source is plausible given the FT data, it was not found in the Pb-Pb ages. The majority

of the analyzed grains have Pb-Pb ages that are significantly older (one group 160-720 Ma, and

a subordinate group 1200-2000 Ma; Table 2-2). The Pb-Pb ages then provide a more distinctive

assignment of the source of the 80 and 91 Ma peaks for this sample: given that all crystallization

ages are much older than Late Cretaceous, the FT peaks encompassing these grains are not

Page 101: Copyright by Brook Colleen Daun Riley 2004

82

directly related to Late Cretaceous volcanism, but potentially are related to thermal resetting

associated with Late Cretaceous magmatism as the arc advanced eastward (Coney, 1978;

Dickinson and Snyder, 1978; Keith, 1978).

Vitrinite-Reflectance Data

As an independent estimate of the peak temperatures reached in the sampling areas,

interbedded mudrocks of the Fort Crittenden Formation were sampled for vitrinite-reflectance

(VR) analysis. At higher absolute temperatures, reflectance of vitrinite fragments in the samples

increases, and Ro (mean reflectance) values rise (see Price, 1983). These thermal maturity

values, based on the average Ro value of 20-50 un-oxidized vitrinite fragments per sample, were

then used to estimate maximum temperatures reached by these rocks. As such, the VR data

complement the fission-track and other thermochronology data, but prove difficult to obtain in

sandstone-rich sections where mudrocks are lacking, and/or where organic material has been

oxidized during diagenesis or weathering. Additionally, the calibration of peak-temperature

estimates for Ro values varies somewhat (e.g. Héroux and others, 1979; Staplin, 1982; Price,

1983; Burnham and Sweeney, 1989, Barker and Pawlewicz, 1994). Accordingly, the range of

peak temperature values associated with a given Ro value must be evaluated using sample

context and field relationships.

Because of the relatively coarse nature of the section, vitrinite-bearing mudrocks occur

at restricted intervals; an additional constraint is the necessity of sampling interbedded mudrock

as close as possible to the interval sampled for FT work. Fresh mudrock in the lower part of the

uppermost Cretaceous section was sampled at three locations in the northern and central

Huachuca Mountains (limited to the Fort Crittenden Formation; Figure 2-1). Siltstone and shale

south of Station 23 were sampled (Figure 2-1), but did not yield usable vitrinite because of

Page 102: Copyright by Brook Colleen Daun Riley 2004

83

oxidation. However, shale and siltstone at a stratigraphically similar position 9.5 km to the north

yielded Ro values of 3.00% and 2.03%, that correspond to peak temperatures of 225-300°C (Ro

= 3.00%), and 150-250°C (Ro = 2.03%) (interpreted after Héroux and others, 1979; Staplin,

1982; Burnham and Sweeney, 1989, and Barker and Pawlewicz, 1994). These values provide a

broad constraint on the local maximum temperature conditions. The vitrinite data indicate that

the present erosional level across the region is such that the strata attained temperatures near

the proposed closure temperature for FT in zircons.

It is important to note that annealing of some grains identified in FT data for this study

occurred at significantly lower Ro value than that proposed by previous workers. Green and

others (1996) stated that no annealing in zircons is detected at Ro values less than 4%

(correlated to maximum temperature of >260°C using the model of Burnham and Sweeney

(1989)). Reflectance values associated with zircon FT annealing in this study are significantly

lower than those reported by Green and others (1996), and this observation suggests that

annealing of fission tracks in radiation-damaged zircons occurs at much lower temperatures than

the temperature required to anneal all grains in a variable population.

The Fort Crittenden Formation here illustrates an important lesson in terms of the field

appearance of thermally modified sedimentary rocks. The character of the samples in the field

did not give rise to any suspicion that these sandstones and conglomerates were heated to

temperatures of 200°C or higher. Most samples from this area are only moderately indurated,

with almost no quartz cement, and no veining. The VR data make it evident that rocks at the

present erosional level were heated to 150°C-225°C. Burial depths of ~2 km (Chapter 1) make it

evident that heating by the nearby Tertiary intrusions was significant. Such heating explains the

Page 103: Copyright by Brook Colleen Daun Riley 2004

84

presence of the Paleocene-Eocene reset FT peak ages in sandstones interbedded with these

mudrocks throughout the northwestern and west-central parts of the range (Figure 2-5).

The issue of local versus regional heating is also pertinent to this discussion. Vitrinite-

reflectance data for the entire study area (refer to Chapter 1) suggest that these rocks did not

exceed ~225°C or so (Figure 2-1). In the case of samples in other parts of the study area (Santa

Rita Mountains, Fort Crittenden Formation shale member; Chapter 1), vitrinite-reflectance data

for one sample indicate peak temperatures of 85-135°C (interpreted after Héroux and others,

1979; Staplin, 1982; Burnham and Sweeney, 1989), which should be well below the temperature

range for annealing in zircons, and lower than maximum temperatures recorded elsewhere in the

Huachuca Mountains (Chapter 1). Vitrinite data are sparse, but suggest that heating effects

caused by Tertiary intrusions were variable because of covered plutons and associated

hydrothermal fluid flow. Consequently, peak-temperature determinations do not always show a

correlation with proximity to lower Tertiary intrusive rocks.

Reset FT peak ages and/or single-grain reset FT ages indicate that, with the exception

of two locations, most samples experienced sufficient Paleogene heating to reset the FT ages of

certain grains (Appendix 4). Samples with reset ages include those samples near Paleogene

intrusions and dikes (i.e. Station 9; Figure 2-5), as well as those not near any obvious heat

source exposed at the surface (Station 11, 13; Figure 2-5). It is thus concluded that heating to

150-225°C occurred on a regional scale at this erosional level. An elevated regional thermal

gradient resulted from the eastward migration of arc-related magmatic activity through

southeastern Arizona associated with shallowing of the subducting slab during this time (Snyder

and others, 1976; Coney, 1978; Dickinson and Snyder, 1978; Keith and Wilt, 1986).

Additionally, it is possible that the basin-bounding fault zone in this area and farther northwest

Page 104: Copyright by Brook Colleen Daun Riley 2004

85

along the Sawmill Canyon fault zone in the Santa Rita Mountains aided the channelization of this

heat flow, although fission-track ages from rocks well outside this fault zone would be needed to

support this. Such controls on the FT ages of zircons in Newark basin fill have been

documented by Steckler and others (1993), as discussed in greater detail in Chapter 1.

Pb-Pb Data from Color/Morphology Fractions

Pb-Pb ages were calculated from LA-ICP-MS data for fifty-six of the FT-dated grains

from Station 23, and unfortunately, during sample handling, eleven FT-dated zircons were lost.

Teflon FT mounts hold zircons by their crystal faces and edges rather than by gluing them in and

as such, zircons easily pop out of the mounts. Pb-Pb ages plotted versus FT ages for the same

zircons appear in Figure 2-6. Uncertainties shown are the 95% confidence intervals for fission-

track ages and one standard deviation for Pb-Pb ages.

Several important findings result from the relationships among crystallization age, color,

and FT age. (1) These data show that a primary difference between the pink/purple suite and

the other zircons in this sample is crystallization age (Pb-Pb): the former are dominantly

Proterozoic, ranging from 1200-2000 Ma, whereas the others show diverse ages, with most

between 160 and 720 Ma (Table 2-2; Figure 2-6). An older group of honey and colorless grains

is also present, with six Pb-Pb ages from 1300 to 1800 Ma. (2) The youngest FT ages (reset)

are from the pink/purple fraction, but a relatively large percentage of young reset grains are also

from the honey fractions. (3) There is a much greater spread of FT ages in the pink/purple

zircons, versus the tighter cluster of both FT and Pb-Pb ages for the majority of the honey and

colorless grains. (4) At Station 23, there is no evidence for coeval volcanism during deposition.

Page 105: Copyright by Brook Colleen Daun Riley 2004

Pb-Pb age vs. Fission track grain age

0

100

200

300

400

500

600

700

0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200

Pb-Pb age (Ma)

FT

GA

(M

a)

pink/purple (N = 14 grains)

colorless (N = 22 grains)

honey (N = 20 grains)

Figure 2-6. Pb-Pb age versus fission-track age (FTGA) for the same zircon grains from Station

depositional

age of sample

86

23, Huachuca Mountains. Cited uncertainties for Pb-Pb ages are 1 standard

deviation, and 95% confidence intervals for FT ages.

Page 106: Copyright by Brook Colleen Daun Riley 2004

87

As the grains with older Pb-Pb ages tend to be pink and purple, these data reaffirm the

previous generalization that the development of pink/purple color is mainly related to time since

crystallization. However, the issue is more complicated than simply time since crystallization, as

demonstrated by Garver and Kamp (2002). The accumulation of radiation damage, more

specifically α-damage, is probably a primary control on the development of color in zircons, and

the level of accumulation is controlled by U + Th concentration and single-grain thermal history.

Older grains from all populations have had more time to accumulate radiation damage, and are

also, of course, more likely to have had a more complicated thermal history.

These data also show that grains with greater amounts of α-damage (calculated from

the crystallization age and U and Th concentrations; see below), are preferentially annealed and

lose fission-track damage (Figure 2-6; Table 2-2). Young reset FT ages are most common in

those grains from all color groups that have older crystallization ages, and/or elevated U+Th

content (Table 2-2). Fission-track age distributions for the pink/purple suite are more dispersed

overall than those of other color fractions. This wider range of FT ages for the older pink/purple

group is probably related to these grains having more complicated thermal histories.

Another important relationship is the similarity between the honey and colorless

populations. These grains have similar age distributions (FT and Pb-Pb), which would suggest

that the difference in color is unrelated to thermal history. It is worth noting that the difference

between these two color populations (honey series versus colorless series) may reflect specific

zircon trace-element composition (REE), as suggested by Gastil and others (1967) and Garver

and Kamp (2002). Following these observations of α-damage in grains with older crystallization

ages and younger reset fission-track ages, the next step is to look at crystallinity in single grains,

and how this relates to track retentivity.

Page 107: Copyright by Brook Colleen Daun Riley 2004

88

Raman Microscopy Data

As radiation damage accumulates in a zircon, there should be a decrease in crystallinity,

because radiation damage causes crystal lattice disruption (Murakami and others, 1991;

Nasdala and others, 1995; Nasdala and others, 2001). Resulting from derivation from multiple

sources, zircons in a detrital suite will likely have U and Th concentrations and thermal histories,

and will accordingly have different crystallinities. As such the spread of individual grain ages

within a fraction would then be a function of different thermal histories and/or U + Th

concentrations. The amount of short-range order of the crystal lattice, and therefore the degree

of crystallinity of a zircon, is related to the amount of radiation damage, with α-damage being the

main contributor (Murakami and others, 1991; Nasdala and others, 1995; Nasdala and others,

2001). The factors controlling the amount of α-damage are U + Th contents and the duration of

α-damage accumulation, the latter being a function of single-grain thermal history. Greater α-

damage and resultant lower crystallinity have been proposed to decrease the effective closure

temperature for the fission-track system (Kasuya and Naeser, 1988), and the more damaged

grains will be preferentially reset by post-depositional heating. Raman microprobe analyses are

here used to determine short-range order in the crystal lattice within the FT-counted area and

among different CL-detected zones in fifty-seven color fraction zircons from the Station 23

sample (Figure 2-1; Table 2-2). Unfortunately, ten FT-dated grains were lost from the p, c, and h

mounts during preparation for this analysis.

With α-decay of 235U, 238U, and 232Th in the zircon, atomic displacements related to the

passage of α-particles and movement of α-recoil nuclei produce changes in atomic positions and

consequent variations in bond lengths and bond angles within the crystal lattice. This process

eventually leads to development of interconnected zones of amorphous or non-crystalline

material, collectively known as α-damage (Murakami and others, 1991). Depending on the

Page 108: Copyright by Brook Colleen Daun Riley 2004

89

parent atom, decay by alpha emission to stable daughter Pb occurs between six and eight times,

whereas a single damage track is produced during spontaneous fission of 238U. Because α-

decay is the dominant mode of decay for U and Th, the contribution of fission tracks to the

overall damage state is negligible relative to α-recoil and α-particle tracks (Murakami and others,

1991). Greater damage in more restricted areas of the lattice is produced by α-recoil, whereas

passage of α-particles tends to produce point defects in the early stages of damage

development (Murakami and others, 1991). As atomic displacements accumulate, the lattice

becomes increasingly disordered, and crystallinity decreases; widths of Raman bands within the

spectrum 200-1010 cm-1 increase, relative intensities decrease, and a shift to overall lower wave

numbers is observed (Nasdala and others, 1995; Nasdala and others, 2001). As such, a highly

metamict grain would exhibit wave numbers less than 1000 cm-1, and Raman bands with full

width at half-maximum intensity (FWHM) of >30 cm-1, whereas a completely crystalline zircon

would yield FWHM of 1.8 cm-1, and wave number of 1008.3 cm-1 (both with 0.5 cm-1 uncertainty;

Nasdala and others, 2002). Broadening of the ν3SiO4 Raman band at ~1000 cm-1 has been

found to demonstrate the strongest response to amorphization, and therefore FWHM is a

relatively sensitive indicator of the crystallinity of the area analyzed (Nasdala and others, 1995).

In the following work, observations based primarily on FWHM data are related to crystallization

and cooling ages and crystal chemistry for individual zircons.

All measurements for grains from the Station 23 sample have the expected correlation of

increasing FWHM with decreasing wave number as grains range from less radiation damaged to

more damaged (Figure 2-7). In particular, the pink/purple zircons (fraction p), with Early to

Middle Proterozoic Pb-Pb ages, have overall wider peaks at lower wave numbers when

compared with all other color fractions. The honey and colorless populations, with much

younger crystallization ages, tend to overlap one another in a broad range from ~3.5 to 6.0 cm-1

Page 109: Copyright by Brook Colleen Daun Riley 2004

Full width at half maximum vs. wave number

1002.0

1003.0

1004.0

1005.0

1006.0

1007.0

1008.0

0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0

FWHM (cm-1

)

Ra

ma

n w

av

e n

um

be

r (c

m-1

)

pink/purple (N = 14 grains)

colorless (N = 22 grains)

honey (N = 21 grains)

Figure 2-7. Full-width at half maximum (FWHM) versus Raman wave number for color

fractions from Station 23, Huachuca Mountains. Cited uncertainties for

Raman FWHM and wave number quantified as described in Nasdala and

others (2001). FWHM and wave number position are measures of the

crystallinity of the analyzed portion of a zircon. Increased alpha-damage

accumulation results in decreased crystallinity, expressed as wider Raman

peaks (larger FWHM) and shifts to lower wave numbers.

90

Page 110: Copyright by Brook Colleen Daun Riley 2004

91

(FWHM) and 1005.0-1007.5 cm-1 (wave number). The overlapping behavior of the honey and

colorless populations indicates that the generation of honey color is probably unrelated to

differences in crystallinity of zircons from this sample. It is apparent that α-damage in zircons

from all color populations is annealed to some degree, and would be expected as a result of the

Paleogene heating. Despite this partial annealing, differences in behavior among these

populations can still be readily identified.

Another important factor in the accumulation of α-damage is the U and Th content,

termed effective uranium concentration (eU; e.g. Gastil and others, 1967). Model eU

concentrations for each grain were calculated based on both the FT and LA-ICP-MS data, as the

concentrations of U from the mass spectrometry were generally 0.5-1.0 times those derived from

the fission-track work. This disagreement in U concentrations between the two methods may be

due to several factors, including analytical differences resulting from factors such as differing

ablation rate among zircons with different crystallinities (including the standard zircon UT-01). U

concentrations derived from the FT data were used, and effective Th concentrations were

calculated based on the U:Th ratio from the ICP-MS work. Concentrations of U for each grain

based on the fission-track work were compared to those derived from the laser work, and a ratio

was calculated for FT U:laser U concentrations for each zircon. These values were then used to

scale the Th concentrations calculated from the laser work, assuming the machine response for

the two elements to be similar. The ranges of Th concentrations derived in this manner agree

favorably with Garver and Kamp (2002), who stated that the typical Th:U ratio is ~0.5 in zircon.

It is also important to note that in typical zircon (Th<U), the contribution to total α-decay events

by U accounts for 80% or more of the total damage.

Page 111: Copyright by Brook Colleen Daun Riley 2004

92

Trends in bandwidth versus eU reflect the similar behavior of the honey and colorless

populations, which are distinct from the pink/purple grains (Figure 2-8). Pink/purple zircons

retain more α-damage (greater FWHM) than colorless and honey grains. In addition, the

pink/purple series has a shallower positive slope as both bandwidth and eU increase, indicating

that with increasing U+Th, there is an increase in the amount of damage retained in a crystal

regardless of FT cooling age. This is in contrast to the honey and colorless series, which do not

show an increase in accumulated damage with increasing eU concentration.

Ranges of eU values also vary among the color populations. Most honey and colorless

grains range from 600 to 1500 ppm eU, whereas pink/purple grains have overall lower eU (200-

700 ppm, with only a few grains up to 1300 ppm). Note however that a few lower-eU honey and

colorless grains plot with a similar trend to the pink/purple population (Figure 2-8). The common

theme among these lower eU honey and colorless zircons is older Pb-Pb ages, relative to the

other grains from the population (ranging from 1300 to 1790 Ma for those five zircons; Table 2-

2). Despite the fact that eU concentrations for colorless and honey grains are overall higher than

those for pink/purple fraction grains, Raman band widths are narrower and show less dispersion

as compared to the pink/purple zircons (Figure 2-8). In other words, despite higher eU contents

for colorless and honey zircons, these grains are overall less damaged than the pink/purple

fraction. This less damaged character of the colorless and honey populations may reflect two

factors: first, the honey and colorless grains have overall younger crystallization ages than the

pink/purple grains (Table 2-2), allowing less total time to accumulate damage prior to the

Paleogene reheating event, despite the higher eU concentrations. The colorless and honey

populations may also have had less complicated thermal histories owing to their younger

crystallization ages. As such, these zircons could have behaved similarly during the heating

event, and may not have accumulated as much damage as the older pink/purple zircons,

Page 112: Copyright by Brook Colleen Daun Riley 2004

Full width at half maximum (FWHM) vs. eU

0

100

200

300

400

500

600

700

800

900

1000

1100

1200

1300

1400

1500

1600

0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0

FWHM (cm-1

)

eU

(p

pm

)

pink/purple UT-01 (N = 14 grains)

colorless UT-01 (N = 22 grains)

honey UT-01 (N = 20 grains)

Figure 2-8. Full-width at half maximum (FWHM) versus U+Th concentration (effective uranium,

or eU (= U+Th in ppm)) for color fractions from Station 23, Huachuca

Mountains. Cited uncertainties for Raman FWHM quantified as described

in Nasdala and others (2001). eU concentrations from fission track and

laser ablation ICP-MS data, with 95% confidence intervals (refer to text for

details). Note that increased alpha-damage accumulation results in

decreased crystallinity, which is expressed as wider Raman peaks (greater

FWHM).

93

Page 113: Copyright by Brook Colleen Daun Riley 2004

94

thereby producing the overall narrower bandwidths and smaller range of values as compared

with the pink/purple zircons. Alternatively, there may have been some homogenization of

bandwidths (and damage states) associated with the heating event, giving rise to the narrower

range of FWHM values. However, given sufficient development of α-decay prior to Paleogene

heating, differences among color populations were not completely lost to annealing. These

points are discussed below.

The distribution of the different color fractions also varies in bandwidth-FTGA space,

directly reflecting the decreased crystallinity of the pink/purple grains, and their fission-track age

(Figure 2-9). The relationship between bandwidth and FTGA has a positive slope, with the

pink/purple grains forming the high-damage end of the spectrum, and colorless and honey grains

overlap at the lower damage end of the spectrum. Several zircons are off this trend: three

pink/purple grains with the youngest FTGA, and the three pink/purple and colorless grains with

the oldest FTGA. The common factor among the three pink/purple zircons with young reset

FTGA, in addition to Early and Middle Proterozoic Pb-Pb ages, is very high eU, ranging from

694-1222 ppm (Table 2-2). At the older end of the range of FT ages, the common theme of the

colorless and pink/purple outliers is relatively low eU, ranging from 235-364 ppm. Interestingly,

these three grains also have old crystallization ages (1328-1981 Ma; Table 2-2), but at least in

part because of low eU, maintain older FTGA. Looking at the color populations separately, the

pink/purple distribution has a negative slope, as one might expect: where present crystallinities

are lowest (highest FWHM), FTGA are similarly low, and the youngest of these are the group

that form the young reset peak age.

Page 114: Copyright by Brook Colleen Daun Riley 2004

Full-width at half maximum vs. Fission track grain age

10

100

1000

0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0

FWHM (cm -1

)

FT

GA

(M

a)

pink/purple (N = 14 grains)

colorless (N = 22 grains)

honey (N = 21 grains)

Figure 2-9. Full-width at half maximum (FWHM) versus fission-track grain age (FTGA) for color

fractions from Station 23, Huachuca Mountains. Cited uncertainties for

Raman FWHM quantified as described in Nasdala and others (2001); 95%

confidence intervals shown for FT ages. Note that the pink/purple fraction

has the youngest reset FT ages, in addition to retaining the greatest alpha-

damage.

95

Page 115: Copyright by Brook Colleen Daun Riley 2004

96

Effective Dose/Effective Dose Factor

A “complete storage” value for accumulated α-damage based on eU and time since

cooling can be calculated (Nasdala and others, 2001). However, heating causes loss of α-

damage, and zircons from Station 23 store variable percentages of total α-damage possible,

given their crystallization ages and eU concentrations (compare with the “complete storage” line

calculated by Nasdala and others (2001; Figure 2-10a, Table 2-4 this work)). The “complete

storage” line was fitted to 33 Raman analyses from zircons considered to have remained at or

near surface temperatures following crystallization. When compared with these reference

zircons that define the complete storage line, the amount of damage stored in the pink/purple

series is much greater than that for either the honey or colorless zircons. There is also a wider

range of effective doses for these grains than for the colorless and honey populations. Honey

and colorless zircons store 7-80% of the maximum possible damage, with most grains having

10-40% of the total possible damage (Table 2-4). The honey and colorless populations also

demonstrate no correlation between increasing preservation of α-damage and crystallinity; i.e.

as preserved damage increases, there is no concomitant decrease in crystallinity. By contrast,

the pink/purple suite tends to store less of the total radiation damage possible, typically less than

25% of the total, and shows a narrower range of preserved damage. Pink/purple grains also

show a slight decrease in crystallinity with increasing damage stored. Given the older

crystallization ages of the pink/purple grains, it seems likely that the annealing of these grains

relates back to the observation that more radiation-damaged areas tend to anneal preferentially

relative to less damaged zones (Nasdala and others, 2001). These workers identified relatively

complete damage preservation only in zones with lower dosage (dominantly point defects), and

thus consider heavily damaged areas to be less stable and more easily annealed than point

defects.

Page 116: Copyright by Brook Colleen Daun Riley 2004

Comparison of

color fraction data with 'complete storage' line

0.0

5.0

10.0

15.0

20.0

25.0

30.0

0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 0.45 0.50

calculated -dose (*1016

/mg),

given Pb-Pb age

FW

HM

(c

m-1

)

unannealed zirconscomplete storage linepink/purple UT-01 (N = 14 grains)colorless UT-01 (N = 22 grains)honey UT-01 (N = 20 grains)Linear (complete storage line)

Effective dose factor vs. eU

0

100

200

300

400

500

600

700

800

900

1000

1100

1200

1300

1400

1500

1600

0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0

effective dose factor

(decimal % -damage stored)

eU

(p

pm

)

pink/purple (N = 14 grains)

colorless (N = 22 grains)

honey (N = 20 grains)

Effective dose factor vs. Fission track grain age

0

100

200

300

400

500

600

700

800

900

1000

0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0

effective dose factor

(decimal -damage stored)

FT

GA

(M

a)

pink/purple (N = 14 grains)

colorless (N = 22 grains)

honey (N = 20 grains)

Effective dose vs. eU

0

100

200

300

400

500

600

700

800

900

1000

1100

1200

1300

1400

1500

1600

0.00 0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08

effective dose ( -decay events /mg *1016

)

(~ -damage stored)

eU

(p

pm

)

pink/purple UT-01 corr (N = 14 grains)

colorless UT-01 corr (N = 22 grains)

honey UT-01 corr (N = 20 grains)

Effective dose vs. Fission track grain age

0

100

200

300

400

500

600

700

0.00 0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08

effective dose ( -decay events /mg *1016

)

(~ -damage stored)

FT

GA

(M

a)

pink/purple UT-01 corr (N = 14 grains)

colorless UT-01 corr (N = 22 grains)

honey UT-01 corr (N = 20 grains)

α

α

α

α

α

α

α

a.

b.

d.

c.

e.

full retention of

α-damage

97

Page 117: Copyright by Brook Colleen Daun Riley 2004

Figure 2-10a. Comparison of color fractions from Station 23, Huachuca Mountains with 'complete storage' line and analyses of 33 zircons considered to have remained at sub-annealing temperatures since crystallization (Nasdala and others, 2001). Dose is complete storage given the crystallization age and eU concentration of a grain. Cited uncertainties for doses are one standard deviation, and dose and FWHM uncertainties are quantified as described in Nasdala and others (2001). Note that the effect of annealing is to decrease the FWHM (increasing crystallinity by annealing alpha-damage; shown schematically with heavy arrows).

Figure 2-10b. Comparison of effective dose factor with eU from color fraction zircons from Station 23. Effective dose factor is the alpha-damage stored given the present crystallinity of a grain, given here as decimal percent with one standard deviation uncertainty. eU concentrations from fission-track and laser ablation ICP-MS data, with 95% confidence intervals (refer to text for details).

Figure 2-10c. Effective dose factor compared to fission-track age of color fraction zircons from Station 23. Effective dose factor values given as decimal percent with one standard deviation; 95% confidence intervals shown for FT ages.

Figure 2-10d. Effective dose compared to eU concentration for color fraction zircons from Station 23. The effective dose is the amount of alpha-damage preserved in a zircon based on the current Raman bandwidth (FWHM) measurement. Cited uncertainties for both effective doses and eU concentrations are one standard deviation.

Figure 2-10e. Comparison of effective dose to FT age for color fraction zircons from Station 23. Cited uncertainties for effective doses are one standard deviation; 95% confidence intervals shown for FT ages.

Page 118: Copyright by Brook Colleen Daun Riley 2004

Tab

le 2

-4.

Radia

tion d

am

age d

ose d

ata

for

colo

r fr

action z

ircons f

rom

Sta

tion 2

3,

Huachuca M

ounta

ins.

gra

in #

eff

ec

tive

do

se

fa

cto

r

(%)

err

or

(1 S

D;

%)

eff

ec

tive

do

se

(-d

ec

ay e

ve

nts

/mg

(*1

016))

err

or

(1 S

D;

* 1

016 /

mg

)

tota

l p

os

sib

le d

os

e

(-d

ec

ay e

ve

nts

/mg

(*1

016))

err

or

(1 S

D;

* 1

016 /

mg

)

pin

k/p

urp

le

L0

62

12

2.9

0.0

35

1.1

E-0

50

.30

0.0

74

d 1

95

12

2.3

0.0

34

1.5

E-0

50

.28

0.0

51

d 1

31

13

3.9

0.0

43

1.8

E-0

50

.34

0.1

0

d 1

65

13

2.1

0.0

52

9.0

E-0

60

.40

0.0

67

d 0

05

14

3.9

0.0

47

1.5

E-0

50

.33

0.0

90

d 1

61

16

4.1

0.0

75

2.1

E-0

50

.46

0.1

1

d 0

70

16

3.6

0.0

66

1.7

E-0

50

.40

0.0

89

d 1

27

18

3.9

0.0

51

1.4

E-0

50

.28

0.0

62

d 0

12

19

3.7

0.0

37

9.1

E-0

60

.20

0.0

38

d 1

44

19

4.2

0.0

36

1.1

E-0

50

.19

0.0

41

L0

49

20

5.6

0.0

47

2.0

E-0

50

.24

0.0

66

L3

04

22

2.9

0.0

40

1.1

E-0

50

.18

0.0

24

L3

30

27

9.2

0.0

40

1.2

E-0

50

.15

0.0

49

d 0

13

29

6.4

0.0

53

8.1

E-0

60

.18

0.0

41

co

lorl

ess

c2

22

21

24

.40

.01

92

.0E

-05

0.1

60

.06

1

c1

72

81

53

.30

.02

11

.8E

-05

0.1

40

.03

2

c2

25

01

52

.60

.02

21

.5E

-05

0.1

50

.02

6

c1

77

21

63

.30

.02

72

.3E

-05

0.1

70

.03

3

c2

28

51

83

.70

.03

02

.5E

-05

0.1

70

.03

6

c1

11

01

83

.40

.03

59

.0E

-06

0.2

00

.03

8

c2

06

51

85

.60

.01

81

.5E

-05

0.1

00

.03

0

c1

21

61

86

.90

.02

41

.9E

-05

0.1

30

.05

1

c2

52

82

14

.90

.02

31

.7E

-05

0.1

10

.02

5

c2

06

42

25

.10

.01

71

.6E

-05

0.0

74

0.0

17

c2

04

42

55

.70

.03

71

.0E

-05

0.1

50

.03

4

c1

30

02

56

.90

.01

71

.4E

-05

0.0

69

0.0

19

c2

54

42

75

.80

.02

82

.0E

-05

0.1

00

.02

2

c1

59

82

75

.50

.02

52

.7E

-05

0.0

90

.01

9

c1

29

12

96

.70

.02

56

.4E

-06

0.0

86

0.0

20

c1

43

73

04

.00

.02

49

.0E

-06

0.0

81

0.0

11

c2

29

73

16

.90

.02

21

.5E

-05

0.0

71

0.0

16

c1

22

33

21

70

.02

41

.6E

-05

0.0

77

0.0

42

c2

69

53

57

.50

.02

21

.6E

-05

0.0

64

0.0

14

c1

37

64

37

.10

.02

91

.6E

-05

0.0

69

0.0

11

c1

08

26

31

60

.02

52

.0E

-05

0.0

40

0.0

10

c2

03

11

86

74

0.2

22

1.8

E-0

50

.12

0.0

47

98

αα

Page 119: Copyright by Brook Colleen Daun Riley 2004

Ta

ble

2-4

, co

ntin

ue

d

gra

in #

eff

ec

tive

do

se

fa

cto

r

(%)

err

or

(1 S

D;

%)

eff

ec

tive

do

se

(-d

ec

ay e

ve

nts

/mg

(*1

016))

err

or

(1 S

D;

* 1

016 /

mg

)

tota

l p

os

sib

le d

os

e

(-d

ec

ay e

ve

nts

/mg

(*1

016))

err

or

(1 S

D;

* 1

016 /

mg

)

ho

ne

y

h2

18

97

2.4

0.0

22

1.5

E-0

50

.33

0.1

2

h2

22

11

23

.60

.02

61

.3E

-05

0.2

30

.07

1

h2

24

91

44

.10

.02

21

.6E

-05

0.1

60

.04

6

h1

48

21

64

.70

.02

41

.7E

-05

0.1

50

.04

5

h2

51

11

76

.20

.04

01

.3E

-05

0.2

40

.09

2

h2

09

51

74

.40

.02

21

.3E

-05

0.1

30

.03

3

h2

11

91

83

.30

.02

21

.8E

-05

0.1

30

.02

4

h2

29

21

93

.80

.02

21

.1E

-05

0.1

10

.02

2

h2

37

42

26

.10

.01

62

.0E

-05

0.0

76

0.0

21

h1

30

02

44

.70

.02

51

.6E

-05

0.1

00

.02

0

h1

22

42

44

.20

.02

31

.5E

-05

0.1

00

.01

7

h1

10

92

59

.50

.02

21

.9E

-05

0.0

88

0.0

33

h2

35

82

54

.90

.03

21

.3E

-05

0.1

30

.02

4

h2

24

02

65

.30

.02

51

.8E

-05

0.1

00

.02

0

h2

27

63

35

.60

.01

81

.4E

-05

0.0

54

0.0

09

3

h2

39

03

35

.20

.02

51

.3E

-05

0.0

75

0.0

12

h2

03

13

98

.00

.03

01

.4E

-05

0.0

76

0.0

16

h2

24

84

58

.10

.02

31

.6E

-05

0.0

50

0.0

09

0

h1

10

17

42

10

.03

72

.1E

-05

0.0

51

0.0

14

h1

18

08

01

40

.03

21

.4E

-05

0.0

40

0.0

07

2

No

tes:

Eff

ective

do

se

fa

cto

r is

th

e r

atio

of

the

accu

mu

late

d d

ose

to

th

e t

ota

l d

ose

po

ssib

le (

giv

en

cry

sta

lliz

atio

n a

ge

an

d e

U),

mu

ltip

lie

d b

y 1

00

; i.e

. p

erc

en

t d

am

ag

e s

tore

d.

Eff

ective

do

se

is b

ase

d o

n R

am

an

FW

HM

da

ta a

nd

co

mp

ari

so

n w

ith

th

e c

om

ple

te s

tora

ge

lin

e o

f N

asd

ala

an

d o

the

rs (

20

01

).

99

αα

Page 120: Copyright by Brook Colleen Daun Riley 2004

100

The current distribution of damage levels, wherein we see little change in

bandwidths/crystallinity within a population, may reflect homogenization and annealing of α-

damage during Paleogene heating. The current level of damage, reflected in the FWHM Raman

parameter, is probably not the result of bandwidths within a color population all being the same

prior to Paleogene heating: it is unlikely simply given the variation of both Pb-Pb and FT ages

that grains within a color population have very similar thermal histories. Given that more

damaged crystals anneal preferentially (Nasdala and others, 2001), a larger percent of the

damage in the high-damage grains would have been annealed by Paleogene heating. Thus the

older/high eU grains would have reduced FWHM values (i.e. better crystalline), and this event

would have had a lesser effect on grains with less prior α-damage, because these grains had

little damage to begin with (Figure 2-10a).

One can relate accumulated α-damage (given the current crystallinity) to the total

possible α-damage given crystallization age in terms of a percent α-damage stored; this is

termed the effective dose factor (refer to Appendix 3). Comparing the effective dose factor with

eU concentration (Figure 2-10b) shows that the pink/purple zircon fraction has relatively low eU

and relatively low effective dose factor when compared with the honey and colorless zircons,

which lie in a somewhat larger range in both fields. The general trend for zircons from this

sample is that as eU increases, effective dose factor increases, despite having been partially

annealed in the Paleogene.

The effective dose factor may also be compared to the FT ages (Figure 2-10c). This

plot reinforces the observation that the pink/purple grains store a somewhat smaller percentage

of their total possible α-damage than colorless and honey zircons. As well, colorless and honey

grains have a much higher degree of variability in how much damage is stored versus the

Page 121: Copyright by Brook Colleen Daun Riley 2004

101

pink/purple fraction. This would lead to variability in preservation of pre-heating fission-track

ages within populations useful for provenance information. In other words, a honey or colorless

grain may not be suspected as having a reset FT age, but the age may indeed be reset because

significant damage was stored in the zircon prior to the annealing event. Other grain parameters

such as eU and crystallization age will help to identify these potentially reset zircon FT age as

well, but unless thermal history is constrained, this may still pose a problem in determining

partially reset grains.

The accumulated α-damage dose may also be compared with eU concentration (Figure

2-10d). In this case, all populations show a steep positive slope, where increased eU correlates

with slightly increased effective α-damage doses. The slope of the pink/purple fraction is

somewhat shallower than that of the other populations, indicating that with increasing eU for

pink/purple grains, a greater amount of α-damage is retained as compared with the other

populations.

A comparison of effective dose and FT age shows that effective doses are higher for the

pink/purple fraction than for the honey or colorless fractions (Figure 2-10e). The pink/purple

grains have a vague negative correlation between effective dose and FTGA: at increased

effective doses, fission-track ages are younger (to be expected). However, the same is not

obvious in the honey and colorless fractions; if anything there is a very low-slope positive

correlation, where higher doses are correlated with higher FTGA.

FT Ages versus Minimum Damage Storage Ages

Useful observations are also found in comparing effective doses to doses calculated

using the FT ages (Figure 11a). In Figure 11a, the effective dose given accumulation of α-

Page 122: Copyright by Brook Colleen Daun Riley 2004

effective dose comparison

0.000

0.010

0.020

0.030

0.040

0.050

0.060

0.070

0.080

0.000 0.010 0.020 0.030 0.040 0.050 0.060 0.070 0.080

effective dose given FTGA ( -decay events /mg *1016

)

eff

ec

tiv

e d

os

e g

ive

n m

inim

um

da

ma

ge

sto

rag

e a

ge

(-d

ec

ay

ev

en

ts /

mg

*1

016)

pink/purple (N = 14 grains)colorless (N = 22 grains)honey (N = 20 grains)1:1 lineLinear (1:1 line)

FTGA compared to minimum damage storage age

0

100

200

300

400

500

600

700

800

900

0 100 200 300 400 500 600 700 800 900

FTGA (Ma)

min

imu

m d

am

ag

e s

tora

ge

ag

e (

Ma

)

pink/purple (N = 14 grains)colorless (N = 22 grains)honey (N = 20 grains)1:1 lineLinear (1:1 line)

Figure 2-11a. Comparison of effective doses using those calculated from the fission-track ages,

a.

b.

and those calculated based on present crystallinities (from Raman

microprobe data, FWHM). Uncertainties shown are one standard deviation.

Figure 2-11b. Comparison of minimum damage storage ages (based on Raman microprobe

data, FWHM) with fission-track ages. Uncertainties shown on FTGA are

95% confidence intervals.

102

α

α

Page 123: Copyright by Brook Colleen Daun Riley 2004

103

damage since cooling through the FT closure temperature is compared to the actual measured

dose for each zircon. The actual effective dose (same parameter as that in Figures 10d, 10e)

utilizes the present crystallinity of the grain (in terms of measured FWHM), and provides a

minimum age for α-damage accumulation based on the present level of damage. Figure 2-11b

compares the FT age with the minimum damage storage age for each zircon.

Most grains have accumulated more α-damage than they should have if accumulation

only started since FT closure (Figure 2-11a). Therefore given the amount of α-damage the

grains currently store, more time is required than since FT closure. The fact that the minimum

damage storage ages are older than FT ages for most grains indicates that some α-damage is

more stable during thermal annealing than fission damage, as suggested by Nasdala and others

(2001). If this were not the case, both the FT age and the minimum damage storage age should

be nearly identical in all cases (Figure 2-11). Grains with minimum damage storage age similar

to FT age suggests that all types of α-damage was annealed at the same time as FT resetting.

Clearly, given the distributions shown in Figure 2-11, Paleogene annealing did not anneal all of

the α-damage, but did reset the FT ages of certain grains.

Some colorless and honey-colored grains have slightly less α-damage than would be

expected considering their FT age. There are several possibilities for such behavior. (1)

Minimum damage storage ages shown in Figure 2-11b are minimum storage ages, because they

are based on an assumed simple thermal history (i.e. one in which α-damage in the zircon is not

partially annealed multiple times). If these ages are actually older, which is likely because the

grains may not have had a simple thermal history, then these older damage storage ages would

pull the points up on the y-axis. However, this does not change the relationship of those grains

which plot below the 1:1 line on Figure 2-11a: doses given the FT age are still relatively higher

Page 124: Copyright by Brook Colleen Daun Riley 2004

104

with respect to doses given the minimum damage storage ages, and points on the age

comparison plot will remain below the 1:1 line. (2) One conclusion from the finding that α-

damage ages are older than FT ages is that some types of α-damage might be resistant to

annealing compared with fission damage, and the closure temperatures for damage preservation

might overlap more directly with closure temperatures for fission damage (one possible situation

presented by Rahn and others, in press). In this case, the α-damage might be dominantly point

defects, which may remain stable to higher temperatures than more damaged areas created by

α-recoil (Nasdala and others, 2001). This latter scenario may be reflected in the behavior of

those grains which fall near the 1:1 line on either the effective dose or age comparisons (Figure

2-11).

It is likely that eU (in combination with sufficient retention time for α-damage) may be a

critical factor in determining the behavior of a zircon during heating to ~250°C or so: the higher

eU values indicate zircons with a propensity to have α-damage annealed under the same

conditions as FT damage. The higher eU values of zircons that have less α-damage than would

be expected given their FT ages (Figure 2-11) may help to set up a situation wherein either or

both of the following may have happened: (1) in the source area, at approximately 100 Ma

(based on both the FT ages and the minimum damage storage ages of those zircons that fall

below the 1:1 lines on Figure 2-11), rocks containing these zircons were heated to >400°C and

both fission damage and α-damage were completely annealed; (2) all of these grains

accumulated significant α-damage prior to heating at ~100 Ma, allowing resetting of both their

FT ages and minimum damage storage ages during the ~100 Ma thermal event without bringing

the rocks up to full annealing temperatures. The exception to this is a colorless zircon, that has

a lower eU value (235 ppm; Table 2-2), but older Pb-Pb, FT, and minimum damage storage

ages than those zircons which also plot below the 1:1 lines on Figure 2-11. The older Pb-Pb age

Page 125: Copyright by Brook Colleen Daun Riley 2004

105

for this colorless zircon likely enables it to behave similarly to other honey and colorless zircons

that plot below the 1:1 relationships in Figure 2-11, but that have higher eU values.

It is also important to note that those grains that have minimum damage storage age ≈

FT age (1:1 line) are honey and colorless zircons (Figure 2-11), and that pink/purple grains

retain significant α-damage. For pink/purple zircons, the minimum damage storage ages are

greater than the FT ages, and doses are greater than those expected given only the FT age.

This observation indicates that the pink/purple grains probably had more damage going into the

~100 Ma annealing event, and thus exit the heating event with greater damage.

Consider the following scenario, by analogy with the present distribution of damage in

the different color populations (Figure 2-7). If, given a simple thermal history, the pink/purple

suite has more damage than honey and colorless zircons prior to a ~100 Ma annealing event in

the source area, then some damage could carry through this thermal annealing. On the other

hand, if the damage level of the pink/purple suite prior to the ~100 Ma event is equal to that of

the honey and colorless grains, then some other factor about the pink/purple grains would allow

some of that damage to carry through the thermal annealing. If the damage level of the honey

and colorless suites is much greater than that for the pink/purple zircons going into the ~100 Ma

event, then this is unexpected, and there is some other controlling factor.

Given the situation discussed above, and the following parameters, damage values for

pink/purple zircons are ~2.5 times that of the honey and colorless zircons going into a ~100 Ma

event, given simple thermal histories for both pink/purple and honey and colorless zircons, and

the following typical single-grain parameters:

Page 126: Copyright by Brook Colleen Daun Riley 2004

106

pink/purple zircons honey and colorless zircons

Pb-Pb age = 1685 Ma Pb-Pb age = 480 Ma

eU = 600 ppm eU = 850 ppm

dose prior to 100 Ma = dose prior to 100 Ma =

0.27 *1016 α-decay events/mg 0.10 *1016 α-decay events/mg

The ages and eU values are averages for all grains from a color population, and honey

and colorless zircons were treated as one population. Th was taken to be 0.5U (Garver and

Kamp, 2002). According to these calculations, it is likely that at least some pink/purple zircons

entered the ~100 Ma thermal annealing with greater α-damage than most honey and colorless

zircons, thus allowing them to: (1) exit the thermal event with greater damage; and (2)

experience preferential annealing as a result of their increased α-damage level. Clearly, the

same analogy may be drawn for damage states prior to the ~60 Ma thermal event that all zircons

experienced.

Most of the honey and colorless grains have similar FT age and minimum damage

storage age (Figure 2-11b), and the remaining zircons have an excess of α-damage in relation to

the FT age. For the honey and colorless grains whose minimum damage storage ages and

FTGA are similar, thermal histories are likely relatively simple. There are two likely histories for

such zircons: (1) these grains were originally derived from rapidly-cooled volcanic rocks that

remained at sub-annealing temperatures until re-heating (annealing); (2) older grains (older Pb-

Pb ages; Table 2-2), might have been completely annealed at some point during their thermal

history, and following annealing remained at cool temperatures until the final thermal

perturbation. Either scenario would produce thermally concordant grains (similar ages for

accumulation of α-damage and fission damage). For those grains whose minimum α-damage

storage ages are much older than the FT ages (i.e. the pink-purple series), a more complicated

Page 127: Copyright by Brook Colleen Daun Riley 2004

107

thermal history is likely. Pink/purple grains may have been heated and cooled during multiple

episodes since crystallization, and have older minimum storage ages than honey and colorless

grains.

The Raman microprobe data thus reveal certain critical details in the interpretation of the

FT and Pb-Pb age data for the color fractions. First, most zircons are not greatly damaged at

present, presumably due to Paleogene annealing, although most still retain sufficient differences

to distinguish color populations: (a) the pink/purple series retains more α-damage than the

honey and colorless series zircons; (b) several high eU and/or older honey-colored zircons also

have reset FT ages. All other assumptions being equal, these observations mean that damaged

pink/purple and honey-colored zircons had more α-damage going into the heating event, and

apparently were the most likely to have reset FT ages. This conclusion is borne out in the FT

data, wherein we see that the youngest FT ages, and the largest total percent of a population,

are from the pink/purple and honey fractions (Figure 2-3). Effective U appears to be an

important indicator of grains susceptible to thermal annealing: grains with high eU and

Proterozoic crystallization ages tend to be reset, whereas low eU grains with similarly older

crystallization ages retain older cooling ages for the source rocks. In general the reset grains,

particularly the pink/purple suite, retain the highest amounts, but the smallest percentage of the

total α-damage possible; nominal storage for pink/purple series grains is approximately 20%.

This resetting trend is likely indicative of preferential annealing of more damaged areas or more

damaged grains.

Thus far, it has been shown that in terms of FTGA, crystallization age, FWHM/Raman

band shift, and eU, the distributions of honey and colorless grains overlap. This finding suggests

that these populations behaved in a similar fashion, given the thermal and physical conditions

Page 128: Copyright by Brook Colleen Daun Riley 2004

108

particular to this sample. Accordingly, for this particular distribution, honey and colorless grains

may be treated as essentially one thermal population. Further work remains to be done to

determine the applicability of this for other data sets. Additionally, as suggested by Gastil and

others (1967), there may be specific chemical distinctions, and it is unknown what influence

chemical variation may exert on thermal behavior, if any. The results of REE analysis for zircons

from Station 23 follow in an attempt to address this issue.

REE Data

Based on suggestions of color generation related to REE chemistry (Fielding, 1970;

Gaudette and others, 1983), these FT-dated grains were also analyzed for heavy and light REE

using LA-ICP-MS, with the same spot location as the Pb, U, and Th analyses. REE

concentration data for unknowns and standards appears in Table 2-5. Estimations of error for

light REE (LREE) and heavy REE (HREE) concentrations, based on sequential measurements

of the standard zircon (UT-01), are also noted. As expected for zircons, the HREE content is

higher than the LREE in all color populations (e.g. Fielding, 1970; Gromet and Silver, 1983;

Hinton and Upton, 1991; Hoskin and Ireland, 2000). Most of the LREE are at concentrations just

above the detection limit (~0.1 ppm) in most grains, with some notable exceptions in the

pink/purple fraction. Values for every REE for the pink/purple fraction are somewhat lower but

generally overlapping with the colorless and honey fractions. No correlation of color to REE

composition was detected.

REE concentrations from unknowns in this study were normalized and compared to the

well-studied Elie Ness zircons (ENZ) from Scotland (Hinton and Upton, 1991). The REE in the

majority of unknowns do not deviate greatly from ENZ (Figure 2-12). There is a greater spread

Page 129: Copyright by Brook Colleen Daun Riley 2004

Tab

le 2

-5.

Rare

eart

h e

lem

ent

concentr

ation d

ata

(ppm

) fo

r colo

r fr

action z

ircons f

rom

Sta

tion 2

3,

Huachuca M

ounta

ins.

gra

in #

La

Ce

Nd

Sm

Eu

Gd

Tb

Dy

Ho

Er

Tm

Yb

Lu

pin

k/p

urp

le

d0

05

33

11

07

75

78

36

77

85

36

14

63

32

33

45

d0

12

11

90

20

13

45

52

81

28

33

26

55

3

d0

13

12

80

21

14

44

92

21

03

25

17

74

0

d0

70

11

21

21

41

81

46

76

32

76

74

82

12

4

d1

27

11

00

20

13

13

31

23

35

10

d1

31

18

01

11

94

78

37

16

84

22

95

66

d1

44

11

90

10

94

44

21

10

42

72

24

50

d1

61

19

46

56

62

28

63

72

94

48

25

33

61

27

51

09

66

57

16

5

d1

65

11

40

10

11

45

22

41

13

26

19

24

8

d1

95

11

60

11

12

44

72

21

00

27

20

74

3

L0

49

15

02

01

95

65

29

12

42

81

96

46

L0

62

21

39

22

32

15

71

33

14

33

22

31

56

L3

04

04

02

01

85

73

32

13

93

63

00

46

L3

30

21

01

26

56

91

54

69

29

77

15

39

83

co

lorl

ess

c1

08

24

74

12

22

96

10

75

32

42

68

62

98

7

c1

11

00

90

22

32

71

14

54

23

85

75

04

74

c1

21

60

24

12

25

91

01

92

97

43

31

03

81

31

41

c1

22

30

28

02

22

66

95

46

21

45

65

00

77

c1

29

11

40

21

18

45

82

51

07

24

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93

5

c1

30

01

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11

44

31

88

52

42

00

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c1

37

63

25

12

12

66

92

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23

65

94

51

10

0

c1

43

71

22

12

13

36

95

48

22

55

33

65

81

c1

59

87

51

22

12

05

71

38

17

33

93

18

75

c1

72

80

18

01

11

24

54

27

14

03

73

28

93

c1

77

23

23

12

11

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70

36

21

35

34

11

11

4

c2

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11

19

01

11

65

70

30

15

83

93

60

89

c2

04

41

18

02

12

15

80

40

18

94

13

11

68

c2

06

41

32

01

11

55

71

36

18

14

23

45

86

c2

06

51

17

02

11

44

63

34

17

84

43

46

86

c2

22

21

19

01

11

34

58

29

15

04

03

36

84

c2

25

00

24

01

01

14

47

25

12

43

12

69

56

c2

28

57

46

23

10

58

91

87

96

43

81

11

94

11

61

c2

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47

02

12

25

81

39

19

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03

97

71

c2

52

81

24

02

22

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51

25

96

85

54

12

4

c2

54

40

90

21

32

71

12

55

24

65

94

62

93

c2

69

51

14

02

12

46

90

47

21

74

73

34

91

109

Page 130: Copyright by Brook Colleen Daun Riley 2004

Ta

ble

2-5

, co

ntin

ue

d

gra

in #

La

Ce

Nd

Sm

Eu

Gd

Tb

Dy

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10

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63

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77

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02

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11

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13

2

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110

Page 131: Copyright by Brook Colleen Daun Riley 2004

REE variation

Station 23 color fraction zircon

0.01

0.10

1.00

10.00

100.00

1000.00

10000.00

100000.00

56 57 58 59 60 61 62 63 64 65 66 67 68 69 70 71 72

EN

Z-n

orm

ali

ze

d v

alu

e

Figure 2-12. Normalized rare-earth-element data for color fraction zircons from Station 23,

La Ce Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu

pink/purple (N = 14 grains)

colorless (N = 22 grains)honey (N = 21 grains)

Huachuca Mountains. Elie Ness zircon (ENZ) average, to which unknowns

are normalized, is the result of the average of seven analyses reported for

the ENZ megacryst by Hinton and Upton (1991).

111

Page 132: Copyright by Brook Colleen Daun Riley 2004

112

of normalized values in the pink/purple series than for the colorless or honey grains, and a few

pink/purple grains plot with abundances of 10-10,000 times that of the ENZ for the LREE. More

importantly, with the exception of some zircons from the pink/purple series, there is little

deviation in relative abundances among the different color fractions. As such, the difference

among these groups, in particular the colorless and honey grains, appears to be unrelated to

rare earth element chemistry, at least in these zircons. This finding is in contrast to the work of

Fielding (1970), and Gaudette and others (1981); both studies linked the development of color to

crystal chemistry, specifically that of U and certain REE.

Fielding (1970) investigated color zonation in serial sections of a Late Permian

pink/purple zircon from a pegmatite in the New England batholith. This work concluded that

bands of red color are correlated with areas with lower in Fe, Al, Mn, and Pr, and that the

reduction of Nb+5 to Nb+4 in combination with a structural defect capable of providing electrons

for this reduction aids in forming color centers. Fielding (1970) also noted an enrichment in

HREE over LREE (as expected for zircon, particularly that derived from a pegmatite), and higher

concentrations of Er in color bands. Gaudette and others (1981) presented evidence for the

relationship between Eu concentrations and brown color in detrital zircons from the Potsdam

Formation (New York State): ion microprobe data from 21 zircons indicates a positive Eu

anomaly in brown grains, whereas there is no Eu anomaly for colorless grains.

These studies unfortunately do not focus on zircons from a wide variety of sources, and

sampled grains are probably not numerous enough to make broad generalizations about the

control exerted by trace-element chemistry on color formation. Similar problems with not

capturing the full range of zircon types are no doubt encountered in the present study. It is likely

that there is a combination of chemical factors that contribute to color development in zircons.

Page 133: Copyright by Brook Colleen Daun Riley 2004

113

For example, Krogh and Davis (1974) suggest that alteration of metamict zircon allows

enrichment in water, as well as Fe, Al, and Ca oxides. These impurities, in combination with

REE or other chemical variations and/or accumulation of radiation damage, may contribute to

color generation. As pointed out by Fielding (1970), there are also crystallographic

considerations; his work demonstrated that there is a tendency to isolate impurities and defects

along the (111) plane of zircon in the samples examined, and that colorless sections are typically

parallel to (110). Much work remains to be done on a full suite of genetically and temporally

distinct igneous zircons, including major- and minor-element chemistry and Raman microscopy,

to better determine the various contributing factors and their relative importance.

DISCUSSION

FT Age Data

In both the p and h fractions, zircons with FT ages between 60 and 70 Ma are present,

and the youngest peaks for these two fractions overlap at two sigma (63 Ma and 70 Ma; Table 2-

3). Significant variability of single-grain ages exists within the p fraction, as demonstrated by

peaks at 63 Ma and 175 Ma, the latter of which is a composite of ~150 Ma grains and several

older grain ages (Figure 2-3). This variability is probably related to the presence of grains with

different thermal histories in the same fraction. Differing thermal histories are likely, as zircons

have different Pb-Pb ages and variability in short-range lattice order within individual color

fractions (based on Raman microscopy data; Tables 2 and 4). Considering that there are young

reset grains from all the color populations, some key observations bear re-emphasis:

(1) All pink/purple zircons have Early and Middle Proterozoic crystallization ages,

whereas the majority of the colorless and honey young reset zircons have Ordovician-

Early Jurassic crystallization ages.

Page 134: Copyright by Brook Colleen Daun Riley 2004

114

(2) All young FT-reset grains have elevated eU values, suggesting that only those

grains with α-damage prior to Paleogene annealing were reset.

(2) There is only one young reset colorless grain (c2_031; Table 2-2), which suggests

that this population will generally reflect provenance characteristics rather than being

reset, as in the case of high-damage colored zircons.

(3) All of the honey and colorless young reset zircons have relatively small FWHM (3.5-

4.6 cm-1), versus the pink/purple, which have FWHM two or more times greater (8.6-11.8

cm-1). This finding indicates that the pink/purple zircons retained greater amounts of α-

damage after Paleogene heating.

Cumulative probability density curves for each of the three color fractions (Figure 2-3)

show that peaks are similar to the bulk sample, indicating that color does not relate in a simple

fashion to either fission-track age or α-damage level. This observation suggests that there is a

complex interaction between radiation damage of the crystal lattice and thermal annealing of

zircons.

Both the colorless and honey fractions have peak ages between 75 and 120 Ma,

comprising the entire c fraction, and nearly half of the grains in the h fraction (Figure 2-3; Table

2-3). These are reasonable provenance ages for multi-cycle sediments that were shed into this

basin. This observation suggests that FT ages of colorless and honey zircons are most useful in

understanding provenance of the sediments.

Raman Crystallinity Data

Effective U, retention time (time since complete α-damage annealing), and thermal

history are the determining factors in how radiation-damaged a grain is at present, as measured

Page 135: Copyright by Brook Colleen Daun Riley 2004

115

by Raman bandwidth. Crystallization age is also important in grains with rapid cooling to <200°C

and simple thermal histories, in which case the retention time may approximate the

crystallization age. Possible end members and intermediate scenarios are shown in Figure 2-

13; these scenarios are developed for zircons with simple thermal histories. In cases where

zircons have higher levels of α-damage (i.e. long retention times and/or high eU concentrations),

the potential for preferentially resetting fission-track ages at temperatures of 150°C-250°C

increases (as shown by increasingly darker shading of rectangles in Figure 2-13. However,

given younger retention ages and/or lower eU values, accumulated α-damage decreases,

thereby allowing higher retentivities in the fission-track system.

Relatively old crystallization ages, combined with lower eU values, allow certain

colorless and honey zircons to behave similarly to pink/purple grains in FWHM-eU space (i.e.

these old colorless/honey grains display a positive correlation between increasing eU and

decreasing crystallinity similar to the pink/purple grains; in contrast, other zircons from these two

populations show no decrease in crystallinity with increasing eU). Despite the fact that eU

concentrations are lower for pink/purple fraction zircons, these grains are more damaged. This

behavior may be attributable to an overall longer time since crystallization for the pink/purple

zircons, allowing for significant accumulation of α-damage prior to the onset of Laramide

magmatism. The fact that even very high eU grains in the honey and colorless suite do not have

wide Raman bandwidths may indicate that these grains were highly damaged in micro-areas

which were preferentially annealed during Paleogene heating.

The colorless and honey grains have a narrower distribution of bandwidths as compared

with the pink/purple zircons (Figure 2-7, Figure 2-8). Such behavior may indicate: (a) shorter,

less complicated thermal histories in grains with overall younger crystallization ages; or (b)

Page 136: Copyright by Brook Colleen Daun Riley 2004

116

homogenization of the bandwidths of these populations during the Paleogene heating event.

The more crystalline nature of the honey and colorless populations may reflect both processes.

It is likely that prior to heating (60 Ma), the pink/purple grains had higher but variable

preserved α-damage levels, compared to the other populations. Heating anneals α-damage,

with the final product being a zero-damage zircon. Given enough time and sufficiently high

temperatures (temperatures greater than perhaps 400°C), all grains would be homogenized into

zero-damage zircons. This temperature estimate is based on the concept of the color-removal

zone and its thermal bounds, proposed by Garver and Kamp (2002). These authors suggested

that zircons derived from the reset FT color zone and from the reset FT colorless zone have

synorogenic cooling ages, experienced peak temperatures of 250-400°C, and approximately

80% of grains are colorless as a result of thermal annealing. Accordingly, above about 400°C,

color should be almost completely removed from most grains, at which point the majority of the

α-damage may also have been annealed.

Overlapping Behavior: Honey vs. Colorless Zircons

The differences in color between honey and colorless zircons in the Station 23 sample

cannot be attributed to differences in FT age, crystallization age, crystallinity, or REE

geochemistry. It is possible that there is variation in other major- or minor-element chemistry

that may affect color, and/or there may be inter-sample variation in the factors which contribute

to the development of honey color in zircons. This overlapping behavior presents the

opportunity for further study to understand the differences between the colorless and honey

series, and to define the factors which contribute to development of honey color. A well-selected

suite of igneous zircons from multiple genetic and temporal contexts would provide the best

means of understanding the generation of honey color. Zircons from an igneous series with

Page 137: Copyright by Brook Colleen Daun Riley 2004

117

independently known and relatively simple thermal histories would provide the best starting point

for such a study. The basis of the data set would be FT ages for color-separated zircons. Other

desirable data include REE, Fe, Al, Ca, and Mn concentrations to thoroughly define the

geochemical variations among colorless and honey colored zircons. To define the α-damage

contribution to both color development and FT system behavior, Pb-Pb ages and Th and U

values, and short- and long-range lattice order measurements (via Raman microscopy and X-ray

diffraction, respectively) should be collected for color-separated grains.

Activation Energy for Damage Annealing

Clearly there is a decreased activation energy associated with annealing more damaged

zircon than annealing less damaged zircon: more α-damaged zircons have been preferentially

reset (Nasdala and others, 2001). The precise genesis of this phenomenon is unclear.

Activation energy for annealing damage probably varies as a complicated relationship between

eU and retention time. Decreased activation energy for annealing fission tracks in a highly α-

damaged grain probably relates to the relative ease of moving ions in a damaged lattice rather

than in a perfect crystalline lattice. In the case of a highly damaged crystal lattice, the material is

more glass-like (i.e. little structural order, and thus easier to rearrange weakly-bonded material).

In the case of a crystalline zircon, strongly bonded ions are ordered within the lattice structure.

The activation energy required to move ions back into place in the former situation is likely

decreased by the presence of weaker bonds in a more poorly ordered lattice. It is concluded

that each grain, depending on the eU, retention time, and thermal history, can have a different

activation energy for the annealing of either fission tracks or α-damage.

Page 138: Copyright by Brook Colleen Daun Riley 2004

118

Criteria for Recognizing Reset Grains

From the age and crystallinity data presented above, it seems clear that the

relationships among thermal history, zircon color, and radiation damage are not straightforward.

For some time, it has been recognized that accumulation of α-damage is a function of eU,

retention time, and thermal history. Additionally, studies have linked the development of color to

accumulated α-damage since FT closure temperature (Garver and Kamp, 2002). At this point,

the occurrence of the FT-reset grains and their characteristics must be considered in this

context. Can one predict which grains will be reset by a low-temperature thermal event?

Given any eU concentration, a zircon at temperatures less than about 300°C-350°C

becomes increasingly α-damaged with time, and crystal lattices become increasingly disordered

(Figure 2-13). α-damage is complex, and it is clear that at low temperatures (150°C-250°C)

some fraction of the damage is repaired, but some remains and this latter fraction requires much

higher energies to anneal (i.e. color appears to anneal at 350°C-400°C; Garver and Kamp 2002).

α-damage causes disorder, which facilitates the annealing of fission tracks. All other things

being equal, a high-damage grain should have a lower closure temperature than a low-damage

grains (Kasuya and Naeser, 1988). Therefore, one would like to know, in a predictive sense,

which grains in a variably damaged population would be annealed if the strata were subjected to

low-temperature heating (150°C-250°C). Is it only total α-damage or is there some other basic

crystal property that determines track retention?

Because of uncertainties associated with variable thermal histories and levels of

accumulated radiation damage prior to the most recent heating for grains within a single color

population, total dose value alone cannot be used to distinguish grains that are potentially reset,

but it is probably of first-order importance. Provided with crystallinity measurements and U and

Page 139: Copyright by Brook Colleen Daun Riley 2004

time

alp

ha

da

ma

ge

metamict

retention age;

Pb-Pb age

500 Ma 1000 Ma250 Ma 1500 Ma 2000 Ma

low eU <250 ppm

moderate eU 250-400

high eU 400-900 ppm

very high eU

>900 ppm

Figure 2-13. Qualitative relationship between time, alpha-damage, and effective uranium (eU)

best range to

preserve time since

cooling to <250°C

(provenance ages)

most likely to be

reset by post-

depositional low-T

events

concentration. Note that as eU increases, and/or retention time increases,

the propensity to develop damage to the point where fission tracks are

preferentially annealed in more damaged grains also rises (shown by

increasingly darker shaded rectangles). Note that these scenarios represent

the simplest cases, where zircons are not appreciably re-heated following

cooling to less than ~180°C at the retention age, which may or may not be

the same as the crystallization age.

119

Page 140: Copyright by Brook Colleen Daun Riley 2004

120

Th concentrations, accumulated α-damage and the percent damage stored (effective dose

factor) may prove an effective means of establishing the potential for reset. Effective U content

alone is insufficient to determine potential for reset: if a zircon has a short retention time (i.e.

young crystallization age, and/or time since complete α-damage annealing), there remains

insufficient time to develop radiation damage even if the grain has high eU and is not annealed

subsequently. Zircon color alone is similarly problematic. Many of the young reset zircons are

pink/purple, but a number also come from the honey suite, and there is one reset colorless grain.

By the same logic, a number of the lower eU pink/purple, honey, and colorless zircons retain

provenance ages. As such one color population may comprise multiple thermal populations

because there is the possibility, if not likelihood, of sampling zircon with a diversity of low-

temperature thermal histories in a single sandstone.

In the data presented in this part of the study, several points are critical:

(1) Reset FT ages occur in specific grains with higher eU values and/or older

crystallization ages.

(2) Despite FT annealing and resetting of FT ages in certain zircons, some α-damage

remains in certain grains following an annealing event with widespread elevated

temperatures on the order of 200°C.

(3) Grains with older crystallization ages retain significant α-damage at the present,

despite the fact that they have been heated and cooled at least once.

(4) Honey color in zircons in this data set appears to be unrelated to α-damage, and

unrelated to REE content.

(5) Pink and purple color in zircons correlates to old crystallization age and elevated α-

damage levels, and is unrelated to REE content.

Page 141: Copyright by Brook Colleen Daun Riley 2004

121

Conclusions that can be drawn from these points are: (1) grains in the pink/purple color series

have the greatest possibility of having old crystallization ages and/or high α-damage; and (2)

non-pink/purple grains which have high eU and long retention times should also be suspect.

Clearly, single-grain thermal history and the amount of accumulated radiation damage attained

prior to an annealing event are the controlling factors in grain response to heating. Because

thermal histories vary among grains within a detrital suite, eU concentrations and retention times

provide a means of quantifying the present level of α-damage, and in identifying potentially reset

grains.

Additionally, there might also be a threshold for grains in terms of their current damage

levels, wherein one might suspect that these grains were very highly damaged prior to partial

annealing. Grains coming out of the most recent heating event with higher damage levels likely

went in with higher levels, and all other things being equal, are the grains most likely to have

been reset. This point does not mean that a highly damaged zircon will come out of the heating

event completely undamaged; it simply means that the more damaged micro-areas will have

been preferentially annealed. Based on data presented herein, one might consider a possible

value of FWHM of 8 cm-1 as indicative of a grain that entered a heating event with significant α-

damage, but this is problematic for the following reasons:

(1) The threshold FWHM value selected depends on how much α-damage a grain

accumulated prior to the heating event. One might envision a case of two grains that

emerge from a heating event with equal FWHM, and thus equal crystallinities at present.

However, resulting from different thermal histories, one grain may have contained more

stable point defects, and thus entered the annealing event with similar crystallinity to the

present value. The other zircon might have been highly damaged to begin with, but

because it was much more damaged, it also preferentially annealed more than the other

Page 142: Copyright by Brook Colleen Daun Riley 2004

122

(and because it was more damaged, would have been much more susceptible to the

annealing of fission tracks than the zircon in the first scenario).

(2) All color groups retain some grains with reset FT ages, and the colorless and honey

reset zircons have much lower FWHM than the pink/purple reset grains. Additionally, all

colorless and honey reset grains have FWHM < 8 cm-1.

It may also be helpful to consider maximum paleotemperature as a potential guide for

identifying reset fission-track ages. However, because the amount of resetting depends upon

other factors (eU, retention time), peak temperature should provide only a general guideline in

combination with other single-grain parameters. The simplest end member cases are

represented in Figure 2-14. Partial to full annealing of fission tracks might be expected to occur

in near-amorphous zircon at a temperature of perhaps as low as 180°C (Figure 2-14). Along the

same lines, almost no annealing of fission tracks may occur in fully crystalline zircon even at

temperatures as high as 260°C (Figure 2-14) (Brandon and others, 1998).

In the heated samples, it is clear that grains belonging to the 50-60 Ma peak have been

reset because these ages are younger than the depositional age. However, it is uncertain how

much, if any, damage was annealed in the other older grains. There are several options, but

one possibility is that resetting (FT and α-damage) only occurs above some threshold α-damage

value. This possibility is supported by the fact that older peak ages in samples that lack a young

reset peak are similar to older peak ages in samples that have a young reset peak (Chapter 1).

As such, in multi-component FT data sets, the first-order methods of differentiating

thermal populations, and determining which data yield provenance information and which yield

data on post-depositional thermal activity, are as follows:

Page 143: Copyright by Brook Colleen Daun Riley 2004

123

(1) Separate zircons by color, and evaluate FTGA accordingly. This relatively simple

task can provide an efficient means of determining grains which might have been reset

by post-depositional thermal events.

(2) Evaluate etch behavior: grains in which fission tracks etch more rapidly do so

because of higher levels of radiation damage. This relative etching efficiency may be

used as a first-order proxy for damage levels (c.f. Gleadow, 1978).

(3) Evaluate FTGA with respect to model eU. There is a clear indication in data

presented herein that honey and colorless grains with higher eU values may be

preferentially reset, and thus provide constraints on post-depositional thermal activity.

(4) Obtain VR data: this is an efficient and inexpensive way to estimate maximum

paleotemperature.

If additional differentiation becomes necessary, crystallization ages and Th concentrations might

also assist in further defining thermal populations. Additionally, α-damage levels ascertained by

the use of Raman microscopy may provide supplementary data. However, one must recognize

that this is only a proxy for damage prior to the last reheating, and is highly dependent on

thermal history. Such data are most helpful when thermal histories are relatively simple.

CONCLUSIONS

This study provides the first correlation of FT ages, Pb-Pb crystallization ages, α-

damage levels, and trace-element geochemistry for the same detrital zircons with different

histories, but all subjected to a mild Tertiary heating event. Raman microscopy data and the

homogeneity of REE crystal chemistry for these grains provides a means of evaluating the major

contributing factors in the development and annealing of fission damage, α-damage, and the

development of color in zircons. These data provide the following observations and conclusions:

Page 144: Copyright by Brook Colleen Daun Riley 2004

annealing temperature °C

pe

rce

nt

FT

an

ne

alin

g

0

150°

Figure 2-14. Inferred relationship between annealing of fission tracks, annealing temperature,

50

100

235° 260°210°

high

alpha-

damagelow

alpha-

damage

180°0°

moderate

alpha-

damage

and accumulated alpha-damage. As in Figure 2-13, these scenarios

represent the simplest cases, where zircons are not appreciably re-heated

following cooling at the retention age, except during the annealing event.

Note that the relationships between the amount of damage annealed, the

annealing temperature for a grain with a certain level of damage, and the

shape of the curve that describes these relationships, remain to be

constrained by further work on a suite of igneous zircons for which the

124

thermal history is known.

Page 145: Copyright by Brook Colleen Daun Riley 2004

125

(1) Some grains that have young reset fission-track ages retain significant α-damage

despite having experienced the thermal input required for annealing fission tracks.

There is an overlapping range of stability for α-damage and fission damage.

Additionally, there is a higher thermal stability of α-damage relative to fission damage,

which is likely related to the amount and type of α-damage in a crystal (Nasdala and

others, 2001).

(2) Placing these observations in context, this study presents the criteria for determining

the presence of zircons with reset FT ages in multi-component populations. Critical

factors include FT age(s) in the context of known depositional age, color, eU content, as

well as supporting evidence in the form of the FTGA distributions of older rocks in the

section.

(3) Pb-Pb ages, total and effective α-doses, and spot crystallinity measurements

provide a means of more accurately identifying potentially reset grains which might not

otherwise be obvious.

(4) Pink/purple grains are currently more α-damaged than colorless or honey-colored

zircons, with most pink/purple zircons having FWHM > 6 cm-1.

(5) In general, fission-track ages of colorless detrital zircons provide a means of dating

the provenance of sandstones. In many cases, honey-colored grains will also yield

consistent provenance ages. Care must be taken in the selection of grains and in the

interpretation of grain age distributions to avoid high-eU zircons.

(6) More radiation-damaged zircons, such as those from the pink/purple series in the

present study, will be more likely to have been reset via post-depositional thermal

activity with temperatures perhaps as low as 180°C, up to 260°C, and as such provide a

means of dating local or regional cooling following magmatism. Again, care must be

taken to identify grains with relatively high eU contents. General context for the

Page 146: Copyright by Brook Colleen Daun Riley 2004

126

interpretation of either provenance or post-depositional thermal activity is provided

simply and cost-effectively by the addition of vitrinite-reflectance data from interbedded

mudrocks.

(7) Honey and colorless zircons demonstrate overlapping behavior in terms of fission-

track age, Pb-Pb age, eU, crystallinity, and REE geochemistry.

Page 147: Copyright by Brook Colleen Daun Riley 2004

A

pp

en

dix

1—

Ag

e d

ata

fo

r U

pp

er

Cre

tac

eo

us

an

d k

ey p

os

t-U

pp

er

Cre

tac

eo

us

ig

ne

ou

s r

oc

ks

in

s

ou

the

as

tern

Ari

zo

na

form

ati

on

locati

on

ag

eevid

en

ce

cit

ati

on

Tert

iary

qu

art

z v

ein

sS

anta

Rita M

ounta

ins

Oli

go

cen

e?

youngest

rock s

how

n a

s c

ross-c

ut

by t

hese

Dre

wes (

1971);

Marv

in

vein

s is r

hyolit

ic t

uff

/tu

ffaceous s

andsto

ne

and o

thers

(1973);

Marv

in

unit o

f G

ringo G

ulc

h v

olc

anic

s (

post-

60 M

a);

and o

thers

(1978)

Dre

wes (

1971)

links t

hese r

ocks t

o O

ligocene

Gro

svenor

Hill

s v

olc

anic

s;

dik

e s

warm

in B

ox

Canyon d

ate

d b

y M

arv

in a

nd o

thers

(1973)

at

26.5

Ma ±

1.3

m.y

. (K

-Ar,

sanid

ine),

als

o lik

ely

rela

ted

Tert

iary

rh

yo

lite

Santa

Rita M

ounta

ins

~28 M

a ±

2 m

.y.

K-A

rD

rew

es (

1971)

p

orp

hyry

Helv

eti

a s

tocks

Santa

Rita M

ounta

ins

54.9

Ma ±

1.3

m.y

.K

-Ar

on b

iotite

Dre

wes (

1976);

Marv

in a

nd

54.8

Ma ±

2.0

m.y

.K

-Ar

on b

iotite

oth

ers

(1973);

Marv

in a

nd

53.3

Ma ±

2.0

m.y

.K

-Ar

on b

iotite

oth

ers

(1978)

qu

art

z m

on

zo

nit

eS

anta

Rita M

ounta

ins

55.3

Ma ±

2.0

m.y

.K

-Ar

on b

iotite

Dre

wes (

1972)

s

tock,

Helv

eti

a a

rea

qu

art

z l

ati

te p

orp

hyry

Santa

Rita M

ounta

ins

55.2

Ma ±

2.0

m.y

.K

-Ar

on b

iotite

Marv

in a

nd o

thers

(1973);

p

lug

s E

of

Helv

eti

a57.1

Ma ±

2.1

m.y

.K

-Ar

on b

iotite

Marv

in a

nd o

thers

(1978)

57.6

Ma ±

2.1

m.y

.K

-Ar

on b

iotite

qu

art

z l

ati

te p

orp

yry

Santa

Rita M

ounta

ins

57.1

Ma ±

1.9

m.y

.K

-Ar

on b

iotite

Dre

wes (

1972)

p

lug

, G

reate

rvil

le

a

rea

Gre

ate

rvil

le p

lug

sS

anta

Rita M

ounta

ins

57.2

Ma ±

2.1

m.y

.K

-Ar

on b

iotite

Dre

wes (

1976)

57.8

Ma ±

2.1

m.y

.K

-Ar

on b

iotite

qu

art

z l

ati

te p

orp

hyry

Santa

Rita M

ounta

ins

57.0

Ma ±

2.3

m.y

.K

-Ar

on b

iotite

Marv

in a

nd o

thers

(1973);

n

ear

Gre

ate

rvil

leM

arv

in a

nd o

thers

(1978)

127

Page 148: Copyright by Brook Colleen Daun Riley 2004

Appendix

1,

continued

form

ati

on

locati

on

ag

eevid

en

ce

cit

ati

on

gra

no

dio

rite

an

dP

ata

gonia

Mounta

ins

59 M

a ±

3 m

.y.

K-A

r on b

iotite

Marv

in a

nd o

thers

(1973)

a

sso

cia

ted

qu

art

z59 M

a ±

5 m

.y.

K-A

r on h

orn

ble

nde

m

on

zo

nit

e59 M

a ±

3 m

.y.

K-A

r on b

iotite

Red

Mo

un

tain

co

mp

lex

Pata

gonia

Mounta

ins

62-5

8 M

are

gio

nal re

lationship

sK

eith a

nd S

wan (

1995);

Keith a

nd W

ilt (

1986)

Gri

ng

o G

ulc

h v

olc

an

ics

Santa

Rita M

ounta

ins

61.3

Ma ±

4.3

m.y

.K

-Ar

on h

orn

ble

nde,

dacite p

orp

hyry

Marv

in a

nd o

thers

(1973);

62 M

a ±

3 m

.y.

K-A

r on b

iotite

, m

icro

gra

nodio

rite

Dre

wes (

1976);

Marv

in

and o

thers

(1978)

Gri

ng

o G

ulc

h p

luto

nS

anta

Rita M

ounta

ins

61.9

Ma ±

6.0

m.y

.K

-Ar

on b

iotite

, horn

ble

nde

Dre

wes (

1976);

Marv

in a

nd

c

onsid

ere

d ~

pene-

62.0

Ma ±

6.0

m.y

.K

-Ar

on b

iotite

, horn

ble

nde

oth

ers

(1973)

c

onte

mpora

neous w

ith

G

ringo G

ulc

h v

olc

anic

s,

o

ther

nearb

y r

ocks

(

Dre

wes,

1976)

qu

art

z l

ati

te p

lug

sS

anta

Rita M

ounta

ins

64-6

0 M

aA

r-A

r on b

iotite

, horn

ble

nde

Keith a

nd W

ilt (

1986)

(

Helv

eti

a s

tocks)

qu

art

z l

ati

te p

lug

sS

anta

Rita M

ounta

ins

64-6

0 M

aA

r-A

r on b

iotite

, horn

ble

nde

Keith a

nd W

ilt (

1986)

(

Gri

ng

o G

ulc

h

p

luto

n/v

olc

an

ics)

rocks a

sso

cia

ted

wit

hS

anta

Rita M

ounta

ins

67-6

5 M

ahorn

ble

nde

Keith a

nd W

ilt (

1986)

P

b-Z

n-A

g

d

ep

osit

s T

yn

dall

/

S

ale

ro/I

van

ho

e

m

ines

Jo

sep

hin

e C

an

yo

nS

anta

Rita M

ounta

ins

68.8

Ma ±

7.0

m.y

.K

-Ar

Dre

wes (

1976)

d

iori

te

128

Page 149: Copyright by Brook Colleen Daun Riley 2004

Appendix

1,

continued

form

ati

on

locati

on

ag

eevid

en

ce

cit

ati

on

po

rph

yri

tic

da

cit

e d

ike

SS

anta

Rita M

ounta

ins

69 M

a ±

3 m

.y.

K-A

r on h

orn

ble

nde

Marv

in a

nd o

thers

(1973);

o

f S

ilver

Cave

Dre

wes (

1976);

Marv

in

and o

thers

(1978)

Mad

era

Can

yo

nS

anta

Rita M

ounta

ins

69.6

Ma ±

2.1

m.y

.K

-Ar

Dre

wes (

1976)

g

ran

od

iori

te

Ele

ph

an

t H

ea

d q

ua

rtz

Santa

Rita M

ounta

ins

69.9

Ma ±

3.0

m.y

.K

-Ar

on b

iotite

Dre

wes (

1976)

m

on

zo

nit

e70.8

Ma ±

2.9

m.y

.K

-Ar

on b

iotite

(

Qu

an

trell

sto

ck)

Ele

ph

an

t H

ea

d/Q

ua

ntr

ell

Santa

Rita M

ounta

ins

71-6

8 M

aK

eith a

nd W

ilt (

1986)

s

tocks

Jo

se

ph

ine

Can

yo

nS

anta

Rita M

ounta

ins

70-6

8 M

aA

r-A

r on b

iotite

Keith a

nd W

ilt (

1986)

d

iori

te

vo

lcan

ics o

f Jo

nes

Canelo

Hill

s72 M

aK

-Ar

on b

iotite

Hayes (

1970)

M

esa (

up

per

un

it

w

eld

ed

tu

ff);

u

nderlyin

g

c

onglo

mera

te lik

ely

F

ort

Critt

enden

F

orm

ation

Co

ron

a s

tock

Santa

Rita M

ounta

ins

72-7

1 M

aK

eith a

nd W

ilt (

1986)

Co

ron

a s

tock

Santa

Rita M

ounta

ins

75.5

Ma ±

2.7

m.y

.K

-Ar

on b

iotite

Marv

in a

nd o

thers

(1973);

Marv

in a

nd o

thers

(1978)

qu

art

z d

iori

te E

of

Mt.

Santa

Rita M

ounta

ins

75.3

Ma ±

2.9

m.y

.K

-Ar

on b

iotite

Marv

in a

nd o

thers

(1973);

F

ag

an

Ran

ch

Marv

in a

nd o

thers

(1978)

129

Page 150: Copyright by Brook Colleen Daun Riley 2004

Appendix

1,

continued

form

ati

on

locati

on

ag

eevid

en

ce

cit

ati

on

Sale

ro F

orm

ati

on

Santa

Rita M

ounta

ins

74.0

Ma ±

2.2

m.y

.K

-Ar

on b

iotite

, w

eld

ed t

uff

mem

ber

Dre

wes (

1968);

Inm

an

c

onfo

rmable

ato

p F

ort

(1982)

C

ritt

enden F

orm

ation

in S

anta

Rita M

ounta

ins

(

Hayes a

nd D

rew

es,

1

978)

Sale

ro F

orm

ati

on

Santa

Rita M

ounta

ins

74.3

Ma ±

3.3

m.y

.K

-Ar

on b

iotite

, rh

yodacite w

eld

ed t

uff

Dre

wes (

1968);

Inm

an

(1982)

Sale

ro F

orm

ati

on

Santa

Rita M

ounta

ins

79-7

3 M

aA

r-A

r on b

iotite

, w

eld

ed t

uff

mem

ber

Keith a

nd W

ilt (

1986)

vo

lcan

ics o

f D

ove C

an

yo

nC

anelo

Hill

s73 M

a ±

4 m

.y.

K-A

r on b

iotite

Marv

in a

nd o

thers

(1973);

Marv

in a

nd o

thers

(1978)

trach

yan

desit

e o

fS

W o

f C

anelo

Hill

s73.9

Ma ±

3.0

m.y

.K

-Ar

on b

iotite

Marv

in a

nd o

thers

(1973);

M

ead

ow

Vall

ey

Marv

in a

nd o

thers

(1978)

an

desit

es o

f C

orr

al

Canelo

Hill

s,

W f

lank

75 M

aK

-Ar

on b

iotite

Hayes (

1987)

C

an

yo

n

(

confo

rmably

overlain

b

y F

ort

Critt

enden

F

orm

ation)

Note

s:

For

appro

xim

ate

ages (

desig

nate

d w

ith a

~ b

efo

re t

he c

ited a

ge):

ages a

re a

s c

ited in t

he t

ext

of

refe

renced g

eolo

gic

map;

uncert

ain

ties f

or

these

ages a

re a

ppro

xim

ate

. W

here

no info

rmation o

n t

he isoto

pic

syste

m o

r m

inera

l(s)

date

d w

as p

rovid

ed in t

he o

rigin

al re

fere

nce,

these f

ield

s a

re left

bla

nk.

130

Page 151: Copyright by Brook Colleen Daun Riley 2004

131

Appendix 2—Sample suite field descriptions for fission-track work, Santa Rita and Huachuca Mountains, southeastern Arizona

The following are brief field descriptions for each sample included in this study. Note that compositions were estimated in the field using hand samples, and accordingly may not exactly match point-counted values. abbreviations F = % framework grains Q = % quartz M = % matrix (silt-sized and finer) F = % feldspar C = % cement R = % lithic fragments P = % porosity

Page 152: Copyright by Brook Colleen Daun Riley 2004

132

station #/field sample # field description Station 9/990625-3 —Fort Crittenden Formation sandstone FT sample from Station 9

along Glance Ridge transect, Huachuca Mountains. —geologic map: Hayes and Raup (1968); topographic map: Pyeatt Ranch (3490000 m N, 549000 m E). —sample is a pink-gray (weathered and fresh) medium grained to granule subrounded to rounded sandstone; by hand sample, F75M10C10P5:Q40F20R30; contains significant pseudomatrix and somewhat squashed, but still coherent, mudclasts; some of feldspar may be altered, but difficult to tell in hand sample; at least partially calcite cemented; Fe-oxide common; this sandstone bed is approximately 20 cm thick, bounded by silty mudstones; evidence for low angle trough cross beds, and basal contact scours down into silty mudstone below (approximately 1-2 cm relief on basal scour surface); there are other beds of this type throughout the section exposed in Ferosa Canyon, interbedded with mudstones, siltstones, and very fine sandstones; all have sharp contacts, including upper contacts; sandstone beds generally ~20 cm thick, finer lithologies somewhat thicker, on the order of 30-70 cm thick; moderately indurated. —no strike/dip.

Page 153: Copyright by Brook Colleen Daun Riley 2004

133

Station 11/990626-1 —Glance conglomerate FT sample from Station 11 along Wakefield transect, Huachuca Mountains —geologic map: Hayes and Raup (1968); topographic map: Miller Peak (3475000 m N, 562000 n E). —general lithology is red-maroon (fresh and weathered) sand rich granule, pebble, and cobble subrounded to well rounded conglomerate; significant mud/clay content (reddish-maroon), which has since become pseudomatrix; major clast lithologies include, but not limited to, volcanics, limestone, granite, andesite, sandstone; clast sizes range from sand sized to cobbles >6 cm in longest exposed dimension (grain size described excludes true matrix grain sizes); “matrix” supported conglomerate; crude structureless bedding, with intercalated sandy and more conglomeratic lenses; bedding generally on the order of 30-50 cm, but variable; moderately indurated; stratigraphic up uncertain. —strike/dip (with some question due to poor outcrop): N29W 88SW.

Page 154: Copyright by Brook Colleen Daun Riley 2004

134

Station 13/990628-1 —Fort Crittenden Formation sandstone/conglomerate FT sample from Station 13 along Cemetery transect, Huachuca Mountains. —geologic map: Hayes and Raup (1968); topographic map: Montezuma Pass (3468000 m N, 560000 m E). —sample is a green-gray brown (weathered/fresh) medium to coarse grained rounded sandstone with sparse granule and pebble horizons and lenses, as well as intercalated granules within finer sandstone beds; by hand sample, F80M7C3P10:Q50F12R38; at least partially calcite cemented; beds are relatively structureless internally, and outcrop does not show evidence for beds having internal lamination, tabular, or trough cross bedding; beds have moderately sharp tops and sharp bases, and are uniform within outcrop; sandstones generally thick bedded (~30 cm thick), with some thinner beds (3-5 cm thick); sandstone moderately friable, poor to fair induration; beds fine upward within scope of outcrop. —strike/dip: N42W 39NE.

Page 155: Copyright by Brook Colleen Daun Riley 2004

135

Station 14/990628-2 —Cintura Formation sandstone FT sample from Station 14 along Cemetery transect, Huachuca Mountains. —geologic map: Hayes and Raup (1968); topographic map: Montezuma Pass (3468000 m N, 560000 m E). —sample is a brownish gray (weathered) to light brown (fresh) fine to medium grained rounded sandstone (grain size and rounding difficult to discern in hand sample due to homogeneous grain type, quartz cement, well-indurated nature); by hand sample, F95M0C5P0:Q97F2R1 (again, difficult to tell for above reasons); at least partially quartz cemented, and potentially slightly recrystallized (though no local veining seen); no local evidence for internal stratification, though up section near contact with Fort Crittenden Formation, there are very large scale low angle trough cross beds well exposed in Bear Creek; beds here are essentially internally structureless, have sharp tops and bases, and are of a consistent thickness (>35 cm thick), color, and character; bounded above and below by similar sandstones; very well indurated. —strike/dip: N67W 58SW.

Page 156: Copyright by Brook Colleen Daun Riley 2004

136

Station 23/990722-2 —Fort Crittenden Formation sandstone/conglomerate FT sample from Station 23 along Gate 7 transect, Huachuca Mountains. —geologic map: Hayes and Raup (1968); topographic map: Huachuca Peak (3478000 m N, 554000 m E). —sample is a brown (weathered) to gray (fresh) medium to coarse grained subangular to subrounded sandstone; this and other outcrops also have lenses and beds of coarse, granular, and pebbly sandstone and conglomerate, the finer of which were also included in the sample; the gross lithologies of these beds appear very similar to finer constituents; by hand sample on medium grained sandstone fraction, F87M1C8P5:Q50F10R40; partially cemented by calcite; no local evidence for fine scale laminae, tabular, or trough cross beds, but there are relatively fine scale individual beds 1-2 cm thick; overall thinly to thickly bedded (1-2 cm-40 cm); moderately to poorly indurated, (both levels of induration sampled equally); beds overall have gradational tops and bases, except where basal bed is conglomeratic, and bases of sandstone above are sharper; no evidence within outcrop for basal scour, but clear evidence for basal lags; sampled interval in this area is approximately 2 m thick, which seems to be average for Fort Crittenden Formation in this area; outcrop bounded above and below by finer lithologies (based on outcrop character). —strike/dip: N43W 87NE.

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Station 33/990802-1 —Lower Temporal Formation arkosic fanglomerate unit FT sample from Station 33 along Last Chance transect, Santa Rita Mountains. —geologic map: Drewes (1971a); topographic map: Patagonia (3497000 m N, 520000 m E). —general lithology is a white-gray (weathered) to gray-white-green with obvious pink feldspar (fresh) granule to sandy pseudomatrix supported subangular granule conglomerate with sparse small subrounded cobbles; significant fine and mud/clay content which is likely the alteration product of tuffaceous materials, which has since become pseudomatrix (pseudomatrix:clast ratio ~60:40); major clast lithology includes, but not limited to, volcanics; some of the sandy detritus may also be granitic, but due to outcrop weathering it is difficult to discern more about the clast content; likely significant tuffaceous material included in this fanglomerate; clast sizes range from abundant sandy detritus to small cobbles 1-2 cm in longest exposed dimension; no evidence for basal scour, cross bedding, tabular cross strata, or basal lag; may have relatively thin (1-2 cm?) lamination, but very difficult to tell due to weathering profile; lumpy, amorphous, weathering-back texture; poorly indurated; many portions of outcrop have slight to significant Mn staining, and there are small hematite veins locally (rare); also some yellow streaks, some along joints; hematite and yellow streaks (jarosite? goethite?) likely associated with abundant Tertiary quartz veining within this area; gradational tops and bases; outcrop at least 10-15 m thick, but cannot here see the base of this unit. —strike/dip unavailable due to weathering profile, outcrop character of sample; will use Drewes (1971a) strike/dip in same area.

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Station 38/990803-3 —Turney Ranch Formation sandstone FT sample from Station 38 along Cave Creek transect, Santa Rita Mountains. —geologic map: Drewes (1971a); topographic map: Mt. Wrightson (3510000 m N, 521000 m E). —sample is a light to dark pink (weathered) to pink lavender (fresh) medium to coarse (subordinate) grained subrounded sandstone; by hand sample, looks like F87M0C10?P3:Q80F5?R15; difficult to tell due to grain size what the potential RF fraction is; two main lithologies sampled in proportion to the proportions within the outcrop; lighter pink structureless, internally homogeneous medium to coarse sandstone is interbedded with thinly bedded, darker pink, finer grained sandstone, which itself has plane parallel laminations; generally will have one lighter pink sandstone bed approximately 5-10 cm thick, topped by 5-10 thinner (1-2 cm each), finer darker pink sandstone beds with intervening homogeneous lighter pink beds of similar thickness, and this sequence repeats throughout outcrop area; contacts between finer and coarser sandstone beds generally sharp; well indurated; no evidence for basal scour or lag, cross stratification; within area of outcrop there are also some fine beds of reddish siltstone, and some mudstone in the receding cutback of Sawmill Canyon; no obvious fining upward sequences, with the exception of the repetition as described above; sampled interval is bounded above and below by rocks of similar lithology and outcrop character; outcrop covers the full extent of the floor of Sawmill Canyon, and top and base of unit are not visible from sample site. —strike/dip: N36W 69SW.

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Station 42/990805-3 —Fort Crittenden Formation upper red conglomerate member sandstone/conglomerate FT sample from Station 42 along Ditch Mountain transect, Santa Rita Mountains. —geologic map: Drewes (1971a); topographic map: Mt. Wrightson (3507000 m N, 523000 m E). —general lithologies are maroon-brown (weathered) to purple-brown (fresh) “matrix” supported, rounded pebble and small cobble conglomerate and coarse sandstone; sandstones and conglomerates are well-interleaved, and cobbles/pebbles are well mixed within “matrix” of finer particles; major clast lithologies in the conglomerate include, but are not limited to, abundant sandstone, abundant red mudstone, abundant red claystone, sparse green sandstone, sparse chert, sparse finely laminated limestone (which looks like clasts of Apache Canyon Formation or Mural Formation, Bisbee Group); there may also be significant granitic detritus, but it is difficult to tell if it’s granitic, or if it is recycled sandstone; it is also difficult to discern whether or not these were large clasts which have since been degraded, or if the detritus was sand-sized during deposition; clast sizes range from mud and probable clay grain sizes up to a maximum longest exposed dimension of 10-12 cm; sandstones are well-mixed vertically with conglomerates, and appear as lenses as well as discrete beds; granule and sand compositions are difficult to discern in sandstones, but they appear to be broadly similar to the clasts in the conglomerates; by hand sample on medium sand fraction, F80M5C5P10:Q55F15R30; there is some evidence for basal scour and lag at bases of conglomerate beds where they cut into sandstones beneath; this is the only clear evidence that these beds are stratigraphically upright; sandstones have limited calcite cement; vague plane laminae in some sandstones, on the order of 1-2 cm thick, but no evidence for other types of stratification or cross stratification; the conglomerate is crudely, thinly to thickly bedded, and beds are on the order of 2-10 cm thick; tops of both the sandstone and conglomerate are generally gradational, and bases of most conglomerates and sandstones are sharp (though there are sparse gradational bases in both within the interval sampled); all beds are moderately to well indurated, particularly in comparison with surrounding beds; beds above and below are very similar lithologically, and show similar outcrop character; outcrop continuous within this gulch. —strike/dip: N16W 64NE.

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Station 44/990805-5 —Lower Bathtub Formation polymictic conglomerate FT sample from Station 44 along Ditch Mountain transect, Santa Rita Mountains. —geologic map: Drewes (1971a); topographic map: Mt. Wrightson (3506000 m N, 520000 m E). —general lithology is a brown (weathered/fresh), clast-supported subrounded to rounded large cobble conglomerate; dominant clast lithology is an almost porphyritic andesite; subordinate clast lithologies include rhyolite and chert; it is difficult due to exposure to tell percentages of clast types; grain sizes range from mud to the largest clasts which are approximately 15-20 cm in longest exposed dimension; grain sizes and lithologies are well mixed, the former perhaps suggesting a debris flow origin; no evidence for basal scour or lag, lamination, or cross stratification; internal contacts appear gradational; interval is crudely bedded, with beds on the order of 0.5-1 m in thickness; sampled interval is likely bounded above and below by finer lithologies, based on outcrop character (difficult to discern due to poor outcrop); sampled interval is approximately 2 m thick, with covered top and base. —strike/dip: N30W 24SW.

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Station 45/000724-1 —Fort Crittenden Formation basal conglomerate subunit sandstone FT sample from Station 45 along N Brushy transect, Huachuca Mountains. —geologic map: Hayes and Raup (1968); topographic map: Pyeatt Ranch (3486000 m N, 551800 m E). —sample is an olive (weathered) to gray (fresh) coarse to medium grained angular to subangular sandstone; by hand sample, F80M5C5P10:Q30F2R78; RF fraction mostly VRF (dark purple-gray, angular); moderately well sorted mineralogically, well size sorted; at least partially cemented by calcite; finer intervals well-indurated; coarser intervals moderately indurated; common plane parallel laminations (individual bed sets 0.5-1 cm and thinner) to low angle trough cross-bedding (bed sets 5-10 cm); sharp upper and lower contacts between beds; interval sampled is a ~1.5 m thick group of interbeds of sandstone within cobble to small boulder conglomerate. —bedding-parallel slickensides ornamented by hematite common to sparse on several bedding planes beneath sampled interval (bedding parallel faults?—flexural slip?); very minor calcite veining in the area. —sample is located within Hayes’ (1986) basal conglomerate subunit, near upper portion. —strike/dip: N33W 26SW.

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Station 46/000724-2 —Fort Crittenden Formation upper conglomerate subunit sandstone FT sample from Station 46 along N Brushy transect, Huachuca Mountains. —geologic map: Hayes and Raup (1968); topographic map: Pyeatt Ranch (3486000 m N, 551600 m E). —sample is a pink-beige (weathered) to pink-gray (fresh) coarse grained sub-rounded to rounded sandstone with rare rounded pebbles to granules (attempted not to sample pebbles and granular intervals); by hand sample, F85M0C5P10:Q70F3R27; RF fraction include VRF; moderately well sorted mineralogically; well size sorted; at least partially cemented by calcite; very well indurated; significant amount of Fe oxide; sparse to common very low angle trough cross-bedding in bed sets 10-20 cm thick; bases and tops of individual beds gradational; interval sampled is very thick (>50 m thick; refer to Hayes (1986) section), and approximately 75 cm above a pebble to small cobble conglomerate lag (possible channel lag) that overlies a significant thickness of conglomerate (>10 m thick; refer to Hayes (1986) section). —sample is from near the base of a thick sandstone interval near upper part of Hayes’ (1986) upper conglomerate subunit (approximately located stratigraphically on Hayes’ (1986) detailed measured section north of Brushy Canyon). —strike/dip: N34W 50SW.

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Station 47/000724-3 —Fort Crittenden Formation shale subunit sandstone FT sample from Station 47 along N Brushy transect, Huachuca Mountains. —geologic map: Hayes and Raup (1968); topographic map: Pyeatt Ranch (3486000 m N, 550000 m E). —sample is a brown-gray (weathered) to gray (fresh) medium grained subrounded sandstone; by hand sample, looks like F90M0C10P0:Q80F0R20; R may be chert grains or VRF; moderately well sorted mineralogically; well size sorted; at least partially cemented by calcite; well indurated; common low angle trough cross-bedding in bed sets 5-10 cm thick; sharp bases and tops with interbedded mudstone and shale, with these fine intervals ranging from centimeters to 1 m thick; sample from a ~1 m thick interval of sandstone interbedded with other thicker and thinner sandstones, mudstones, and shales. —highly variable amounts of calcite veining in the area, from abundant to rare; unavoidable, but no portion of sample was veined or associated with veined areas. —sample within the upper part of Hayes’ (1986) shale subunit, Hayes’ (1986) geologic map where dips change from SW to NE. —strike/dip: N37W 35SW.

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Station 49/000725-1 —Fort Crittenden Formation upper conglomerate? subunit sandstone FT sample from Station 49 along Ferosa transect, Huachuca Mountains. —geologic map: Hayes and Raup (1968); topographic map: Pyeatt Ranch (3489000 m N, 550000 m E). —sample is a red-orange-brown (weathered) to white (fresh) coarse grained sub-angular to sub-rounded sandstone with lags and thin intervals of granules (attempted to avoid the latter in sampling); by hand sample, F90M0C7P3:Q70F10?R20; RF are dark gray to black moderately well rounded grains; rare large (~4 cm in largest exposed dimension) rounded mud rip-up clasts; partially quartz cemented; moderately well indurated; structureless beds 15-20 cm thick (similar beds this thick nearby; difficult to tell here due to jointing); sample from an ~2 m thick interval of sandstone beds with interbedded conglomerate (laterally and vertically gradational with sandstone within 2 m). —sample near top? of upper conglomerate subunit; difficult to tell here due to faulting, folding in this area; particularly difficult to tell going further south along Ferosa Canyon, where there are fault slivers of upper conglomerate next to slivers of basal conglomerate in a repetitive fashion; does not appear to be interbedding of upper and basal (and there wasn’t interbedding or a gradational nature to this contact in Hayes’ (1986) section north of Brushy Canyon); however, it is difficult in this area find other evidence for faulting other than juxtaposition of these units, presence of faults and veining northward along Ferosa Canyon. —strike/dip: N34W 24NE (overturned?—no facing indicators here, map indicates overturning).

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Station 52/000730-2 —Fort Crittenden Formation shale member sandstone FT sample from Station 52 along Ditch Mountain transect, Santa Rita Mountains. —geologic map: Drewes (1971a); topographic map: Mt. Wrightson (3511000 m N, 520000 m E). —sample is a pink-brown (weathered) to purple-gray (fresh) fine to medium grained, subrounded to subangular sandstone; by hand sample, F90M0C8P2:Q93F2R5; sample is well mineralogically sorted, well size sorted; large mud rip-up clasts (2-4 cm in longest exposed dimension) on some bedding planes; sample is very well indurated, at least partially calcite cemented; low angle trough crossbeds common within most layers, in bedsets 15-20 cm thick; beds range from 7-8 cm thick to 30-40 cm thick; sharp tops and bases; sample is from a 2 meter thick sandstone package bounded atop by red shale and below by similar sandstone; thin granule conglomeratic intervals present (2-5 cm and above and within each unit). —strike/dip: N20W 82SW.

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Appendix 3—Description of techniques used in this study

Fission-track Thermochronology

Fission track thermochronology is based on the formation of damage tracks in a crystal lattice

from the spontaneous fission of 238U in nature, and the retention and accumulation of these

damage tracks when samples remain below the closure temperature (235°C ± 25°C for zircon;

Brandon and Vance, 1992). Over time, trace amounts of uranium incorporated into a mineral

structure decay spontaneously by alpha emission or by fission. The fission process creates

spontaneous tracks, or trails of severe damage of the crystal lattice due to the high masses of the

daughter nuclei (atomic numbers 30 through 65; Faure, 1986) moving away from each other as a

large amount of energy is released (approximately 200 MeV; Faure 1986). The density of

spontaneous fission tracks depends upon 238U concentration and the length of time since cooling

through the temperature of track annealing (closure temperature).

The amount of 235U in the zircon, and therefore the amount of 238U in the zircon, is estimated by

measurement of the density of induced fission tracks in an external detector. This method

involves mounting mineral grains in Teflon, and grinding and polishing the mount to reveal a fresh

internal surface of the grain. A pre-annealed mica sheet is attached to this surface to serve as

the external detector; the mica print records the fission of 235U induced during slow neutron

irradiation (which causes only 235U to fission) within a reactor facility.

Both spontaneous fission tracks and induced fission tracks are counted on a polished, acid-

etched surface of the mineral or the detector. Enlargement of the damage zone by etching

reveals the tracks. Track densities are measured by counting etched fission track pits in reflected

light at high magnification (1250x). Spontaneous track densities are measured following

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irradiation. Generally, densities of tracks must be on the order of 10/cm2 (Fleischer and others,

1975); below this lower limit, a statistically significant number of tracks are difficult to count.

Measured parameters include: the spontaneous track density within the mineral (ρs); the induced

track density within the external detector (ρi); the reactor neutron flux at the time of irradiation (Φ);

and the zeta (ζ) calibration factor for each counter. The latter is a pre-determined calibration

factor between the analyst and internationally accepted natural age standards.

The density of spontaneous fission tracks (ρs) is given by the equation ρs = (tλ)(Nvc238R238η238),

where t = time over which tracks have accumulated; λ = decay constant for fission of 238U

(1.551x10-10 y-1); Nv = number of atoms per unit volume in mineral; c238 = fraction of atoms in the

mineral that are 238U; R238 = length of etchable track of 238U fission fragment in the grain; η238 =

etching efficiency of the mineral (a ratio of the number of tracks revealed to the number that

intersect the etched surface for a given material and etch condition; Fleischer and others, 1975).

The density of induced fission tracks (ρi) is given by the equation ρi = (σΦ)(Nvc235R235η235), where

σ = cross-section for inducing fission of 235U; Φ = thermal neutron flux (neutrons/unit area); Nv =

number of atoms per unit volume in detector; c235 = fraction of atoms in the detector that are 235U;

R235 = length of etchable track of 235U fission fragment in the detector; η235 = etching efficiency

within the detector.

The neutron flux (Φ) is measured by including a dosimeter glass and attached mica at either end

of the tube of grain/mica mounts (Fleischer and others, 1975). The dosimeter glass contains a

known concentration of uranium. By counting the density of a statistically significant number of

track etch pits in the attached mica (which has recorded induced fission tracks in the dosimeter

during neutron bombardment), the neutron flux can be calculated using the following equation: ρd

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= BΦ, where B = σNvRdCdUηD (a constant); σ = cross section for inducing fission of 235U in the

dosimeter; Φ = thermal neutron flux (neutrons/unit area); Nv = number of atoms per unit volume in

dosimeter glass; CdU = fraction of atoms in dosimeter that are 235U in the dosimeter; R235 = length

of an etchable 235U track in the dosimeter; η235 = etching efficiency of the dosimeter. In the

equation above, B is a constant that does not require independent measurement provided that it

remains constant (Fleischer and others, 1975).

The above equations combine to give an equation for the age of the mineral since the last partial

or full resetting:

tgs

iw d= +

1 1λ

ρρ

ζ ρ λln , ( ) ( ) ( ) ( )σ σ ζt s i d z wN N N w= + + +1 1 1 2/ / / / ,

where t = age; λ = total decay constant for 238U (1.551x10-10 y-1); g = geometry factor for mica

external detector (= 2); ρs = spontaneous track density (tracks/cm2); ρi = induced track density in

external detector (tracks/cm2); ρd = spontaneous track density in dosimeter (tracks/cm2); Ns =

density of spontaneous tracks counted; Ni = density of induced tracks counted; Nd = density of

dosimeter tracks counted; ζw = weighted mean zeta calibration factor (see below); σζw = weighted

error of weighted mean zeta factor (see below).

The Zeta factor (ζ) varies among different counters; Zeta is a correction for the difference

between the calculated age of a known standard and the “true” age of that standard as

determined by independent means. The equations that describe this value and the associated

uncertainty are as follows:

ζσ ζ

σw

z j

j

n

z

j

n

j

j

=

2

2

1

1

, σ σζw jzj

n

= −

−∑ 2

1

,

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where ( )ζλ

ρρ ρ

λj

t i

s de gstd p

p

= −

1

( ) ( ) ( ) ( )σ σz s i d std stdj N N N t= + + + +1 1 1 2/ / /

tstd = known age of standard

σstd = known error of standard age

Several assumptions are inherent in using the above equations (Fleischer and others, 1975).

The Zeta value is assumed to be constant; ζ is a function of ρs, ρi, and ρd, which are (or should

be) constant. The counted tracks must have been derived only from the spontaneous fission of

uranium or of 235U in the case of induced fission. Methods of etching and track identification must

be the same for spontaneous and induced track counts. Based on counting a series of zircon

standards including zircons from the Fish Canyon tuff (Colorado; 27.90 Ma ± .50 m.y.) and the

Buluk tuff (Kenya; 16.40 Ma ± .20 m.y.), the author’s weighted mean ζ is 352.74 ± 8.09 (one

standard deviation).

Component statistical peak ages were fitted to the single-grain age data using the methodology

and programs presented in Brandon (1992, 1996). In general where less than 15 single-grain

ages were measured, the χ2 age is reported (Galbraith, 1981).

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Cathodoluminescence

Color FT mounts were carbon-coated and cathodoluminescence (CL) images of each FT-dated

grain were taken using an Oxford Instruments photomultiplier-based CL detector mounted on a

JEOL T330A scanning electron microscope; accelerating voltages range from 10-15 kV, as

described in Milliken (1994). CL images assist in differentiating zonation within a grain, degree of

heterogeneity within individual grains, and zonation present within the counted region. The

magnitude of CL response of geologic materials, particularly zircons, is the result of multiple

factors which are difficult to distinguish. These include the degree of metamictization (Chuanyi

and others, 1992) and varying, competing responses from trace element contributions (Hanchar

and Rudnick, 1995). As such, the use of CL remains a qualitative guide for other quantitative

portions of this work.

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Raman Microscopy

Short-range order of the crystal lattice, and therefore the degree of crystallinity of a zircon is

related to the amount of radiation damage, with α-damage being the overwhelming contributor

(Murakami and others, 1991; Nasdala and others, 1995; Nasdala and others, 2001). Raman

microprobe analyses were utilized to determine the short-range order of the crystal lattice within

the FT-counted area, and variations in lattice order among different CL-detected zones.

Representative Raman measurements (2-6 measurements per grain) were made based on the

FT-counted locations, and to characterize zonation detected in the CL images. Raman

measurements were made at the University of Mäinz using a Jobin Yvon LabRam-HR equipped

with an Olympus optical microscope (100x objective, numerical aperture 0.9). Spectra were

excited using the He-Ne 632.8 nm line (3 mW at the sample surface). Wave number accuracies

are ± 0.5 cm-1, with spectral resolution of approximately 0.5 cm-1. Methods, data reduction, and

errors are further discussed in Nasdala and others (2001).

The total possible α-damage dose, or the total amount of damage possible given the eU value

and the crystallization age, are calculated by the following formula:

Da = 8 * (cU*NA*0.9928/M238*106) * (eλ238t-1) + 7 * (cU*NA*0.0072/M235*106) * (eλ235 t-1) + 6 * (cTh*NA/M232*106) * (eλ232 t-1),

where Da = number of a-decay events per mg zircon; cU and cTh are the U and Th concentrations

in the zircon (ppm); NA is Avogadro’s number; M238, M235, and M232 are the molecular weights of

the parent isotopes; λ238, λ235, and λ232 are the decay constants for each of the parent isotopes;

and t is age (in this case, the crystallization age).

Accumulated α-damage dose, or the amount of damage stored based on the present crystallinity

of the grain, is calculated given the eU value and the amount of time required to achieve the

present level of damage. The equation cited above is utilized to calculate this value, with t in this

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case is the minimum damage storage age (the time required to achieve the present level of α-

damage).

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U-Th-Pb and Rare-earth-element Analysis

To complement the crystallinity measurements and determine the total possible and accumulated

α-damage within each crystal, FT-dated zircons were analyzed for Pb, U, and Th within the FT-

counted area using laser ablation inductively-coupled mass spectrometry (LA-ICP-MS). FT-dated

grains were also analyzed for heavy and light REE using LA-ICP-MS, using the same spot

location as the Pb, U, and Th analyses.

The University of Texas LA-ICP-MS system (Platform quadrapole ICP-MS) utilizes an LUV 213

Nd:YAG laser which generates a 200 mJ beam at 1064 nm. The laser beam is polarized and

then passes through a series of harmonic resonators resulting in a final laser beam of up to 5 mJ

of 213 nm ultraviolet light. Based on grain behavior and machine response, the laser was used at

40-50% maximum power with 30-40 µm actual spot sizes. Material from the ablation pit is

injected into the plasma, extracted to the Hexapole cell, ionized, and passed through the

quadrapole mass analyzer to a single Daly-cup detector. For each grain a series of 78 scans of

all masses of interest was made (28Si, 91Zr, 96Zr, all REE, 176Hf, 179Hf, 206Pb, 207Pb, 208Pb, 232Th,

and 238U).

For calculation of Pb-Pb ages, the number of counts per second (CPS) of 206Pb and 207Pb were

ratioed against one another for multiple sequential analyses (up to 78) of each grain during the

sample run. The total number of scans for each grain was divided into three groups, and the

blank-subtracted averages of these groups were used to calculate the concentration ages for the

majority of grains for which FT, crystallinity measurements, and REE compositions were

determined. Precision estimates for the ages were determined by finding the standard deviation

of the three counts-per-second averages over the course of the 78 runs; the standard deviation of

these values is then used as the uncertainty (one standard deviation).

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232Th, 238U, 235U, and REE concentrations were calculated based on CPS measurements from the

LA-ICP-MS. Reduction of these data for the unknown zircons involves comparison of counts per

second for a given element over the run time with solution concentration data for a standard

zircon (zircon UT-01, from the University of Texas at Austin Vargas Mineral Collection), and with

concentrations of Zr from electron microprobe analysis of the unknown zircons (analyzed at

Rensselaer Polytechnic Institute by K. Becker; Appendix 6). The UT-01 standard zircon was

dissolved and analyzed using the Platform quadrapole ICP-MS (analysis completed by J.

Lansdown, University of Texas). Data reduction procedure for calculation of the concentrations

follows.

A concentration/CPS (slope) for the element of interest is calculated by taking the concentration

of the element (determined by solution analysis of UT-01) and dividing this value by the

concentration of 96Zr (determined by solution analysis of UT-01), yielding a concentration ratio.

The CPS of the element of interest divided by CPS 96Zr yields a CPS ratio. The concentration

ratio is divided by the CPS ratio for each run of UT-01. An average of these values yields an

average concentration/CPS; this is the number (slope) by which the CPS and microprobe 96Zr

values are multiplied in the following procedure. The same procedure was completed for Hf, to

verify that similar values resulted. This analysis treats the solution concentration values for both

238U and 96Zr as ‘true’ values. This is not an issue for comparison of relative concentrations of

each element, since the same 96Zr concentration is used for each element as the standard.

The blank-subtracted CPS of the element of interest is divided by the blank-subtracted CPS of

96Zr (for a given grain). This value is multiplied by the concentration/CPS (slope) for the isotope

of interest, and by the microprobe value for 96Zr for that grain; this yields a parts-per-million (ppm)

concentration of the element of interest in a given grain. This analysis treats the microprobe-

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determined concentration values for 96Zr for each grain as ‘true’ values, in addition to using the

slope (above), which treats the solution values as ‘true.’

Because of the size of the unknown zircons (most 50-75 µm in longest exposed dimension), and

the laser spot sizes (30-45 µm), multiple sequential scan series of each grain were not possible.

Estimates of errors for the concentrations were derived by comparing concentrations of the

element of interest for multiple laser ablation runs of UT-01, calculating an average concentration

for UT-01, and a standard deviation for those data. The blank-subtracted CPS of the element of

interest is divided by the blank-subtracted CPS of 96Zr. This value is multiplied by the

concentration/CPS value (slope) derived for UT-01, and by the ppm Zr (determined for UT-01 by

solution analysis) to derive a concentration of the element of interest in that analysis of UT-01.

These values are then averaged, and compared using the standard deviation as the uncertainty.

The same procedure was completed for Hf, with resulting similar concentrations and standard

deviations. Detection limits for laser ablation analyses were determined by a comparison of laser

analyses of NIST glasses with low concentrations to estimate lower detection limits (0.3 ppm).

COMPARISON OF SPOT SIZES FOR VARIOUS METHODS

Spot sizes varied among the different types of analyses. Spot sizes for Raman microprobe

analysis and LA-ICP-MS approximate the FT-counted area, and CL images were used to verify a

lack of zonation in the analyzed region. Raman measurements were made based on the FT-

counted location, as well as to represent different zones present in the CL images. LA-ICP-MS

data effectively encompass the entire FT-counted region.

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Appendix 4—Complete fission track data for Jura-Cretaceous sandstone samples, Santa Rita and Huachuca Mountains, southeastern Arizona

abbreviations/symbols RhoS = density of spontaneous tracks (/cm2) Ns = number of spontaneous tracks counted RhoI = density of induced tracks (/cm2) Ni = number of induced tracks counted squares = number of squares counted (area of one counting square for University of Texas

Axioskop = 6.160x10-7 cm2) U+/-2s = ppm uranium, ± 2 standard deviations

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Upper Cretaceous Fort Crittenden Formation, Station 9 990625-3 (Axioskop, 010412-19) >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.968E+05 RELATIVE ERROR (%): 1.92 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 1 2.50E+07 ( 123) 1.79E+07 ( 88) 8 732 158 72.4 54.8 95.5 2 1.41E+07 ( 182) 9.12E+06 ( 118) 21 374 70 79.9 63.0 101.3 3 8.93E+06 ( 99) 6.49E+06 ( 72) 18 266 63 71.6 52.3 98.4 4 1.33E+07 ( 49) 8.93E+06 ( 33) 6 366 127 77.2 48.7 123.8 5 2.01E+07 ( 62) 1.56E+07 ( 48) 5 639 185 67.2 45.4 100.2 6 1.05E+07 ( 103) 6.70E+06 ( 66) 16 275 68 81.1 59.0 112.3 7 6.80E+06 ( 67) 5.99E+06 ( 59) 16 245 64 59.2 41.1 85.5 8 1.52E+07 ( 262) 1.25E+07 ( 216) 28 514 73 63.1 52.2 76.1 9 7.51E+06 ( 74) 9.23E+06 ( 91) 16 379 80 42.5 30.8 58.4 10 1.43E+07 ( 53) 1.00E+07 ( 37) 6 410 135 74.5 48.1 116.6 11 7.98E+06 ( 118) 6.43E+06 ( 95) 24 263 55 64.4 48.9 84.7 12 1.38E+07 ( 102) 1.08E+07 ( 80) 12 444 100 66.4 49.0 90.2 >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.957E+05 RELATIVE ERROR (%): 1.90 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 13 1.35E+07 ( 116) 1.12E+07 ( 97) 14 463 95 61.8 47.0 81.2 14 1.33E+07 ( 98) 6.22E+06 ( 46) 12 256 76 110.0 76.9 159.7 15 1.38E+07 ( 51) 1.27E+07 ( 47) 6 523 153 56.3 37.1 85.6 16 1.61E+07 ( 89) 1.42E+07 ( 79) 9 586 133 58.5 42.7 80.3 17 1.46E+07 ( 54) 1.38E+07 ( 51) 6 568 160 55.0 36.8 82.3 18 2.44E+07 ( 60) 1.38E+07 ( 34) 4 568 195 91.2 59.1 143.3 19 3.31E+07 ( 102) 1.30E+07 ( 40) 5 535 169 131.3 90.6 194.3 20 1.96E+07 ( 145) 8.93E+06 ( 66) 12 367 91 113.4 84.3 154.2 21 2.05E+07 ( 126) 1.07E+07 ( 66) 10 441 109 98.7 72.8 135.1 22 2.02E+07 ( 174) 6.26E+06 ( 54) 14 258 70 165.6 121.7 228.9 23 1.79E+07 ( 231) 9.89E+06 ( 128) 21 407 73 93.1 74.6 116.2 24 2.31E+07 ( 71) 1.62E+07 ( 50) 5 668 190 73.6 50.6 107.9 25 2.52E+07 ( 186) 1.42E+07 ( 105) 12 585 116 91.3 71.5 116.5 26 1.32E+07 ( 73) 1.75E+07 ( 97) 9 720 148 39.2 28.4 53.6 27 1.33E+07 ( 74) 1.17E+07 ( 65) 9 483 121 59.1 41.7 83.8 28 1.34E+07 ( 99) 8.12E+06 ( 60) 12 334 87 85.4 61.4 119.8 29 1.27E+07 ( 78) 9.90E+06 ( 61) 10 408 105 66.3 46.8 94.3 990625-3 (Axioskop, 010412-19) Number of grains = 29 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 26 1.32E+07 ( 73) 1.75E+07 ( 97) 39.2 28.4 53.6 100.0 39.3 28.5 53.9 9 7.51E+06 ( 74) 9.23E+06 ( 91) 42.5 30.8 58.4 71.2 40.6 32.5 50.8 17 1.46E+07 ( 54) 1.38E+07 ( 51) 55.0 36.8 82.3 37.7 43.7 35.9 53.1

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15 1.38E+07 ( 51) 1.27E+07 ( 47) 56.3 37.1 85.6 35.7 45.8 38.3 54.7 16 1.61E+07 ( 89) 1.42E+07 ( 79) 58.5 42.7 80.3 27.3 48.5 41.4 56.8 27 1.33E+07 ( 74) 1.17E+07 ( 65) 59.1 41.7 83.8 28.2 50.1 43.3 58.0 7 6.80E+06 ( 67) 5.99E+06 ( 59) 59.2 41.1 85.5 32.0 51.2 44.6 58.8 13 1.35E+07 ( 116) 1.12E+07 ( 97) 61.8 47.0 81.2 28.1 53.0 46.7 60.2 8 1.52E+07 ( 262) 1.25E+07 ( 216) 63.1 52.2 76.1 18.9 55.7 49.8 62.4 11 7.98E+06 ( 118) 6.43E+06 ( 95) 64.4 48.9 84.7 19.8 56.7 50.9 63.1 29 1.27E+07 ( 78) 9.90E+06 ( 61) 66.3 46.8 94.3 21.9 57.3 51.6 63.6 12 1.38E+07 ( 102) 1.08E+07 ( 80) 66.4 49.0 90.2 23.4 58.0 52.4 64.2 5 2.01E+07 ( 62) 1.56E+07 ( 48) 67.2 45.4 100.2 26.6 58.4 52.8 64.6 3 8.93E+06 ( 99) 6.49E+06 ( 72) 71.6 52.3 98.4 23.9 59.2 53.7 65.3 1 2.50E+07 ( 123) 1.79E+07 ( 88) 72.4 54.8 95.5 19.7 60.2 54.7 66.2 24 2.31E+07 ( 71) 1.62E+07 ( 50) 73.6 50.6 107.9 19.6 60.7 55.3 66.7 10 1.43E+07 ( 53) 1.00E+07 ( 37) 74.5 48.1 116.6 20.7 61.1 55.7 67.1 4 1.33E+07 ( 49) 8.93E+06 ( 33) 77.2 48.7 123.8 20.9 61.5 56.1 67.4 2 1.41E+07 ( 182) 9.12E+06 ( 118) 79.9 63.0 101.3 9.7 63.0 57.6 68.9 6 1.05E+07 ( 103) 6.70E+06 ( 66) 81.1 59.0 112.3 7.2 63.7 58.3 69.7 28 1.34E+07 ( 99) 8.12E+06 ( 60) 85.4 61.4 119.8 4.5 64.6 59.1 70.5 18 2.44E+07 ( 60) 1.38E+07 ( 34) 91.2 59.1 143.3 3.2 65.1 59.7 71.0 25 2.52E+07 ( 186) 1.42E+07 ( 105) 91.3 71.5 116.5 0.6 66.7 61.3 72.7 23 1.79E+07 ( 231) 9.89E+06 ( 128) 93.1 74.6 116.2 0.1 68.5 63.1 74.5 21 2.05E+07 ( 126) 1.07E+07 ( 66) 98.7 72.8 135.1 0.0 69.6 64.1 75.6 14 1.33E+07 ( 98) 6.22E+06 ( 46) 110.0 76.9 159.7 0.0 70.5 65.0 76.5 20 1.96E+07 ( 145) 8.93E+06 ( 66) 113.4 84.3 154.2 0.0 71.9 66.3 78.0 19 3.31E+07 ( 102) 1.30E+07 ( 40) 131.3 90.6 194.3 0.0 73.1 67.4 79.2 22 2.02E+07 ( 174) 6.26E+06 ( 54) 165.6 121.7 228.9 0.0 75.4 69.6 81.7 POOL 1.46E+07( 3121) 1.01E+07( 2153) 0.0 75.4 69.6 81.7 MEAN URANIUM CONCENTRATION +/-2SE (ppm): 414.3, 23.9 POOLED AGE WITH 63% CONF. INTERVAL(Ma): 75.4, 72.4 -- 78.5 ( -3.0 +3.1) 95% CONF. INTERVAL(Ma): 69.6 -- 81.7 ( -5.8 +6.3) CHI^2 PROBABILITY: 0.0% CENTRAL AGE WITH 63% CONF. INTERVAL(Ma): 74.4, 69.8 -- 79.3 ( -4.6 +4.9) 95% CONF. INTERVAL(Ma): 65.7 -- 84.2 ( -8.7 +9.9) AGE DISPERSION (%): 26.0 CHI^2 AGE WITH 63% CONF. INTERVAL (Ma): 65.1, 62.3 -- 68.1 ( -2.8 +3.0) 95% CONF. INTERVAL (Ma): 59.7 -- 71.0 ( -5.4 +5.9) NUMBER AND PERCENTAGE OF GRAINS: 22, 76%

Page 182: Copyright by Brook Colleen Daun Riley 2004

990625-3Upper Cretaceous Fort Crittenden Formation

Station 9, Huachuca Mountains

n = 29 grains (12 from 15 h etch, 17 from 11 h etch)

FT grain age (Ma)

30 50 70 300 50010 100

Pro

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z=

0.1

)

0

1

2

3

4

5

6

162

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163

Lower Cretaceous Glance conglomerate, Station 11 990626-1 (Axioskop, 020628-020702) >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.946E+05 RELATIVE ERROR (%): 1.88 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 1 2.33E+07 ( 172) 8.52E+06 ( 63) 12 352 89 139.3 104.1 186.1 2 2.11E+07 ( 156) 1.14E+07 ( 84) 12 469 104 95.2 72.8 124.6 3 1.99E+07 ( 98) 9.94E+06 ( 49) 8 411 118 102.9 72.5 148.2 4 2.60E+07 ( 192) 1.38E+07 ( 102) 12 570 115 96.6 75.6 123.4 5 1.92E+07 ( 248) 1.14E+07 ( 147) 21 469 79 86.8 70.3 107.1 6 2.14E+07 ( 158) 1.22E+07 ( 90) 12 503 107 90.1 69.3 117.2 7 2.39E+07 ( 265) 8.30E+06 ( 92) 18 343 72 147.2 115.6 187.2 8 2.44E+07 ( 150) 1.35E+07 ( 83) 10 557 124 92.7 70.6 121.6 9 2.11E+07 ( 117) 1.06E+07 ( 59) 9 440 115 102.1 74.1 142.1 10 1.96E+07 ( 121) 1.20E+07 ( 74) 10 496 116 84.3 62.6 114.3 11 2.68E+07 ( 165) 1.23E+07 ( 76) 10 510 118 111.1 84.4 146.2 12 2.04E+07 ( 151) 7.85E+06 ( 58) 12 324 86 133.6 98.3 184.2 13 3.06E+07 ( 151) 1.30E+07 ( 64) 8 536 135 121.3 90.1 165.2 14 2.65E+07 ( 147) 1.32E+07 ( 73) 9 544 129 103.1 77.6 136.9 15 3.33E+07 ( 164) 1.40E+07 ( 69) 8 578 140 121.5 91.5 161.3 16 2.09E+07 ( 206) 1.32E+07 ( 130) 16 545 98 81.5 65.1 102.1 17 2.48E+07 ( 153) 1.22E+07 ( 75) 10 503 117 104.5 79.0 138.1 18 2.39E+07 ( 147) 9.90E+06 ( 61) 10 409 105 123.8 91.4 169.8 19 1.54E+07 ( 114) 1.08E+07 ( 80) 12 447 101 73.2 54.8 97.7 20 1.66E+07 ( 184) 8.12E+06 ( 90) 18 335 72 104.8 81.1 135.4 21 1.43E+07 ( 88) 8.28E+06 ( 51) 10 342 96 88.9 62.4 128.2 22 2.15E+07 ( 199) 1.07E+07 ( 99) 15 443 90 103.1 80.6 131.8 23 1.76E+07 ( 260) 7.98E+06 ( 118) 24 330 62 113.0 90.4 141.2 24 2.00E+07 ( 332) 9.26E+06 ( 154) 27 383 63 110.7 90.8 134.9 25 1.64E+07 ( 363) 8.97E+06 ( 199) 36 371 54 93.9 78.3 112.5 26 1.89E+07 ( 210) 8.21E+06 ( 91) 18 339 72 118.2 92.0 151.7 27 2.61E+07 ( 257) 1.40E+07 ( 138) 16 578 101 95.7 77.3 118.4 28 2.44E+07 ( 240) 8.93E+06 ( 88) 16 369 80 139.4 108.8 178.6 29 2.49E+07 ( 245) 1.02E+07 ( 101) 16 423 86 124.2 98.1 157.3 30 1.62E+07 ( 120) 1.01E+07 ( 75) 12 419 98 82.1 61.3 109.9 >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.935E+05 RELATIVE ERROR (%): 1.85 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 31 3.54E+07 ( 218) 1.44E+07 ( 89) 10 599 129 124.9 97.2 160.4 32 2.97E+07 ( 183) 1.19E+07 ( 73) 10 491 116 127.6 97.0 167.8 33 2.65E+07 ( 163) 1.27E+07 ( 78) 10 525 120 106.6 81.1 140.1 34 5.25E+07 ( 291) 1.08E+07 ( 60) 9 449 117 244.3 185.0 322.2 35 3.21E+07 ( 237) 1.34E+07 ( 99) 12 555 113 122.2 96.2 155.1 990626-1 (Axioskop, 020628-020702) ------ GRAIN AGES IN ORIGINAL ORDER ------

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Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 36 2.46E+07 ( 227) 1.36E+07 ( 126) 15 565 103 92.2 73.8 115.3 37 2.72E+07 ( 201) 1.83E+07 ( 135) 12 757 133 76.4 61.0 95.5 38 2.42E+07 ( 149) 1.49E+07 ( 92) 10 619 131 82.9 63.6 107.9 39 1.70E+07 ( 251) 1.01E+07 ( 149) 24 418 70 86.3 70.0 106.4 40 3.53E+07 ( 435) 4.55E+06 ( 56) 20 188 51 386.8 293.5 508.4 41 2.94E+07 ( 145) 1.70E+07 ( 84) 8 707 156 88.3 67.2 115.8 42 3.85E+07 ( 166) 1.37E+07 ( 59) 7 567 149 143.8 106.5 197.0 990626-1 (Axioskop, 020628-020702) Number of grains = 42 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 19 1.54E+07 ( 114) 1.08E+07 ( 80) 73.2 54.8 97.7 100.0 73.2 54.8 97.7 37 2.72E+07 ( 201) 1.83E+07 ( 135) 76.4 61.0 95.5 82.7 75.3 62.8 90.3 16 2.09E+07 ( 206) 1.32E+07 ( 130) 81.5 65.1 102.1 83.2 77.8 67.1 90.1 30 1.62E+07 ( 120) 1.01E+07 ( 75) 82.1 61.3 109.9 91.8 78.6 68.7 90.0 38 2.42E+07 ( 149) 1.49E+07 ( 92) 82.9 63.6 107.9 95.7 79.5 70.2 90.0 10 1.96E+07 ( 121) 1.20E+07 ( 74) 84.3 62.6 114.3 97.7 80.1 71.2 90.1 39 1.70E+07 ( 251) 1.01E+07 ( 149) 86.3 70.0 106.4 97.4 81.4 73.1 90.7 5 1.92E+07 ( 248) 1.14E+07 ( 147) 86.8 70.3 107.1 97.9 82.4 74.4 91.2 41 2.94E+07 ( 145) 1.70E+07 ( 84) 88.3 67.2 115.8 98.5 82.9 75.1 91.5 21 1.43E+07 ( 88) 8.28E+06 ( 51) 88.9 62.4 128.2 99.1 83.2 75.5 91.7 6 2.14E+07 ( 158) 1.22E+07 ( 90) 90.1 69.3 117.2 99.2 83.8 76.3 92.1 36 2.46E+07 ( 227) 1.36E+07 ( 126) 92.2 73.8 115.3 98.9 84.7 77.3 92.8 8 2.44E+07 ( 150) 1.35E+07 ( 83) 92.7 70.6 121.6 99.0 85.3 78.0 93.2 25 1.64E+07 ( 363) 8.97E+06 ( 199) 93.9 78.3 112.5 98.1 86.4 79.3 94.1 2 2.11E+07 ( 156) 1.14E+07 ( 84) 95.2 72.8 124.6 98.2 86.9 79.9 94.5 27 2.61E+07 ( 257) 1.40E+07 ( 138) 95.7 77.3 118.4 97.8 87.6 80.7 95.2 4 2.60E+07 ( 192) 1.38E+07 ( 102) 96.6 75.6 123.4 97.7 88.2 81.3 95.6 9 2.11E+07 ( 117) 1.06E+07 ( 59) 102.1 74.1 142.1 97.4 88.6 81.7 96.0 3 1.99E+07 ( 98) 9.94E+06 ( 49) 102.9 72.5 148.2 97.2 89.0 82.1 96.4 22 2.15E+07 ( 199) 1.07E+07 ( 99) 103.1 80.6 131.8 95.6 89.7 82.8 97.0 14 2.65E+07 ( 147) 1.32E+07 ( 73) 103.1 77.6 136.9 94.8 90.1 83.4 97.5 17 2.48E+07 ( 153) 1.22E+07 ( 75) 104.5 79.0 138.1 93.7 90.7 83.9 98.0 20 1.66E+07 ( 184) 8.12E+06 ( 90) 104.8 81.1 135.4 92.0 91.2 84.5 98.5 33 2.65E+07 ( 163) 1.27E+07 ( 78) 106.6 81.1 140.1 90.1 91.8 85.0 99.1 24 2.00E+07 ( 332) 9.26E+06 ( 154) 110.7 90.8 134.9 77.8 93.0 86.2 100.2 11 2.68E+07 ( 165) 1.23E+07 ( 76) 111.1 84.4 146.2 73.1 93.5 86.8 100.8 23 1.76E+07 ( 260) 7.98E+06 ( 118) 113.0 90.4 141.2 61.6 94.4 87.6 101.6 26 1.89E+07 ( 210) 8.21E+06 ( 91) 118.2 92.0 151.7 48.2 95.2 88.4 102.4 13 3.06E+07 ( 151) 1.30E+07 ( 64) 121.3 90.1 165.2 39.4 95.8 89.0 103.0 15 3.33E+07 ( 164) 1.40E+07 ( 69) 121.5 91.5 161.3 30.6 96.4 89.6 103.7 35 3.21E+07 ( 237) 1.34E+07 ( 99) 122.2 96.2 155.1 19.4 97.2 90.5 104.5 18 2.39E+07 ( 147) 9.90E+06 ( 61) 123.8 91.4 169.8 15.2 97.8 91.0 105.1 29 2.49E+07 ( 245) 1.02E+07 ( 101) 124.2 98.1 157.3 8.7 98.6 91.8 106.0 31 3.54E+07 ( 218) 1.44E+07 ( 89) 124.9 97.2 160.4 5.3 99.4 92.5 106.7 32 2.97E+07 ( 183) 1.19E+07 ( 73) 127.6 97.0 167.8 3.3 100.0 93.2 107.4 12 2.04E+07 ( 151) 7.85E+06 ( 58) 133.6 98.3 184.2 2.0 100.6 93.7 107.9 1 2.33E+07 ( 172) 8.52E+06 ( 63) 139.3 104.1 186.1 0.8 101.3 94.4 108.7 990626-1 (Axioskop, 020628-020702) Number of grains = 42 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 28 2.44E+07 ( 240) 8.93E+06 ( 88) 139.4 108.8 178.6 0.2 102.3 95.3 109.7 42 3.85E+07 ( 166) 1.37E+07 ( 59) 143.8 106.5 197.0 0.1 102.9 96.0 110.4

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7 2.39E+07 ( 265) 8.30E+06 ( 92) 147.2 115.6 187.2 0.0 104.1 97.1 111.6 34 5.25E+07 ( 291) 1.08E+07 ( 60) 244.3 185.0 322.2 0.0 106.3 99.2 114.0 40 3.53E+07 ( 435) 4.55E+06 ( 56) 386.8 293.5 508.4 0.0 110.6 103.2 118.5 POOL 2.33E+07( 8239) 1.09E+07( 3837) 0.0 110.6 103.2 118.5 MEAN URANIUM CONCENTRATION +/-2SE (ppm): 448.3, 22.2 POOLED AGE WITH 63% CONF. INTERVAL(Ma): 110.6, 106.8 -- 114.6 ( -3.8 +4.0) 95% CONF. INTERVAL(Ma): 103.2 -- 118.5 ( -7.4 +7.9) CHI^2 PROBABILITY: 0.0% CENTRAL AGE WITH 63% CONF. INTERVAL(Ma): 108.8, 103.4 -- 114.5 ( -5.4 +5.7) 95% CONF. INTERVAL(Ma): 98.5 -- 120.2 ( -10.3 +11.4) AGE DISPERSION (%): 23.8 CHI^2 AGE WITH 63% CONF. INTERVAL (Ma): 100.6, 97.0 -- 104.3 ( -3.6 +3.7) 95% CONF. INTERVAL (Ma): 93.7 -- 107.9 ( -6.9 +7.4) NUMBER AND PERCENTAGE OF GRAINS: 36, 86%

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990626-1Lower Cretaceous Glance conglomerate

Station 11, Huachuca Mountains

n = 42 grains (30 from 17 h etch, 12 from 12 h etch)

FT grain age (Ma)

30 50 70 300 50070010 1000

1

2

3

4

5

6

7

8

9

10

Pro

ba

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en

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z=

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Upper Cretaceous Fort Crittenden Formation, Station 13 990628-1 (Axioskop, 010419-010502) >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.925E+05 RELATIVE ERROR (%): 1.83 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 1 1.73E+07 ( 96) 1.05E+07 ( 58) 9 435 115 84.7 60.6 119.6 2 1.89E+07 ( 70) 1.68E+07 ( 62) 6 698 178 58.0 40.6 83.0 3 1.79E+07 ( 66) 1.62E+07 ( 60) 6 675 175 56.5 39.2 81.5 4 2.07E+07 ( 115) 5.95E+06 ( 33) 9 248 86 176.7 119.8 268.2 5 1.23E+07 ( 228) 1.42E+07 ( 262) 30 590 76 44.7 37.1 53.8 6 1.78E+07 ( 197) 9.29E+06 ( 103) 18 386 77 97.5 76.4 124.2 7 2.31E+07 ( 142) 9.42E+06 ( 58) 10 392 103 124.9 91.6 172.6 8 1.41E+07 ( 61) 7.65E+06 ( 33) 7 318 111 94.5 61.1 148.9 9 9.44E+06 ( 93) 9.84E+06 ( 97) 16 409 84 49.0 36.8 65.4 10 1.43E+07 ( 88) 1.19E+07 ( 73) 10 493 116 61.9 44.8 85.6 11 4.09E+07 ( 151) 1.19E+07 ( 44) 6 495 150 174.2 124.3 249.3 12 1.58E+07 ( 117) 1.08E+07 ( 80) 12 450 102 74.6 55.9 99.4 13 1.68E+07 ( 124) 1.15E+07 ( 85) 12 478 105 74.4 56.3 98.4 14 1.98E+07 ( 73) 9.20E+06 ( 34) 6 383 131 109.6 72.2 169.7 15 1.81E+07 ( 178) 1.22E+07 ( 120) 16 507 94 75.8 59.8 96.0 16 1.38E+07 ( 170) 5.28E+06 ( 65) 20 220 55 132.6 99.4 176.7 17 1.04E+07 ( 64) 1.54E+07 ( 95) 10 642 133 34.7 24.8 48.2 18 1.50E+07 ( 111) 1.43E+07 ( 106) 12 597 118 53.6 40.9 70.2 19 1.23E+07 ( 114) 1.14E+07 ( 105) 15 473 94 55.5 42.4 72.7 20 1.28E+07 ( 71) 1.52E+07 ( 84) 9 630 139 43.5 31.2 60.4 21 1.48E+07 ( 91) 8.77E+06 ( 54) 10 365 100 86.3 61.0 123.2 22 1.40E+07 ( 69) 7.51E+06 ( 37) 8 312 103 95.3 63.2 146.2 23 1.38E+07 ( 34) 1.34E+07 ( 33) 4 557 194 52.9 31.8 88.1 24 2.53E+07 ( 218) 1.17E+07 ( 101) 14 487 98 109.9 86.4 139.7 >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.914E+05 RELATIVE ERROR (%): 1.81 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 25 3.66E+07 ( 361) 3.65E+06 ( 36) 16 153 51 493.8 354.6 708.5 26 1.79E+07 ( 110) 1.69E+07 ( 104) 10 705 140 53.9 41.0 70.8 27 2.33E+07 ( 172) 1.45E+07 ( 107) 12 605 119 81.7 63.9 104.5 28 2.46E+07 ( 91) 1.24E+07 ( 46) 6 520 154 100.7 70.0 146.9 29 2.11E+07 ( 52) 8.93E+06 ( 22) 4 373 158 119.8 72.0 207.0 30 3.12E+07 ( 77) 1.30E+07 ( 32) 4 542 191 122.1 80.3 190.5 31 1.66E+07 ( 123) 8.79E+06 ( 65) 12 367 92 96.4 70.9 132.4 990628-1 (Axioskop, 010419-010502) Number of grains = 31 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 17 1.04E+07 ( 64) 1.54E+07 ( 95) 34.7 24.8 48.2 100.0 34.7 24.8 48.2

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20 1.28E+07 ( 71) 1.52E+07 ( 84) 43.5 31.2 60.4 32.0 38.7 30.8 48.7 5 1.23E+07 ( 228) 1.42E+07 ( 262) 44.7 37.1 53.8 37.8 42.3 36.4 49.1 9 9.44E+06 ( 93) 9.84E+06 ( 97) 49.0 36.8 65.4 41.8 43.5 38.0 49.9 23 1.38E+07 ( 34) 1.34E+07 ( 33) 52.9 31.8 88.1 48.9 44.1 38.6 50.4 18 1.50E+07 ( 111) 1.43E+07 ( 106) 53.6 40.9 70.2 39.1 45.6 40.3 51.6 26 1.79E+07 ( 110) 1.69E+07 ( 104) 53.9 41.0 70.8 36.5 46.7 41.6 52.5 19 1.23E+07 ( 114) 1.14E+07 ( 105) 55.5 42.4 72.7 33.0 47.8 42.8 53.4 3 1.79E+07 ( 66) 1.62E+07 ( 60) 56.5 39.2 81.5 35.5 48.4 43.4 53.9 2 1.89E+07 ( 70) 1.68E+07 ( 62) 58.0 40.6 83.0 36.2 49.0 44.1 54.4 10 1.43E+07 ( 88) 1.19E+07 ( 73) 61.9 44.8 85.6 29.2 49.8 45.0 55.2 13 1.68E+07 ( 124) 1.15E+07 ( 85) 74.4 56.3 98.4 5.0 51.7 46.8 57.0 12 1.58E+07 ( 117) 1.08E+07 ( 80) 74.6 55.9 99.4 1.1 53.2 48.3 58.5 15 1.81E+07 ( 178) 1.22E+07 ( 120) 75.8 59.8 96.0 0.1 55.2 50.3 60.5 27 2.33E+07 ( 172) 1.45E+07 ( 107) 81.7 63.9 104.5 0.0 57.1 52.2 62.5 1 1.73E+07 ( 96) 1.05E+07 ( 58) 84.7 60.6 119.6 0.0 58.2 53.2 63.6 21 1.48E+07 ( 91) 8.77E+06 ( 54) 86.3 61.0 123.2 0.0 59.1 54.2 64.6 8 1.41E+07 ( 61) 7.65E+06 ( 33) 94.5 61.1 148.9 0.0 59.9 54.9 65.3 22 1.40E+07 ( 69) 7.51E+06 ( 37) 95.3 63.2 146.2 0.0 60.7 55.6 66.2 31 1.66E+07 ( 123) 8.79E+06 ( 65) 96.4 70.9 132.4 0.0 62.0 56.9 67.6 6 1.78E+07 ( 197) 9.29E+06 ( 103) 97.5 76.4 124.2 0.0 64.1 58.9 69.7 28 2.46E+07 ( 91) 1.24E+07 ( 46) 100.7 70.0 146.9 0.0 65.0 59.8 70.6 14 1.98E+07 ( 73) 9.20E+06 ( 34) 109.6 72.2 169.7 0.0 65.8 60.6 71.4 24 2.53E+07 ( 218) 1.17E+07 ( 101) 109.9 86.4 139.7 0.0 68.0 62.7 73.8 29 2.11E+07 ( 52) 8.93E+06 ( 22) 119.8 72.0 207.0 0.0 68.6 63.3 74.4 30 3.12E+07 ( 77) 1.30E+07 ( 32) 122.1 80.3 190.5 0.0 69.4 64.1 75.3 7 2.31E+07 ( 142) 9.42E+06 ( 58) 124.9 91.6 172.6 0.0 71.0 65.5 76.9 16 1.38E+07 ( 170) 5.28E+06 ( 65) 132.6 99.4 176.7 0.0 72.8 67.3 78.8 11 4.09E+07 ( 151) 1.19E+07 ( 44) 174.2 124.3 249.3 0.0 74.9 69.2 81.0 4 2.07E+07 ( 115) 5.95E+06 ( 33) 176.7 119.8 268.2 0.0 76.4 70.7 82.6 25 3.66E+07 ( 361) 3.65E+06 ( 36) 493.8 354.6 708.5 0.0 83.2 77.0 89.9 POOL 1.78E+07( 3727) 1.10E+07( 2296) 0.0 83.2 77.0 89.9 MEAN URANIUM CONCENTRATION +/-2SE (ppm): 457.4, 25.4 POOLED AGE WITH 63% CONF. INTERVAL(Ma): 83.2, 80.0 -- 86.5 ( -3.2 +3.3) 95% CONF. INTERVAL(Ma): 77.0 -- 89.9 ( -6.2 +6.7) CHI^2 PROBABILITY: 0.0% CENTRAL AGE WITH 63% CONF. INTERVAL(Ma): 81.9, 75.0 -- 89.4 ( -6.9 +7.5) 95% CONF. INTERVAL(Ma): 68.9 -- 97.3 ( -13.0 +15.4) AGE DISPERSION (%): 43.8 CHI^2 AGE WITH 63% CONF. INTERVAL (Ma): 53.2, 50.6 -- 55.8 ( -2.6 +2.7) 95% CONF. INTERVAL (Ma): 48.3 -- 58.5 ( -4.9 +5.4) NUMBER AND PERCENTAGE OF GRAINS: 13, 42%

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Pro

ba

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z=

0.1

)990628-1

Upper Cretaceous Fort Crittenden FormationStation 13, Huachuca Mountains

n = 31 grains (24 from 15 h etch, 7 from 11 h etch)

FT grain age (Ma)

30 50 70 300 50070010 1000

1

2

3

4

5

6

7

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170

Lower Cretaceous Cintura Formation, Station 14 990628-2b/A (U16Z) & 990628-2b/a (U26Z) >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.903E+05 RELATIVE ERROR (%): 1.79 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 1 2.54E+07 ( 188) 1.08E+06 ( 8) 12 45 31 1083.7 571.4 2346.4 2 2.80E+07 ( 138) 1.62E+06 ( 8) 8 68 47 813.1 421.3 1809.1 3 3.98E+07 ( 245) 1.79E+06 ( 11) 10 75 44 1036.4 596.9 1979.4 4 2.29E+07 ( 141) 5.52E+06 ( 34) 10 231 79 208.2 143.3 311.5 5 2.52E+07 ( 217) 5.10E+06 ( 44) 14 214 65 247.0 179.0 348.7 6 3.23E+07 ( 199) 4.87E+06 ( 30) 10 204 74 329.5 226.1 497.8 7 1.91E+07 ( 106) 7.03E+06 ( 39) 9 295 94 137.3 94.7 203.5 8 2.11E+07 ( 156) 3.92E+06 ( 29) 12 164 61 268.5 181.5 412.0 9 2.62E+07 ( 194) 1.89E+06 ( 14) 12 79 42 666.2 399.5 1203.9 10 3.26E+07 ( 321) 4.06E+06 ( 40) 16 170 54 396.9 288.0 561.9 11 1.89E+07 ( 93) 8.12E+06 ( 40) 8 340 108 117.7 80.7 175.0 >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.892E+05 RELATIVE ERROR (%): 1.77 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 12 2.77E+07 ( 256) 1.30E+06 ( 12) 15 55 31 993.5 584.1 1844.9 13 3.04E+07 ( 375) 5.93E+06 ( 73) 20 249 59 255.2 198.3 327.8 14 2.31E+07 ( 171) 6.22E+06 ( 46) 12 262 77 186.4 134.5 263.7 >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.975E+05 RELATIVE ERROR (%): 1.51 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 15 1.59E+07 ( 343) 4.45E+06 ( 96) 35 182 37 183.9 146.2 231.1 16 2.37E+07 ( 204) 4.75E+06 ( 41) 14 194 61 255.1 183.0 364.7 17 2.33E+07 ( 287) 6.25E+06 ( 77) 20 256 59 191.5 148.6 246.4 18 2.26E+07 ( 279) 5.76E+06 ( 71) 20 236 56 201.6 155.2 261.6 19 2.13E+07 ( 328) 4.22E+06 ( 65) 25 173 43 257.6 197.4 335.6 990628-2b/A (U16Z) & 990628-2b/a (U26Z) >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.968E+05 RELATIVE ERROR (%): 1.49 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07

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------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 20 1.65E+07 ( 122) 4.73E+06 ( 35) 12 194 65 179.3 123.1 268.5 21 2.88E+07 ( 266) 2.71E+06 ( 25) 15 111 44 531.1 358.5 822.4 22 2.50E+07 ( 246) 5.28E+06 ( 52) 16 216 60 242.4 180.1 332.5 23 2.16E+07 ( 200) 1.62E+07 ( 150) 15 666 110 69.2 55.7 86.0 24 2.35E+07 ( 116) 5.88E+06 ( 29) 8 241 89 205.2 136.8 318.7 25 2.24E+07 ( 331) 9.13E+06 ( 135) 24 374 65 126.6 103.2 155.4 26 1.97E+07 ( 327) 3.97E+06 ( 66) 27 163 40 252.4 193.8 328.4 27 1.60E+07 ( 158) 8.93E+06 ( 88) 16 366 79 92.8 71.3 120.8 28 1.52E+07 ( 225) 4.40E+06 ( 65) 24 180 45 177.4 134.5 233.8 29 2.31E+07 ( 171) 5.82E+06 ( 43) 12 239 73 204.3 146.4 291.7 30 2.58E+07 ( 143) 4.87E+06 ( 27) 9 200 76 270.1 180.0 421.6 31 1.47E+07 ( 127) 5.91E+06 ( 51) 14 242 68 128.8 92.7 181.8 32 2.22E+07 ( 137) 9.58E+06 ( 59) 10 393 102 120.2 88.2 166.0 33 2.53E+07 ( 374) 4.40E+06 ( 65) 24 180 45 292.2 224.7 379.4 990628-2b/A (U16Z) & 990628-2b/a (U26Z) Number of grains = 33 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 23 2.16E+07 ( 200) 1.62E+07 ( 150) 69.2 55.7 86.0 100.0 69.2 55.6 86.1 27 1.60E+07 ( 158) 8.93E+06 ( 88) 92.8 71.3 120.8 8.4 78.1 65.7 92.9 11 1.89E+07 ( 93) 8.12E+06 ( 40) 117.7 80.7 175.0 2.9 84.0 71.6 98.5 32 2.22E+07 ( 137) 9.58E+06 ( 59) 120.2 88.2 166.0 0.9 90.3 78.1 104.4 25 2.24E+07 ( 331) 9.13E+06 ( 135) 126.6 103.2 155.4 0.1 100.8 89.0 114.2 31 1.47E+07 ( 127) 5.91E+06 ( 51) 128.8 92.7 181.8 0.1 103.6 91.9 116.7 7 1.91E+07 ( 106) 7.03E+06 ( 39) 137.3 94.7 203.5 0.0 106.0 94.4 119.0 28 1.52E+07 ( 225) 4.40E+06 ( 65) 177.4 134.5 233.8 0.0 113.5 101.7 126.7 20 1.65E+07 ( 122) 4.73E+06 ( 35) 179.3 123.1 268.5 0.0 117.1 105.1 130.3 15 1.59E+07 ( 343) 4.45E+06 ( 96) 183.9 146.2 231.1 0.0 125.6 113.5 139.0 14 2.31E+07 ( 171) 6.22E+06 ( 46) 186.4 134.5 263.7 0.0 129.2 117.0 142.7 17 2.33E+07 ( 287) 6.25E+06 ( 77) 191.5 148.6 246.4 0.0 134.8 122.5 148.3 18 2.26E+07 ( 279) 5.76E+06 ( 71) 201.6 155.2 261.6 0.0 139.9 127.4 153.5 29 2.31E+07 ( 171) 5.82E+06 ( 43) 204.3 146.4 291.7 0.0 142.7 130.2 156.3 24 2.35E+07 ( 116) 5.88E+06 ( 29) 205.2 136.8 318.7 0.0 144.5 131.9 158.2 4 2.29E+07 ( 141) 5.52E+06 ( 34) 208.2 143.3 311.5 0.0 146.6 134.0 160.3 22 2.50E+07 ( 246) 5.28E+06 ( 52) 242.4 180.1 332.5 0.0 151.1 138.4 165.0 5 2.52E+07 ( 217) 5.10E+06 ( 44) 247.0 179.0 348.7 0.0 154.9 142.0 169.0 26 1.97E+07 ( 327) 3.97E+06 ( 66) 252.4 193.8 328.4 0.0 160.3 147.2 174.6 16 2.37E+07 ( 204) 4.75E+06 ( 41) 255.1 183.0 364.7 0.0 163.4 150.2 177.8 13 3.04E+07 ( 375) 5.93E+06 ( 73) 255.2 198.3 327.8 0.0 168.7 155.2 183.2 19 2.13E+07 ( 328) 4.22E+06 ( 65) 257.6 197.4 335.6 0.0 172.9 159.3 187.6 8 2.11E+07 ( 156) 3.92E+06 ( 29) 268.5 181.5 412.0 0.0 174.9 161.2 189.7 30 2.58E+07 ( 143) 4.87E+06 ( 27) 270.1 180.0 421.6 0.0 176.7 163.0 191.5 33 2.53E+07 ( 374) 4.40E+06 ( 65) 292.2 224.7 379.4 0.0 181.7 167.8 196.8 6 3.23E+07 ( 199) 4.87E+06 ( 30) 329.5 226.1 497.8 0.0 184.7 170.6 199.9 10 3.26E+07 ( 321) 4.06E+06 ( 40) 396.9 288.0 561.9 0.0 190.3 175.9 205.8 21 2.88E+07 ( 266) 2.71E+06 ( 25) 531.1 358.5 822.4 0.0 195.7 181.0 211.6 9 2.62E+07 ( 194) 1.89E+06 ( 14) 666.2 399.5 1203.9 0.0 200.0 185.0 216.2 2 2.80E+07 ( 138) 1.62E+06 ( 8) 813.1 421.3 1809.1 0.0 203.3 188.1 219.7 12 2.77E+07 ( 256) 1.30E+06 ( 12) 993.5 584.1 1844.9 0.0 209.7 194.0 226.5 3 3.98E+07 ( 245) 1.79E+06 ( 11)1036.4 596.9 1979.4 0.0 215.7 199.7 233.0 1 2.54E+07 ( 188) 1.08E+06 ( 8)1083.7 571.4 2346.4 0.0 220.3 204.0 237.9 POOL 2.30E+07( 7184) 5.24E+06( 1641) 0.0 220.3 204.0 237.9 MEAN URANIUM CONCENTRATION +/-2SE (ppm): 219.8, 13.4

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POOLED AGE WITH 63% CONF. INTERVAL(Ma): 220.3, 211.8 -- 229.2 ( -8.5 +8.8) 95% CONF. INTERVAL(Ma): 204.0 -- 237.9 ( -16.3 +17.6) CHI^2 PROBABILITY: 0.0% CENTRAL AGE WITH 63% CONF. INTERVAL(Ma): 222.1, 200.1 -- 246.5 ( -22.0 +24.4) 95% CONF. INTERVAL(Ma): 180.9 -- 272.4 ( -41.1 +50.3) AGE DISPERSION (%): 56.3 CHI^2 AGE WITH 63% CONF. INTERVAL (Ma): 84.0, 77.4 -- 91.1 ( -6.6 +7.1) 95% CONF. INTERVAL (Ma): 71.6 -- 98.5 ( -12.4 +14.5) NUMBER AND PERCENTAGE OF GRAINS: 3, 9%

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z=

0.1

)

990628-2Lower Cretaceous Cintura Formation

Station 14, Huachuca Mountains

n = 33 grains (11 from 15 h etch, 3 from 11 h etch,

FT grain age (Ma)

30 50 70 300 500 70010 100 10000

1

2

3

4

5

6

5 from 13.5 h etch, 14 from 9.5 h etch)

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Upper Cretaceous Fort Crittenden Formation, Station 23 (bulk sample) 990722-2 (Axioskop, 010401-10) >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.881E+05 RELATIVE ERROR (%): 1.75 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 1 1.41E+07 ( 261) 4.60E+06 ( 85) 30 194 43 153.3 119.6 196.3 2 1.52E+07 ( 84) 3.79E+06 ( 21) 9 160 69 199.0 123.4 336.8 3 1.76E+07 ( 152) 1.36E+07 ( 117) 14 573 108 65.4 51.2 83.6 4 1.10E+07 ( 102) 4.55E+06 ( 42) 15 192 59 122.0 84.6 179.0 5 9.74E+06 ( 84) 1.01E+07 ( 87) 14 426 92 48.9 35.7 66.8 6 1.17E+07 ( 65) 8.30E+06 ( 46) 9 350 104 71.3 48.2 106.4 7 7.03E+06 ( 130) 3.68E+06 ( 68) 30 155 38 96.3 71.3 131.2 8 1.40E+07 ( 69) 7.10E+06 ( 35) 8 300 101 99.2 65.3 153.5 9 1.76E+07 ( 130) 1.01E+07 ( 75) 12 429 100 86.9 65.2 115.8 10 1.56E+07 ( 115) 9.47E+06 ( 70) 12 400 96 82.9 61.1 113.3 11 1.64E+07 ( 91) 5.59E+06 ( 31) 9 236 85 146.9 97.3 228.3 12 2.06E+07 ( 76) 1.03E+07 ( 38) 6 434 141 100.6 67.5 152.6 13 1.78E+07 ( 197) 1.11E+07 ( 123) 18 469 86 80.6 64.0 101.4 14 1.14E+07 ( 63) 8.12E+06 ( 45) 9 343 102 70.7 47.5 106.0 15 2.06E+07 ( 114) 7.22E+06 ( 40) 9 305 96 142.8 99.3 210.0 16 1.21E+07 ( 52) 1.41E+07 ( 61) 7 598 154 43.2 29.2 63.6 17 1.42E+07 ( 35) 1.26E+07 ( 31) 4 531 190 57.1 34.2 95.6 18 9.33E+06 ( 23) 5.68E+06 ( 14) 4 240 126 82.6 41.0 173.3 19 1.99E+07 ( 147) 9.74E+06 ( 72) 12 411 98 102.2 76.9 135.8 20 1.83E+07 ( 180) 7.71E+06 ( 76) 16 326 75 118.5 90.4 155.3 21 1.79E+07 ( 55) 1.01E+07 ( 31) 5 425 152 89.3 56.7 143.5 22 1.85E+07 ( 114) 9.42E+06 ( 58) 10 398 105 99.0 71.6 138.3 23 1.06E+07 ( 39) 8.39E+06 ( 31) 6 354 127 63.5 38.7 105.2 24 1.28E+07 ( 63) 4.67E+06 ( 23) 8 197 82 137.1 84.4 231.2 25 2.76E+07 ( 102) 1.33E+07 ( 49) 6 560 160 104.7 74.0 150.4 26 1.59E+07 ( 88) 1.05E+07 ( 58) 9 442 117 76.6 54.4 108.6 27 1.64E+07 ( 182) 1.23E+07 ( 136) 18 518 91 67.4 53.7 84.6 28 1.25E+07 ( 123) 3.65E+06 ( 36) 16 154 51 170.8 117.6 254.5 29 2.16E+07 ( 80) 1.06E+07 ( 39) 6 446 143 103.2 69.7 155.4 30 1.66E+07 ( 102) 1.06E+07 ( 65) 10 446 111 79.2 57.5 109.9 >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.871E+05 RELATIVE ERROR (%): 1.72 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 31 3.29E+07 ( 405) 4.38E+06 ( 54) 20 186 51 365.8 276.1 483.5 32 2.17E+07 ( 107) 1.56E+07 ( 77) 8 662 152 69.9 51.7 95.1 33 2.21E+07 ( 109) 2.35E+07 ( 116) 8 998 188 47.2 36.2 61.6 34 2.39E+07 ( 118) 1.54E+07 ( 76) 8 654 151 77.7 58.0 103.9 35 2.33E+07 ( 115) 1.42E+06 ( 7) 8 60 44 766.6 379.2 1830.5 990722-2 (Axioskop, 010401-10) ------ GRAIN AGES IN ORIGINAL ORDER ------

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Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 36 1.62E+07 ( 199) 1.06E+07 ( 131) 20 451 80 76.2 60.8 95.5 37 2.39E+07 ( 177) 1.19E+07 ( 88) 12 505 109 100.5 77.5 130.2 38 2.60E+07 ( 401) 1.09E+07 ( 168) 25 462 73 119.4 99.1 143.9 39 1.98E+07 ( 122) 8.44E+06 ( 52) 10 358 100 117.5 84.5 165.8 40 2.01E+07 ( 198) 1.16E+07 ( 114) 16 490 93 87.0 68.8 110.0 41 1.70E+07 ( 262) 1.45E+07 ( 223) 25 614 85 59.1 49.1 71.2 42 2.65E+07 ( 98) 1.03E+07 ( 38) 6 436 141 128.9 88.2 192.7 43 2.15E+07 ( 106) 6.70E+06 ( 33) 8 284 99 160.1 108.0 244.0 44 1.84E+07 ( 170) 1.60E+07 ( 148) 15 679 114 57.7 46.0 72.4 45 1.93E+07 ( 143) 7.71E+06 ( 57) 12 327 87 125.6 92.0 173.8 46 2.11E+07 ( 156) 1.01E+07 ( 75) 12 430 100 103.8 78.6 137.1 47 2.30E+07 ( 298) 1.12E+07 ( 145) 21 475 80 102.9 83.9 126.2 48 2.00E+07 ( 148) 9.06E+06 ( 67) 12 384 94 110.1 82.3 147.2 49 2.94E+07 ( 217) 9.88E+06 ( 73) 12 419 99 147.8 113.1 193.0 50 2.52E+07 ( 186) 1.49E+07 ( 110) 12 631 122 84.7 66.6 107.7 51 2.71E+07 ( 100) 8.93E+06 ( 33) 6 378 131 151.1 101.6 231.0 52 2.44E+07 ( 135) 1.73E+07 ( 96) 9 734 152 70.5 54.0 91.9 53 1.16E+07 ( 43) 4.33E+06 ( 16) 6 184 91 133.8 74.6 254.0 54 3.23E+07 ( 179) 1.71E+07 ( 95) 9 726 151 94.2 73.2 121.3 55 3.50E+07 ( 194) 9.92E+06 ( 55) 9 421 114 175.8 130.2 241.5 56 2.44E+07 ( 240) 1.40E+07 ( 138) 16 594 103 87.2 70.3 108.1 57 2.95E+07 ( 109) 7.85E+06 ( 29) 6 333 123 186.8 124.0 291.2 58 2.64E+07 ( 195) 1.49E+06 ( 11) 12 63 37 829.4 472.4 1610.5 59 2.23E+07 ( 165) 1.04E+07 ( 77) 12 442 101 106.9 81.3 140.5 60 2.76E+07 ( 102) 1.70E+07 ( 63) 6 723 183 81.4 58.9 113.3 990722-2 (Axioskop, 010401-10) Number of grains = 60 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 16 1.21E+07 ( 52) 1.41E+07 ( 61) 43.2 29.2 63.6 100.0 43.2 29.2 63.6 33 2.21E+07 ( 109) 2.35E+07 ( 116) 47.2 36.2 61.6 68.4 45.8 36.8 57.1 5 9.74E+06 ( 84) 1.01E+07 ( 87) 48.9 35.7 66.8 87.2 46.8 39.0 56.2 17 1.42E+07 ( 35) 1.26E+07 ( 31) 57.1 34.2 95.6 83.9 47.9 40.3 56.9 44 1.84E+07 ( 170) 1.60E+07 ( 148) 57.7 46.0 72.4 61.6 51.3 44.5 59.1 41 1.70E+07 ( 262) 1.45E+07 ( 223) 59.1 49.1 71.2 50.8 53.9 47.9 60.7 23 1.06E+07 ( 39) 8.39E+06 ( 31) 63.5 38.7 105.2 57.7 54.4 48.3 61.1 3 1.76E+07 ( 152) 1.36E+07 ( 117) 65.4 51.2 83.6 45.4 56.0 50.2 62.5 27 1.64E+07 ( 182) 1.23E+07 ( 136) 67.4 53.7 84.6 33.0 57.6 52.0 63.9 32 2.17E+07 ( 107) 1.56E+07 ( 77) 69.9 51.7 95.1 29.5 58.6 53.0 64.7 52 2.44E+07 ( 135) 1.73E+07 ( 96) 70.5 54.0 91.9 24.8 59.6 54.1 65.7 14 1.14E+07 ( 63) 8.12E+06 ( 45) 70.7 47.5 106.0 27.2 60.0 54.6 66.1 6 1.17E+07 ( 65) 8.30E+06 ( 46) 71.3 48.2 106.4 29.3 60.5 55.0 66.5 36 1.62E+07 ( 199) 1.06E+07 ( 131) 76.2 60.8 95.5 15.4 62.0 56.6 67.9 26 1.59E+07 ( 88) 1.05E+07 ( 58) 76.6 54.4 108.6 14.3 62.6 57.3 68.5 34 2.39E+07 ( 118) 1.54E+07 ( 76) 77.7 58.0 103.9 11.3 63.4 58.1 69.3 30 1.66E+07 ( 102) 1.06E+07 ( 65) 79.2 57.5 109.9 9.5 64.1 58.8 69.9 13 1.78E+07 ( 197) 1.11E+07 ( 123) 80.6 64.0 101.4 5.0 65.3 60.0 71.1 60 2.76E+07 ( 102) 1.70E+07 ( 63) 81.4 58.9 113.3 4.3 65.9 60.6 71.7 18 9.33E+06 ( 23) 5.68E+06 ( 14) 82.6 41.0 173.3 5.2 66.1 60.8 71.8 10 1.56E+07 ( 115) 9.47E+06 ( 70) 82.9 61.1 113.3 4.2 66.7 61.4 72.5 50 2.52E+07 ( 186) 1.49E+07 ( 110) 84.7 66.6 107.7 2.1 67.8 62.5 73.5 9 1.76E+07 ( 130) 1.01E+07 ( 75) 86.9 65.2 115.8 1.3 68.5 63.2 74.2 40 2.01E+07 ( 198) 1.16E+07 ( 114) 87.0 68.8 110.0 0.6 69.5 64.2 75.2 56 2.44E+07 ( 240) 1.40E+07 ( 138) 87.2 70.3 108.1 0.3 70.6 65.3 76.3 21 1.79E+07 ( 55) 1.01E+07 ( 31) 89.3 56.7 143.5 0.3 70.9 65.6 76.6 54 3.23E+07 ( 179) 1.71E+07 ( 95) 94.2 73.2 121.3 0.1 71.8 66.5 77.6

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7 7.03E+06 ( 130) 3.68E+06 ( 68) 96.3 71.3 131.2 0.0 72.5 67.2 78.3 22 1.85E+07 ( 114) 9.42E+06 ( 58) 99.0 71.6 138.3 0.0 73.1 67.8 78.9 8 1.40E+07 ( 69) 7.10E+06 ( 35) 99.2 65.3 153.5 0.0 73.5 68.2 79.3 37 2.39E+07 ( 177) 1.19E+07 ( 88) 100.5 77.5 130.2 0.0 74.4 69.1 80.2 12 2.06E+07 ( 76) 1.03E+07 ( 38) 100.6 67.5 152.6 0.0 74.8 69.4 80.6 19 1.99E+07 ( 147) 9.74E+06 ( 72) 102.2 76.9 135.8 0.0 75.5 70.2 81.3 47 2.30E+07 ( 298) 1.12E+07 ( 145) 102.9 83.9 126.2 0.0 76.9 71.5 82.8 29 2.16E+07 ( 80) 1.06E+07 ( 39) 103.2 69.7 155.4 0.0 77.3 71.9 83.1 46 2.11E+07 ( 156) 1.01E+07 ( 75) 103.8 78.6 137.1 0.0 78.0 72.5 83.8 25 2.76E+07 ( 102) 1.33E+07 ( 49) 104.7 74.0 150.4 0.0 78.4 73.0 84.3 990722-2 (Axioskop, 010401-10) Number of grains = 60 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 59 2.23E+07 ( 165) 1.04E+07 ( 77) 106.9 81.3 140.5 0.0 79.1 73.7 85.0 48 2.00E+07 ( 148) 9.06E+06 ( 67) 110.1 82.3 147.2 0.0 79.8 74.3 85.7 39 1.98E+07 ( 122) 8.44E+06 ( 52) 117.5 84.5 165.8 0.0 80.4 74.9 86.3 20 1.83E+07 ( 180) 7.71E+06 ( 76) 118.5 90.4 155.3 0.0 81.3 75.8 87.3 38 2.60E+07 ( 401) 1.09E+07 ( 168) 119.4 99.1 143.9 0.0 83.2 77.5 89.2 4 1.10E+07 ( 102) 4.55E+06 ( 42) 122.0 84.6 179.0 0.0 83.6 78.0 89.7 45 1.93E+07 ( 143) 7.71E+06 ( 57) 125.6 92.0 173.8 0.0 84.3 78.6 90.4 42 2.65E+07 ( 98) 1.03E+07 ( 38) 128.9 88.2 192.7 0.0 84.8 79.1 90.9 53 1.16E+07 ( 43) 4.33E+06 ( 16) 133.8 74.6 254.0 0.0 85.0 79.3 91.1 24 1.28E+07 ( 63) 4.67E+06 ( 23) 137.1 84.4 231.2 0.0 85.3 79.6 91.5 15 2.06E+07 ( 114) 7.22E+06 ( 40) 142.8 99.3 210.0 0.0 86.0 80.2 92.1 11 1.64E+07 ( 91) 5.59E+06 ( 31) 146.9 97.3 228.3 0.0 86.5 80.7 92.6 49 2.94E+07 ( 217) 9.88E+06 ( 73) 147.8 113.1 193.0 0.0 87.7 81.9 93.9 51 2.71E+07 ( 100) 8.93E+06 ( 33) 151.1 101.6 231.0 0.0 88.2 82.4 94.5 1 1.41E+07 ( 261) 4.60E+06 ( 85) 153.3 119.6 196.3 0.0 89.7 83.7 96.0 43 2.15E+07 ( 106) 6.70E+06 ( 33) 160.1 108.0 244.0 0.0 90.3 84.3 96.6 28 1.25E+07 ( 123) 3.65E+06 ( 36) 170.8 117.6 254.5 0.0 91.0 85.0 97.4 55 3.50E+07 ( 194) 9.92E+06 ( 55) 175.8 130.2 241.5 0.0 92.2 86.1 98.6 57 2.95E+07 ( 109) 7.85E+06 ( 29) 186.8 124.0 291.2 0.0 92.8 86.8 99.3 2 1.52E+07 ( 84) 3.79E+06 ( 21) 199.0 123.4 336.8 0.0 93.4 87.3 99.9 31 3.29E+07 ( 405) 4.38E+06 ( 54) 365.8 276.1 483.5 0.0 97.1 90.7 103.8 35 2.33E+07 ( 115) 1.42E+06 ( 7) 766.6 379.2 1830.5 0.0 98.3 91.9 105.1 58 2.64E+07 ( 195) 1.49E+06 ( 11) 829.4 472.4 1610.5 0.0 100.4 93.8 107.3 POOL 1.92E+07( 8315) 9.66E+06( 4177) 0.0 100.4 93.8 107.3 MEAN URANIUM CONCENTRATION +/-2SE (ppm): 408.0, 19.1 POOLED AGE WITH 63% CONF. INTERVAL(Ma): 100.4, 97.0 -- 103.9 ( -3.4 +3.5) 95% CONF. INTERVAL(Ma): 93.8 -- 107.3 ( -6.5 +7.0) CHI^2 PROBABILITY: 0.0% CENTRAL AGE WITH 63% CONF. INTERVAL(Ma): 100.6, 94.5 -- 107.2 ( -6.1 +6.5) 95% CONF. INTERVAL(Ma): 89.0 -- 113.9 ( -11.7 +13.2) AGE DISPERSION (%): 40.7 CHI^2 AGE WITH 63% CONF. INTERVAL (Ma): 68.5, 65.8 -- 71.4 ( -2.8 +2.9) 95% CONF. INTERVAL (Ma): 63.2 -- 74.2 ( -5.3 +5.7) NUMBER AND PERCENTAGE OF GRAINS: 23, 38%

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Upper Cretaceous Fort Crittenden Formation, Station 23 (pink/purple fraction) 990722-2p (BX60/Axioskop, 011115-011116 & 011125, p = d+L) >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 3.102E+05 RELATIVE ERROR (%): 2.11 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.700E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 1 1.71E+07 ( 103) 1.26E+07 ( 76) 9 494 115 73.7 54.2 100.6 2 2.91E+07 ( 117) 1.02E+07 ( 41) 6 400 125 153.9 107.4 225.2 3 2.45E+07 ( 148) 2.04E+07 ( 123) 9 800 148 65.3 51.1 83.4 4 1.41E+07 ( 330) 1.30E+07 ( 306) 35 512 62 58.6 49.7 69.2 5 2.57E+07 ( 138) 9.70E+06 ( 52) 8 381 106 143.3 103.7 201.2 6 2.70E+07 ( 163) 1.06E+07 ( 64) 9 416 105 137.7 102.6 186.9 7 2.59E+07 ( 278) 6.72E+06 ( 72) 16 264 63 206.5 158.9 268.0 8 2.90E+07 ( 291) 4.98E+06 ( 50) 15 195 56 310.0 230.3 425.8 9 2.60E+07 ( 174) 9.85E+06 ( 66) 10 386 96 141.6 106.4 188.4 10 2.97E+07 ( 239) 1.19E+07 ( 96) 12 468 97 134.1 105.3 170.7 11 1.95E+07 ( 157) 7.46E+06 ( 60) 12 293 76 141.4 104.5 193.8 >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 3.083E+05 RELATIVE ERROR (%): 2.03 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 12 3.03E+07 ( 112) 1.14E+07 ( 42) 6 449 139 143.1 99.9 209.1 13 2.52E+07 ( 248) 9.03E+06 ( 89) 16 356 77 149.0 116.4 190.5 14 3.52E+07 ( 390) 9.92E+06 ( 110) 18 392 76 189.1 152.3 234.7 15 4.25E+07 ( 157) 4.33E+06 ( 16) 6 171 84 508.2 310.3 893.3 990722-2p (BX60/Axioskop, 011115-011116 & 011125, p = d+L) Number of grains = 15 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 4 1.41E+07 ( 330) 1.30E+07 ( 306) 58.6 49.7 69.2 100.0 58.6 49.7 69.2 3 2.45E+07 ( 148) 2.04E+07 ( 123) 65.3 51.1 83.4 45.2 60.6 52.5 69.9 1 1.71E+07 ( 103) 1.26E+07 ( 76) 73.7 54.2 100.6 37.2 62.6 54.8 71.5 10 2.97E+07 ( 239) 1.19E+07 ( 96) 134.1 105.3 170.7 0.0 74.2 65.7 83.7 6 2.70E+07 ( 163) 1.06E+07 ( 64) 137.7 102.6 186.9 0.0 80.3 71.6 90.1 11 1.95E+07 ( 157) 7.46E+06 ( 60) 141.4 104.5 193.8 0.0 85.4 76.5 95.4 9 2.60E+07 ( 174) 9.85E+06 ( 66) 141.6 106.4 188.4 0.0 90.2 81.1 100.3 12 3.03E+07 ( 112) 1.14E+07 ( 42) 143.1 99.9 209.1 0.0 92.9 83.7 103.1 5 2.57E+07 ( 138) 9.70E+06 ( 52) 143.3 103.7 201.2 0.0 95.9 86.6 106.2 13 2.52E+07 ( 248) 9.03E+06 ( 89) 149.0 116.4 190.5 0.0 100.9 91.4 111.3 2 2.91E+07 ( 117) 1.02E+07 ( 41) 153.9 107.4 225.2 0.0 103.0 93.5 113.5 14 3.52E+07 ( 390) 9.92E+06 ( 110) 189.1 152.3 234.7 0.0 111.6 101.7 122.5 7 2.59E+07 ( 278) 6.72E+06 ( 72) 206.5 158.9 268.0 0.0 117.4 107.2 128.6 8 2.90E+07 ( 291) 4.98E+06 ( 50) 310.0 230.3 425.8 0.0 125.3 114.6 137.0 15 4.25E+07 ( 157) 4.33E+06 ( 16) 508.2 310.3 893.3 0.0 130.4 119.3 142.4 POOL 2.48E+07( 3045) 1.03E+07( 1265) 0.0 130.4 119.3 142.4

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MEAN URANIUM CONCENTRATION +/-2SE (ppm): 404.0, 28.4 POOLED AGE WITH 63% CONF. INTERVAL(Ma): 130.4, 124.6 -- 136.4 ( -5.8 +6.0) 95% CONF. INTERVAL(Ma): 119.3 -- 142.4 ( -11.1 +12.1) CHI^2 PROBABILITY: 0.0% CENTRAL AGE WITH 63% CONF. INTERVAL(Ma): 138.0, 120.9 -- 157.6 ( -17.1 +19.6) 95% CONF. INTERVAL(Ma): 106.4 -- 178.9 ( -31.6 +40.9) AGE DISPERSION (%): 48.6 CHI^2 AGE WITH 63% CONF. INTERVAL (Ma): 62.6, 58.5 -- 67.0 ( -4.1 +4.4) 95% CONF. INTERVAL (Ma): 54.8 -- 71.5 ( -7.8 +8.9) NUMBER AND PERCENTAGE OF GRAINS: 3, 20%

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Upper Cretaceous Fort Crittenden Formation, Station 23 (colorless fraction) 990722-2c (Axioskop, 011209-011214) >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 3.047E+05 RELATIVE ERROR (%): 1.89 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 1 1.96E+07 ( 242) 1.28E+07 ( 158) 20 512 84 81.5 66.3 100.3 2 1.77E+07 ( 131) 1.77E+07 ( 131) 12 708 126 53.3 41.6 68.3 3 2.11E+07 ( 156) 5.95E+06 ( 44) 12 238 72 187.3 133.9 267.6 4 2.08E+07 ( 128) 1.20E+07 ( 74) 10 480 113 91.7 68.7 122.4 5 2.26E+07 ( 167) 1.12E+07 ( 83) 12 448 100 106.6 81.6 139.2 6 2.37E+07 ( 175) 1.18E+07 ( 87) 12 470 102 106.6 82.1 138.4 7 3.06E+07 ( 151) 2.11E+07 ( 104) 8 843 168 77.2 59.9 99.6 8 2.65E+07 ( 147) 1.57E+07 ( 87) 9 627 136 89.7 68.5 117.3 9 2.64E+07 ( 325) 1.82E+07 ( 224) 20 726 101 77.3 64.7 92.5 10 2.67E+07 ( 148) 1.23E+07 ( 68) 9 490 120 115.1 86.1 153.7 11 2.33E+07 ( 86) 1.65E+07 ( 61) 6 659 170 75.3 53.6 106.3 12 2.08E+07 ( 192) 1.42E+07 ( 131) 15 566 101 78.0 62.1 98.0 13 3.04E+07 ( 225) 1.52E+07 ( 112) 12 605 116 106.6 84.6 134.4 14 3.15E+07 ( 155) 1.44E+07 ( 71) 8 575 138 115.5 87.0 153.3 15 2.66E+07 ( 131) 1.10E+07 ( 54) 8 438 120 128.8 93.4 180.3 16 2.49E+07 ( 184) 1.96E+07 ( 145) 12 783 133 67.6 54.1 84.6 17 2.65E+07 ( 196) 1.34E+07 ( 99) 12 535 109 105.0 82.1 134.3 18 2.15E+07 ( 212) 1.50E+07 ( 148) 16 600 101 76.3 61.4 94.7 19 2.51E+07 ( 247) 1.63E+07 ( 161) 16 652 106 81.7 66.5 100.3 >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 3.065E+05 RELATIVE ERROR (%): 1.96 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 20 3.08E+07 ( 171) 1.57E+07 ( 87) 9 623 135 104.8 80.6 136.2 21 1.86E+07 ( 206) 6.67E+06 ( 74) 18 265 62 147.8 113.0 193.2 22 2.44E+07 ( 135) 1.48E+07 ( 82) 9 587 131 87.9 66.5 116.0 23 3.27E+07 ( 242) 1.37E+07 ( 101) 12 543 110 127.6 100.7 161.7 24 3.99E+07 ( 516) 3.94E+06 ( 51) 21 157 44 520.1 392.2 687.7 25 1.90E+07 ( 187) 1.36E+07 ( 134) 16 540 95 74.7 59.5 93.9 26 3.41E+07 ( 294) 1.61E+07 ( 139) 14 640 111 113.0 91.7 139.1 27 2.74E+07 ( 541) 1.11E+07 ( 218) 32 439 62 132.5 112.2 156.4 28 4.98E+07 ( 184) 2.00E+07 ( 74) 6 795 187 132.2 100.6 173.5 29 2.85E+07 ( 158) 1.37E+07 ( 76) 9 544 126 110.7 83.9 146.0 30 3.02E+07 ( 149) 1.93E+07 ( 95) 8 765 160 83.8 64.5 108.9 990722-2c (Axioskop, 011209-011214) Number of grains = 30 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 2 1.77E+07 ( 131) 1.77E+07 ( 131) 53.3 41.6 68.3 100.0 53.3 41.6 68.3 16 2.49E+07 ( 184) 1.96E+07 ( 145) 67.6 54.1 84.6 15.1 60.9 51.4 72.3

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25 1.90E+07 ( 187) 1.36E+07 ( 134) 74.7 59.5 93.9 11.9 65.5 56.8 75.5 11 2.33E+07 ( 86) 1.65E+07 ( 61) 75.3 53.6 106.3 18.2 66.8 58.4 76.3 18 2.15E+07 ( 212) 1.50E+07 ( 148) 76.3 61.4 94.7 19.3 69.1 61.3 77.9 7 3.06E+07 ( 151) 2.11E+07 ( 104) 77.2 59.9 99.6 23.6 70.3 62.9 78.7 9 2.64E+07 ( 325) 1.82E+07 ( 224) 77.3 64.7 92.5 25.6 72.0 65.1 79.7 12 2.08E+07 ( 192) 1.42E+07 ( 131) 78.0 62.1 98.0 31.1 72.8 66.0 80.2 1 1.96E+07 ( 242) 1.28E+07 ( 158) 81.5 66.3 100.3 31.0 73.9 67.4 81.1 19 2.51E+07 ( 247) 1.63E+07 ( 161) 81.7 66.5 100.3 32.5 74.9 68.5 81.9 30 3.02E+07 ( 149) 1.93E+07 ( 95) 83.8 64.5 108.9 35.0 75.5 69.1 82.4 22 2.44E+07 ( 135) 1.48E+07 ( 82) 87.9 66.5 116.0 34.0 76.1 69.8 83.0 8 2.65E+07 ( 147) 1.57E+07 ( 87) 89.7 68.5 117.3 31.1 76.9 70.6 83.7 4 2.08E+07 ( 128) 1.20E+07 ( 74) 91.7 68.7 122.4 28.4 77.5 71.3 84.3 20 3.08E+07 ( 171) 1.57E+07 ( 87) 104.8 80.6 136.2 11.1 78.9 72.6 85.7 17 2.65E+07 ( 196) 1.34E+07 ( 99) 105.0 82.1 134.3 3.7 80.2 73.9 87.0 13 3.04E+07 ( 225) 1.52E+07 ( 112) 106.6 84.6 134.4 1.0 81.7 75.4 88.5 6 2.37E+07 ( 175) 1.18E+07 ( 87) 106.6 82.1 138.4 0.4 82.8 76.4 89.6 5 2.26E+07 ( 167) 1.12E+07 ( 83) 106.6 81.6 139.2 0.2 83.7 77.4 90.5 29 2.85E+07 ( 158) 1.37E+07 ( 76) 110.7 83.9 146.0 0.1 84.6 78.3 91.5 26 3.41E+07 ( 294) 1.61E+07 ( 139) 113.0 91.7 139.1 0.0 86.3 79.9 93.1 10 2.67E+07 ( 148) 1.23E+07 ( 68) 115.1 86.1 153.7 0.0 87.1 80.7 94.0 14 3.15E+07 ( 155) 1.44E+07 ( 71) 115.5 87.0 153.3 0.0 87.9 81.5 94.8 23 3.27E+07 ( 242) 1.37E+07 ( 101) 127.6 100.7 161.7 0.0 89.4 83.0 96.4 15 2.66E+07 ( 131) 1.10E+07 ( 54) 128.8 93.4 180.3 0.0 90.2 83.7 97.2 28 4.98E+07 ( 184) 2.00E+07 ( 74) 132.2 100.6 173.5 0.0 91.3 84.8 98.4 27 2.74E+07 ( 541) 1.11E+07 ( 218) 132.5 112.2 156.4 0.0 94.3 87.7 101.5 21 1.86E+07 ( 206) 6.67E+06 ( 74) 147.8 113.0 193.2 0.0 95.7 89.0 102.8 3 2.11E+07 ( 156) 5.95E+06 ( 44) 187.3 133.9 267.6 0.0 97.0 90.2 104.2 24 3.99E+07 ( 516) 3.94E+06 ( 51) 520.1 392.2 687.7 0.0 104.0 96.8 111.8 POOL 2.62E+07( 6181) 1.34E+07( 3166) 0.0 104.0 96.8 111.8 MEAN URANIUM CONCENTRATION +/-2SE (ppm): 536.0, 27.8 POOLED AGE WITH 63% CONF. INTERVAL(Ma): 104.0, 100.3 -- 107.9 ( -3.7 +3.9) 95% CONF. INTERVAL(Ma): 96.8 -- 111.8 ( -7.2 +7.7) CHI^2 PROBABILITY: 0.0% CENTRAL AGE WITH 63% CONF. INTERVAL(Ma): 101.2, 94.4 -- 108.4 ( -6.7 +7.2) 95% CONF. INTERVAL(Ma): 88.4 -- 115.8 ( -12.8 +14.6) AGE DISPERSION (%): 32.0 CHI^2 AGE WITH 63% CONF. INTERVAL (Ma): 80.2, 77.0 -- 83.6 ( -3.3 +3.4) 95% CONF. INTERVAL (Ma): 73.9 -- 87.0 ( -6.3 +6.8) NUMBER AND PERCENTAGE OF GRAINS: 16, 53%

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Upper Cretaceous Fort Crittenden Formation, Station 23 (honey fraction) 990722-2h (Axioskop, 011214-011219) >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 3.010E+05 RELATIVE ERROR (%): 1.76 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 1 2.29E+07 ( 254) 1.52E+07 ( 168) 18 613 97 79.5 65.0 97.3 2 3.04E+07 ( 281) 1.19E+07 ( 110) 15 481 93 133.6 106.7 167.3 3 2.04E+07 ( 151) 1.75E+07 ( 129) 12 706 126 61.6 48.5 78.3 4 2.52E+07 ( 186) 1.22E+07 ( 90) 12 492 105 108.2 83.8 139.7 5 2.27E+07 ( 140) 7.63E+06 ( 47) 10 308 90 155.9 111.7 221.6 6 2.08E+07 ( 462) 8.52E+06 ( 189) 36 345 52 128.2 107.4 152.9 7 1.92E+07 ( 142) 1.65E+07 ( 122) 12 667 123 61.3 47.9 78.4 8 2.23E+07 ( 206) 1.68E+07 ( 155) 15 678 111 70.0 56.4 86.7 9 1.66E+07 ( 123) 1.37E+07 ( 101) 12 552 111 64.0 49.0 83.6 10 2.08E+07 ( 231) 1.51E+07 ( 167) 18 609 97 72.8 59.3 89.4 11 1.67E+07 ( 278) 1.23E+07 ( 204) 27 496 72 71.8 59.5 86.6 12 1.73E+07 ( 256) 1.29E+07 ( 190) 24 520 77 71.0 58.4 86.2 13 2.41E+07 ( 238) 1.22E+07 ( 120) 16 492 91 104.0 83.1 130.2 14 2.30E+07 ( 170) 2.08E+07 ( 154) 12 842 139 58.2 46.5 72.8 15 1.90E+07 ( 176) 1.16E+07 ( 107) 15 468 92 86.4 67.6 110.3 16 2.48E+07 ( 244) 1.12E+07 ( 110) 16 451 87 116.2 92.3 146.2 >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 3.028E+05 RELATIVE ERROR (%): 1.83 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 17 2.52E+07 ( 93) 1.22E+07 ( 45) 6 489 146 109.2 75.9 159.6 18 2.00E+07 ( 197) 1.88E+07 ( 185) 16 754 114 56.5 45.9 69.5 19 2.96E+07 ( 219) 1.85E+07 ( 137) 12 745 130 84.5 67.9 105.2 20 2.74E+07 ( 270) 1.40E+07 ( 138) 16 563 98 103.3 83.6 127.5 21 2.69E+07 ( 199) 1.20E+07 ( 89) 12 484 104 117.7 91.3 151.6 22 2.40E+07 ( 237) 1.72E+07 ( 170) 16 693 109 73.8 60.2 90.5 990722-2h (Axioskop, 011214-011219) Number of grains = 22 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 18 2.00E+07 ( 197) 1.88E+07 ( 185) 56.5 45.9 69.5 100.0 56.5 45.9 69.5 14 2.30E+07 ( 170) 2.08E+07 ( 154) 58.2 46.5 72.8 84.3 57.3 49.0 67.1 7 1.92E+07 ( 142) 1.65E+07 ( 122) 61.3 47.9 78.4 87.4 58.4 50.9 67.0 3 2.04E+07 ( 151) 1.75E+07 ( 129) 61.6 48.5 78.3 93.2 59.2 52.3 67.0 9 1.66E+07 ( 123) 1.37E+07 ( 101) 64.0 49.0 83.6 94.3 59.9 53.3 67.3 8 2.23E+07 ( 206) 1.68E+07 ( 155) 70.0 56.4 86.7 77.0 61.8 55.5 68.8 12 1.73E+07 ( 256) 1.29E+07 ( 190) 71.0 58.4 86.2 63.7 63.5 57.5 70.2 11 1.67E+07 ( 278) 1.23E+07 ( 204) 71.8 59.5 86.6 56.1 64.9 59.1 71.3 10 2.08E+07 ( 231) 1.51E+07 ( 167) 72.8 59.3 89.4 53.6 65.9 60.2 72.1 22 2.40E+07 ( 237) 1.72E+07 ( 170) 73.8 60.2 90.5 51.2 66.7 61.2 72.8

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1 2.29E+07 ( 254) 1.52E+07 ( 168) 79.5 65.0 97.3 34.6 68.0 62.5 74.0 19 2.96E+07 ( 219) 1.85E+07 ( 137) 84.5 67.9 105.2 18.3 69.2 63.8 75.1 15 1.90E+07 ( 176) 1.16E+07 ( 107) 86.4 67.6 110.3 10.8 70.2 64.7 76.1 20 2.74E+07 ( 270) 1.40E+07 ( 138) 103.3 83.6 127.5 0.3 72.3 66.8 78.3 13 2.41E+07 ( 238) 1.22E+07 ( 120) 104.0 83.1 130.2 0.0 74.1 68.5 80.1 4 2.52E+07 ( 186) 1.22E+07 ( 90) 108.2 83.8 139.7 0.0 75.4 69.8 81.4 17 2.52E+07 ( 93) 1.22E+07 ( 45) 109.2 75.9 159.6 0.0 76.0 70.4 82.1 16 2.48E+07 ( 244) 1.12E+07 ( 110) 116.2 92.3 146.2 0.0 77.8 72.2 84.0 21 2.69E+07 ( 199) 1.20E+07 ( 89) 117.7 91.3 151.6 0.0 79.2 73.5 85.4 6 2.08E+07 ( 462) 8.52E+06 ( 189) 128.2 107.4 152.9 0.0 82.6 76.8 88.9 2 3.04E+07 ( 281) 1.19E+07 ( 110) 133.6 106.7 167.3 0.0 84.6 78.6 91.0 5 2.27E+07 ( 140) 7.63E+06 ( 47) 155.9 111.7 221.6 0.0 85.8 79.8 92.2 POOL 2.22E+07( 4753) 1.36E+07( 2922) 0.0 85.8 79.8 92.2 MEAN URANIUM CONCENTRATION +/-2SE (ppm): 551.2, 28.1 POOLED AGE WITH 63% CONF. INTERVAL(Ma): 85.8, 82.6 -- 89.0 ( -3.1 +3.2) 95% CONF. INTERVAL(Ma): 79.8 -- 92.2 ( -6.0 +6.5) CHI^2 PROBABILITY: 0.0% CENTRAL AGE WITH 63% CONF. INTERVAL(Ma): 85.6, 80.1 -- 91.6 ( -5.5 +5.9) 95% CONF. INTERVAL(Ma): 75.1 -- 97.6 ( -10.5 +12.0) AGE DISPERSION (%): 26.1 CHI^2 AGE WITH 63% CONF. INTERVAL (Ma): 70.2, 67.3 -- 73.1 ( -2.8 +3.0) 95% CONF. INTERVAL (Ma): 64.7 -- 76.1 ( -5.4 +5.9) NUMBER AND PERCENTAGE OF GRAINS: 13, 59%

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183

Pro

ba

bili

ty d

en

sity (

%/∆

z=

0.1

)990722-2 composite

Upper Cretaceous Fort Crittenden FormationStation 23, Huachuca Mountains

n = 127 grains

FT grain age (Ma)

30 50 70 300 50070010 100 1000

0

2

4

6

8

10

12

14

16

18

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184

Middle Jurassic Temporal Formation, Station 33 990802-1 (Axioskop, 020121) >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.838E+05 RELATIVE ERROR (%): 1.67 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 1 1.37E+07 ( 254) 1.47E+07 ( 271) 30 629 79 46.7 39.0 55.8 2 1.73E+07 ( 192) 8.30E+06 ( 92) 18 356 75 103.1 80.1 132.6 3 3.12E+07 ( 308) 1.20E+07 ( 118) 16 513 96 128.8 103.7 160.0 4 2.24E+07 ( 414) 1.43E+07 ( 265) 30 615 78 77.6 65.9 91.3 5 2.04E+07 ( 151) 1.56E+07 ( 115) 12 667 126 65.1 50.9 83.4 6 2.30E+07 ( 255) 1.05E+07 ( 116) 18 449 84 108.7 86.8 135.9 7 2.36E+07 ( 349) 1.46E+07 ( 216) 24 627 88 80.2 67.2 95.7 8 2.09E+07 ( 387) 1.19E+07 ( 220) 30 511 71 87.3 73.4 103.8 9 1.68E+07 ( 186) 9.11E+06 ( 101) 18 391 79 91.1 71.2 116.5 10 1.99E+07 ( 196) 9.74E+06 ( 96) 16 418 86 100.9 78.7 129.3 11 2.06E+07 ( 407) 7.66E+06 ( 151) 32 328 54 133.1 109.8 161.3 12 2.37E+07 ( 146) 1.72E+07 ( 106) 10 738 145 68.3 52.9 88.0 13 2.00E+07 ( 492) 6.90E+06 ( 170) 40 296 46 142.9 119.2 171.1 14 2.48E+07 ( 275) 1.60E+07 ( 177) 18 685 105 77.1 63.4 93.7 15 1.96E+07 ( 242) 7.22E+06 ( 89) 20 310 66 134.0 104.7 171.3 16 1.09E+07 ( 188) 8.58E+06 ( 148) 28 368 62 63.1 50.6 78.7 17 1.89E+07 ( 291) 7.86E+06 ( 121) 25 337 62 118.8 95.6 147.5 18 1.54E+07 ( 426) 1.42E+07 ( 394) 45 610 65 53.8 46.5 62.4 19 2.01E+07 ( 496) 1.19E+07 ( 292) 40 508 62 84.3 72.3 98.3 20 2.51E+07 ( 494) 1.18E+07 ( 233) 32 507 68 105.0 89.2 123.7 21 2.17E+07 ( 534) 8.73E+06 ( 215) 40 374 52 122.9 104.1 145.0 22 2.13E+07 ( 368) 1.26E+07 ( 217) 28 540 75 84.1 70.6 100.3 23 1.80E+07 ( 222) 1.62E+07 ( 199) 20 693 101 55.5 45.5 67.6 24 2.55E+07 ( 251) 1.57E+07 ( 155) 16 674 110 80.3 65.3 98.7 25 1.90E+07 ( 234) 1.66E+07 ( 205) 20 714 102 56.8 46.7 68.9 26 2.55E+07 ( 439) 9.91E+06 ( 171) 28 425 66 126.9 105.6 152.4 27 2.69E+07 ( 332) 1.06E+07 ( 130) 20 452 81 126.1 102.4 155.2 990802-1 (Axioskop, 020121) Number of grains = 27 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 1 1.37E+07 ( 254) 1.47E+07 ( 271) 46.7 39.0 55.8 100.0 46.7 39.0 55.8 18 1.54E+07 ( 426) 1.42E+07 ( 394) 53.8 46.5 62.4 20.1 50.9 45.2 57.4 23 1.80E+07 ( 222) 1.62E+07 ( 199) 55.5 45.5 67.6 32.6 52.0 46.7 58.0 25 1.90E+07 ( 234) 1.66E+07 ( 205) 56.8 46.7 68.9 40.1 53.0 47.9 58.5 16 1.09E+07 ( 188) 8.58E+06 ( 148) 63.1 50.6 78.7 26.4 54.2 49.3 59.6 5 2.04E+07 ( 151) 1.56E+07 ( 115) 65.1 50.9 83.4 19.7 55.2 50.3 60.5 12 2.37E+07 ( 146) 1.72E+07 ( 106) 68.3 52.9 88.0 12.3 56.2 51.3 61.4 14 2.48E+07 ( 275) 1.60E+07 ( 177) 77.1 63.4 93.7 0.6 58.5 53.7 63.7 4 2.24E+07 ( 414) 1.43E+07 ( 265) 77.6 65.9 91.3 0.0 61.2 56.4 66.4 7 2.36E+07 ( 349) 1.46E+07 ( 216) 80.2 67.2 95.7 0.0 63.2 58.4 68.4 24 2.55E+07 ( 251) 1.57E+07 ( 155) 80.3 65.3 98.7 0.0 64.4 59.6 69.6 22 2.13E+07 ( 368) 1.26E+07 ( 217) 84.1 70.6 100.3 0.0 66.1 61.3 71.3 19 2.01E+07 ( 496) 1.19E+07 ( 292) 84.3 72.3 98.3 0.0 68.1 63.2 73.3 8 2.09E+07 ( 387) 1.19E+07 ( 220) 87.3 73.4 103.8 0.0 69.5 64.6 74.7 9 1.68E+07 ( 186) 9.11E+06 ( 101) 91.1 71.2 116.5 0.0 70.2 65.4 75.5

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185

10 1.99E+07 ( 196) 9.74E+06 ( 96) 100.9 78.7 129.3 0.0 71.2 66.3 76.4 2 1.73E+07 ( 192) 8.30E+06 ( 92) 103.1 80.1 132.6 0.0 72.1 67.2 77.4 20 2.51E+07 ( 494) 1.18E+07 ( 233) 105.0 89.2 123.7 0.0 74.3 69.3 79.7 6 2.30E+07 ( 255) 1.05E+07 ( 116) 108.7 86.8 135.9 0.0 75.4 70.4 80.8 17 1.89E+07 ( 291) 7.86E+06 ( 121) 118.8 95.6 147.5 0.0 76.8 71.7 82.3 21 2.17E+07 ( 534) 8.73E+06 ( 215) 122.9 104.1 145.0 0.0 79.4 74.2 84.9 27 2.69E+07 ( 332) 1.06E+07 ( 130) 126.1 102.4 155.2 0.0 80.9 75.6 86.5 26 2.55E+07 ( 439) 9.91E+06 ( 171) 126.9 105.6 152.4 0.0 82.7 77.4 88.5 3 3.12E+07 ( 308) 1.20E+07 ( 118) 128.8 103.7 160.0 0.0 84.0 78.6 89.8 11 2.06E+07 ( 407) 7.66E+06 ( 151) 133.1 109.8 161.3 0.0 85.7 80.2 91.5 15 1.96E+07 ( 242) 7.22E+06 ( 89) 134.0 104.7 171.3 0.0 86.6 81.1 92.5 13 2.00E+07 ( 492) 6.90E+06 ( 170) 142.9 119.2 171.1 0.0 88.6 83.0 94.6 POOL 2.05E+07( 8529) 1.15E+07( 4783) 0.0 88.6 83.0 94.6 MEAN URANIUM CONCENTRATION +/-2SE (ppm): 494.0, 21.8 POOLED AGE WITH 63% CONF. INTERVAL(Ma): 88.6, 85.7 -- 91.6 ( -2.9 +3.0) 95% CONF. INTERVAL(Ma): 83.0 -- 94.6 ( -5.6 +6.0) CHI^2 PROBABILITY: 0.0% CENTRAL AGE WITH 63% CONF. INTERVAL(Ma): 88.3, 82.5 -- 94.4 ( -5.7 +6.1) 95% CONF. INTERVAL(Ma): 77.4 -- 100.7 ( -10.9 +12.4) AGE DISPERSION (%): 30.3 CHI^2 AGE WITH 63% CONF. INTERVAL (Ma): 56.2, 53.6 -- 58.8 ( -2.5 +2.6) 95% CONF. INTERVAL (Ma): 51.3 -- 61.4 ( -4.8 +5.3) NUMBER AND PERCENTAGE OF GRAINS: 7, 26%

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186

Pro

babili

ty d

ensity (

%/∆

z=

0.1

)990802-1

Upper Jurassic Temporal FormationStation 33, Santa Rita Mountains

n = 27 grains (27 from 15 h etch)

FT grain age (Ma)

30 50 70 300 50010 1000

1

2

3

4

5

6

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Lower Cretaceous Turney Ranch Formation, Station 38 990803-3 (Axioskop, 011010-011121) >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.817E+05 RELATIVE ERROR (%): 1.63 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 1 2.16E+07 ( 80) 3.79E+06 ( 14) 6 164 86 275.3 157.6 521.5 2 1.94E+07 ( 334) 1.91E+06 ( 33) 28 83 29 482.2 341.4 703.9 3 1.99E+07 ( 147) 1.10E+07 ( 81) 12 473 106 89.0 67.7 117.1 4 1.60E+07 ( 197) 4.55E+06 ( 56) 20 196 53 172.1 127.8 235.7 5 1.34E+07 ( 207) 6.04E+06 ( 93) 25 261 55 109.1 85.1 139.8 6 1.26E+07 ( 209) 3.85E+06 ( 64) 27 166 42 159.0 120.0 210.5 7 1.31E+07 ( 121) 1.08E+06 ( 10) 15 47 29 566.7 308.1 1173.1 8 1.13E+07 ( 439) 4.51E+06 ( 175) 63 195 30 123.1 102.6 147.6 9 8.17E+06 ( 141) 3.25E+06 ( 56) 28 140 38 123.7 90.4 171.7 10 1.35E+07 ( 50) 2.16E+06 ( 8) 6 94 64 298.3 144.3 717.6 11 1.28E+07 ( 142) 4.06E+06 ( 45) 18 175 52 154.5 110.3 221.0 12 1.86E+07 ( 80) 9.04E+06 ( 39) 7 391 125 100.9 68.2 152.0 13 1.16E+07 ( 57) 8.52E+06 ( 42) 8 368 114 67.0 44.3 102.3 14 1.86E+07 ( 103) 6.13E+06 ( 34) 9 265 91 148.3 100.3 225.2 >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.806E+05 RELATIVE ERROR (%): 1.61 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 15 3.43E+07 ( 148) 1.39E+06 ( 6) 7 60 47 1091.9 525.3 2719.0 16 1.26E+07 ( 116) 4.98E+06 ( 46) 15 216 64 123.4 87.3 177.5 17 1.76E+07 ( 152) 5.22E+06 ( 45) 14 226 67 164.6 117.9 234.7 18 2.26E+07 ( 390) 8.12E+06 ( 140) 28 352 60 135.9 111.5 165.7 19 2.56E+07 ( 189) 5.01E+06 ( 37) 12 217 71 247.1 174.3 360.3 20 2.94E+07 ( 163) 7.58E+06 ( 42) 9 329 101 188.7 134.5 271.1 21 2.16E+07 ( 93) 7.19E+06 ( 31) 7 312 112 146.3 97.1 227.0 22 2.76E+07 ( 153) 9.56E+06 ( 53) 9 415 114 141.0 102.9 196.5 23 2.35E+07 ( 145) 8.93E+06 ( 55) 10 387 105 128.9 94.2 179.2 24 9.97E+06 ( 43) 1.39E+06 ( 6) 7 60 47 337.7 148.5 947.2 25 3.33E+07 ( 205) 1.53E+07 ( 94) 10 662 138 106.5 83.1 136.4 26 2.24E+07 ( 124) 6.67E+06 ( 37) 9 289 95 163.3 112.9 242.1 27 1.50E+07 ( 139) 4.76E+06 ( 44) 15 207 62 154.1 109.6 221.3 28 2.68E+07 ( 99) 7.85E+06 ( 29) 6 340 126 166.1 109.6 260.2 29 2.52E+07 ( 186) 1.04E+07 ( 77) 12 452 104 117.7 90.0 153.9 30 2.07E+07 ( 153) 7.44E+06 ( 55) 12 323 87 136.0 99.6 188.5 31 1.79E+07 ( 199) 4.24E+06 ( 47) 18 184 54 205.7 149.8 288.4 32 1.73E+07 ( 149) 5.22E+06 ( 45) 14 226 67 161.4 115.5 230.3 33 2.16E+07 ( 160) 7.98E+06 ( 59) 12 346 90 132.6 98.1 181.9 34 1.93E+07 ( 107) 1.14E+07 ( 63) 9 493 125 83.4 60.6 115.8 35 1.97E+07 ( 109) 6.31E+06 ( 35) 9 274 92 151.8 103.5 228.7 990803-3 (Axioskop, 011010-011121) ------ GRAIN AGES IN ORIGINAL ORDER ------

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Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 36 1.81E+07 ( 234) 3.87E+06 ( 50) 21 168 47 227.0 167.5 313.8 37 1.37E+07 ( 152) 5.95E+06 ( 66) 18 258 64 112.2 83.9 150.0 38 2.03E+07 ( 125) 5.19E+06 ( 32) 10 225 79 189.8 128.8 288.6 39 1.47E+07 ( 217) 7.44E+06 ( 110) 24 323 62 96.5 76.4 121.9 40 2.10E+07 ( 310) 1.10E+07 ( 162) 24 475 76 93.7 77.0 114.0 41 2.48E+07 ( 229) 1.18E+07 ( 109) 15 512 99 102.7 81.4 129.5 42 1.82E+07 ( 101) 6.49E+06 ( 36) 9 282 94 137.0 93.2 206.2 43 1.89E+07 ( 70) 1.00E+07 ( 37) 6 434 142 92.8 61.6 142.1 44 1.46E+07 ( 45) 9.42E+06 ( 29) 5 408 151 76.2 46.9 125.9 990803-3 (Axioskop, 011010-011121) Number of grains = 44 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 13 1.16E+07 ( 57) 8.52E+06 ( 42) 67.0 44.3 102.3 100.0 67.0 44.3 102.3 44 1.46E+07 ( 45) 9.42E+06 ( 29) 76.2 46.9 125.9 67.8 70.9 51.9 97.5 34 1.93E+07 ( 107) 1.14E+07 ( 63) 83.4 60.6 115.8 69.4 76.6 61.3 95.6 3 1.99E+07 ( 147) 1.10E+07 ( 81) 89.0 67.7 117.1 68.2 81.4 68.2 97.2 43 1.89E+07 ( 70) 1.00E+07 ( 37) 92.8 61.6 142.1 76.1 83.1 70.5 97.9 40 2.10E+07 ( 310) 1.10E+07 ( 162) 93.7 77.0 114.0 72.5 87.4 76.6 99.7 39 1.47E+07 ( 217) 7.44E+06 ( 110) 96.5 76.4 121.9 74.9 89.4 79.3 100.7 12 1.86E+07 ( 80) 9.04E+06 ( 39) 100.9 68.2 152.0 79.8 90.2 80.3 101.2 41 2.48E+07 ( 229) 1.18E+07 ( 109) 102.7 81.4 129.5 76.0 92.3 82.9 102.8 25 3.33E+07 ( 205) 1.53E+07 ( 94) 106.5 83.1 136.4 71.4 94.1 84.9 104.3 5 1.34E+07 ( 207) 6.04E+06 ( 93) 109.1 85.1 139.8 66.5 95.8 86.8 105.7 37 1.37E+07 ( 152) 5.95E+06 ( 66) 112.2 83.9 150.0 63.7 97.0 88.2 106.7 29 2.52E+07 ( 186) 1.04E+07 ( 77) 117.7 90.0 153.9 53.6 98.7 89.9 108.3 8 1.13E+07 ( 439) 4.51E+06 ( 175) 123.1 102.6 147.6 22.7 102.3 93.7 111.8 16 1.26E+07 ( 116) 4.98E+06 ( 46) 123.4 87.3 177.5 22.4 103.1 94.6 112.5 9 8.17E+06 ( 141) 3.25E+06 ( 56) 123.7 90.4 171.7 21.4 104.1 95.5 113.4 23 2.35E+07 ( 145) 8.93E+06 ( 55) 128.9 94.2 179.2 18.3 105.1 96.6 114.4 33 2.16E+07 ( 160) 7.98E+06 ( 59) 132.6 98.1 181.9 14.1 106.3 97.8 115.5 18 2.26E+07 ( 390) 8.12E+06 ( 140) 135.9 111.5 165.7 4.3 109.0 100.5 118.2 30 2.07E+07 ( 153) 7.44E+06 ( 55) 136.0 99.6 188.5 3.6 110.0 101.5 119.2 42 1.82E+07 ( 101) 6.49E+06 ( 36) 137.0 93.2 206.2 3.5 110.6 102.1 119.7 22 2.76E+07 ( 153) 9.56E+06 ( 53) 141.0 102.9 196.5 2.6 111.6 103.1 120.7 21 2.16E+07 ( 93) 7.19E+06 ( 31) 146.3 97.1 227.0 2.3 112.2 103.7 121.4 14 1.86E+07 ( 103) 6.13E+06 ( 34) 148.3 100.3 225.2 1.8 112.9 104.4 122.1 35 1.97E+07 ( 109) 6.31E+06 ( 35) 151.8 103.5 228.7 1.4 113.7 105.2 122.9 27 1.50E+07 ( 139) 4.76E+06 ( 44) 154.1 109.6 221.3 0.8 114.7 106.2 123.9 11 1.28E+07 ( 142) 4.06E+06 ( 45) 154.5 110.3 221.0 0.5 115.7 107.1 124.9 6 1.26E+07 ( 209) 3.85E+06 ( 64) 159.0 120.0 210.5 0.2 117.1 108.6 126.4 32 1.73E+07 ( 149) 5.22E+06 ( 45) 161.4 115.5 230.3 0.1 118.2 109.6 127.4 26 2.24E+07 ( 124) 6.67E+06 ( 37) 163.3 112.9 242.1 0.0 119.0 110.4 128.3 17 1.76E+07 ( 152) 5.22E+06 ( 45) 164.6 117.9 234.7 0.0 120.0 111.4 129.3 28 2.68E+07 ( 99) 7.85E+06 ( 29) 166.1 109.6 260.2 0.0 120.7 112.0 130.0 4 1.60E+07 ( 197) 4.55E+06 ( 56) 172.1 127.8 235.7 0.0 122.0 113.3 131.4 20 2.94E+07 ( 163) 7.58E+06 ( 42) 188.7 134.5 271.1 0.0 123.3 114.6 132.7 38 2.03E+07 ( 125) 5.19E+06 ( 32) 189.8 128.8 288.6 0.0 124.3 115.5 133.7 31 1.79E+07 ( 199) 4.24E+06 ( 47) 205.7 149.8 288.4 0.0 126.0 117.2 135.5 36 1.81E+07 ( 234) 3.87E+06 ( 50) 227.0 167.5 313.8 0.0 128.2 119.3 137.8 990803-3 (Axioskop, 011010-011121) Number of grains = 44 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI--

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19 2.56E+07 ( 189) 5.01E+06 ( 37) 247.1 174.3 360.3 0.0 130.1 121.1 139.8 1 2.16E+07 ( 80) 3.79E+06 ( 14) 275.3 157.6 521.5 0.0 131.0 121.9 140.8 10 1.35E+07 ( 50) 2.16E+06 ( 8) 298.3 144.3 717.6 0.0 131.6 122.5 141.4 24 9.97E+06 ( 43) 1.39E+06 ( 6) 337.7 148.5 947.2 0.0 132.1 123.0 142.0 2 1.94E+07 ( 334) 1.91E+06 ( 33) 482.2 341.4 703.9 0.0 137.1 127.6 147.2 7 1.31E+07 ( 121) 1.08E+06 ( 10) 566.7 308.1 1173.1 0.0 138.9 129.4 149.2 15 3.43E+07 ( 148) 1.39E+06 ( 6)1091.9 525.3 2719.0 0.0 141.6 131.8 152.0 POOL 1.76E+07( 7012) 6.10E+06( 2434) 0.0 141.6 131.8 152.0 MEAN URANIUM CONCENTRATION +/-2SE (ppm): 263.4, 13.7 POOLED AGE WITH 63% CONF. INTERVAL(Ma): 141.6, 136.5 -- 146.8 ( -5.0 +5.2) 95% CONF. INTERVAL(Ma): 131.8 -- 152.0 ( -9.7 +10.4) CHI^2 PROBABILITY: 0.0% CENTRAL AGE WITH 63% CONF. INTERVAL(Ma): 145.4, 135.9 -- 155.7 ( -9.6 +10.2) 95% CONF. INTERVAL(Ma): 127.3 -- 166.1 ( -18.1 +20.7) AGE DISPERSION (%): 37.9 CHI^2 AGE WITH 63% CONF. INTERVAL (Ma): 113.7, 109.3 -- 118.3 ( -4.4 +4.6) 95% CONF. INTERVAL (Ma): 105.2 -- 122.9 ( -8.5 +9.2) NUMBER AND PERCENTAGE OF GRAINS: 25, 57%

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Pro

babili

ty d

ensity (

%/∆

z=

0.1

)990803-3

Lower Cretaceous Turney Ranch FormationStation 38, Santa Rita Mountains

n = 44 grains (14 from 17 h etch, 30 from 12 h etch)

FT grain age (Ma)

30 50 70 300 50070010 100 10000

1

2

3

4

5

6

7

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upper red conglomerate member, Upper Cretaceous Fort Crittenden Formation, Station 42 990805-3 (Axioskop, 010306-30) >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.795E+05 RELATIVE ERROR (%): 1.59 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 1 1.62E+07 ( 140) 8.23E+06 ( 71) 14 358 86 95.8 71.9 127.8 2 1.22E+07 ( 45) 4.33E+06 ( 16) 6 188 93 136.3 76.4 257.8 3 1.46E+07 ( 81) 3.61E+06 ( 20) 9 157 70 195.5 120.0 335.5 4 1.40E+07 ( 138) 3.15E+06 ( 31) 16 137 49 215.0 145.9 327.4 5 1.15E+07 ( 106) 5.52E+06 ( 51) 15 240 67 101.5 72.2 144.7 6 8.66E+06 ( 48) 5.41E+06 ( 30) 9 236 86 78.3 48.7 127.8 7 1.62E+07 ( 100) 6.82E+06 ( 42) 10 297 92 116.1 80.5 170.6 8 1.66E+07 ( 205) 6.01E+06 ( 74) 20 262 61 134.3 102.7 175.4 9 9.42E+06 ( 116) 5.28E+06 ( 65) 20 230 57 87.3 64.0 120.2 10 1.51E+07 ( 149) 7.91E+06 ( 78) 16 345 79 92.9 70.5 122.5 11 1.98E+07 ( 220) 2.44E+06 ( 27) 18 106 41 387.7 262.9 595.8 12 1.63E+07 ( 201) 1.01E+07 ( 125) 20 442 80 78.5 62.5 98.6 13 1.33E+07 ( 115) 4.29E+06 ( 37) 14 187 61 151.0 104.0 224.7 14 1.69E+07 ( 125) 8.52E+06 ( 63) 12 371 94 97.0 71.2 133.5 15 2.60E+07 ( 128) 5.48E+06 ( 27) 8 239 91 228.5 151.4 358.6 16 1.10E+07 ( 68) 5.84E+06 ( 36) 10 254 85 92.3 60.9 142.2 17 2.23E+07 ( 329) 1.49E+06 ( 22) 24 65 27 693.5 461.2 1095.5 18 1.51E+07 ( 93) 5.19E+06 ( 32) 10 226 80 141.3 94.1 217.9 19 1.93E+07 ( 286) 7.44E+06 ( 110) 24 324 62 126.4 101.0 158.0 20 9.20E+06 ( 68) 5.14E+06 ( 38) 12 224 72 87.5 58.1 133.7 21 1.81E+07 ( 67) 2.16E+06 ( 8) 6 94 65 393.4 194.8 926.3 22 2.30E+07 ( 170) 2.57E+06 ( 19) 12 112 51 423.5 267.9 710.9 23 1.80E+07 ( 155) 3.71E+06 ( 32) 14 162 57 233.6 160.1 351.9 24 1.60E+07 ( 158) 5.58E+06 ( 55) 16 243 66 139.8 102.6 193.6 25 2.10E+07 ( 155) 1.15E+07 ( 85) 12 501 109 88.8 67.9 116.0 26 1.91E+07 ( 141) 3.92E+06 ( 29) 12 171 63 234.3 157.7 361.1 27 1.79E+07 ( 199) 3.16E+06 ( 35) 18 137 46 273.4 191.8 401.7 28 1.32E+07 ( 122) 5.52E+06 ( 51) 15 240 67 116.7 83.7 165.0 29 1.71E+07 ( 158) 1.84E+06 ( 17) 15 80 38 439.0 271.1 760.6 30 7.22E+06 ( 178) 2.80E+06 ( 69) 40 122 30 125.1 94.5 165.4 >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.784E+05 RELATIVE ERROR (%): 1.58 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 31 1.67E+07 ( 185) 3.52E+06 ( 39) 18 154 49 228.1 161.9 330.0 32 1.33E+07 ( 49) 8.66E+06 ( 32) 6 378 133 74.6 47.0 120.3 33 1.95E+07 ( 48) 1.01E+07 ( 25) 4 444 176 93.3 56.7 157.8 34 3.21E+07 ( 99) 1.49E+07 ( 46) 5 653 193 104.6 73.2 151.8 35 2.25E+07 ( 83) 7.58E+06 ( 28) 6 331 125 143.4 93.0 228.3 990805-3 (Axioskop, 010306-30)

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------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 36 1.62E+07 ( 40) 1.10E+07 ( 27) 4 479 183 72.2 43.4 122.2 37 2.06E+07 ( 76) 3.52E+06 ( 13) 6 154 84 278.0 156.2 540.8 38 1.30E+07 ( 32) 2.44E+06 ( 6) 4 106 84 251.3 107.0 724.4 39 1.60E+07 ( 237) 6.09E+06 ( 90) 24 266 57 127.3 99.6 162.8 40 9.74E+06 ( 90) 4.44E+06 ( 41) 15 194 61 106.7 73.2 158.3 41 2.56E+07 ( 315) 4.22E+06 ( 52) 20 185 51 290.1 217.2 395.3 42 2.41E+07 ( 119) 4.67E+06 ( 23) 8 204 84 247.8 159.4 403.8 43 1.90E+07 ( 117) 7.31E+06 ( 45) 10 319 95 126.2 89.1 182.0 44 1.78E+07 ( 175) 8.02E+06 ( 79) 16 350 79 107.2 82.0 140.2 45 2.84E+07 ( 105) 1.30E+07 ( 48) 6 568 164 106.3 75.1 152.9 46 2.06E+07 ( 228) 8.57E+06 ( 95) 18 375 78 116.2 91.1 148.1 47 2.60E+07 ( 192) 1.30E+07 ( 96) 12 568 117 97.0 75.6 124.3 48 1.81E+07 ( 134) 6.63E+06 ( 49) 12 290 83 132.6 95.3 187.8 49 1.00E+07 ( 74) 9.74E+06 ( 72) 12 426 101 50.3 35.8 70.5 50 2.06E+07 ( 304) 5.61E+06 ( 83) 24 245 54 176.4 138.0 225.2 51 2.61E+07 ( 241) 5.84E+06 ( 54) 15 255 70 215.0 160.3 293.8 52 1.76E+07 ( 65) 1.08E+07 ( 40) 6 473 149 79.2 52.7 120.5 53 2.25E+07 ( 83) 4.06E+06 ( 15) 6 177 90 263.8 153.6 488.6 54 2.27E+07 ( 56) 1.01E+07 ( 25) 4 444 176 108.7 67.1 181.6 55 2.96E+07 ( 73) 1.62E+07 ( 40) 4 710 224 88.8 59.8 134.1 56 1.83E+07 ( 45) 5.28E+06 ( 13) 4 231 126 166.3 89.4 334.9 57 2.70E+07 ( 133) 6.09E+06 ( 30) 8 266 97 213.2 143.8 327.2 58 1.65E+07 ( 549) 6.25E+06 ( 208) 54 273 39 128.0 108.3 151.2 59 1.41E+07 ( 52) 5.41E+06 ( 20) 6 237 105 125.8 74.4 222.1 60 2.38E+07 ( 88) 1.35E+07 ( 50) 6 591 167 85.7 60.0 123.9 990805-3 (Axioskop, 010306-30) Number of grains = 60 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 49 1.00E+07 ( 74) 9.74E+06 ( 72) 50.3 35.8 70.5 100.0 50.5 36.0 70.8 36 1.62E+07 ( 40) 1.10E+07 ( 27) 72.2 43.4 122.2 22.0 56.0 42.7 73.6 32 1.33E+07 ( 49) 8.66E+06 ( 32) 74.6 47.0 120.3 26.3 60.6 47.9 76.6 6 8.66E+06 ( 48) 5.41E+06 ( 30) 78.3 48.7 127.8 30.2 63.9 51.7 78.9 12 1.63E+07 ( 201) 1.01E+07 ( 125) 78.5 62.5 98.6 23.8 70.4 60.0 82.5 52 1.76E+07 ( 65) 1.08E+07 ( 40) 79.2 52.7 120.5 32.3 71.5 61.5 83.0 60 2.38E+07 ( 88) 1.35E+07 ( 50) 85.7 60.0 123.9 34.1 73.4 63.8 84.5 9 9.42E+06 ( 116) 5.28E+06 ( 65) 87.3 64.0 120.2 34.2 75.4 66.2 86.0 20 9.20E+06 ( 68) 5.14E+06 ( 38) 87.5 58.1 133.7 39.4 76.4 67.3 86.7 25 2.10E+07 ( 155) 1.15E+07 ( 85) 88.8 67.9 116.0 38.6 78.3 69.6 88.1 55 2.96E+07 ( 73) 1.62E+07 ( 40) 88.8 59.8 134.1 44.1 79.1 70.5 88.6 16 1.10E+07 ( 68) 5.84E+06 ( 36) 92.3 60.9 142.2 48.1 79.8 71.4 89.2 10 1.51E+07 ( 149) 7.91E+06 ( 78) 92.9 70.5 122.5 46.6 81.3 73.1 90.4 33 1.95E+07 ( 48) 1.01E+07 ( 25) 93.3 56.7 157.8 52.1 81.7 73.5 90.8 1 1.62E+07 ( 140) 8.23E+06 ( 71) 95.8 71.9 127.8 50.1 83.0 75.0 91.9 14 1.69E+07 ( 125) 8.52E+06 ( 63) 97.0 71.2 133.5 50.1 84.0 76.1 92.7 47 2.60E+07 ( 192) 1.30E+07 ( 96) 97.0 75.6 124.3 47.7 85.3 77.6 93.9 5 1.15E+07 ( 106) 5.52E+06 ( 51) 101.5 72.2 144.7 47.4 86.1 78.5 94.6 34 3.21E+07 ( 99) 1.49E+07 ( 46) 104.6 73.2 151.8 46.0 87.0 79.3 95.3 45 2.84E+07 ( 105) 1.30E+07 ( 48) 106.3 75.1 152.9 43.8 87.8 80.2 96.1 40 9.74E+06 ( 90) 4.44E+06 ( 41) 106.7 73.2 158.3 43.3 88.5 80.9 96.8 44 1.78E+07 ( 175) 8.02E+06 ( 79) 107.2 82.0 140.2 37.1 89.7 82.2 97.9 54 2.27E+07 ( 56) 1.01E+07 ( 25) 108.7 67.1 181.6 39.1 90.1 82.6 98.3 7 1.62E+07 ( 100) 6.82E+06 ( 42) 116.1 80.5 170.6 34.2 90.9 83.4 99.1 46 2.06E+07 ( 228) 8.57E+06 ( 95) 116.2 91.1 148.1 21.0 92.7 85.2 100.8 28 1.32E+07 ( 122) 5.52E+06 ( 51) 116.7 83.7 165.0 18.1 93.5 86.1 101.7

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30 7.22E+06 ( 178) 2.80E+06 ( 69) 125.1 94.5 165.4 9.8 95.0 87.5 103.1 59 1.41E+07 ( 52) 5.41E+06 ( 20) 125.8 74.4 222.1 9.7 95.4 87.9 103.5 43 1.90E+07 ( 117) 7.31E+06 ( 45) 126.2 89.1 182.0 7.2 96.3 88.8 104.4 19 1.93E+07 ( 286) 7.44E+06 ( 110) 126.4 101.0 158.0 2.6 98.3 90.8 106.4 39 1.60E+07 ( 237) 6.09E+06 ( 90) 127.3 99.6 162.8 1.2 99.8 92.3 107.9 58 1.65E+07 ( 549) 6.25E+06 ( 208) 128.0 108.3 151.2 0.2 102.8 95.3 110.9 48 1.81E+07 ( 134) 6.63E+06 ( 49) 132.6 95.3 187.8 0.1 103.5 96.0 111.6 8 1.66E+07 ( 205) 6.01E+06 ( 74) 134.3 102.7 175.4 0.1 104.6 97.1 112.7 2 1.22E+07 ( 45) 4.33E+06 ( 16) 136.3 76.4 257.8 0.1 104.9 97.3 113.0 24 1.60E+07 ( 158) 5.58E+06 ( 55) 139.8 102.6 193.6 0.0 105.8 98.2 113.9 18 1.51E+07 ( 93) 5.19E+06 ( 32) 141.3 94.1 217.9 0.0 106.3 98.7 114.4 990805-3 (Axioskop, 010306-30) Number of grains = 60 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 35 2.25E+07 ( 83) 7.58E+06 ( 28) 143.4 93.0 228.3 0.0 106.7 99.2 114.9 13 1.33E+07 ( 115) 4.29E+06 ( 37) 151.0 104.0 224.7 0.0 107.5 99.9 115.6 56 1.83E+07 ( 45) 5.28E+06 ( 13) 166.3 89.4 334.9 0.0 107.8 100.2 116.0 50 2.06E+07 ( 304) 5.61E+06 ( 83) 176.4 138.0 225.2 0.0 110.3 102.6 118.5 3 1.46E+07 ( 81) 3.61E+06 ( 20) 195.5 120.0 335.5 0.0 111.0 103.2 119.3 57 2.70E+07 ( 133) 6.09E+06 ( 30) 213.2 143.8 327.2 0.0 112.3 104.5 120.6 4 1.40E+07 ( 138) 3.15E+06 ( 31) 215.0 145.9 327.4 0.0 113.6 105.7 122.0 51 2.61E+07 ( 241) 5.84E+06 ( 54) 215.0 160.3 293.8 0.0 115.8 107.8 124.3 31 1.67E+07 ( 185) 3.52E+06 ( 39) 228.1 161.9 330.0 0.0 117.5 109.5 126.2 15 2.60E+07 ( 128) 5.48E+06 ( 27) 228.5 151.4 358.6 0.0 118.7 110.6 127.4 23 1.80E+07 ( 155) 3.71E+06 ( 32) 233.6 160.1 351.9 0.0 120.1 112.0 128.9 26 1.91E+07 ( 141) 3.92E+06 ( 29) 234.3 157.7 361.1 0.0 121.4 113.2 130.2 42 2.41E+07 ( 119) 4.67E+06 ( 23) 247.8 159.4 403.8 0.0 122.5 114.2 131.4 38 1.30E+07 ( 32) 2.44E+06 ( 6) 251.3 107.0 724.4 0.0 122.8 114.5 131.7 53 2.25E+07 ( 83) 4.06E+06 ( 15) 263.8 153.6 488.6 0.0 123.6 115.3 132.6 27 1.79E+07 ( 199) 3.16E+06 ( 35) 273.4 191.8 401.7 0.0 125.6 117.1 134.6 37 2.06E+07 ( 76) 3.52E+06 ( 13) 278.0 156.2 540.8 0.0 126.3 117.8 135.4 41 2.56E+07 ( 315) 4.22E+06 ( 52) 290.1 217.2 395.3 0.0 129.5 120.8 138.7 11 1.98E+07 ( 220) 2.44E+06 ( 27) 387.7 262.9 595.8 0.0 132.0 123.2 141.4 21 1.81E+07 ( 67) 2.16E+06 ( 8) 393.4 194.8 926.3 0.0 132.8 123.9 142.2 22 2.30E+07 ( 170) 2.57E+06 ( 19) 423.5 267.9 710.9 0.0 134.8 125.8 144.4 29 1.71E+07 ( 158) 1.84E+06 ( 17) 439.0 271.1 760.6 0.0 136.6 127.6 146.4 17 2.23E+07 ( 329) 1.49E+06 ( 22) 693.5 461.2 1095.5 0.0 141.1 131.8 151.1 POOL 1.72E+07( 8351) 5.93E+06( 2885) 0.0 141.1 131.8 151.1 MEAN URANIUM CONCENTRATION +/-2SE (ppm): 258.1, 12.6 POOLED AGE WITH 63% CONF. INTERVAL(Ma): 141.1, 136.3 -- 146.1 ( -4.8 +5.0) 95% CONF. INTERVAL(Ma): 131.8 -- 151.1 ( -9.3 +10.0) CHI^2 PROBABILITY: 0.0% CENTRAL AGE WITH 63% CONF. INTERVAL(Ma): 137.0, 128.2 -- 146.5 ( -8.9 +9.5) 95% CONF. INTERVAL(Ma): 120.2 -- 156.2 ( -16.8 +19.2) AGE DISPERSION (%): 43.9 CHI^2 AGE WITH 63% CONF. INTERVAL (Ma): 99.8, 95.9 -- 103.9 ( -3.9 +4.1) 95% CONF. INTERVAL (Ma): 92.3 -- 107.9 ( -7.5 +8.1) NUMBER AND PERCENTAGE OF GRAINS: 31, 52%

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Pro

babili

ty d

ensity (

%/∆

z=

0.1

)990805-3

Upper Red Conglomerate, Upper Cretaceous Fort Crittenden FormationStation 42, Santa Rita Mountains

n = 60 grains (30 from 17 h etch, 30 from 12 h etch)

FT grain age (Ma)

30 50 70 300 50070010 100 1000

0

1

2

3

4

5

6

7

8

9

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195

Middle Jurassic Bathtub Formation, Station 44 990805-5 (Axioskop, 020204-020207) >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.774E+05 RELATIVE ERROR (%): 1.56 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 1 1.70E+07 ( 63) 6.22E+06 ( 23) 6 273 113 132.0 81.4 222.8 2 1.90E+07 ( 187) 6.80E+06 ( 67) 16 298 73 134.2 101.3 177.5 3 1.47E+07 ( 190) 1.41E+07 ( 182) 21 617 93 50.7 41.2 62.6 4 1.57E+07 ( 194) 8.93E+06 ( 110) 20 392 76 85.4 67.3 108.3 5 2.02E+07 ( 224) 2.01E+07 ( 223) 18 882 121 48.9 40.3 59.2 6 2.00E+07 ( 123) 1.44E+07 ( 89) 10 634 135 66.9 50.8 88.2 7 2.11E+07 ( 104) 1.24E+07 ( 61) 8 543 140 82.8 59.9 115.5 8 1.82E+07 ( 101) 5.77E+06 ( 32) 9 253 89 152.1 101.9 233.6 9 1.96E+07 ( 169) 1.02E+07 ( 88) 14 448 96 92.8 71.5 120.4 10 2.25E+07 ( 83) 9.47E+06 ( 35) 6 415 140 114.7 76.7 175.3 11 1.68E+07 ( 248) 1.43E+07 ( 212) 24 629 89 56.9 47.0 68.8 12 1.10E+07 ( 216) 4.52E+06 ( 89) 32 198 42 117.0 91.1 150.2 13 1.66E+07 ( 92) 1.46E+07 ( 81) 9 641 143 55.3 40.6 75.5 14 1.70E+07 ( 126) 6.36E+06 ( 47) 12 279 81 129.6 92.3 185.1 15 1.75E+07 ( 86) 8.52E+06 ( 42) 8 374 115 99.2 68.0 147.1 16 1.24E+07 ( 153) 1.69E+07 ( 208) 20 741 105 35.8 28.9 44.4 17 1.43E+07 ( 88) 1.51E+07 ( 93) 10 662 139 46.1 34.0 62.4 18 2.74E+07 ( 118) 2.34E+07 ( 101) 7 1028 207 56.7 43.3 74.2 19 2.19E+07 ( 162) 4.46E+06 ( 33) 12 196 68 234.9 162.1 351.4 20 2.53E+07 ( 187) 1.03E+07 ( 76) 12 451 104 118.5 90.6 155.0 21 2.13E+07 ( 118) 9.20E+06 ( 51) 9 404 113 112.0 80.2 158.7 22 2.06E+07 ( 152) 6.63E+06 ( 49) 12 291 83 149.7 108.2 210.8 23 2.00E+07 ( 185) 1.71E+07 ( 158) 15 750 121 56.9 45.7 70.7 24 1.88E+07 ( 139) 9.47E+06 ( 70) 12 415 100 95.8 71.7 127.9 25 1.95E+07 ( 120) 9.42E+06 ( 58) 10 413 109 100.3 72.9 139.7 26 1.61E+07 ( 89) 5.41E+06 ( 30) 9 237 86 143.0 94.2 223.8 27 1.76E+07 ( 65) 1.65E+07 ( 61) 6 724 186 51.9 36.0 74.9 28 1.89E+07 ( 105) 1.17E+07 ( 65) 9 514 128 78.5 57.1 108.7 29 2.44E+07 ( 120) 1.24E+07 ( 61) 8 543 140 95.4 69.7 132.1 30 1.26E+07 ( 140) 1.41E+07 ( 156) 18 617 101 43.6 34.5 55.1 >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.763E+05 RELATIVE ERROR (%): 1.55 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 31 3.06E+07 ( 113) 5.68E+06 ( 21) 6 250 108 255.4 161.3 426.1 32 2.53E+07 ( 156) 1.31E+07 ( 81) 10 579 130 92.6 70.6 121.5 33 3.14E+07 ( 116) 2.30E+07 ( 85) 6 1013 221 65.8 49.6 87.3 34 3.07E+07 ( 189) 5.19E+06 ( 32) 10 229 81 280.4 193.9 419.4 35 2.37E+07 ( 175) 9.20E+06 ( 68) 12 405 99 123.3 93.0 163.4 990805-5 (Axioskop, 020204-020207) ------ GRAIN AGES IN ORIGINAL ORDER ------

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Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 36 3.41E+07 ( 126) 1.49E+07 ( 55) 6 655 177 110.5 80.1 154.5 37 2.64E+07 ( 325) 8.60E+06 ( 106) 20 379 74 147.0 117.6 183.7 38 2.48E+07 ( 153) 9.09E+06 ( 56) 10 400 107 131.5 96.5 181.9 39 2.13E+07 ( 197) 1.39E+07 ( 128) 15 610 109 74.3 59.2 93.2 40 2.47E+07 ( 152) 1.61E+07 ( 99) 10 708 144 74.0 57.3 95.7 41 2.46E+07 ( 182) 8.52E+06 ( 63) 12 375 95 138.2 103.6 184.2 42 2.15E+07 ( 238) 2.09E+07 ( 232) 18 922 124 49.7 41.2 60.0 43 2.93E+07 ( 271) 7.36E+06 ( 68) 15 324 79 190.0 145.5 247.9 44 1.81E+07 ( 167) 4.11E+06 ( 38) 15 181 59 210.0 147.9 306.2 45 2.08E+07 ( 192) 1.75E+07 ( 162) 15 772 124 57.3 46.3 71.1 46 2.76E+07 ( 102) 1.16E+07 ( 43) 6 512 156 114.3 79.6 167.2 47 2.37E+07 ( 175) 1.10E+07 ( 81) 12 483 108 103.8 79.5 135.4 48 2.33E+07 ( 115) 1.10E+07 ( 54) 8 483 132 102.8 73.9 144.8 49 3.06E+07 ( 151) 1.85E+07 ( 91) 8 813 172 79.9 61.4 104.0 50 2.62E+07 ( 129) 8.73E+06 ( 43) 8 384 117 144.2 101.8 208.4 51 2.62E+07 ( 258) 1.21E+07 ( 119) 16 532 99 104.4 83.6 130.3 990805-5 (Axioskop, 020204-020207) Number of grains = 51 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 16 1.24E+07 ( 153) 1.69E+07 ( 208) 35.8 28.9 44.4 100.0 35.8 28.9 44.4 30 1.26E+07 ( 140) 1.41E+07 ( 156) 43.6 34.5 55.1 20.7 39.2 33.3 46.1 17 1.43E+07 ( 88) 1.51E+07 ( 93) 46.1 34.0 62.4 28.5 40.6 35.1 47.0 5 2.02E+07 ( 224) 2.01E+07 ( 223) 48.9 40.3 59.2 17.0 43.4 38.4 49.0 42 2.15E+07 ( 238) 2.09E+07 ( 232) 49.7 41.2 60.0 15.5 45.0 40.4 50.1 3 1.47E+07 ( 190) 1.41E+07 ( 182) 50.7 41.2 62.6 16.7 46.0 41.6 50.8 27 1.76E+07 ( 65) 1.65E+07 ( 61) 51.9 36.0 74.9 22.0 46.3 41.9 51.1 13 1.66E+07 ( 92) 1.46E+07 ( 81) 55.3 40.6 75.5 21.7 46.9 42.6 51.6 18 2.74E+07 ( 118) 2.34E+07 ( 101) 56.7 43.3 74.2 17.9 47.6 43.4 52.3 11 1.68E+07 ( 248) 1.43E+07 ( 212) 56.9 47.0 68.8 10.4 48.9 44.8 53.4 23 2.00E+07 ( 185) 1.71E+07 ( 158) 56.9 45.7 70.7 8.9 49.7 45.6 54.1 45 2.08E+07 ( 192) 1.75E+07 ( 162) 57.3 46.3 71.1 7.9 50.3 46.3 54.7 33 3.14E+07 ( 116) 2.30E+07 ( 85) 65.8 49.6 87.3 4.2 51.0 47.0 55.4 6 2.00E+07 ( 123) 1.44E+07 ( 89) 66.9 50.8 88.2 2.0 51.7 47.7 56.1 40 2.47E+07 ( 152) 1.61E+07 ( 99) 74.0 57.3 95.7 0.3 52.8 48.8 57.2 39 2.13E+07 ( 197) 1.39E+07 ( 128) 74.3 59.2 93.2 0.0 54.0 50.0 58.4 28 1.89E+07 ( 105) 1.17E+07 ( 65) 78.5 57.1 108.7 0.0 54.7 50.6 59.1 49 3.06E+07 ( 151) 1.85E+07 ( 91) 79.9 61.4 104.0 0.0 55.7 51.6 60.1 7 2.11E+07 ( 104) 1.24E+07 ( 61) 82.8 59.9 115.5 0.0 56.3 52.2 60.8 4 1.57E+07 ( 194) 8.93E+06 ( 110) 85.4 67.3 108.3 0.0 57.6 53.4 62.1 32 2.53E+07 ( 156) 1.31E+07 ( 81) 92.6 70.6 121.5 0.0 58.7 54.5 63.2 9 1.96E+07 ( 169) 1.02E+07 ( 88) 92.8 71.5 120.4 0.0 59.8 55.5 64.3 29 2.44E+07 ( 120) 1.24E+07 ( 61) 95.4 69.7 132.1 0.0 60.5 56.3 65.1 24 1.88E+07 ( 139) 9.47E+06 ( 70) 95.8 71.7 127.9 0.0 61.4 57.1 66.0 15 1.75E+07 ( 86) 8.52E+06 ( 42) 99.2 68.0 147.1 0.0 62.0 57.6 66.6 25 1.95E+07 ( 120) 9.42E+06 ( 58) 100.3 72.9 139.7 0.0 62.7 58.4 67.4 48 2.33E+07 ( 115) 1.10E+07 ( 54) 102.8 73.9 144.8 0.0 63.4 59.0 68.1 47 2.37E+07 ( 175) 1.10E+07 ( 81) 103.8 79.5 135.4 0.0 64.5 60.1 69.2 51 2.62E+07 ( 258) 1.21E+07 ( 119) 104.4 83.6 130.3 0.0 66.0 61.5 70.8 36 3.41E+07 ( 126) 1.49E+07 ( 55) 110.5 80.1 154.5 0.0 66.7 62.2 71.6 21 2.13E+07 ( 118) 9.20E+06 ( 51) 112.0 80.2 158.7 0.0 67.4 62.9 72.3 46 2.76E+07 ( 102) 1.16E+07 ( 43) 114.3 79.6 167.2 0.0 68.0 63.4 72.9 10 2.25E+07 ( 83) 9.47E+06 ( 35) 114.7 76.7 175.3 0.0 68.5 63.9 73.4 12 1.10E+07 ( 216) 4.52E+06 ( 89) 117.0 91.1 150.2 0.0 69.7 65.1 74.7 20 2.53E+07 ( 187) 1.03E+07 ( 76) 118.5 90.6 155.0 0.0 70.8 66.1 75.8 35 2.37E+07 ( 175) 9.20E+06 ( 68) 123.3 93.0 163.4 0.0 71.8 67.0 76.9

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14 1.70E+07 ( 126) 6.36E+06 ( 47) 129.6 92.3 185.1 0.0 72.5 67.7 77.6 990805-5 (Axioskop, 020204-020207) Number of grains = 51 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 38 2.48E+07 ( 153) 9.09E+06 ( 56) 131.5 96.5 181.9 0.0 73.4 68.6 78.6 1 1.70E+07 ( 63) 6.22E+06 ( 23) 132.0 81.4 222.8 0.0 73.8 68.9 78.9 2 1.90E+07 ( 187) 6.80E+06 ( 67) 134.2 101.3 177.5 0.0 74.8 70.0 80.0 41 2.46E+07 ( 182) 8.52E+06 ( 63) 138.2 103.6 184.2 0.0 75.9 70.9 81.1 26 1.61E+07 ( 89) 5.41E+06 ( 30) 143.0 94.2 223.8 0.0 76.4 71.4 81.7 50 2.62E+07 ( 129) 8.73E+06 ( 43) 144.2 101.8 208.4 0.0 77.1 72.1 82.5 37 2.64E+07 ( 325) 8.60E+06 ( 106) 147.0 117.6 183.7 0.0 79.0 73.9 84.4 22 2.06E+07 ( 152) 6.63E+06 ( 49) 149.7 108.2 210.8 0.0 79.8 74.7 85.3 8 1.82E+07 ( 101) 5.77E+06 ( 32) 152.1 101.9 233.6 0.0 80.4 75.2 85.9 43 2.93E+07 ( 271) 7.36E+06 ( 68) 190.0 145.5 247.9 0.0 82.2 76.9 87.8 44 1.81E+07 ( 167) 4.11E+06 ( 38) 210.0 147.9 306.2 0.0 83.3 78.0 89.0 19 2.19E+07 ( 162) 4.46E+06 ( 33) 234.9 162.1 351.4 0.0 84.5 79.1 90.2 31 3.06E+07 ( 113) 5.68E+06 ( 21) 255.4 161.3 426.1 0.0 85.3 79.9 91.1 34 3.07E+07 ( 189) 5.19E+06 ( 32) 280.4 193.9 419.4 0.0 86.8 81.3 92.7 POOL 2.05E+07( 7829) 1.15E+07( 4383) 0.0 86.8 81.3 92.7 MEAN URANIUM CONCENTRATION +/-2SE (ppm): 503.5, 21.9 POOLED AGE WITH 63% CONF. INTERVAL(Ma): 86.8, 84.0 -- 89.7 ( -2.8 +2.9) 95% CONF. INTERVAL(Ma): 81.3 -- 92.7 ( -5.5 +5.9) CHI^2 PROBABILITY: 0.0% CENTRAL AGE WITH 63% CONF. INTERVAL(Ma): 92.7, 86.5 -- 99.4 ( -6.2 +6.7) 95% CONF. INTERVAL(Ma): 80.9 -- 106.3 ( -11.8 +13.6) AGE DISPERSION (%): 43.8 CHI^2 AGE WITH 63% CONF. INTERVAL (Ma): 51.7, 49.7 -- 53.9 ( -2.1 +2.2) 95% CONF. INTERVAL (Ma): 47.7 -- 56.1 ( -4.0 +4.4) NUMBER AND PERCENTAGE OF GRAINS: 14, 27%

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Pro

babili

ty d

ensity (

%/∆

z=

0.1

)990805-5

Upper Jurassic Bathtub FormationStation 44, Santa Rita Mountains

n = 51 grains (30 from 17 h etch, 21 from 12 h etch)

FT grain age (Ma)

30 50 70 300 500 70010 100 10000

1

2

3

4

5

6

7

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basal conglomerate subunit, Upper Cretaceous Fort Crittenden Formation, Station 45 000724-1b/a (U20Y) & 000724-1d/c (U26Z) >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.973E+05 RELATIVE ERROR (%): 1.66 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 1 2.26E+07 ( 668) 1.17E+07 ( 345) 48 478 54 100.6 87.4 115.7 2 1.79E+07 ( 275) 8.96E+06 ( 138) 25 367 64 103.3 83.7 127.4 3 2.56E+07 ( 189) 8.93E+06 ( 66) 12 365 90 147.4 111.2 195.2 4 3.44E+07 ( 297) 7.88E+06 ( 68) 14 323 79 223.5 171.5 290.8 5 2.26E+07 ( 292) 1.04E+07 ( 135) 21 427 75 112.0 90.9 138.1 6 1.75E+07 ( 517) 6.02E+06 ( 178) 48 246 38 150.1 125.8 179.1 7 1.86E+07 ( 240) 5.26E+06 ( 68) 21 215 52 181.2 138.2 237.3 8 2.86E+07 ( 247) 1.41E+07 ( 122) 14 579 106 104.9 84.0 130.9 9 2.84E+07 ( 175) 7.47E+06 ( 46) 10 306 90 196.0 141.6 276.8 10 1.53E+07 ( 170) 7.85E+06 ( 87) 18 321 69 101.1 77.8 131.3 11 3.09E+07 ( 343) 1.39E+07 ( 154) 18 569 93 115.4 94.8 140.4 12 3.16E+07 ( 175) 3.61E+06 ( 20) 9 148 65 440.1 281.5 727.9 13 1.68E+07 ( 249) 5.55E+06 ( 82) 24 227 51 156.4 121.5 201.1 >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.992E+05 RELATIVE ERROR (%): 1.71 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 14 1.69E+07 ( 416) 6.90E+06 ( 170) 40 281 44 127.5 106.0 153.4 15 1.14E+07 ( 105) 5.63E+06 ( 52) 15 229 64 105.5 75.2 150.1 16 2.39E+07 ( 147) 1.01E+07 ( 62) 10 409 105 123.7 91.5 169.3 17 2.04E+07 ( 151) 6.90E+06 ( 51) 12 281 79 154.1 111.9 215.8 >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.922E+05 RELATIVE ERROR (%): 1.58 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 18 2.31E+07 ( 456) 6.04E+06 ( 119) 32 251 47 193.7 157.7 237.9 19 1.80E+07 ( 133) 1.34E+07 ( 99) 12 558 113 68.5 52.6 89.2 20 2.21E+07 ( 204) 1.84E+07 ( 170) 15 766 120 61.4 49.8 75.7 21 2.06E+07 ( 190) 7.03E+06 ( 65) 15 293 73 147.8 111.4 196.0 22 2.02E+07 ( 373) 8.66E+06 ( 160) 30 361 58 118.7 98.0 143.7 23 1.83E+07 ( 339) 5.30E+06 ( 98) 30 221 45 175.0 139.3 219.7 000724-1b/a (U20Y) & 000724-1d/c (U26Z) >>NEW PARAMETERS--ZETA METHOD<<

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EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.916E+05 RELATIVE ERROR (%): 1.63 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 24 2.51E+07 ( 278) 1.10E+07 ( 122) 18 459 84 115.7 93.1 143.8 25 3.06E+07 ( 226) 5.01E+06 ( 37) 12 209 69 305.6 217.1 442.8 26 2.49E+07 ( 276) 7.12E+06 ( 79) 18 297 67 176.2 136.9 226.5 000724-1b/a (U20Y) & 000724-1d/c (U26Z) Number of grains = 26 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 20 2.21E+07 ( 204) 1.84E+07 ( 170) 61.4 49.8 75.7 100.0 61.4 49.8 75.6 19 1.80E+07 ( 133) 1.34E+07 ( 99) 68.5 52.6 89.2 50.1 64.1 54.2 75.9 1 2.26E+07 ( 668) 1.17E+07 ( 345) 100.6 87.4 115.7 0.0 84.6 75.5 94.7 10 1.53E+07 ( 170) 7.85E+06 ( 87) 101.1 77.8 131.3 0.0 86.7 77.8 96.5 2 1.79E+07 ( 275) 8.96E+06 ( 138) 103.3 83.7 127.4 0.0 89.4 80.9 98.9 8 2.86E+07 ( 247) 1.41E+07 ( 122) 104.9 84.0 130.9 0.0 91.4 83.1 100.6 15 1.14E+07 ( 105) 5.63E+06 ( 52) 105.5 75.2 150.1 0.0 92.2 83.9 101.3 5 2.26E+07 ( 292) 1.04E+07 ( 135) 112.0 90.9 138.1 0.0 94.5 86.4 103.5 11 3.09E+07 ( 343) 1.39E+07 ( 154) 115.4 94.8 140.4 0.0 97.0 89.0 105.8 24 2.51E+07 ( 278) 1.10E+07 ( 122) 115.7 93.1 143.8 0.0 98.7 90.7 107.4 22 2.02E+07 ( 373) 8.66E+06 ( 160) 118.7 98.0 143.7 0.0 100.8 92.9 109.3 16 2.39E+07 ( 147) 1.01E+07 ( 62) 123.7 91.5 169.3 0.0 101.6 93.8 110.2 14 1.69E+07 ( 416) 6.90E+06 ( 170) 127.5 106.0 153.4 0.0 104.1 96.2 112.6 3 2.56E+07 ( 189) 8.93E+06 ( 66) 147.4 111.2 195.2 0.0 105.6 97.7 114.1 21 2.06E+07 ( 190) 7.03E+06 ( 65) 147.8 111.4 196.0 0.0 107.1 99.2 115.6 6 1.75E+07 ( 517) 6.02E+06 ( 178) 150.1 125.8 179.1 0.0 110.7 102.7 119.4 17 2.04E+07 ( 151) 6.90E+06 ( 51) 154.1 111.9 215.8 0.0 111.7 103.7 120.4 13 1.68E+07 ( 249) 5.55E+06 ( 82) 156.4 121.5 201.1 0.0 113.4 105.3 122.1 23 1.83E+07 ( 339) 5.30E+06 ( 98) 175.0 139.3 219.7 0.0 116.0 107.9 124.8 26 2.49E+07 ( 276) 7.12E+06 ( 79) 176.2 136.9 226.5 0.0 118.1 109.8 126.9 7 1.86E+07 ( 240) 5.26E+06 ( 68) 181.2 138.2 237.3 0.0 119.8 111.5 128.7 18 2.31E+07 ( 456) 6.04E+06 ( 119) 193.7 157.7 237.9 0.0 123.3 114.8 132.3 9 2.84E+07 ( 175) 7.47E+06 ( 46) 196.0 141.6 276.8 0.0 124.5 116.0 133.7 4 3.44E+07 ( 297) 7.88E+06 ( 68) 223.5 171.5 290.8 0.0 127.0 118.4 136.3 25 3.06E+07 ( 226) 5.01E+06 ( 37) 305.6 217.1 442.8 0.0 129.5 120.7 138.9 12 3.16E+07 ( 175) 3.61E+06 ( 20) 440.1 281.5 727.9 0.0 131.8 122.9 141.3 POOL 2.14E+07( 7131) 8.43E+06( 2808) 0.0 131.8 122.9 141.3 MEAN URANIUM CONCENTRATION +/-2SE (ppm): 344.9, 17.3 POOLED AGE WITH 63% CONF. INTERVAL(Ma): 131.8, 127.2 -- 136.6 ( -4.6 +4.8) 95% CONF. INTERVAL(Ma): 122.9 -- 141.3 ( -8.9 +9.5) CHI^2 PROBABILITY: 0.0% CENTRAL AGE WITH 63% CONF. INTERVAL(Ma): 135.6, 125.3 -- 146.7 ( -10.3 +11.1) 95% CONF. INTERVAL(Ma): 116.2 -- 158.2 ( -19.4 +22.6) AGE DISPERSION (%): 36.0 CHI^2 AGE WITH 63% CONF. INTERVAL (Ma): 64.1, 58.9 -- 69.9 ( -5.3 +5.7) 95% CONF. INTERVAL (Ma): 54.2 -- 75.9 ( -9.9 +11.7) NUMBER AND PERCENTAGE OF GRAINS: 2, 8%

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Pro

ba

bili

ty d

en

sity (

%/∆

z=

0.1

)000724-1

Upper Cretaceous Fort Crittenden FormationStation 45, Huachuca Mountains

n = 26 grains (6 from 14 h etch; 3 from 13 h etch;

FT grain age (Ma)

30 50 70 300 500 70010 1000

1

2

3

4

5

6

13 from 10 h etch; 4 from 5 h etch)

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upper conglomerate subunit, Upper Cretaceous Fort Crittenden Formation, Station 46 000724-2 b/A (U20Y) & d/c (U26Z) >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.937E+05 RELATIVE ERROR (%): 1.57 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 1 2.16E+07 ( 319) 7.37E+06 ( 109) 24 306 59 149.2 119.6 186.1 2 2.11E+07 ( 208) 8.93E+06 ( 88) 16 370 80 120.6 93.7 155.2 3 2.34E+07 ( 144) 8.93E+06 ( 55) 10 370 100 134.0 97.8 186.2 4 1.95E+07 ( 108) 1.03E+07 ( 57) 9 426 113 97.3 70.1 136.5 5 3.46E+07 ( 256) 1.07E+07 ( 79) 12 443 100 164.7 127.7 212.3 6 1.61E+07 ( 149) 7.36E+06 ( 68) 15 305 74 111.7 83.7 149.1 7 2.64E+07 ( 130) 7.31E+06 ( 36) 8 303 101 183.8 127.0 273.2 8 3.75E+07 ( 231) 1.95E+07 ( 120) 10 807 149 98.6 78.7 123.4 9 2.53E+07 ( 437) 1.03E+07 ( 178) 28 428 65 125.6 104.8 150.4 10 2.34E+07 ( 360) 6.43E+06 ( 99) 25 266 54 184.8 147.4 231.4 >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.955E+05 RELATIVE ERROR (%): 1.61 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 11 2.12E+07 ( 209) 6.49E+06 ( 64) 16 267 67 166.7 125.9 220.7 >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.903E+05 RELATIVE ERROR (%): 1.74 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 12 3.08E+07 ( 190) 3.25E+06 ( 20) 10 136 60 465.6 298.7 767.9 13 3.33E+07 ( 246) 3.11E+06 ( 23) 12 130 54 522.4 346.6 826.1 14 1.59E+07 ( 196) 4.22E+06 ( 52) 20 177 49 189.7 139.7 262.4 15 1.87E+07 ( 138) 4.60E+06 ( 34) 12 193 66 203.8 140.1 305.2 000724-2 b/A (U20Y) & d/c (U26Z) ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 16 3.21E+07 ( 198) 1.01E+07 ( 62) 10 421 107 160.6 120.6 213.6 17 3.45E+07 ( 255) 1.27E+07 ( 94) 12 532 111 137.0 107.8 174.1 18 3.08E+07 ( 379) 2.52E+07 ( 311) 20 1056 125 62.1 53.0 72.8 000724-2 b/A (U20Y) & d/c (U26Z) Number of grains = 18 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------

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Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 18 3.08E+07 ( 379) 2.52E+07 ( 311) 62.1 53.0 72.8 100.0 62.1 53.0 72.8 4 1.95E+07 ( 108) 1.03E+07 ( 57) 97.3 70.1 136.5 1.2 67.6 58.4 78.1 8 3.75E+07 ( 231) 1.95E+07 ( 120) 98.6 78.7 123.4 0.1 75.2 66.3 85.4 6 1.61E+07 ( 149) 7.36E+06 ( 68) 111.7 83.7 149.1 0.0 79.8 70.8 89.8 2 2.11E+07 ( 208) 8.93E+06 ( 88) 120.6 93.7 155.2 0.0 85.4 76.5 95.5 9 2.53E+07 ( 437) 1.03E+07 ( 178) 125.6 104.8 150.4 0.0 94.2 85.2 104.1 3 2.34E+07 ( 144) 8.93E+06 ( 55) 134.0 97.8 186.2 0.0 96.7 87.7 106.6 17 3.45E+07 ( 255) 1.27E+07 ( 94) 137.0 107.8 174.1 0.0 100.7 91.7 110.6 1 2.16E+07 ( 319) 7.37E+06 ( 109) 149.2 119.6 186.1 0.0 105.7 96.6 115.6 16 3.21E+07 ( 198) 1.01E+07 ( 62) 160.6 120.6 213.6 0.0 108.7 99.6 118.7 5 3.46E+07 ( 256) 1.07E+07 ( 79) 164.7 127.7 212.3 0.0 112.4 103.1 122.5 11 2.12E+07 ( 209) 6.49E+06 ( 64) 166.7 125.9 220.7 0.0 115.2 105.8 125.3 7 2.64E+07 ( 130) 7.31E+06 ( 36) 183.8 127.0 273.2 0.0 117.1 107.7 127.3 10 2.34E+07 ( 360) 6.43E+06 ( 99) 184.8 147.4 231.4 0.0 121.9 112.3 132.2 14 1.59E+07 ( 196) 4.22E+06 ( 52) 189.7 139.7 262.4 0.0 124.3 114.7 134.7 15 1.87E+07 ( 138) 4.60E+06 ( 34) 203.8 140.1 305.2 0.0 126.1 116.4 136.6 12 3.08E+07 ( 190) 3.25E+06 ( 20) 465.6 298.7 767.9 0.0 130.8 120.8 141.6 13 3.33E+07 ( 246) 3.11E+06 ( 23) 522.4 346.6 826.1 0.0 136.9 126.5 148.1 POOL 2.51E+07( 4153) 9.38E+06( 1555) 0.0 136.9 126.5 148.1 MEAN URANIUM CONCENTRATION +/-2SE (ppm): 388.8, 23.2 POOLED AGE WITH 63% CONF. INTERVAL(Ma): 136.9, 131.5 -- 142.5 ( -5.4 +5.6) 95% CONF. INTERVAL(Ma): 126.5 -- 148.1 ( -10.4 +11.2) CHI^2 PROBABILITY: 0.0% CENTRAL AGE WITH 63% CONF. INTERVAL(Ma): 149.3, 134.2 -- 166.1 ( -15.1 +16.8) 95% CONF. INTERVAL(Ma): 121.1 -- 184.0 ( -28.2 +34.6) AGE DISPERSION (%): 42.1 CHI^2 AGE WITH 63% CONF. INTERVAL (Ma): 67.6, 62.7 -- 72.7 ( -4.8 +5.2) 95% CONF. INTERVAL (Ma): 58.4 -- 78.1 ( -9.1 +10.5) NUMBER AND PERCENTAGE OF GRAINS: 2, 11%

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Pro

ba

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ty d

en

sity (

%/∆

z=

0.1

)000724-2

Upper Cretaceous Fort Crittenden FormationStation 46, Huachuca Mountains

n = 18 grains (4 from 13 h etch; 13 from 10 h etch; 1 from 5 h etch)

FT grain age (Ma)

30 50 70 300 500 70010 1000

1

2

3

4

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shale unit, Upper Cretaceous Fort Crittenden Formation, Station 47 000724-3 long etch (Axioskop, 030826) >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.896E+05 RELATIVE ERROR (%): 1.81 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 1 3.71E+07 ( 183) 7.91E+06 ( 39) 8 333 107 234.5 166.3 339.5 2 1.99E+07 ( 184) 5.74E+06 ( 53) 15 241 66 174.5 128.4 241.4 3 1.90E+07 ( 234) 6.66E+06 ( 82) 20 280 62 143.3 111.1 184.8 4 2.79E+07 ( 258) 5.84E+06 ( 54) 15 246 67 238.9 178.5 325.9 5 2.57E+07 ( 380) 5.01E+06 ( 74) 24 210 49 255.4 198.8 327.7 000724-3 long etch (Axioskop, 030826) Number of grains = 5 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 3 1.90E+07 ( 234) 6.66E+06 ( 82) 143.3 111.1 184.8 100.0 143.3 111.1 184.8 2 1.99E+07 ( 184) 5.74E+06 ( 53) 174.5 128.4 241.4 33.1 155.7 127.5 190.0 1 3.71E+07 ( 183) 7.91E+06 ( 39) 234.5 166.3 339.5 7.2 173.6 145.6 206.8 4 2.79E+07 ( 258) 5.84E+06 ( 54) 238.9 178.5 325.9 2.8 189.2 162.1 220.8 5 2.57E+07 ( 380) 5.01E+06 ( 74) 255.4 198.8 327.7 0.7 205.9 179.7 235.8 POOL 2.45E+07( 1239) 5.98E+06( 302) 0.7 205.9 179.7 235.8 MEAN URANIUM CONCENTRATION +/-2SE (ppm): 251.2, 30.3 POOLED AGE WITH 63% CONF. INTERVAL(Ma): 205.9, 192.1 -- 220.7 ( -13.8 +14.8) 95% CONF. INTERVAL(Ma): 179.7 -- 235.8 ( -26.2 +29.9) CHI^2 PROBABILITY: 0.7% CENTRAL AGE WITH 63% CONF. INTERVAL(Ma): 203.4, 182.4 -- 226.7 ( -21.0 +23.3) 95% CONF. INTERVAL(Ma): 164.3 -- 251.6 ( -39.1 +48.2) AGE DISPERSION (%): 18.9 CHI^2 AGE WITH 63% CONF. INTERVAL (Ma): 189.2, 174.9 -- 204.7 ( -14.3 +15.5) 95% CONF. INTERVAL (Ma): 162.1 -- 220.8 ( -27.1 +31.6) NUMBER AND PERCENTAGE OF GRAINS: 4, 80%

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upper? conglomerate subunit, Upper Cretaceous Fort Crittenden Formation, Station 49 000725-1 (Axioskop, 020708-020709) >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.863E+05 RELATIVE ERROR (%): 1.52 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 1 2.17E+07 ( 187) 1.09E+07 ( 94) 14 463 96 99.2 77.1 127.5 >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.882E+05 RELATIVE ERROR (%): 1.52 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 2 3.21E+07 ( 237) 7.31E+06 ( 54) 12 308 84 218.8 163.0 299.1 3 2.25E+07 ( 166) 9.06E+06 ( 67) 12 383 94 123.8 93.1 164.6 4 3.11E+07 ( 134) 1.25E+07 ( 54) 7 529 144 124.7 90.5 174.2 5 2.20E+07 ( 217) 1.11E+07 ( 109) 16 467 90 100.0 79.1 126.3 000725-1 (Axioskop, 020708-020709) Number of grains = 5 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 1 2.17E+07 ( 187) 1.09E+07 ( 94) 99.2 77.1 127.5 100.0 99.2 77.1 127.5 5 2.20E+07 ( 217) 1.11E+07 ( 109) 100.0 79.1 126.3 96.6 99.8 83.7 119.0 3 2.25E+07 ( 166) 9.06E+06 ( 67) 123.8 93.1 164.6 41.9 106.0 90.9 123.5 4 3.11E+07 ( 134) 1.25E+07 ( 54) 124.7 90.5 174.2 45.6 109.1 94.8 125.7 2 3.21E+07 ( 237) 7.31E+06 ( 54) 218.8 163.0 299.1 0.0 124.9 109.7 142.3 POOL 2.50E+07( 941) 1.00E+07( 376) 0.0 124.9 109.7 142.3 MEAN URANIUM CONCENTRATION +/-2SE (ppm): 425.5, 45.7 POOLED AGE WITH 63% CONF. INTERVAL(Ma): 124.9, 116.9 -- 133.5 ( -8.0 +8.6) 95% CONF. INTERVAL(Ma): 109.7 -- 142.3 ( -15.2 +17.3) CHI^2 PROBABILITY: 0.0% CENTRAL AGE WITH 63% CONF. INTERVAL(Ma): 125.5, 110.7 -- 142.2 ( -14.8 +16.7) 95% CONF. INTERVAL(Ma): 98.2 -- 160.3 ( -27.3 +34.8) AGE DISPERSION (%): 23.9 CHI^2 AGE WITH 63% CONF. INTERVAL (Ma): 109.1, 101.6 -- 117.3 ( -7.6 +8.1) 95% CONF. INTERVAL (Ma): 94.8 -- 125.7 ( -14.4 +16.5) NUMBER AND PERCENTAGE OF GRAINS: 4, 80%

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shale member, Upper Cretaceous Fort Crittenden Formation, Station 52 000730-2 (Axioskop, 020710) >>NEW PARAMETERS--ZETA METHOD<< EFFECTIVE TRACK DENSITY FOR FLUENCE MONITOR (tracks/cm^2): 2.790E+05 RELATIVE ERROR (%): 1.64 EFFECTIVE URANIUM CONTENT OF MONITOR (ppm): 12.17 ZETA FACTOR AND STANDARD ERROR (yr cm^2): 352.74 8.09 SIZE OF COUNTER SQUARE (cm^2): 6.160E-07 ------ GRAIN AGES IN ORIGINAL ORDER ------ Grain RhoS (Ns) RhoI (Ni) Squares U+/-2s Grain Age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- 1 3.13E+07 ( 231) 5.14E+06 ( 38) 12 224 73 291.4 207.8 420.2 2 3.52E+07 ( 195) 8.66E+06 ( 48) 9 378 109 196.4 143.3 274.7 3 2.78E+07 ( 137) 2.84E+06 ( 14) 8 124 65 459.7 271.3 846.8 4 4.42E+07 ( 218) 1.36E+07 ( 67) 8 593 146 157.0 119.2 206.7 5 3.04E+07 ( 375) 9.74E+06 ( 120) 20 425 79 151.4 122.7 186.7 6 2.15E+07 ( 185) 7.77E+06 ( 67) 14 339 83 133.5 100.8 176.8 7 3.69E+07 ( 182) 6.09E+06 ( 30) 8 266 97 290.5 198.7 440.4 8 3.08E+07 ( 456) 5.07E+06 ( 75) 24 221 51 290.6 227.5 370.7 9 3.28E+07 ( 182) 1.32E+07 ( 73) 9 574 135 120.7 91.8 158.7 10 3.04E+07 ( 225) 6.49E+06 ( 48) 12 283 82 226.0 165.8 314.7 11 2.81E+07 ( 415) 9.00E+06 ( 133) 24 392 69 151.2 123.7 184.7 12 2.95E+07 ( 291) 5.48E+06 ( 54) 16 239 65 259.2 194.4 352.3 13 3.34E+07 ( 288) 6.73E+06 ( 58) 14 293 77 237.9 179.4 314.8 000730-2 (Axioskop, 020710) Number of grains = 13 ------ GRAIN AGES ORDERED WITH INCREASING AGE ------ Grain RhoS (Ns) RhoI (Ni) Grain age (Ma) P(X2) Sum age (Ma) no. (cm^-2) (cm^-2) Age --95% CI-- (%) Age --95% CI-- 9 3.28E+07 ( 182) 1.32E+07 ( 73) 120.7 91.8 158.7 100.0 120.7 91.8 158.7 6 2.15E+07 ( 185) 7.77E+06 ( 67) 133.5 100.8 176.8 60.7 127.3 104.2 155.5 11 2.81E+07 ( 415) 9.00E+06 ( 133) 151.2 123.7 184.7 40.5 139.2 120.2 161.2 5 3.04E+07 ( 375) 9.74E+06 ( 120) 151.4 122.7 186.7 51.1 143.1 126.2 162.2 4 4.42E+07 ( 218) 1.36E+07 ( 67) 157.0 119.2 206.7 59.8 145.3 129.1 163.4 2 3.52E+07 ( 195) 8.66E+06 ( 48) 196.4 143.3 274.7 29.7 150.2 134.1 168.1 10 3.04E+07 ( 225) 6.49E+06 ( 48) 226.0 165.8 314.7 5.1 156.8 140.6 174.8 13 3.34E+07 ( 288) 6.73E+06 ( 58) 237.9 179.4 314.8 0.4 164.7 148.4 182.8 12 2.95E+07 ( 291) 5.48E+06 ( 54) 259.2 194.4 352.3 0.0 172.4 155.9 190.7 7 3.69E+07 ( 182) 6.09E+06 ( 30) 290.5 198.7 440.4 0.0 177.6 160.9 196.0 8 3.08E+07 ( 456) 5.07E+06 ( 75) 290.6 227.5 370.7 0.0 188.8 171.7 207.6 1 3.13E+07 ( 231) 5.14E+06 ( 38) 291.4 207.8 420.2 0.0 193.7 176.4 212.6 3 2.78E+07 ( 137) 2.84E+06 ( 14) 459.7 271.3 846.8 0.0 198.4 180.8 217.6 POOL 3.08E+07( 3380) 7.52E+06( 825) 0.0 198.4 180.8 217.6 MEAN URANIUM CONCENTRATION +/-2SE (ppm): 328.2, 25.3 POOLED AGE WITH 63% CONF. INTERVAL(Ma): 198.4, 189.2 -- 208.0 ( -9.2 +9.6) 95% CONF. INTERVAL(Ma): 180.8 -- 217.6 ( -17.6 +19.2) CHI^2 PROBABILITY: 0.0% CENTRAL AGE WITH 63% CONF. INTERVAL(Ma): 203.2, 183.9 -- 224.5 ( -19.3 +21.3) 95% CONF. INTERVAL(Ma): 167.0 -- 247.0 ( -36.1 +43.8) AGE DISPERSION (%): 31.9 CHI^2 AGE WITH 63% CONF. INTERVAL (Ma): 156.8, 148.3 -- 165.7 ( -8.5 +8.9) 95% CONF. INTERVAL (Ma): 140.6 -- 174.8 ( -16.2 +18.0) NUMBER AND PERCENTAGE OF GRAINS: 7, 54%

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Appendix 5—Compositional data for Upper Cretaceous Fort Crittenden Formation sandstones, Santa Rita and Huachuca Mountains, southeastern

Arizona

station # Qm Qp Ls Lv Lm K P U % Qm % Qp % Qt % Ls % Lv % Lm % Lt % K % P % F % U Station 13 60 67 26 51 10 72 7 7 20 22 42 9 17 3 29 24 2 26 2 Station 23 67 34 33 18 5 110 29 4 22 11 34 11 6 2 19 37 10 46 1 Station 42 113 33 72 19 10 37 8 8 38 11 49 24 6 3 34 12 3 15 3 Station 45 81 25 21 3 73 76 10 11 27 8 35 7 1 24 32 25 3 29 4 Station 46 77 67 16 0 78 48 7 7 26 22 48 5 0 26 31 16 2 18 2 Station 47 65 85 31 8 75 7 14 15 22 28 50 10 3 25 38 2 5 7 5 Station 49 96 65 11 49 52 3 12 12 32 22 54 4 16 17 37 1 4 5 4 Station 51 105 53 3 129 2 1 4 3 35 18 53 1 43 1 45 0 1 2 1 Station 52 139 116 6 1 13 9 4 12 46 39 85 2 0 4 7 3 1 4 4 Station 61 74 23 21 24 43 71 33 11 25 8 32 7 8 14 29 24 11 35 4 Notes: Point counts for composition of sandstones made at 10x magnification, 300 points total. Qm = monocrystalline quartz; Qp = polycrystalline quartz (excluding microcrystalline quartz); Ls = sedimentary lithic fragments; Lm = metamorphic lithic fragments; Lv = volcanic lithic fragments; K = potassium feldspar (both relict and fresh); P = plagioclase feldspar; U = unidentified grain; Qt = total quartz (excluding microcrystalline quartz); Lt = total lithic fragments; F = total feldspar.

Page 229: Copyright by Brook Colleen Daun Riley 2004

Ap

pe

nd

ix 6

—E

lec

tro

n m

icro

pro

be

an

aly

se

s o

f 5

7 z

irco

ns

fro

m S

tati

on

23

, H

ua

ch

uc

a M

ou

nta

ins

po

int

#g

rain

#Z

rO2 (

%)

SiO

2 (

%)

HfO

2 (

%)

Y2O

3 (

%)

Ce

2O

3 (

%)

tota

l

pin

k/p

urp

le f

rac

tio

n

1d

127

65.8

5

32.3

5

1.4

0

0.0

0

-

99.6

1

1d

144

65.5

6

32.7

5

1.4

6

0.0

9

0.0

2

99.8

8

1d

161

66.4

2

32.4

1

1.1

9

0.1

1

0.0

3

100.1

6

2d

161

53.0

7

25.6

2

1.0

4

0.2

4

0.0

4

80.0

2

1d

165

66.3

3

32.6

6

1.4

4

0.1

0

0.0

1

100.5

4

2d

165

66.0

6

32.6

7

1.3

9

0.1

1

0.0

2

100.2

4

1d

070

65.6

5

32.5

6

1.4

9

0.2

2

0.0

2

99.9

3

1d

195

67.0

9

32.1

9

1.3

2

0.1

0

0.0

2

100.7

1

1d

005

61.0

1

29.3

5

1.4

4

0.0

2

0.0

6

91.8

8

2d

005

67.5

7

29.8

8

1.6

3

0.0

1

0.0

4

99.1

3

1d

131

65.1

4

32.9

9

1.2

9

0.1

5

0.0

2

99.5

9

2d

131

65.3

8

32.7

2

1.3

6

0.2

4

0.0

1

99.7

1

1d

012

65.6

5

33.0

7

1.3

7

0.1

0

0.0

4

100.2

2

2d

012

66.0

1

32.5

9

1.3

5

0.1

0

0.0

0

100.0

6

1d

013

66.8

1

33.1

3

1.2

9

0.1

0

0.0

4

101.3

7

2d

013

66.4

1

33.0

3

1.3

1

0.0

9

0.0

1

100.8

4

1L

330

65.3

4

32.7

6

1.1

3

0.3

3

0.0

5

99.6

1

2L

330

65.6

3

33.1

2

1.1

3

0.2

7

0.0

0

100.1

6

1L

304

66.2

2

33.0

0

1.4

8

0.1

3

0.0

3

100.8

6

2L

304

65.8

8

32.9

7

1.4

8

0.1

2

-

100.4

6

1L

062

65.8

2

32.8

3

1.2

6

0.2

4

0.0

3

100.1

9

2L

062

66.2

8

32.9

1

1.3

2

0.2

2

0.0

2

100.7

6

1L

049

65.8

2

32.8

9

1.3

4

-

0.0

2

100.0

7

2L

049

66.3

5

33.1

3

1.3

3

0.0

9

0.0

3

100.9

2

209

Page 230: Copyright by Brook Colleen Daun Riley 2004

Appendix

6,

continued

po

int

#g

rain

#Z

rO2 (

%)

SiO

2 (

%)

HfO

2 (

%)

Y2O

3 (

%)

Ce

2O

3 (

%)

tota

l

co

lorl

ess f

racti

on

1c1_110

65.3

3

32.8

1

1.4

9

0.1

0

0.0

2

99.7

5

2c1_110

66.0

0

32.5

4

1.4

0

0.2

0

0.0

1

100.1

5

1c1_223

65.3

1

32.8

1

1.5

1

0.1

9

-

99.8

2

2c1_223

65.9

1

32.5

2

1.4

5

0.2

0

0.0

2

100.1

0

1c1_376

65.7

9

32.8

7

1.2

6

0.2

9

-

100.2

1

2c1_376

65.2

7

32.8

1

1.2

3

0.3

2

0.0

0

99.6

3

1c1_437

65.8

0

32.6

8

1.5

7

0.2

2

0.0

2

100.3

0

2c1_437

66.1

5

32.7

0

1.5

5

0.2

4

0.0

4

100.6

9

1c1_216

64.3

6

31.5

8

1.2

4

0.2

4

0.0

2

97.4

4

2c1_216

66.6

1

32.9

2

1.3

8

0.2

3

0.0

3

101.1

7

1c1_082

65.1

6

32.4

7

1.3

8

0.2

6

0.0

1

99.2

9

2c1_082

66.1

5

32.3

3

1.3

8

0.2

5

0.0

2

100.1

2

1c1_291

66.1

0

32.8

5

1.1

6

0.2

2

0.0

4

100.3

7

2c1_291

65.4

7

32.3

1

1.1

9

0.2

3

0.0

1

99.2

2

1c1_300

65.4

9

33.2

3

1.6

7

0.0

6

-

100.4

4

2c1_300

65.5

9

33.2

2

1.6

6

0.0

9

-

100.5

6

1c1_598

64.6

0

32.6

3

1.4

4

0.2

5

0.0

5

98.9

7

1c1_728

65.0

6

33.0

4

1.5

6

0.2

2

0.0

3

99.9

1

2c1_728

66.1

5

33.2

5

1.3

8

0.1

9

0.0

1

100.9

9

1c1_772

65.1

4

32.6

1

1.3

5

0.1

9

0.0

7

99.3

6

2c1_772

65.9

6

33.1

8

1.4

0

0.1

3

0.0

4

100.7

0

1c2_695

65.2

7

32.5

5

1.2

5

0.2

8

0.0

2

99.3

8

2c2_695

66.4

2

33.1

9

1.2

9

0.0

9

0.0

6

101.0

5

1c2_031

65.8

8

32.1

8

1.3

4

0.1

1

0.0

8

99.6

0

2c2_031

66.5

8

32.3

6

1.2

8

0.1

4

0.0

1

100.3

7

1c2_222

66.0

3

32.3

2

1.4

6

0.1

0

0.0

4

99.9

5

2c2_222

66.0

3

32.3

3

1.3

8

0.0

9

0.0

5

99.8

9

1c2_250

65.2

8

32.1

2

1.7

3

0.1

2

0.0

6

99.3

1

2c2_250

65.5

2

32.1

2

1.6

8

0.1

3

0.0

5

99.5

0

1c2_044

63.7

5

30.4

2

1.3

9

0.1

6

0.0

3

95.7

4

2c2_044

65.5

5

31.6

9

1.3

3

0.1

5

-

98.7

1

1c2_064

66.9

9

32.3

4

1.2

5

0.2

3

0.0

0

100.8

1

2c2_064

66.8

5

32.3

8

1.2

9

0.2

0

0.0

2

100.7

4

210

Page 231: Copyright by Brook Colleen Daun Riley 2004

Appendix

6,

continued

po

int

#g

rain

#Z

rO2 (

%)

SiO

2 (

%)

HfO

2 (

%)

Y2O

3 (

%)

Ce

2O

3 (

%)

tota

l

co

lorl

ess f

racti

on

, co

nti

nu

ed

1c2_065

66.8

4

32.3

6

1.1

7

0.2

2

0.0

0

100.5

9

2c2_065

67.3

6

32.3

9

1.2

0

0.1

1

0.0

2

101.0

8

1c2_297

65.4

7

31.7

4

1.4

9

0.1

7

0.0

3

98.9

0

2c2_297

65.0

3

31.8

7

1.4

9

0.2

0

0.0

4

98.6

3

1c2_528

65.0

2

32.2

4

1.1

8

0.3

5

0.0

3

98.8

3

2c2_528

65.8

5

32.4

7

1.4

2

0.0

5

0.0

1

99.8

0

1c2_285

66.1

7

32.2

8

1.2

4

0.2

6

0.0

4

99.9

9

2c2_285

65.3

7

31.7

3

1.2

2

0.3

1

0.0

3

98.6

8

1c2_544

66.1

4

32.6

4

1.1

6

0.2

3

0.0

1

100.1

9

2c2_544

65.4

6

32.0

3

1.1

6

0.2

2

0.0

1

98.8

7

ho

ney f

racti

on

1h

1_300

66.2

8

32.5

4

1.6

5

0.2

2

0.0

6

100.7

5

2h

1_300

65.4

7

31.9

9

1.6

2

0.2

5

0.0

3

99.3

7

1h

1_180

66.3

1

32.4

7

1.3

4

0.3

1

0.0

1

100.4

4

2h

1_180

66.5

8

32.5

1

1.3

6

0.3

0

0.0

1

100.7

6

1h

1_101

67.0

2

32.0

2

1.1

0

0.2

4

0.0

2

100.4

1

2h

1_101

67.1

7

32.0

5

1.1

8

0.2

4

0.0

1

100.6

5

1h

1_109

66.4

5

32.1

0

1.3

3

0.2

7

0.0

5

100.2

0

2h

1_109

66.8

3

32.1

9

1.3

3

0.2

8

0.0

4

100.6

6

1h

1_224

66.7

4

32.1

6

1.2

2

0.2

3

0.0

3

100.3

8

2h

1_224

67.3

4

32.3

6

1.2

1

0.2

0

0.0

3

101.1

4

1h

1_482

66.3

9

32.6

6

1.5

3

0.2

5

0.0

4

100.8

7

2h

1_482

66.9

5

32.5

9

1.5

5

0.2

1

0.0

3

101.3

2

1h

2_031

66.0

0

32.2

1

1.4

8

0.2

4

0.0

2

99.9

5

1h

2_095

63.0

3

31.0

8

1.3

1

0.2

2

0.0

3

95.6

7

1h

2_221

65.0

4

32.1

0

1.3

5

0.1

8

0.0

4

98.7

1

1h

2_119

66.6

3

32.8

8

1.2

2

0.1

3

0.0

3

100.8

8

1h

2_189

64.8

0

32.0

1

1.4

4

0.2

4

-

98.5

0

1h

2_240

65.6

4

32.3

6

1.3

1

0.2

6

0.0

1

99.5

8

1h

2_248

61.9

6

29.9

4

1.5

0

0.1

3

0.0

3

93.5

4

1h

2_249

66.3

6

32.9

3

1.3

1

0.1

9

0.0

2

100.8

1

2h

2_249

66.3

0

32.9

5

1.3

3

0.1

9

0.0

2

100.7

8

211

Page 232: Copyright by Brook Colleen Daun Riley 2004

Appendix

6,

continued

po

int

#g

rain

#Z

rO2 (

%)

SiO

2 (

%)

HfO

2 (

%)

Y2O

3 (

%)

Ce

2O

3 (

%)

tota

l

ho

ne

y f

rac

tio

n,

co

nti

nu

ed

1h

2_374

65.8

7

32.0

8

1.5

2

0.1

4

0.0

0

99.6

1

2h

2_374

63.6

9

30.8

4

1.5

2

0.0

9

0.0

3

96.1

7

1h

2_276

66.4

3

32.7

4

1.4

0

0.0

9

-

100.6

6

2h

2_276

66.5

1

32.5

1

1.3

7

0.1

3

0.0

8

100.6

1

1h

2_277

60.2

9

29.5

0

1.3

7

0.1

5

0.0

3

91.3

4

2h

2_277

66.6

2

32.8

9

1.4

7

0.1

5

0.0

3

101.1

6

1h

2_358

64.9

0

31.6

3

1.4

2

0.2

2

0.0

6

98.2

3

2h

2_358

64.4

9

31.1

9

1.4

3

0.2

3

0.0

3

97.3

7

1h

2_292

66.4

0

32.0

4

1.3

8

0.2

4

0.0

2

100.0

8

2h

2_292

66.5

4

31.9

1

1.4

3

0.2

0

-

100.0

9

1h

2_390

67.0

7

32.7

1

1.1

5

0.2

2

0.0

1

101.1

5

2h

2_390

65.7

1

33.0

2

1.2

1

0.2

4

0.0

5

100.2

3

1h

2_511

65.9

5

32.9

6

1.0

1

0.5

0

0.0

1

100.4

3

2h

2_511

66.1

8

33.0

7

1.0

6

0.4

2

0.0

9

100.8

3

Note

s:

Ele

ctr

on m

icro

pro

be a

naly

ses m

ade b

y K

. B

ecker

at

Renssela

er

Poly

technic

Institu

te,

Tro

y,

NY

. B

eam

/counting p

ara

mete

rs:

15kv;

50nA

;120 s

econds m

axim

um

counting t

ime;

25-3

0 m

m b

eam

dia

mete

r.

Mean d

ete

ction lim

its:

HfO

2 =

0.0

68%

; Y

2O

3 =

0.0

22%

; C

e2O

3 =

0.0

68%

.

212

Page 233: Copyright by Brook Colleen Daun Riley 2004

213

References

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zircons with different degrees of metamictization: Acta Mineralogica Sinica, v. 12, p. 323-328.

Coney, P.J., 1972, Cordilleran tectonics and North America plate motion: American Journal of

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Vita

Brook Colleen Daun Riley was born on the 28th of April, 1973 in Tucson, Arizona, to

parents Bill and Dianne Riley. She grew up in the mountains of southeastern Arizona, and

attended the University of Arizona from 1991-1996. Following receipt of a B.S. in Geosciences

from the University of Arizona, the author attended the University of New Mexico Department of

Earth and Planetary Sciences. During May of 1997, the author began an extended internship

with Exxon Production Company in Houston, Texas, and subsequently transferred to the Ph.D.

program at the University of Texas in 1998. During the author’s time at the University of Texas,

she has been fortunate to have taught undergraduate field camp, field methods, structural

geology, and sedimentology, as well as graduate-level carbonate geology. During the summer of

1998, Brook completed an internship with BHP Petroleum in Houston, Texas. The author’s

publications include work from her senior thesis on detrital zircon geochronology of the Roberts

Mountains and Golconda allochthons in north-central Nevada, the results of independent field

studies in the Huachuca Mountains, and abstracts related to her Ph.D. work.

Permanent address: 1012 English Street Houston, Texas 77009

This dissertation was typed by the author.