EnvironmentalSafetyHealthGeotechnica] T

O'Reil ly, Talbot & Okun «- <maaaiiaaaEI& -+ 293 Brid^ street A S S C A T E S ]I ° ' I Su,te500

Springfield, MA 01103

Tel 413 788 6222

Fax 413 788 883°May 24, 1999 Emai1 °ffice@ot°-env com File No 267-02-01 ­

Mr. Charles Crocetti Sanborn, Head & Associates 6 Garvins Falls Road, Suite 1 Concord, New Hampshire 03301-5174 Supcrfund Records Center

Re: SDGBW406 BREAK Woods Hole Group Laboratory OTHhR-Beede Waste Oil/Cash Energy Site Organic Data Validation (PCBs and pesticides)

17 / Soil Samples / S-l, S-8, S-23, S-36, S-40, S-41, S-49, S-69, S-73, S-77, S-85, S-86, S-87, S-88, S-141, S-142 and OW-406 (Field Duplicate Pair / S-69 and OW-406)

1 / Aqueous Equipment Blank / OW-406A 2 / PES / TT01646 and P00226

Dear Mr. Crocetti:

This memo covers the Tier n validation of PCB and pesticide analyses in sample delivery group (SDG) BW406. This SDG includes 17 soil samples, one aqueous equipment blank and two performance evaluation samples (PES). Soil samples were collected from the Beede Waste Oil/Cash Energy Site by Sanborn, Head & Associates, Inc. Copies of field sampling notes were provided with the SDG BW220 volatile organic validation memo dated April 7, 1998.

These samples were analyzed by Woods Hole Group Environmental Laboratory for polychlorinated biphenyls (PCBs) and chlorinated pesticides by EPA Method 8080A. They were also analyzed for other organic parameters (semivolatiles and petroleum hydrocarbons) which are covered in a separate validation memo.

The analytical standard operating procedure (SOP) was included in the November 1997 Quality Assurance Project Plan (QAPP) and was also provided as an attachment to the SDG BW418 organic validation memo dated March 24, 1999 for reference.

Tier II validation was performed on these data by O'Reilly, Talbot & Okun Associates, Inc. (OTO). The Region I. EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses, December 1996 was utilized as the primary guidance source, in accordance with the QAPP. The November 1988 version of those guidelines was also used, as it provides the most recent guidance which specifically covers PCB and pesticide validation. Project specific criteria were utilized for some parameters. Tables summarizing analytical and validation criteria were provided in the QAPP and are also provided as attachments to this memo. A CADRE review was not performed. The following parameters were evaluated during this data review:

T BW406 PCB/Pesticide Validation; Page 2 O'Reilly, Talbot & Okun i"""":<"1

[ A S S 0 C I A T s ]

PCB Pest Parameters evaluated: Overall evaluation of data and potential usability issues

:!• * Data completeness (CSF audit) » * Preservation and technical holding times

Initial and continuing calibrations * * Blanks

Surrogate compounds # - Matrix spike/matrix spike duplicate

* Field duplicates *

* Sensitivity check * - Pesticide Instrument Performance

* Performance Evaluation Samples (PES)/accuracy check Compound quantitation and reported quantitation limits

* Indicates all criteria were met for this parameter. "-" = Not applicable.

The following information is provided in attachments to this data validation memorandum:

Table 1: Recommendation Summary Table - summarizes validation recommendations.

Table 2: Overall Evaluation of Data - summarizes site DQOs and potential usability issues.

Table 3: Data Summary Tables summarize accepted, qualified and rejected data.

The soil data on Table 3 are reported on a dry weight basis. The laboratory did not note this fact on each analytical result sheet, as required by the QAPP. However, the dry weight basis was checked by calculation from raw data by the validator, and confirmed by letter from the laboratory (copy attached).

Overall Evaluation of Data and Potential Usability Issues

These soil data are intended for use in site characterization, risk assessment, and assessment of remedial alternatives. Target quantitation limits were based primarily on New Hampshire Department of Environmental Services S-l soil criteria. The desired quantitation limits were met in undiluted samples. Some of the samples required dilution due to the presence of high concentrations of PCBs. Those samples had multiple analytes with quantitation limits which exceeded target limits. However, overall data usability is not significantly affected, because the compounds present at the highest concentrations are likely to be the ones driving risk and remediation decisions.

PCB data were acceptable without qualification in most samples. PCB detections in four samples were estimated due to variability observed in continuing calibrations. The high concentrations of PCBs present caused interference with pesticide data in several ways. Pesticide continuing calibrations showed decreasing instrument response over the course of run sequences. In addition to degrading instrument response, PCBs caused direct interference with sample results. PCB patterns contain so many peaks that it is likely some

T BW406 PCB/Pesticide Validation; Page 3 O'Reilly, Talbot & Okun k'"""":<""

[ A S S 0 C I A T E S ]

peaks will fall into pesticide retention time windows, resulting in false positives. False negatives or increased quantitation limits may also occur under these conditions, due to the masking of pesticide peaks. The validator believes most if not all of the pesticide data in this SDG may be false positives, despite the lab's efforts at extract clean-up and peak identification. All reported detections of pesticides in this SDG have been estimated.

Additionally, the pesticide performance evaluation sample had three analytes that scored action low and one that was missed entirely. Nondetects for those analytes have been rejected due to the possibility of false negatives.

The following sections provide further information on this sample delivery group.

Initial and Continuing Calibrations

Initial calibration summary forms were not provided for PCBs and pesticides. Raw data was reviewed for this information, and initial calibrations were found to be acceptable. Continuing calibration forms were provided. Calibrations for several analytes did not meet project criteria for maximum percent difference (%D) from initial calibration. The primary (quantitation) column can have no greater than 15%D; 20%D is allowable on the confirmatory column. Continuing calibrations associated with these soils degraded over the course of the run sequences, with up to 13 of 24 pesticide targets failing to meet criteria at the end of the sequence. According to the lab's SOP, the sequence should have been stopped and associated samples reanalyzed under acceptable calibration conditions. However, the lab indicated they did not feel stable calibrations could be achieved for these samples due to the amount of matrix interference (PCBs) present. The lab used the column with the more stable calibration to quantitate each target analyte identified.

Analtye

A1242

A1016

A1242

A1016

y?-BHC

4,4'-DDT

4 pesticides and 2 surrogates

13 of 24 pesticide targets

13 of 24 pesticide targets

Date %D

Column A

12/9/97 21

12/11/97 18

12/11/97 22

12/11/97 21

12/6/97 17

12/6/97 21

12/8/97 16-24

12/8/97 16-34

12/11/97 17-34

Column B

23

(OK)

26

(OK)

21

23

(OK)

27

22-38

Action on Affected Samples

none; not detected in associated runs

none; not detected in associated runs

estimate (J) A1242 in S-85, S-86, S-87, S-88

none; not detected in associated runs

none; not detected in associated runs

estimate 0) 4,4>-DDT in S-41

none; not detected in associated runs (bottle blanks and S-49)

estimate all pesticide hits in S-49, S-69, S-73, S-77, S-85, S-86, S-87, S-88, S-141, S-142, OW-406

none; not detected in associated runs (equipment blank OW-406A only)

BW406 PCB/Pesticide Validation; Page 4 O'Reilly, Talbot & Okun <— auaiaaaaiu —>

[ A S S O C I A T E S ] I

Validation action taken for out-of-control pesticide calibration, per 11/88 guidance, is to estimate positive results for the affected analyte only. However, due to the number of outliers at the end of the run sequences, professional judgment was used to estimate detections of all pesticides, not just those with high %Ds. Pesticide data usability was affected by this lack of instrument stability and the amount of matrix interference present. The following table summarizes compounds which did not meet project criteria and actions taken on associated sample results.

Surrogate Compounds

PCB surrogate spike recoveries met project criteria. Surrogates were not recoverable in samples S-40 and S-86 due to dilutions required to get high concentrations of A1242 on scale. This is an acceptable analytical limitation.

Pesticide surrogate recoveries met criteria with one exception, sample S-87. That sample had a 19% surrogate recovery. Review of chromatograms shows PCB interference in this pesticide run (see attached supporting raw data). The sample was not re-extracted and reanalyzed, as required by the QAPP when surrogate fail, because the failure was due to obvious matrix interference. Detection and quantisation of pesticides in the presence of PCBs is difficult. Pesticide results in sample S-87 should be considered estimates (J detects, UJ nondetects) due to this matrix interference which caused a low surrogate recovery.

Matrix Spike/Matrix Spike Duplicate

Matrix spike/matrix spike duplicate (MS/MSD) results for pesticides were acceptable. The MS/MSD was run on sample S-l, in which PCBs were not detected. That sample was free of matrix interferences observed in other soil samples. A PCB matrix spike was not required. For the 8080A analyses, pesticide recoveries are used as indicators of PCB performance.

Field Duplicates

The field duplicate samples, S-69 and OW-406, were submitted to the laboratory single blind. PCBs were nondetect in both samples; this is an acceptable duplicate condition. Endosulfan sulfate was detected in one sample but not the other. Results were within ±2 times the quantitation limit of one another, and are considered acceptable duplicate results. /?-BHC was reported in both samples, and had an unacceptably high relative percent difference, 77% RPD. The /?-BHC results in these two samples should be considered estimates (J). High variability in field duplicates is typically attributed to poor field and/or laboratory precision. However, in this case, the results were likely affected by the sample matrix. PCBs were present, as shown in the attached supporting pesticide data. PCBs were reported as nondetect in the field duplicates, but are still evident in the pesticide run, which has much lower quantitation limits than the PCB analysis. The /?-BHC detects in the two samples had both been flagged "P" by the laboratory due to greater than 25% difference between quantitation results on the two columns. This further supports the matrix, rather than lab or field error, as the cause of duplicate imprecision.

T BW406 PCB/Pesticide Validation; Page 5 O'Reilly, Talbot & Okun <­

[ A S S O C I A T E S ]

The validator believes most if not all of the pesticides reported in these soil samples are false positives due to PCB peaks falling into pesticide retention time windows. PCBs are difficult to clean out of pesticide extracts due to their similar chemical characteristics. Pesticide results from this SDG should be used with caution.

Performance Evaluation Samples/Accuracy Check

Two PES were submitted for these analyses. Score reports from EPA are attached. PES number TT01646 was a solid PES analyzed for PCBs. It contained Aroclor 1260 which scored within acceptance limits, indicating good analytical accuracy for PCBs.

PES number P00226 was an aqueous pesticide PES. A solid-matrix PES was not available for pesticides. In an attempt to make the PES more relevant to the soil samples, P00226 was extracted as if it were solid (i.e., by sonication instead of in a separately funnel). Because of the preparation techniques used, actions taken based on PES scores have been applied only to soils, not to associated aqueous blanks. Five of the nine pesticide targets in P00226 scored within acceptance limits. Three scored action low, and one was missed entirely. The lab was requested to review their results for possible sources of error. As shown in the attached correspondence, the lab could not identify an error or cause for these low scores. Soil results for these analytes may be biased low and should be considered estimates. Nondetects have been rejected due to the possibility of false negatives.

PES No. Fraction # In limits / Analytes Not Within Score Action total # targets Limits

P00226 Pesticides 5/9 <5-BHC action low Estimate (J) detects

4,4'-DDT action low and reject (R) nondetects for these

heptachlor epoxide action low compounds in all soil methoxychlor target miss samples in this SDG

TT01646 PCBs 1/1 none — none

PES P00226 was associated with a continuing calibration in which 13 of 24 pesticides did not meet continuing criteria. Chromatography performance degraded over the course of this sequence due to the large amounts of PCBs present in the soil samples. This degraded instrument response may have been the cause of low PES results. As shown in the continuing calibration section, detections of all pesticides in affected samples are considered estimates.

In addition to the PES, lab control samples (LCSs) were used to assess analytical accuracy. Solid and aqueous pesticide LCSs had acceptable recoveries for each analyte. The solid LCS was analyzed at the start of a run sequence, and was therefore not affected by the degraded instrument performance seen at the end of some run sequences.

t BW406 PCB/Pesticide Validation; Page 6 O'Reilly, Talbot & Okun

[ A S S O C I A T E S ] I

Compound Ouantitation and Reported Quantitation Limits.

Target quantitation limits for this project were based primarily on New Hampshire Department of Environmental Services S-l soil criteria, as summarized on Table C.15 of the 11/97 Work Plan (attached with DQO form). Quantitation limits were well below S-l criteria in undiluted samples. Samples S-40 and S-86 required dilution factors of 100 and 1000, respectively, to get A1242 on scale. Quantitation limits for other Aroclors in those samples exceed S-l criteria. Additionally, several samples required dilution to get pesticide runs on scale, although the peaks present were likely due to PCBs. Some samples are therefore reported with elevated pesticide quantitation limits, but no detected pesticides. The increased quantitation limits do affect data usability, particularly when S-l criteria are exceeded. Those data points may not be usable for nature and extent of contamination or risk assessment purposes.

A large percentage of the pesticide results were flagged "P" by the laboratory, indicating quantitation varied by more than 25% difference between the two columns. This is likely due to PCB interference, which may co-elute with pesticides or cause entirely false positive results. Results with the "P" flag were reported from the column yielding the lower concentration, in accordance with EPA Method 8080. EPA's newer analytical method, 8082, calls for the higher result to be reported so that results are conservative. For this project, we retain the use of the lower value due to the likelihood of positive bias or false positives resulting from PCBs. "P" flags should be considered "J" qualifiers, indicating uncertainty in the reported value.

The lab used a "#" flag to indicate PCB interference with pesticide analysis. The analyst compared chromatograms from the PCB runs (which were acid cleaned) to pesticide runs (which were not acid cleaned) to identify pesticide peaks. Peaks which were removed by acid were considered potential pesticides (see attached example raw data). When PCB peaks were present in the pesticide windows on both columns, that pesticide was reported as nondetect with a "U#" qualifier. Detection limits for these pesticides are likely somewhat elevated due to the presence of PCBs. The nondetect values are therefore considered estimated quantitation limits, and are reported as "UJ" on the data summary table.

Please feel free to contact me at 413-788-6222 if you have any questions regarding this validation.

Very truly yours,

Valerie D. Watanabe Data Validator

James D. Okun Principal

T BW406 PCB/Pesticide Validation; Page 7 O'Reilly, Talbot & Okun «- *3ESBSI3&->

[ A S S O C I A T E S ] I

cc: D. Szaro/EPA QA (with all attachments) W. Ives/NHDES Site Manager (memo + tables only) J. DiLorenzo/EPA Site Manager (memo + tables only) D. Vorhees/Menzie-Cura (memo + tables only)

Attachments: Table 1: Recommendation Summary Table Table 2: Overall Evaluation of Data Table 3: Data Summary Tables (includes TICs) Data Validation Worksheets PES Score Reports (2) Communication/Phone Logs Supporting Raw Data Project Specific Validation Criteria CSF Audit (DC-2 Form) DQO Form (with attached Table C.15 from Work Plan)

TABLES

TABLE 1 Recommendation Summary Table

BW406 ORGANIC ANALYSIS (PCBs and Pesticides) Beede Waste Oil/Cash Energy Site

Plaistow, New Hampshire

Sample Matrix Recommended Qualifiers Number PCBs Pest

S-l Soil A J/R1

S-8 Soil A J/R1

S-23 Soil A J/R1

S-36 Soil A J/R1

S-40 Soil A J/R1

S-41 Soil A PJ/R1

S-49 Soil A PJ/R1

S-69 Soil A P'5J/R]

S-73 Soil A PJ/R1

S-77 Soil A PJ/R1

S-8 5 Soil P PJ/R1

S-8 6 Soil P PJ/R1

S-87 Soil P P-'J/R1

S-88 Soil P PJ/R1

S-141 Soil A PJ/R1

S-142 Soil A PJ/R1

5OW-406 SoH A J3' J/R1

OW-406A Aq. Eq. Blank A A

7217010 Aq. bottle A A

092997 Soil bottle A A

A ­ Accept results.

J1 ­ Estimate A1242 detection due to continuing calibration with high %D from initial calibration. Quantitation may be affected by analytical variability.

J2 ­ Estimate 4,4'-DDT detection due to continuing calibration with high %D from initial calibration. Quantitation may be affected by analytical variability.

J3 - Estimate positive detections of all pesticides due to continuing calibration with high %Ds for more than half the target analytes. Instrument performance degraded towards the end of the run sequence due to PCBs in the samples. Quantitation of all pesticides may be affected.

J4 - Estimate detected concentrations and quantitation limits (J/UJ) for all pesticides in this sample due to low surrogate spike recovery. Appears to be due to PCBs in the sample.

J5 - Estimate /?-BHC detections in the field duplicates due to high relative percent difference between the two results. Appears to be due to PCB interference rather than lab or field error.

J/R1 - Performance evaluation sample scored action low for <5-BHC, 4,4'-DDT, and heptachlor epoxide. Methoxychlor was missed entirely. Estimate (J) positive detections and reject (R) nondetects for these analytes due to potential for low bias and false negatives.

Pot

entia

l Usa

bilit

y Is

sue

•a S -.

III a s . 119 s

lit I lie ill1 I&P 5 w a J 2 ( U t - ( * - l > ' r S H H y * - i 5 o

D C S t 3 ^ " M 3 M C S S O ' B - S w o "p. S "c ' 8 "^ "eS ™ O ~ * | " U

1 1 g g 11 12 *• f § i 1 i § 1 !l! t iSf, 111! II 11 mi ir !i W ^J Q J""i t/J \J3 S f^ H OJ (H O O M S O t .

s ^ g S g s . s ^ - ^ ^ g ' g ^ - o s ^ l ^3 • 'O cti o rt *c tu £•? * J3 w w f Q ^ ^t T>

' S ^ n ' S ^ ^2 o ' o c i s ^ ^ . S < L ) t w o " S - 2

* §111 It! lifts lilll

gfk^ r5

& '.in £H ^3 ca 'C

cc 3 >

*tH

8 g

3 w'o M '•4-J w _g t-H

CDO. g "a,

W STt p- >J

c* a w CO

pa 80 a UH (X - §g 2

as -a 1 ­Q> w s -3 £* <U S m" ^

O H E CN t* oi s ^

1 <S ° "

1 (2 1

"8_ 13 •& ^ S o M S^

a, 3 o o^

O 3

« sR ^ C3 . » 8 S, O 0) '3 ^ ^ '« M S " - oo *5 _S o >-l 13 O T3 'C ".s3^ &

HI C/3 5 (Si i!!i

C/3 to CS <C W ? CT1

1 3 x fli V)

a) a o "O u a 3 S M

Q ID S 'S

"3 S c g 1cfl R fl i 1J 3 - 2 So g sSS-

•^HS 1 « <US ^ Wo a •rt rt 'C ct ' 3 Q rt c C3 ti ^

2 8 <u <D 53 »C , W W 4_> <4 I—v I—, ^U O O I—3 H-J CO

1 1 1

t> J3 P P £ ID B P P PH-»

P P P P P P P P >—> 3P P 0o o o o o o t-~ t-~ Pi t-- f- Pi CO cn CO Pi CO r- CO CO CO Pi r~- o CO m CO m t— CO CO CO CN CO

o

|m"

12/1

1/97

12/8

/97

12/8

/97(0 CO o CO

ro

11/5

/97

11/3

/97 r- CO CO CO CO CO in CO in CO CO m CO mON

f: oo in co OX 00

ON o ooil co T—«

D P P P P P P P P P P P P P P P P P P P P P PP

Ox Pi Ox Ox Pi ON Ox ON Pi ON OX ox Ox Ox Pi OX Ox Ox ON ON ON OX ON Ox Ox Ox 12

/11/

97ON ON Oxi f- CO CO CO CO CO CO CO r~ r~ CO CO CO CO CO CO CO CO CO Ox OX gx

$ m 00 CO CO $co r-p ON rr co co 00 3

£3 P P P P P P P P H-l P P P P P P P P P P P P P P f-

•* oi ON

12/1

1/9700 r- r

in Ox Ox f­ •* r CN CN CN T •q­f r-4 T CN T T CN CN CN •* TJ­

§00 CO CO in s T3 Ox

t» in

"u S> ON o 2G co m 00 3

u D P P P P 3P P P P t—t H-» P 1—1 p P^P 1—1 P P P

Pi 00 00 CO ^ Pi NO NO Pi NO NO o NO Pi o o o 000 00 oc 00 00 CO o oOW

12/1

1/97

|0 o

NO NO in NO NO NO r r~­ Ox NOt l

CO CN CO NO CO r- CO CO r- r~ NO NO NO CO in CO CO ON CO CO CO OX Ox CO Vs!

§OO l?i CO in ON A

3mO ON CO 2m ON

;D P P P P P P P P P P P P *—> P P P P P P P P PP P

CN CN CN & CN CN Pi m CN Pi CN <N M­r~ f- T r •q- rr •q-

Date

Analy

zed:

12/1

0/97

12/1

0/97

12/1

0/97

12/1

0/97

12/1

0/97

12/1

0/97NO •<*• •q- •«!• •q­ TJ- r •*r r»

12/6

/97

12/6

/97

12/6

/97r­ rr rr Tf s: in ON ON

00 00 in »n m $*•O

u 5I2 OX T—<00 m oo 1

8 3 ^ P p p P P 3P P s>—J P 3P P P P »-T» p P 3p P T

co a. !D & Pi 1 - c 3- Pi T r~- M­t- Pi o o o o o o -3­r~ r- r­ r- or T

CO s Tt in o- o o o o o• •* •t r r CO co CO CO CO

11/5

/97

11/5

/97 CO t r-o\ in o CO TON

CO CO oo CO CO CO CO o F~ $ om $T OX oooo CO m Ox 3

P P P P P P P P P p P P P P P P P P p P P PP P m m in in in in in r r- f» Pi r~ r Pi in iy~i >/ Pi in r- in in in Pi r~ m v>

CO

NO co

o CO 3938

5-4 CO CO CO CO CO CO en r— r-

ON & CO CO CO CO CO CO CO CO

in S CO Ox 3

E> P P >—> P P P p 3 ID P P 3 1—> P > P P 3 P P P P

I Pi 00 00 Pi r- p- oo Pi r- r- r- p- Pi c r~ t-~ O t~­ t­00 oo r- 00 00 oo F t- r ON

o CO f~Ox

r-ON

$

CO t—CO CO CO co co co co CO co CO co co co CO in Ox

1a oo co CO •a in CO o) ON oci CO Ox es> £3 P P P P P P P P P P P P P P P P P P P P P P P

oo oo oo oo oo oo ON Ox o\ o\ ON oo oo oo oo Ox oo 00 oo ON Ox oo 00 00 & Pi pi Pi CO CO CO CO CO CO CO t~- t CO CO CO CO CO CO 0)

Date

Ext

ract

ed:

11/5

/97

1 1

/5/9

7t- CO CO CO in gv ON gx 00 W CO 0. CO -S-1 00 OX r­ (N 3CQ CO CO oo

P P P2$ t> P P P P P P P P P P P P P P P P P P P P >­ ?. CN & (S CS Pi r •~ 1- Pi r CN •*r J- T Pi TT o o o o o or •q- CN <N c-> 0or CN

T T T T

Dat

e E

xtra

cted:

11/5

/97rr p~

in 1 O_N ON t—

CN

^

00 CO CO i OX CN M OS 2 sCO CO oo

• !" •< Is

O c cs S

ampl

e ID

: a JS

Jus

Dat

e S

am

ple

d: W)

3

utio

n F

act

or:

Date

Analy

zed:

Dilu

tion

Fact

or:

VI -4.*

1

|Delta

-BH

C

Gam

ma-

BH

C

| Hepta

chlo

r

| Hepta

chlo

r epoxi

de

"o VI

$1

[End

rm ald

ehyd

e

i

[Die

ldrm

End

osul

fan I

| End

osul

fan n

lE

ndos

ulfa

n sulfa

te

1 1 Met

hoxy

chlo

r [A

lpha

chl

orda

ne

[Gam

ma chl

orda

ne

[Tox

aphe

ne

[Endnnke

tone

NO O4 00 TT CN CO 9Tl- in S

lAlp

ha-B

HC

CN CN CN o CN CN) CN

Pes

ticid

es

Q W

BQ 0 o o O o o S CJ 81*111 1 §cn no

H to OH 1 < IU m

*rn•«r ,"S­

r •*"

13

CD CD CD CD CD CD CD CD CD CD D CD D CD CD CD CD CD 3 en CO rn en en en en £ erf £ erf en en en erf en 5 en en erf m en I* en ro m en en en en m

cs r~"5 ONON

ON in oo So

2§ 1es en 3 ON ON

OT o en

12/1

1/97

12

/11/

9712

/11/

9712

/11/

9712

/11/

9712

/11/

9712

/8/9

712

/11/

97

10/2

3/97

10

/23/

97

11/1

0/97

11

/10/

971

1/5

/97

11/1

0/97

11/5

/97

M CD &o CD CD » CD CD CD ^ J= » CD CD CD CD CD CD CD CD CD CD CD ^ o o o 00 o o otu NO 00O o o O O o

OW

-406

A

7217

010 o o o o o o o or­

"o,0

3*

cr

ON 0£

in oo en ON en

<

1

CD CD tD E> CD CD CD CD CD CD CD CD CD CD CD CD CD ID CD D CD CD CD CD PH PH V-to o o O O 0 o oo oO O 0 00ooo

11/1

0/97

12

/11/

97

000 00 o o or>ON

en ON <

00 s •3, en

&CD CD CD &D CD CD CD -> CD CD CD CD D CD CD D 1—> CD CD D D CD erf cs es U"l cs cs CS •a- cs cs

r-ON ON in

1

NO Oi ON t

2 ON

oo in en m ON en OO 3

CD CD CD CD CD CD CD CD ID D CD D D D £ ON ON ON ON ON ON ON cs cs cs cs CS ON ON ON erf ON cs ON ON ON cs cs ON ON erf en en en en en en en en Ed * * en en en en en en en en NO

11/5

/97

ON go cs

CD CD CD CD CD CD CD CD CD CD CD D D ON ON ON ON ON ON ON rs CN cs cs cs ON ON ON cs ON ON ON cs cs ON ON erf erf erf erf en en en en en en en en en en en en en en en en

r- r-ON ON <n 2°

f- r-ON ON in CS oo en en

ON 3CO 3en

in

11/3

/97

in 00 en ON

PS PH CO en

in I CD CD CD 3 CD CD CD CD CD CD CD CD CD CD CD CD

o o o O 000 r- c- erf erf erf ;r- ; erf r- o en en en en en en

f-ON

12/8

/97

12/8

/97c-­

>n ON ON oo en >n oo oo ON

en

CO en ON 3

en i r- r­

in ON ON

^

o

o

o

CD CD CD 3 CD 3 3 CD CD CD t-i 33 CD 1-1 CD CD 3 O o o O 00 00 oo *oo oo erf NO NO NO erf 00 NO en NO erf o oo o cs cs § cs O I—" en en NO en en 00 en en NO sc-- en

ON 00 r-o en00 ON o

3 CS en ON

CD CD CD CD CD CD 3 CD CD CD CD CD D CD

CN o o o o o o o o O o erf o 0erf 000erf o erf o o o o o o o o o o ot­<7N o o o 8 r- ON ON ON ON 00 oo 00 oo ON 00 00 oo ON ON o oo

ON ON oo 00 oo oo 00 00 ON ON 1—1 m en en en en en 00 en OO o o NO 00 >n en en en en en en >n en & en 8 cs SS o

ON t- cs cs CO m oo 3 1—I r—l

09 CD CD CD CD p CD CD CD CD CD H "* o o O o o o O 00 00 00 erf oo 00 erf NO NO NO erf NO 00 NO erf OO oo NO

NO NO o NO en en en en en en en en en en en en en en

ate

Ana

lyze

d: 1

2/11

/97

o

-3 o

> '-§> r- cs" f-ON in

ate

Ana

lyze

d: 1

2/8/

97ON ON m 00 en in

o1oo OON CO •3

•3 en ON

lutio

n F

act

or.

Sam

ple ID

:

late

Sam

pled

: a

M

2 "3 W5 *

ite E

xtra

cted:

lor

epox

ide

•3

fan

sul

fate

(U u

ite E

xtra

cted:

tf) u

1 1—I WNO cs 00 _o 1•H0_o >n cs en NO O s0cs CN H CO cc 0 pn n "Fidm H

Q Q 'd Q 03 Q w AG %W ^ h43 dCj Q qg

9n 0 0 0 o o 0 m t? 0 "u Cj Cx ^

e pw o o u o o o o1 11 11 1

•aw pa^ 11

PH EC 1 1 1"u '3 1% o oQ WwmPM Q W I

1