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EWG-RPT-023 Rev 0.0 PNNL-29023

X-Ray Diffraction and Product Consistency Test Results for the Phase 6 Study of Nepheline Formation in High-Level Waste Glasses September 2019

CE Lonergan JO Kroll CH Skidmore ZJ Nelson JD Vienna

Prepared for the U.S. Department of Energy under Contract DE-AC05-76RL01830

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X-Ray Diffraction and Product Consistency Test Results for the Phase 6 Study of Nepheline Formation in Hanford High-Level Waste Glasses

September 2019 CE Lonergan JO Kroll CH Skidmore ZJ Nelson JD Vienna Prepared for the U.S. Department of Energy under Contract DE-AC05-76RL01830 Pacific Northwest National Laboratory Richland, Washington 99354


Summary ii

Summary

Hanford high-level waste (HLW) contains relatively high concentrations of Al2O3. A major constraint limiting the waste loading of high-Al2O3 glasses is nepheline (nominally NaAlSiO4) formation upon slow cooling of HLW glasses after melts are poured into steel canisters. The model currently planned to be used at the Hanford Waste Treatment and Immobilization Plant (WTP) for avoiding nepheline formation is unnecessarily conservative and drastically limits waste loading.1

To increase operational flexibility and effectively operate the WTP, the effects of glass composition on glass properties must be determined and glass property-composition models must be developed.2 Determining the impacts of glass composition on nepheline formation and the effects of nepheline on Product Consistency Test (PCT) response is an important part of this effort. During this work data related to the Hanford high-Al2O3 HLW composition region was generated to supplement existing data for model development. Twenty glasses were fabricated, heat treated, and analyzed for crystallinity and PCT response. The heat treatment was designed to mimic the canister centerline cooling (CCC) profile of Hanford HLW glass canisters.3

It was found that only 6 of the 20 prepared glasses (#4, #7, #8, #10, #19, and #20) formed nepheline upon heat treatment. All glasses except for one (#19) precipitated spinel upon quenching and no glasses contained nepheline upon quenching. Of the 20 glasses, the PCT-normalized boron release of the quenched glasses and all but five of the CCC glasses satisfied the environmental assessment glass benchmark value (16.695 g/L).4 The CCC glass samples that exceeded the limit were #8 (48.21 g/L), #10 (19.77 g/L), #13 (20.17 g/L), #19 (60.85 g/L), and #20 (61.08 g/L). Those glasses coincide with the highest amounts of nepheline found in the CCC glasses, except for #13, which did not form nepheline after CCC.

1 Vienna JD, D-S Kim, DC Skorski, and J Matyas. 2013. Glass Property Models and Constraints for Estimating the Glass to Be Produced at Hanford by Implementing Current Advanced Glass Formulation Efforts. PNNL-22631 (ORP-58289), Rev. 1, Pacific Northwest National Laboratory, Richland, Washington. Available at http://www.pnnl.gov/main/publications/external/technical_reports/PNNL-22631Rev1.pdf. 2 Peeler DK, JD Vienna, MJ Schweiger, and KM Fox. 2015. Advanced High-Level Waste Glass Research and Development Plan. PNNL-24450, Pacific Northwest National Laboratory Richland, Washington. Available at http://www.pnnl.gov/main/publications/external/technical_reports/PNNL-24450.pdf. 3 Petkus L. October 19, 2003. “Canister Centerline Cooling Data, 24590-PADC-F00029 Rev 1.” Memorandum to C Musick. River Protection Project, Waste Treatment Plant, Richland, Washington. 4 Jantzen CM, NE Bibler, DC Beam, CL Crawford, and MA Pickett. 1993. Characterization of the Defense Waste Processing Facility (DWPF) Environmental Assessment (EA) Glass Standard Reference Material. WSRC-TR-92-346, Rev. 1, Westinghouse Savannah River Company, Aiken, South Carolina.


Acknowledgments iii

Acknowledgments

The authors gratefully acknowledge the financial support provided by the U.S. Department of Energy Office of River Protection Waste Treatment and Immobilization Plant Project, managed by Tom Fletcher, with technical oversight by Albert Kruger.

The authors thank Kevin Fox of Savannah River National Laboratory for his help in the analysis and testing of the glasses. We also thank Dong-Sang Kim (PNNL) for his technical review, Matt Wilburn of (PNNL) for the editorial review, and Hans Brandal and Veronica Perez (PNNL) for programmatic support during the conduct of this work.


Acronyms and Abbreviations iv

Acronyms and Abbreviations

ARM-1 Approved Reference Material

BDL below detection limit

CCC canister centerline cooling

DI de-ionized

DOE U.S. Department of Energy

EA environmental assessment

HDI How Do I…?

HLW high-level waste

IC ion chromatography

ICP-AES inductively coupled plasma – atomic emission spectroscopy

JMP 13 JMP® version 13.0.0 (SAS Institute Inc. 2016)

KH potassium hydroxide fusion

LM lithium metaborate fusion

ND nepheline discriminator

NN neural network

NR normalized release

OB optical basicity

ORP Office of River Protection

PCT Product Consistency Test

PF sodium peroxide fusion

PNNL Pacific Northwest National Laboratory

QA quality assurance

R&D research and development

SEM scanning electron microscopy

SRNL Savannah River National Laboratory

TanH hyperbolic tangent

XRD X-ray diffraction

WTP Waste Treatment and Immobilization Plant


Contents v

Contents

Summary ....................................................................................................................................................... ii

Acknowledgments ........................................................................................................................................ iii

Acronyms and Abbreviations ...................................................................................................................... iv

Contents ........................................................................................................................................................ v

1.0 Introduction ...................................................................................................................................... 1

1.1 Quality Assurance ............................................................................................................... 3

1.1.1 PNNL QA Program ............................................................................................ 3

1.1.2 ORP Glass Support Work QA Program ............................................................. 3

2.0 Experimental Methods ..................................................................................................................... 5

2.1 Composition Matrix Design ................................................................................................ 5

2.2 Glass Fabrication ................................................................................................................ 9

2.3 Glass Composition Analysis ............................................................................................... 9

2.4 Canister Centerline Cooling Heat Treatment .................................................................... 10

2.5 Scanning Electron Microscopy Analysis .......................................................................... 10

2.6 X-Ray Diffraction Analysis .............................................................................................. 11

2.7 Product Consistency Testing............................................................................................. 11

3.0 Results and Discussion .................................................................................................................. 12

3.1 Crystal Fraction Analysis Upon Quenching and Post-Canister Centerline Cooling Treatment .......................................................................................................................... 12

3.2 SEM Analysis ................................................................................................................... 14

3.3 Product Consistency Testing Analysis .............................................................................. 17

4.0 Summary ........................................................................................................................................ 20

5.0 References ...................................................................................................................................... 21

Appendix A – Measured and Targeted Glass Compositions .................................................................... A.1

Appendix B – X-Ray Diffraction Data ......................................................................................................B.1


Contents vi

Figures

Figure 1. Predicted probability of nepheline formation versus nepheline concentration, as determined by XRD. The highest concentrations of nepheline are found in the following CCC samples. X = NP6-20, □ – NP6-19, and ▼ = NP6-08. (Glasses in red precipitated nepheline upon CCC heat treatment while glasses represented by black circles did not.) ........................................................................................................ 14

Figure 2. SEM images, in secondary mode, of various quenched glasses. ................................................. 15

Figure 3. SEM images of several glasses after CCC heat treatments. ........................................................ 16

Figure 4. Boron ln(NR) rates for quenched glasses versus CCC glasses. Glasses in red precipitated nepheline upon CCC heat treatment while the black circles did not. X = NP6-20, □ – NP6-19, and ▼ = NP6-08. .................................................................... 18

Figure 5. A plot of the difference in crystal concentrations (CCC minus quenched values) vs. the difference in normalized B release values for CCC glasses minus quenched glasses. Glasses in red precipitated nepheline upon CCC heat treatment and glasses presented in black did not. X = NP6-20, □ – NP6-19, and ▼ = NP6-08. ............ 19

Tables

Table 1. Composition of “Others” mixture (in mass fraction). ..................................................................... 6

Table 2. Upper and lower bounds for components (in mass fraction). ......................................................... 7

Table 3. Compositions of 20 statistically designed glasses. ......................................................................... 8

Table 4. Preparation and measurement methods used in reporting the concentrations of the analytes in this study (Fox et al. 2019). .............................................................................. 9

Table 5. CCC heat treatment schedule. ....................................................................................................... 10

Table 6. Crystal identification and quantification in as-quenched glasses. ................................................ 12

Table 7. Crystal identification and quantification results using XRD for the glasses in this study post-CCC treatment. ......................................................................................................... 13

Table 8. PCT method A release rates for B, Li, Na, and Si normalized to target compositions. Values below are averaged from the triplicate measurements (< = below detection limit). ................................................................................................................. 17


Introduction 1

1.0 Introduction

The U.S. Department of Energy (DOE) manages approximately 210,000 m3 of radioactive waste in

underground tanks on the Hanford Site. The Hanford Waste Treatment and Immobilization Plant (WTP) is currently being constructed to vitrify the waste in borosilicate glasses. Prior to processing the low-activity waste (LAW) fraction will be removed from the high-level waste (HLW) and processed separately. Each fraction will be blended with glass-forming chemicals, melted at ~1150°C, and then the molten glass will be poured into stainless steel canisters to cool and solidify (DOE 2000).

According to the 2008 HLW feed vector used by Vienna et al. (2013), many HLW compositions contain high concentrations of Al2O3. The Al2O3 fraction is projected to range from roughly 10 to 70 mass% on a calcined oxide basis after caustic leaching. The loading of high-Al2O3 HLW may be drastically reduced by the constraint(s) applied to reduce the probability of forming nepheline (nominally NaAlSiO4) upon slow cooling of glasses. Nepheline precipitation from an HLW glass during cooling is a major concern because it can reduce the durability of the resulting glass by removing three moles of glass forming oxides (one mole of Al2O3 and two moles of SiO2) for every mole of Na2O (Kim et al. 1995). When nepheline is present in a waste glass, it is difficult to predict the Product Consistency Test (PCT) response. It has also been documented that eucryptite (LiAlSiO4) has a similar effect on glass durability (McCloy and Vienna 2010). To meet disposal requirements, nepheline formation must be avoided, or the amount of nepheline formed and its impact on the PCT response must be predicted. The ability to predict the amount of nepheline formed and the PCT response would provide a basis for specifying a constraint to avoid HLW glass compositions that would yield unacceptable PCT responses.

The current constraint used to avoid nepheline formation in glasses produced by WTP is unnecessarily conservative and limits waste loading (Vienna et al. 2016). A nepheline discriminator (ND) was developed to reduce the risk of nepheline precipitation during canister centerline cooling (CCC) heat treatment (Li et al. 1997). This approach is based on limiting the normalized SiO2 concentration (NSi) using the following:

0.62 (1)

where gi is the mass fraction of the ith component in the glass. A better discriminator is needed as ND screens out glass compositions that often do not precipitate nepheline, while allowing glass compositions that have been shown to crystallize nepheline. In an effort to reduce some of the conservatism in the ND, optical basicity (OB) was proposed as a constraint (Rodriguez et al. 2011; McCloy et al. 2011). The OB of a glass (Λglass) can be calculated from a glass composition using the following equation:

Ʌ∑ Ʌ∑

(2)

where qi = the number of oxygen atoms in the ith component oxide xi = the mole fraction of the ith component oxide in glass Λi = the molar basicity of the ith component oxide

The revised constraint allows glasses with NSi < 0.62 if the OB of the melt is less than 0.55. This approach did reduce some of the conservatism, but still limits the waste loading of high-Al2O3 glasses (Vienna et al. 2016).


Introduction 2

A neural network (NN) model has also been proposed to estimate the probability of nepheline formation for a specific glass composition (Vienna et al. 2013). This approach was selected because it can account for highly non-linear effects of components. The NN model consists of three nodes using the hyperbolic tangent (TanH) transfer function. The output from the three nodes was compared to a probability cutoff value to assign a binary response (i.e., whether nepheline formed or not) for a glass composition. However, the NN method involves complex calculations that require much more data than is available for typical glass properties, and it is difficult to determine the uncertainties of predictions made with the model (Vienna et al. 2016).

To optimize waste loading, a new approach is needed to limit nepheline precipitation during slow cooling of HLW canisters. It has been demonstrated that B2O3, CaO, Fe2O3, K2O, and Li2O affect nepheline formation (Li et al. 1997). A ternary sub-mixture model that takes advantage of the success of the ND while considering the effects of other components in the melt has been developed (Vienna et al. 2017).

The current nepheline formation models are based on a dataset composed of 747 glasses (Vienna et al. 2017; Stanfill et al. 2019). This dataset was gathered from multiple studies under different methods at different labs. The glasses that are currently part of this dataset do not adequately cover high-Al2O3 regions of interest as defined by the predicted waste compositions from the Hanford tanks. The objective of this subtask is to develop data that will enable the current nepheline model to be refined and validated and eventually to develop an improved nepheline model with good predictability in the high-alumina glass composition region for Hanford HLW glasses. This is the first step in creating a model that can support plant operation and waste form qualification activities. This objective will be achieved by varying glass compositions in the region of interest and measuring both the concentration of crystalline phases formed and the PCT responses of samples heat treated according to the simulated Hanford HLW CCC temperature schedule.

The first phase of this study deployed a strategy of varying seven components of interest (Al2O3, B2O3, CaO, Fe2O3, Li2O, Na2O, SiO2) one-at-a-time around a baseline glass to formulate a total of 15 glass compositions. Only one glass from this study formed nepheline crystals during CCC heat treatment. This demonstrated that the HLW glass composition region for which nepheline-free glasses can be formulated was larger than expected but yielded little data useful for modeling. The Phase 2 nepheline study deployed the same one-component-at-a-time approach, but varied Al2O3, B2O3, Li2O, Na2O, and SiO2 around a revised baseline glass (BL3) that was adjusted so that roughly 10 to 15 mass% nepheline would form during CCC heat treatment. A total of 12 of the 14 unique glasses developed during Phase 2 precipitated nepheline upon CCC, and one of the two remaining glasses contained eucryptite.

The data from the first two phases showed that the composition region for which nepheline precipitated was not easily described by first order effects. In Phase 3, a statistical design surrounding the composition region generated two-at-a-time (2X) and three-at-a-time (3X) changes in Al2O3, B2O3, Li2O, Na2O, and SiO2 using the revised baseline glass (BL3) and lower and upper bounds of each component from the Phase 2 study. The 2X and 3X changes in all possible combinations of pairs or triples of components were made by a statistical program, JMP® version 13.0.0 [SAS Institute Inc. 2016] (JMP 13), and then the “net change” was distributed proportionally among the remaining components that were not involved in the 2X or 3X changes. JMP 13 chose six clusters of glasses from all the possible 2X and 3X combinations computed, from which one cluster of 16 glasses was selected to be tested. Results from Phases 1 through 3 are reported by Kroll et al. (2016).

Phase 4 of the study consisted of a matrix of 45 glasses that was statistically designed to cover the Hanford high-alumina composition region as efficiently as possible using an extreme vertices mixture design by varying Al2O3, B2O3, Bi2O3, CaO, Cr2O3, Fe2O3, Li2O, MgO, MnO, Na2O, P2O5, SiO2, and ZrO2 (Vienna et al. 2014). A total of 14 of the 45 glasses precipitated nepheline after CCC treatment.


Introduction 3

The Phase 5 study aimed at further expanding the dataset of glasses susceptible to nepheline formation, consisting of a set of 26 glasses developed by varying Al2O3, B2O3, CaO, Fe2O3, Li2O, Na2O, P2O5, SiO2, and an “Others” mixture all at the same time. JMP 13 was used to generate the compositions using a mixture design and space filling technique. Single- and multi-component constraints were used to set bounds on component concentrations and limit melt viscosity. A replicate of BL3 was also tested in this study. A total of 11 of the 26 glasses were found to precipitate nepheline upon CCC treatment. A more detailed description of the results from the Phase 5 study is given by Kroll et al. (2018).

The current study (Phase 6) also used JMP 13 statistical software to generate a matrix of 20 glasses using a space filling technique. The aim of this study was to refine the logistic regression sub-mixture model (see Stanfill et al. 2019) by filling in gaps of predicted nepheline formation probabilities. This report summarizes the results of the Phase 6 study, which primarily involves PCT and X-ray diffraction (XRD) analysis for quenched and CCC heat-treated glasses.

1.1 Quality Assurance

This work emphasized demonstrating proof of principle with the intent of solving a specific problem or meeting a practical need. The information associated with this report may be used to support design input.

1.1.1 PNNL QA Program

The Pacific Northwest National Laboratory (PNNL) Quality Assurance (QA) Program is based upon the requirements as defined in the DOE Order 414.1D, Quality Assurance, and 10 CFR 830, Energy/Nuclear Safety Management, Subpart A, “Quality Assurance Requirements” (a.k.a., the Quality Rule). PNNL has chosen to implement the following consensus standards in a graded approach:

ASME NQA-1-2000, Quality Assurance Requirements for Nuclear Facility Applications, Part I, “Requirements for Quality Assurance Programs for Nuclear Facilities”

ASME NQA-1-2000, Part II, Subpart 2.7, “Quality Assurance Requirements for Computer Software for Nuclear Facility Applications,” including problem reporting and corrective action

ASME NQA-1-2000, Part IV, Subpart 4.2, “Guidance on Graded Application of Quality Assurance (QA) for Nuclear-Related Research and Development.”

The PNNL Quality Assurance Program Description/Quality Management M&O Program Description describes the Laboratory-level QA program that applies to all work performed by PNNL. Laboratory-level procedures for implementing the QA requirements described in the standards identified above are deployed through PNNL’s web-based “How Do I…?” (HDI) system, a standards-based system for managing and deploying requirements and procedures to PNNL staff. The HDI procedures (called Workflows and Work Controls) provide detailed guidance for performing tasks, such as protecting classified information and procuring items and services, as well as general guidelines for performing research-related tasks, such as preparing and reviewing calculations and calibrating and controlling measuring and test equipment.

1.1.2 ORP Glass Support Work QA Program

The DOE Office of River Protection (ORP) Glass Support Work project is performed under the PNNL Nuclear Quality Assurance Program (NQAP); this program establishes an ASME NQA-1-2012, 10 CFR 830, Subpart A DOE Order (O) 414.1D compliant QA program for use by research and development (R&D) projects and programs that are compatible with the editions of ASME NQA-1 2000 through 2012.


Introduction 4

The work of this report was performed to the QA level of applied research:

Applied research work activities (or deliverables) apply to nuclear and non-nuclear R&D (work activities or deliverables) that are processes initiated-with-the-intent of solving a specific problem or meeting a practical need. For applied research activities, grading is minimal and largely contingent upon the complexity of the research and the ability to duplicate the research if data were lost. The elements of QA grading, including the level of documentation, were applied to the program-, project-, and task-levels.


Experimental Methods 5

2.0 Experimental Methods

The glasses formulated by statistical design were prepared by standard melt/quench protocols as described in Section 2.2. After preparation, the glasses were subjected to heat treatments and PCT, described in Sections 2.4 and 2.7, respectively, to understand crystal formation and its impacts on leaching response. Additionally, compositions were analyzed to ensure no errors in preparation occurred (procedures described in Section 2.3).

2.1 Composition Matrix Design The aim of this study was to refine the logistic regression sub-mixture model (see Stanfill et al. 2019) by filling in gaps of predicted nepheline formation probabilities. A matrix of 20 glasses was developed using a space-filling design technique with JMP™ version 13 statistical software. An in-depth description of the design effort was published in Piepel et al. (2018). Eight components, Al2O3, B2O3, CaO, Fe2O3, Li2O, Na2O, SiO2, and an “Others” mixture, were varied all-at-a-time. The composition of the Others mixture is listed in mass fraction in Table 1. Multi-component constraints were used to limit melt viscosity to the range of 4 to 10 Pa·s and the probability of nepheline formation as predicted by the logistic regression sub-mixture model to the range of 0.20 to 0.65. The lower and upper limits of the single-component constraints in mass fraction are shown in



Table 2. The 20 glass compositions tested in this study are presented in Table 3.

Table 1. Composition of “Others” mixture (in mass fraction).

Component Mass Fraction

Bi2O3 0.1498

Cr2O3 0.1835

F 0.0586

MgO 0.0234

MnO 0.2375

NiO 0.0215

P2O5 0.1727

PbO 0.0108

RuO2 0.0067

SO3 0.0540

SrO 0.0107

ZrO2 0.0705



Table 2. Upper and lower bounds for components (in mass fraction).

Component Lower Limit Upper Limit

Al2O3 0.2150 0.3200

B2O3 0.1400 0.2400

CaO 0.0000 0.0500

Fe2O3 0.0200 0.0500

Li2O 0.0000 0.0600

Na2O 0.0700 0.1600

SiO2 0.2250 0.3350

Others 0.0300 0.1200



Table 3. Compositions of 20 statistically designed glasses.

Glass ID Al2O3 B2O3 CaO Fe2O3 Li2O Na2O SiO2 Bi2O3 Cr2O3 F MgO MnO NiO P2O5 PbO RuO2 SO3 SrO ZrO2

NP6-01 0.2553 0.1966 0.0371 0.0337 0.0203 0.1266 0.2608 0.0104 0.0128 0.0041 0.0016 0.0165 0.0015 0.0120 0.0008 0.0005 0.0038 0.0007 0.0049

NP6-02 0.2626 0.1458 0.0190 0.0498 0.0567 0.0844 0.2664 0.0173 0.0212 0.0068 0.0027 0.0274 0.0025 0.0199 0.0012 0.0008 0.0062 0.0012 0.0081

NP6-03 0.3168 0.1612 0.0415 0.0222 0.0551 0.0754 0.2693 0.0088 0.0107 0.0034 0.0014 0.0139 0.0013 0.0101 0.0006 0.0004 0.0032 0.0006 0.0041

NP6-04 0.2158 0.1415 0.0441 0.0204 0.0588 0.1031 0.3319 0.0126 0.0155 0.0050 0.0020 0.0200 0.0018 0.0146 0.0009 0.0006 0.0046 0.0009 0.0059

NP6-05 0.2458 0.2004 0.0012 0.0489 0.0022 0.1583 0.2254 0.0176 0.0216 0.0069 0.0028 0.028 0.0025 0.0203 0.0013 0.0008 0.0064 0.0013 0.0083

NP6-06 0.3076 0.1918 0.0193 0.0405 0.0508 0.0980 0.2313 0.0091 0.0111 0.0036 0.0014 0.0144 0.0013 0.0105 0.0007 0.0004 0.0033 0.0006 0.0043

NP6-07 0.2327 0.1925 0.0157 0.0214 0.0163 0.1582 0.3259 0.0056 0.0068 0.0022 0.0009 0.0089 0.0008 0.0064 0.0004 0.0003 0.0020 0.0004 0.0026

NP6-08 0.2212 0.1695 0.0409 0.0482 0.0249 0.1438 0.318 0.0050 0.0061 0.0020 0.0008 0.0079 0.0007 0.0058 0.0004 0.0002 0.0018 0.0004 0.0024

NP6-09 0.2836 0.1583 0.0007 0.0456 0.0544 0.1142 0.3128 0.0046 0.0056 0.0018 0.0007 0.0072 0.0007 0.0053 0.0003 0.0002 0.0016 0.0003 0.0021

NP6-10 0.3167 0.2193 0.0139 0.0435 0.0263 0.1231 0.2258 0.0047 0.0058 0.0019 0.0007 0.0075 0.0007 0.0054 0.0003 0.0002 0.0017 0.0003 0.0022

NP6-11 0.2350 0.1684 0.0086 0.0276 0.0533 0.1233 0.3038 0.0120 0.0147 0.0047 0.0019 0.0190 0.0017 0.0138 0.0009 0.0005 0.0043 0.0009 0.0056

NP6-12 0.2533 0.1834 0.0124 0.0483 0.0400 0.1174 0.2917 0.008 0.0098 0.0032 0.0012 0.0127 0.0011 0.0092 0.0006 0.0004 0.0029 0.0006 0.0038

NP6-13 0.2633 0.2301 0.0079 0.0202 0.0236 0.1456 0.2271 0.0123 0.0151 0.0048 0.0019 0.0195 0.0018 0.0142 0.0009 0.0006 0.0044 0.0009 0.0058

NP6-14 0.2901 0.2079 0.0298 0.0206 0.0410 0.1135 0.2530 0.0066 0.0081 0.0026 0.0010 0.0105 0.0009 0.0076 0.0005 0.0003 0.0024 0.0005 0.0031

NP6-15 0.2829 0.1716 0.0447 0.0451 0.0347 0.0877 0.2277 0.0158 0.0194 0.0062 0.0025 0.0251 0.0023 0.0182 0.0011 0.0007 0.0057 0.0011 0.0075

NP6-16 0.2760 0.1873 0.0021 0.0230 0.0585 0.0953 0.2585 0.0149 0.0182 0.0058 0.0023 0.0236 0.0021 0.0171 0.0011 0.0007 0.0054 0.0011 0.0070

NP6-17 0.2232 0.1767 0.0438 0.0268 0.0030 0.1483 0.2669 0.0167 0.0204 0.0066 0.0026 0.0264 0.0024 0.0192 0.0012 0.0008 0.0060 0.0012 0.0078

NP6-18 0.2505 0.1530 0.0500 0.0375 0.0320 0.1016 0.2778 0.0146 0.0179 0.0057 0.0023 0.0232 0.0021 0.0168 0.0011 0.0007 0.0053 0.0010 0.0069

NP6-19 0.2704 0.2231 0.0356 0.0362 0.0043 0.1542 0.2375 0.0058 0.0071 0.0023 0.0009 0.0092 0.0008 0.0067 0.0004 0.0003 0.0021 0.0004 0.0027

NP6-20 0.2170 0.1508 0.0035 0.0236 0.0359 0.1355 0.3142 0.0179 0.0219 0.0070 0.0028 0.0284 0.0026 0.0206 0.0013 0.0008 0.0065 0.0013 0.0084



2.2 Glass Fabrication

Glasses were prepared in 200-g batches with oxides (Al Bi2O3, Cr2O3, Fe2O3, MnO, NiO, PbO, SiO2, and ZrO2) and carbonates (CaCO3, Li2CO3, Na2CO3, and SrCO3) for components shown above in Table 3. NaF, NaPO3, and Na2SO4 were used as the sources of F, P2O5, and SO3, respectively. Boric acid was used as the B2O3 source, and Al(OH)3 was chosen as the aluminum additive. RuO2 was added as 1.5% RuNO(NO3)3 solution dripped onto the necessary amount of SiO2 and placed in an oven for at least 2 h at 90 °C. Once dried, the SiO2 + RuO2 mixture was placed in a container with the rest of the chemicals and homogenized in a vibratory mill with an agate milling chamber for 4 min in two to four separate additions. Once mixed, the batch was added into a Pt-10%Rh crucible in two to four separate additions and melted at 1150 °C for 1 h. The melt was quenched by pouring onto a stainless-steel plate. After quenching, the glass was ground in the vibratory mill for 4 min, using a tungsten carbide chamber, and melted again at 1150°C for a second melt. After preparation, samples were either sent for chemical analysis (discussed further in Section 2.3) or prepared for heat treatment according to the HLW CCC profile (discussed further in Section 2.4)

2.3 Glass Composition Analysis

Glasses were analyzed by Savannah River National Laboratory (SRNL) and the results were published in Fox et al. (2019). Quenched samples were sent for inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and ion chromatography (IC). The low-level reference material was included in the analysis as a reference to ensure the proper operation of the ICP-AES and IC. Glasses were dissolved at SRNL according to the techniques listed in Table 4; more information can be found in Fox et al. 2019.

Table 4. Preparation and measurement methods used in reporting the concentrations of the analytes in this study (Fox et al. 2019).

Analyte Preparation

Method Measurement

Method Al PF ICP-AES B PF ICP-AES Bi LM ICP-AES Ca PF ICP-AES Cr PF ICP-AES F KH IC Fe LM ICP-AES Li PH ICP-AES Mg LM ICP-AES Mn PF ICP-AES Na LM ICP-AES Ni PF ICP-AES P PF ICP-AES Pb LM ICP-AES Ru LM ICP-AES S LM ICP-AES Si PF ICP-AES Sr LM ICP-AES Zr PF ICP-AES PF = sodium peroxide fusion KH = potassium hydroxide fusion LM = lithium metaborate fusion



2.4 Canister Centerline Cooling Heat Treatment

To perform the CCC heat treatment, a crushed sample of quenched glass with particles sized roughly 5 mm in diameter was placed in either a 1.2 × 1.2 × 1.2 cm or a 2.54 × 2.54 × 2.54 cm Pt-10% Rh foil crucible with a tight-fitting Pt-10% Rh foil lid. The glass-loaded crucibles were placed in a furnace preheated to the melt temperature (1150°C) and allowed to dwell for 30 min. Then, the furnace temperature was quickly reduced to 1050°C (at an estimated rate of -12.5°C/min) and cooled as prescribed in Table 5.

Table 5. CCC heat treatment schedule.

Segment Start Temp

(°C) Stop Temp

(°C) Rate

(°C/min)

1(a) 1150 1150 0.000(a)

2(b) 1150 1050 Free fall(b)

3 1050 980 -1.556

4 980 930 -0.806

5 930 875 -0.591

6 875 825 -0.388

7 825 775 -0.253

8 775 725 -0.278

9 725 400 -0.304

(a) Segment 1 is a 30-min dwell at the glass melt temperature (1150°C).

(b) Segment 2 free fall is at an estimated rate of -12.5°C/min.

When the furnace temperature was below 400°C (below the glass transition temperature), the furnace power was turned off and the glass cooled naturally to room temperature. This profile is the temperature schedule of CCC treatment for Hanford HLW glasses planned for use at WTP.1

2.5 Scanning Electron Microscopy Analysis

A JEOL 5900 scanning electron microscopy (SEM) instrument was used for the SEM images. Samples after quenching and post-CCC treatment were placed in Allied Technologies quickset epoxy to be mounted for polishing. Once mounted, samples were polished using silicon carbide polishing paper in the following grits: 320, 400, 600, 800, and 1200. After the final polishing pad, diamond suspension water-based polishing slurries from Allied Technologies were used to polish the samples to a 1-micron finish.

Once polished, the samples were coated with a 2.5-nm layer of platinum, and a strip of carbon tape was applied, to mitigate electron charge buildup during SEM analysis. Images were taken in backscatter mode and secondary mode.

1 Petkus LL. 2003. “Canister Centerline Cooling Data, Revision 1,” to C.A. Musick, CCN: 074851, October 29, 2003, River Protection Project, Hanford Tank Waste Treatment and Immobilization Plant, Richland, Washington.



2.6 X-Ray Diffraction Analysis

Crystal phase identification and quantification was performed on samples after quenching and after heat treatment. Quantitative XRD analysis of crystal concentration was completed by placing 1 to 3 g of each sub-sample in a 10-cm3 tungsten carbide milling chamber for 15 seconds. The glass sample was then doped with 5 wt% NIST (National Institute of Standards and Technology) 674b ZnO (used as an internal standard) and milled for another 45 seconds to combine the mixture. The XRD pattern was collected using a Bruker D8 Advance X-ray diffractometer (Bruker AXS Inc., Madison, WI, USA) equipped with a Cu-Kα target (λ = 1.5406 Å) with the following parameters: power level = 40 kV and 40 mA; goniometer radius = 250 mm, fixed divergence slit = 0.3°, and a LynxEye™ position-sensitive detector. The scan settings were as follows: range (2θ): 5 – 75°; step size (2θ): 0.015°; minimum hold time: 0.3 sec/step. Bruker AXS© EVA (Version 4) and Topas (Version 4.2) software programs were used to identify and quantify phase assemblages, respectively. Rietveld refinements were performed using whole pattern fitting according to the fundamental parameters approach. The database used for phase identification was the Inorganic Crystal Structure Database Version 2014-2.

2.7 Product Consistency Testing

PCT was performed at SRNL on three replicate samples from both as-quenched and CCC glasses according to Method A of ASTM-C-1285-14. The results of which were published in Fox et al. 2019. Bulk samples were ground and sieved to a particle size of 0.149 to 0.074 mm (-100 +200 mesh) and tested in stainless steel vessels at 90± 2 °C for 7 days (+/-2%). Fifteen milliliters of Type-I ASTM water and 1.5 g of sieved glass were placed into the vessels prior to testing. Also included in the experimental test matrix was the Approved Reference Material (ARM-1) glass, the environmental assessment (EA) benchmark glass (Jantzen et al. 1993) and blanks from the vessel cleaning batch.

After 7 days, the vessels were removed from the oven and allowed to cool to room temperature. After cooling, pH was measured on a small aliquot of the solution and the remaining solution was used to perform ICP-AES analyses. The solution for chemical analysis was filtered and acidified by adding 4 mL of 0.4M HNO3 to 6 mL of leachate (2:3 volume dilution). The leachates for the EA glass were further diluted with de-ionized (DI) water at a factor of 1 mL leachate to 10 mL of DI water.


Results and Discussion 12

3.0 Results and Discussion

The 20 glass compositions were analyzed as described in Section 2.3, and there was no indication of a mis-batch or significant error. The sums of the measured compositions for all glasses varied between 95.53% and 100.72%. The measurements summed for the total values are shown in Appendix A, Table A-1. Overall the Al2O3, Li2O, and Na2O concentrations were low (~ 6 relative wt% or less) for some of the glasses while Fe2O3 was higher than targeted (by less than 5 relative wt% difference). F and SO3 were low for most glasses which may indicate volatility during melting. Further comparisons can be made using the data in Table A-1.

3.1 Crystal Fraction Analysis Upon Quenching and Post-Canister Centerline Cooling Treatment

After melting, the quenched glasses were characterized using XRD to determine if any crystals developed during melting or upon cooling. All glasses contained crystals upon cooling in concentrations of about 6.5 wt% or less. Spinel was measured in every glass except NP6-20, which precipitated an iron silicate. The results are summarized in Table 6 and the XRD data can be found in Appendix B.

Table 6. Crystal identification and quantification in as-quenched glasses.

Glass ID Spinel (wt%)

Iron Silicon Oxide [Fe2SiO4]

(wt%) Total (wt%)

NP6-01 2.59 0 2.59 NP6-02 5.05 0 5.05 NP6-03 3.1 0 3.1 NP6-04 2.5 0 2.5 NP6-05 6.26 0 6.26 NP6-06 5.04 0 5.04 NP6-07 0.69 0 0.69 NP6-08 0.71 0 0.71 NP6-09 1.38 0 1.38 NP6-10 2.38 0 2.38 NP6-11 2.5 0 2.5 NP6-12 2.51 0 2.51 NP6-13 2.72 0 2.72 NP6-14 1.42 0 1.42 NP6-15 6.49 0 6.49 NP6-16 3.25 0 3.25 NP6-17 3.53 0 3.53 NP6-18 4.09 0 4.09 NP6-19 1.5 0 1.5 NP6-20 0 3.56 3.56

All glasses were then subjected to an HLW CCC heat treatment, as described in Section 2.4. After treatment, the glass was characterized by XRD to identify and quantify the crystals present in the glass. Table 7 shows the results for all 20 glasses investigated in this study.



Nepheline was found in 6 of the 20 glasses (NP6-4, 7, 8, 10, 19, and 20) while spinel was found in all but one (NP6-19). Additional phases present include hematite, various silicates, fluorapatite, and others that were in concentrations of less than 0.5 wt%. It is interesting to note that spinel precipitated in NP6-19 upon quenching, but after CCC spinel was not found in the sample, which instead crystallized out nepheline and hematite. Also shown below in Table 7 is the nepheline predictor which was determined for the glasses using a nonlinear, multi-component model described by Piepel et al. (2018).

Table 7. Crystal identification and quantification results using XRD for the glasses in this study post-CCC treatment.

Glass ID Nepheline

(wt%) Spinel (wt%)

Fluorapatite (wt%)

Silicate (variations)

(wt%) Hematite

(wt%) Others (wt%)

Total (wt%)

Nepheline Predictor

NP6-01 0 4.09 0 0 0 0.12 4.21 27.22 NP6-02 0 10.39 0 0 0 0 10.39 57.38 NP6-03 0 9.78 0 1.94 0 0.47 12.19 27.47 NP6-04 4.16 3.31 0 0 0 0.11 7.58 54.44 NP6-05 0 9.47 0 0 0 0.22 9.69 58.56 NP6-06 0 7.99 0 0 0 0.05 8.04 51.26 NP6-07 1.97 0.51 0 0 0 0.07 2.55 21.87 NP6-08 41.69 3.01 0 0 0 0 44.70 49.19 NP6-09 0 5.75 0 0 0 0 5.75 64.16 NP6-10 4.3 5.82 0 1.32 0 0 11.44 25.16 NP6-11 0 4.5 0 0 0 0.06 4.56 60.62 NP6-12 0 6.2 0 0 0 0.08 6.28 23.13 NP6-13 0 4.47 0 0 0 0.14 4.61 40.79 NP6-14 0 2.63 0 0 0 0 2.63 34.76 NP6-15 0 12 1.97 0 0 0.17 14.14 29.47 NP6-16 0 6.97 0 0 0 0.21 7.18 26.82 NP6-17 0 6.78 4.07 0 0 0 10.85 54.22 NP6-18 0 6.37 3.2 0 0 0 9.57 45.25 NP6-19 29.1 0 0 0 2.84 0 31.94 44.85 NP6-20 32.18 5.62 0 0 0 0.12 37.92 56.90

A key issue that this matrix was intended to address is the misclassification rate of glasses that will, or will not, crystallize nepheline. The nepheline predictor shows the estimated probability of nepheline formation for the glasses in the Phase 6 matrix and a plot of the probability versus the nepheline concentration after CCC is shown below.



Figure 1. Predicted probability of nepheline formation versus nepheline concentration, as determined by XRD. The highest concentrations of nepheline are found in the following CCC samples. X = NP6-20, □ – NP6-19, and ▼ = NP6-08. (Glasses in red precipitated nepheline upon CCC heat treatment while glasses represented by black circles did not.)

The prediction of nepheline behavior for this matrix is still not as accurate as needed, as seen by instances of no nepheline formation for glasses with high probabilities of predicted nepheline.

3.2 SEM Analysis

SEM images were taken of several quenched and CCC glasses to understand the morphology of the crystals present in the glass. Five quenched samples (NP6-05, 06, 08, 13, and 16) with a varying range of spinel concentrations, from 3.01 wt% to 7.99 wt%, were imaged with SEM; example images are provided in Figure 2. As noted in the XRD results, all the glasses mentioned above only precipitated spinel crystals upon cooling after melting.



Figure 2. SEM images, in secondary mode, of various quenched glasses.

All five glasses show similar spinel morphologies. Glass NP6-06 also contained a larger (10 µm × 20 µm), oval-shaped cluster of spinel crystals.

Six of the glasses subjected to the CCC treatment were imaged, and the results are shown in Figure 2. The images show spinel (small white features) formation along with nepheline (large gray features). The XRD of NP6-19 indicates no spinel was detected but hematite was present. NP6-8 and NP6-20 have darker



gray regions in the larger nepheline crystals, and it is unclear at this time what those features may be attributed to.

Figure 3. SEM images of several glasses after CCC heat treatments.

NP6-04-CCC

NP6-07-CCC

NP6-08-CCC

NP6-10-CCC

NP6-19-CCC

NP6-20-CCC



3.3 Product Consistency Testing Analysis

PCT was measured on quenched and heat-treated samples by SRNL as described in Section 2.7. Full experimental details and the testing results can be found in Fox et al. 2019.

The normalized release (NR) results, normalized to the target compositions, are shown in Table 8 for Li, B, Na, and Si for quenched and CCC samples of each glass.

Table 8. PCT method A release rates for B, Li, Na, and Si normalized to target compositions. Values below are averaged from the triplicate measurements (< = below detection limit).

Glass ID Status NRB (g/L) NRLi (g/L) NRNa (g/L) NRSi (g/L)

NP6-01 Quenched 0.898 0.895 0.777 0.251 NP6-01 CCC 0.850 0.740 0.586 0.146 NP6-02 Quenched 1.089 1.173 0.798 0.386 NP6-02 CCC 1.457 1.407 1.021 0.455 NP6-03 Quenched 0.880 1.003 0.723 0.256 NP6-03 CCC 0.760 0.646 0.471 0.116 NP6-04 Quenched 0.286 0.380 0.343 0.169 NP6-04 CCC 8.027 5.763 2.353 0.123 NP6-05 Quenched 4.677 3.685 3.448 0.209 NP6-05 CCC 6.756 5.155 4.416 0.228 NP6-06 Quenched 12.072 7.291 8.828 < 0.015 NP6-06 CCC 10.855 6.754 7.691 < 0.015 NP6-07 Quenched 2.069 1.756 1.369 0.283 NP6-07 CCC 2.068 1.817 1.062 0.187 NP6-08 Quenched 0.409 0.425 0.451 0.210 NP6-08 CCC 48.206 52.87 14.762 0.044 NP6-09 Quenched 1.278 1.350 0.800 0.545 NP6-09 CCC 2.901 2.003 1.074 0.448 NP6-10 Quenched 2.626 2.409 2.141 0.102 NP6-10 CCC 19.769 7.608 14.410 0.040 NP6-11 Quenched 1.457 1.343 0.985 0.423 NP6-11 CCC 4.058 2.766 1.433 0.226 NP6-12 Quenched 1.263 1.297 0.895 0.397 NP6-12 CCC 1.364 1.208 0.845 0.394 NP6-13 Quenched 5.923 5.199 4.467 < 0.016 NP6-13 CCC 20.172 8.493 14.427 < 0.016 NP6-14 Quenched 2.006 1.959 1.569 0.309 NP6-14 CCC 2.477 1.826 1.874 < 0.014 NP6-15 Quenched 0.880 0.918 0.817 0.172 NP6-15 CCC 1.250 1.223 1.049 0.249 NP6-16 Quenched 2.644 2.425 1.596 0.410 NP6-16 CCC 3.371 2.688 1.944 < 0.014 NP6-17 Quenched 0.750 < 1.196 0.721 0.250 NP6-17 CCC 1.533 1.599 1.197 0.305 NP6-18 Quenched 0.264 0.366 0.296 0.112 NP6-18 CCC 1.853 1.341 0.780 0.053 NP6-19 Quenched 1.933 1.744 1.763 0.228 NP6-19 CCC 60.847 3.937 38.852 0.071 NP6-20 Quenched 0.978 0.964 0.728 0.408 NP6-20 CCC 61.083 34.349 17.575 0.116



The highest boron releases for CCC samples were found for the following compositions, starting with the largest value: NP6-20 (61.1 g/L), NP6-19 (60.8 g/L), and NP6-08 (48.2 g/L), which coincide with the glasses that contained the largest amount of nepheline after the CCC heat treatment. The boron normalized release rates for quenched glasses are compared to the heat-treated glasses in Figure 4.

Figure 4. Boron ln(NR) rates for quenched glasses versus CCC glasses. Glasses in red precipitated nepheline upon CCC heat treatment while the black circles did not. X = NP6-20, □ – NP6-19, and ▼ = NP6-08.

There appears to be no clear correlation between normalized release for quenched vs. CCC glasses. In general, the nepheline-containing glasses (in red) have significantly higher CCC NR values compared to the quenched glasses (Figure 5).



Figure 5. A plot of the difference in crystal concentrations (CCC minus quenched values) vs. the difference in normalized B release values for CCC glasses minus quenched glasses. Glasses in red precipitated nepheline upon CCC heat treatment and glasses presented in black did not. X = NP6-20, □ – NP6-19, and ▼ = NP6-08.

There is a clear indication that higher levels of crystals tend to have a higher boron release in the CCC PCT analysis, particularly as compared to the quenched NRB values. As seen in Figure 5, the glasses with the highest releases are NP6-08, NP6-19, and NP6-20, which also have the highest nepheline/crystal concentrations.

It is interesting to note that only five of the CCC glasses exceeded the EA benchmark value (16.695 g/L) for normalized boron release. All the glasses with elevated boron release, NP6-(8, 10, 13, 19, and 20)-CCC, contained nepheline upon CCC treatment except for NP6-13, which only precipitated spinel in the as-quenched and post-CCC sample. This is noteworthy as there are other glasses that precipitated nepheline during CCC but did not exceed 16.695 g/L for boron response, and NP6-13 contained no nepheline and exhibited a high normalized release value (NRB = 20.17 g/L).

The glasses with higher releases had relatively high concentrations of Na2O. Additionally, the glasses had less than 6 wt% spinel after CCC as well as less than 3 wt% spinel upon quenching, but other glasses with lower release rates exhibited similar behavior. Further work is recommended to understand this response.


Summary 20

4.0 Summary

Glasses in a matrix developed via a space-filling design were subjected to CCC heat treatments and analyzed using XRD and SEM and tested for the PCT response. The nepheline predictor established that use of previous data did not predict the formation of nepheline well, as this was a compositional region in a highly misclassified compositional space.

XRD results showed that nepheline formed in only 6 of the 20 glasses after heat treatment, while all but one of the glasses contained spinel upon quenching and after heat treatment. SEM confirmed the presence of spinel upon quenching and the presence of spinel inside of the nepheline crystals after CCC.

Interestingly, only 5 of the 20 glasses exceeded the EA PCT response for boron release. While all six glasses that precipitated nepheline upon CCC had relatively higher release rates compared to their quenched counterparts, one of the five glasses exceeding the EA response did not contain nepheline. This result should be investigated further as it would be expected that the presence of nepheline would result in poor performance for PCT.


References 21

5.0 References

ASTM. 2014. Standard Test Methods for Determining Chemical Durability of Nuclear Waste Glasses: The Product Consistency Test (PCT). ASTM C-1285, ASTM International. West Conshohocken, Pennsylvania.

DOE 2000. Design, Construction, and Commissioning of the Hanford Tank Waste Treatment and Immobilization Plant. U.S. Department of Energy, Office of River Protection, Richland, Washington.

Fox KM, TB Edwards, MC Hsieh, and WT Riley. 2019. Chemical Composition Analysis and Product Consistency Tests of the ORP Phase 6 Nepheline Study Glasses. SRNL-STI-2018-00645, Rev. 0, Savannah River National Laboratory, Aiken, South Carolina.

Jantzen CM, NE Bibler, DC Beam, CL Crawford, and MA Pickett. 1993. Characterization of the Defense Waste Processing Facility (DWPF) Environmental Assessment (EA) Glass Standard Reference Material. WSRC-TR-92-346, Rev. 1, Westinghouse Savannah River Company, Aiken, South Carolina.

JMP™ Pro, Ver. 13.0, Computer Software, SAS Institute Inc., Cary, NC (2016).

Kim D-S, D Peeler, and P Hrma. 1995. “Effect of Crystallization on the Chemical Durability of Simulated Nuclear Waste Glasses.” Ceramic Transactions 61:177-185.

Kroll JO, JD Vienna, MJ Schweiger, GF Piepel, and SK Cooley. 2016. Results from Phase 1, 2, and 3 Studies on Nepheline Formation in High-Level Waste Glasses Containing High Concentrations of Alumina. PNNL-26057, Rev. 0.0; EWG-RPT-011, Rev. 0.0, Pacific Northwest National Laboratory, Richland, Washington.

Kroll JO, JD Vienna, ZJ Nelson, and CH Skidmore. 2018. Results from Phase 5 Study on Nepheline Formation in High-Level Waste Glasses Containing High Concentrations of Alumina. PNNL-27555, Rev. 0.0; EWG-RPT-017, Rev0.0, Pacific Northwest National Laboratory, Richland, Washington.

Li H, JD Vienna, P Hrma, DE Smith, and MJ Schweiger. 1997. “Nepheline Precipitation in High-Level Waste Glasses: Compositional Effects and Impact on the Waste Form Acceptability.” Scientific Basis for Nuclear Waste Management XX 465:261-268. Materials Research Society, Pittsburgh, Pennsylvania.

McCloy JS and JD Vienna. 2010. “Glass Composition Constraint Recommendations for Use in Life-Cycle Mission Modeling.” PNNL-19372. Pacific Northwest National Laboratory, Richland, Washington. Available at https://www.pnnl.gov/main/publications/external/technical_reports/PNNL-19372.pdf.

McCloy JS, MJ Schweiger, CP Rodriguez, and JD Vienna. 2011. “Nepheline Crystallization in Nuclear Waste Glasses: Progress toward Acceptance of High-Alumina Formulations.” International Journal of Applied Glass Science 2(3):201-214. Available at http://onlinelibrary.wiley.com/doi/10.1111/j.2041-1294.2011.00055.x/full.

Piepel GF, BA Stanfill, SK Cooley, B Jones, JO Kroll, and JD Vienna. 2018. “Developing a space-filling mixture experiment design when the components are subject to linear and nonlinear constraints” Quality Engineering. https://doi.org/10.1080/08982112.2018.1517887

Rodriguez CP, JS McCloy, MJ Schweiger, JV Crum, and A Winschell. 2011. Optical Basicity and Nepheline Crystallization in High Alumina Glasses. PNNL-20184. Pacific Northwest National


References 22

Laboratory, Richland, Washington. Available at http://www.pnnl.gov/main/publications/external/technical_reports/PNNL-20184.pdf.

Stanfill BA, GF Piepel, JD Vienna, and SK Cooley. 2019. “Nonlinear logistic regression mixture experiment modelling for binary data using dimensionally-reduced components.” Quality and Reliability Engineering International. Submitted.

Vienna JD, D-S Kim, DC Skorski, and J Matyas. 2013. Glass Property Models and Constraints for Estimating the Glass to Be Produced at Hanford by Implementing Current Advanced Glass Formulation Efforts. PNNL-22631, Rev. 1; ORP-58289, Pacific Northwest National Laboratory, Richland, Washington. Available at http://www.pnnl.gov/main/publications/external/technical_reports/PNNL-22631Rev1.pdf.

Vienna JD, D-S Kim, MJ Schweiger, GF Piepel, JO Kroll, and AA Kruger. 2014. Glass Formulation and Testing for U.S. High-Level Tank Wastes Project 17210 Year 1 Status Report: October 15, 2014. PNNL-SA-84872, Pacific Northwest National Laboratory, Richland, Washington. Available at https://www.hanford.gov/files.cfm/Glass_Formulation_Year_1_Report_Final_10-15-14,_PNNL-SA-84872.pdf.

Vienna JD, GF Piepel, DS Kim, JV Crum, CE Lonergan, BA Stanfill, BJ Riley, SK Cooley, and T Jin. 2016. Update of Hanford Glass Property Models and Constraints for Use in Estimating the Glass Mass to be Produced at Hanford by Implementing Current Enhanced Glass Formulation Efforts. PNNL-25835, Pacific Northwest National Laboratory, Richland, Washington. Available at http://www.pnnl.gov/main/publications/external/technical_reports/PNNL-25835.pdf.

Vienna JD, JO Kroll, PR Hrma, JB Lang, and JV Crum. 2017. “Submixture Model to Predict Nepheline Precipitation in Waste Glasses.” International Journal of Applied Glass Science 8(2):143-157. DOI: 10.1111/ijag.12207


Appendix A A.1

Appendix A – Measured and Targeted Glass Compositions

This appendix contains the compositional data measured and reported by SRNL in SRNL-STI-2018-00645 (Fox et al. 2019). BDL = below detection limit.

Table A-1: Comparison of targeted and measured glass compositions

Glass ID

Oxide

BDL (<)

Measured (wt %)

Targeted (wt %)

Difference of Measured versus

Targeted

% Difference of Measured versus

Targeted LRM Al2O3 9.353 9.510 -0.157 -1.7% LRM B2O3 7.447 7.850 -0.403 -5.1% LRM Bi2O3 < 0.112 0.000 0.112

LRM CaO 0.215 0.540 -0.325

LRM Cr2O3 < 0.146 0.190 -0.044

LRM F 0.910 0.860 0.050

LRM Fe2O3 1.371 1.380 -0.009

LRM Li2O < 0.215 0.110 0.105

LRM MgO < 0.166 0.100 0.066

LRM MnO < 0.129 0.080 0.049

LRM Na2O 20.033 20.030 0.003 0.0% LRM NiO < 0.127 0.190 -0.063

LRM P2O5 0.346 0.540 -0.194

LRM PbO 0.092 0.100 -0.008

LRM RuO2 < 0.066 0.000 0.066

LRM SiO2 54.707 54.200 0.507 0.9% LRM SO3 0.220 0.300 -0.080

LRM SrO < 0.059 0.000 0.059

LRM ZrO2 0.928 0.930 -0.002

LRM Sum 96.642 96.910 -0.268 -0.3% NP6-01 Al2O3 24.753 25.500 -0.747 -2.9% NP6-01 B2O3 19.601 19.660 -0.059 -0.3% NP6-01 Bi2O3 0.993 1.040 -0.047

NP6-01 CaO 3.893 3.710 0.183

NP6-01 Cr2O3 1.284 1.280 0.004

NP6-01 F 0.252 0.410 -0.158

NP6-01 Fe2O3 3.903 3.370 0.533

NP6-01 Li2O 1.926 2.030 -0.104

NP6-01 MgO 0.181 0.160 0.021

NP6-01 MnO 1.617 1.650 -0.033

NP6-01 Na2O 12.277 12.660 -0.383 -3.0% NP6-01 NiO < 0.127 0.150 -0.023

NP6-01 P2O5 1.065 1.200 -0.135

NP6-01 PbO 0.079 0.080 -0.001

NP6-01 RuO2 < 0.066 0.050 0.016

NP6-01 SiO2 26.206 26.080 0.126 0.5% NP6-01 SO3 0.328 0.380 -0.052

NP6-01 SrO 0.065 0.070 -0.005

NP6-01 ZrO2 0.443 0.490 -0.047

NP6-01 Sum 99.060 99.970 -0.910 -0.9% NP6-02 Al2O3 25.556 26.300 -0.745 -2.8% NP6-02 B2O3 14.699 14.580 0.119 0.8% NP6-02 Bi2O3 1.413 1.730 -0.317

NP6-02 CaO 1.913 1.900 0.013

NP6-02 Cr2O3 2.035 2.120 -0.085

NP6-02 F 0.461 0.680 -0.219

NP6-02 Fe2O3 5.122 4.980 0.142

NP6-02 Li2O 5.285 5.670 -0.385 -6.8%


Appendix A A.2

Table A-1: Comparison of targeted and measured glass compositions; continued.

Glass ID

Oxide

BDL (<)

Measured (wt %)

Targeted (wt %)


Targeted


Targeted NP6-02 MgO 0.267 0.270 -0.003

NP6-02 MnO 2.718 2.740 -0.022

NP6-02 Na2O 8.122 8.440 -0.318 -3.8%

NP6-02 NiO < 0.127 0.250 -0.123

NP6-02 P2O5 1.644 1.990 -0.346

NP6-02 PbO 0.114 0.120 -0.006

NP6-02 RuO2 < 0.066 0.080 -0.014

NP6-02 SiO2 27.223 26.640 0.583 2.2% NP6-02 SO3 0.501 0.620 -0.119

NP6-02 SrO 0.119 0.120 -0.001

NP6-02 ZrO2 0.591 0.810 -0.219

NP6-02 Sum 97.976 100.040 -2.064 -2.1% NP6-03 Al2O3 29.618 31.700 -2.082 -6.6% NP6-03 B2O3 15.633 16.120 -0.487 -3.0% NP6-03 Bi2O3 0.858 0.880 -0.022

NP6-03 CaO 4.117 4.150 -0.033

NP6-03 Cr2O3 0.955 1.070 -0.115

NP6-03 F 0.270 0.340 -0.071

NP6-03 Fe2O3 2.577 2.220 0.357

NP6-03 Li2O 4.989 5.510 -0.521 -9.5% NP6-03 MgO 0.175 0.140 0.035

NP6-03 MnO 1.298 1.390 -0.092

NP6-03 Na2O 7.299 7.540 -0.241 -3.2% NP6-03 NiO < 0.127 0.130 -0.003

NP6-03 P2O5 0.758 1.010 -0.252

NP6-03 PbO 0.061 0.060 0.001

NP6-03 RuO2 < 0.066 0.040 0.026

NP6-03 SiO2 26.313 26.930 -0.617 -2.3% NP6-03 SO3 0.297 0.320 -0.023

NP6-03 SrO < 0.059 0.060 -0.001

NP6-03 ZrO2 0.310 0.410 -0.100


NP6-04 CaO 4.715 4.410 0.305

NP6-04 Cr2O3 1.481 1.550 -0.069

NP6-04 F 0.370 0.500 -0.130

NP6-04 Fe2O3 2.459 2.040 0.419

NP6-04 Li2O 5.555 5.880 -0.326 -5.5% NP6-04 MgO 0.221 0.200 0.021

NP6-04 MnO 1.969 2.000 -0.031

NP6-04 Na2O 9.982 10.310 -0.328 -3.2% NP6-04 NiO < 0.127 0.180 -0.053

NP6-04 P2O5 1.323 1.460 -0.137

NP6-04 PbO 0.086 0.090 -0.004

NP6-04 RuO2 < 0.066 0.060 0.006

NP6-04 SiO2 33.587 33.190 0.397 1.2% NP6-04 SO3 0.403 0.460 -0.057

NP6-04 SrO 0.088 0.090 -0.003

NP6-04 ZrO2 0.565 0.590 -0.025

NP6-04 Sum 99.458 100.020 -0.562 -0.6% NP6-05 Al2O3 24.564 24.600 -0.037 -0.1%


Appendix A A.3


Glass ID

Oxide

BDL (<)

Measured (wt %)

Targeted (wt %)


Targeted


Targeted NP6-05 B2O3 20.599 20.040 0.559 2.8%

NP6-05 Bi2O3 1.499 1.760 -0.261

NP6-05 CaO < 0.070 0.120 -0.050

NP6-05 Cr2O3 2.068 2.160 -0.092

NP6-05 F 0.488 0.690 -0.202

NP6-05 Fe2O3 5.011 4.890 0.121

NP6-05 Li2O < 0.215 0.220 -0.005

NP6-05 MgO 0.267 0.280 -0.013

NP6-05 MnO 2.825 2.800 0.025

NP6-05 Na2O 15.131 15.830 -0.699 -4.4% NP6-05 NiO < 0.127 0.250 -0.123

NP6-05 P2O5 1.766 2.030 -0.264

NP6-05 PbO 0.125 0.130 -0.005

NP6-05 RuO2 < 0.066 0.080 -0.014

NP6-05 SiO2 23.479 22.540 0.939 4.2% NP6-05 SO3 0.488 0.640 -0.153

NP6-05 SrO 0.129 0.130 -0.001

NP6-05 ZrO2 0.613 0.830 -0.217


NP6-06 CaO 1.784 1.930 -0.146

NP6-06 Cr2O3 1.011 1.110 -0.099

NP6-06 F 0.245 0.360 -0.115

NP6-06 Fe2O3 4.471 4.050 0.421

NP6-06 Li2O 4.763 5.080 -0.317 -6.2% NP6-06 MgO < 0.166 0.140 0.026

NP6-06 MnO 1.353 1.440 -0.087

NP6-06 Na2O 9.729 9.800 -0.071 -0.7% NP6-06 NiO < 0.127 0.130 -0.003

NP6-06 P2O5 0.808 1.050 -0.242

NP6-06 PbO 0.076 0.070 0.006

NP6-06 RuO2 < 0.066 0.040 0.026

NP6-06 SiO2 22.409 23.130 -0.721 -3.1% NP6-06 SO3 0.288 0.330 -0.042

NP6-06 SrO < 0.059 0.060 -0.001

NP6-06 ZrO2 0.320 0.430 -0.110


NP6-07 CaO 1.404 1.570 -0.166

NP6-07 Cr2O3 0.663 0.680 -0.017

NP6-07 F 0.168 0.220 -0.052

NP6-07 Fe2O3 2.588 2.140 0.448

NP6-07 Li2O 1.497 1.630 -0.133

NP6-07 MgO < 0.166 0.090 0.076

NP6-07 MnO 0.831 0.890 -0.059

NP6-07 Na2O 14.997 15.820 -0.824 -5.2% NP6-07 NiO < 0.127 0.080 0.047

NP6-07 P2O5 0.445 0.640 -0.196


Appendix A A.4


Glass ID

Oxide

BDL (<)

Measured (wt %)

Targeted (wt %)


Targeted


Targeted NP6-07 PbO 0.036 0.040 -0.004

NP6-07 RuO2 < 0.066 0.030 0.036

NP6-07 SiO2 31.662 32.590 -0.928 -2.8% NP6-07 SO3 0.195 0.200 -0.005

NP6-07 SrO < 0.059 0.040 0.019

NP6-07 ZrO2 0.295 0.260 0.035


NP6-08 CaO 4.061 4.090 -0.029

NP6-08 Cr2O3 0.506 0.610 -0.104

NP6-08 F 0.161 0.200 -0.039

NP6-08 Fe2O3 5.093 4.820 0.273

NP6-08 Li2O 2.255 2.490 -0.235

NP6-08 MgO < 0.166 0.080 0.086

NP6-08 MnO 0.718 0.790 -0.072

NP6-08 Na2O 13.716 14.380 -0.664 -4.6% NP6-08 NiO < 0.127 0.070 0.057

NP6-08 P2O5 0.315 0.580 -0.266

NP6-08 PbO 0.044 0.040 0.004

NP6-08 RuO2 < 0.066 0.020 0.046

NP6-08 SiO2 30.699 31.800 -1.101 -3.5% NP6-08 SO3 0.185 0.180 0.005

NP6-08 SrO < 0.059 0.040 0.019

NP6-08 ZrO2 0.154 0.240 -0.086


NP6-09 CaO < 0.070 0.070 0.000

NP6-09 Cr2O3 0.546 0.560 -0.014

NP6-09 F 0.118 0.180 -0.063

NP6-09 Fe2O3 4.832 4.560 0.272

NP6-09 Li2O 5.113 5.440 -0.327 -6.0% NP6-09 MgO < 0.166 0.070 0.096

NP6-09 MnO 0.692 0.720 -0.028

NP6-09 Na2O 11.033 11.420 -0.387 -3.4% NP6-09 NiO < 0.127 0.070 0.057

NP6-09 P2O5 0.427 0.530 -0.103

NP6-09 PbO 0.034 0.030 0.004

NP6-09 RuO2 < 0.066 0.020 0.046

NP6-09 SiO2 31.341 31.280 0.061 0.2% NP6-09 SO3 0.149 0.160 -0.011

NP6-09 SrO < 0.059 0.030 0.029

NP6-09 ZrO2 0.175 0.210 -0.035


NP6-10 CaO 1.184 1.390 -0.206


Appendix A A.5


Glass ID

Oxide

BDL (<)

Measured (wt %)

Targeted (wt %)


Targeted


Targeted NP6-10 Cr2O3 0.522 0.580 -0.058

NP6-10 F 0.150 0.190 -0.040

NP6-10 Fe2O3 4.632 4.350 0.282

NP6-10 Li2O 2.411 2.630 -0.219

NP6-10 MgO < 0.166 0.070 0.096

NP6-10 MnO 0.688 0.750 -0.062

NP6-10 Na2O 12.277 12.310 -0.033 -0.3% NP6-10 NiO < 0.127 0.070 0.057

NP6-10 P2O5 0.355 0.540 -0.185

NP6-10 PbO 0.036 0.030 0.006

NP6-10 RuO2 < 0.066 0.020 0.046

NP6-10 SiO2 22.409 22.580 -0.171 -0.8% NP6-10 SO3 0.159 0.170 -0.011

NP6-10 SrO < 0.059 0.030 0.029

NP6-10 ZrO2 0.140 0.220 -0.080


NP6-11 CaO 0.684 0.860 -0.176

NP6-11 Cr2O3 1.412 1.470 -0.059

NP6-11 F 0.355 0.470 -0.115

NP6-11 Fe2O3 3.167 2.760 0.407

NP6-11 Li2O 4.882 5.330 -0.448 -8.4% NP6-11 MgO 0.190 0.190 -0.001

NP6-11 MnO 1.837 1.900 -0.063

NP6-11 Na2O 12.044 12.330 -0.286 -2.3% NP6-11 NiO < 0.127 0.170 -0.043

NP6-11 P2O5 1.159 1.380 -0.221

NP6-11 PbO 0.078 0.090 -0.012

NP6-11 RuO2 < 0.066 0.050 0.016

NP6-11 SiO2 30.218 30.380 -0.162 -0.5% NP6-11 SO3 0.381 0.430 -0.049

NP6-11 SrO 0.091 0.090 0.001

NP6-11 ZrO2 0.583 0.560 0.023


NP6-12 CaO 1.153 1.240 -0.087

NP6-12 Cr2O3 0.990 0.980 0.010

NP6-12 F 0.219 0.320 -0.101

NP6-12 Fe2O3 5.201 4.830 0.371

NP6-12 Li2O 3.940 4.000 -0.060

NP6-12 MgO < 0.166 0.120 0.046

NP6-12 MnO 1.284 1.270 0.014

NP6-12 Na2O 11.579 11.740 -0.161 -1.4% NP6-12 NiO < 0.127 0.110 0.017

NP6-12 P2O5 0.836 0.920 -0.084

NP6-12 PbO 0.064 0.060 0.004

NP6-12 RuO2 < 0.066 0.040 0.026


Appendix A A.6


Glass ID

Oxide

BDL (<)

Measured (wt %)

Targeted (wt %)


Targeted


Targeted NP6-12 SiO2 30.004 29.170 0.834 2.9% NP6-12 SO3 0.263 0.290 -0.027

NP6-12 SrO < 0.059 0.060 -0.001

NP6-12 ZrO2 0.330 0.380 -0.050

NP6-12 Sum 100.719 99.970 0.749 0.7% NP6-13 Al2O3 25.272 26.300 -1.028 -3.9% NP6-13 B2O3 22.733 23.010 -0.278 -1.2% NP6-13 Bi2O3 1.193 1.230 -0.037

NP6-13 CaO 0.490 0.790 -0.300

NP6-13 Cr2O3 1.485 1.510 -0.025

NP6-13 F 0.348 0.480 -0.132

NP6-13 Fe2O3 2.495 2.020 0.475

NP6-13 Li2O 2.254 2.360 -0.106

NP6-13 MgO 0.186 0.190 -0.004

NP6-13 MnO 1.885 1.950 -0.065

NP6-13 Na2O 14.154 14.560 -0.406 -2.8% NP6-13 NiO < 0.127 0.180 -0.053

NP6-13 P2O5 1.170 1.420 -0.250

NP6-13 PbO 0.079 0.090 -0.011

NP6-13 RuO2 < 0.066 0.060 0.006

NP6-13 SiO2 22.281 22.710 -0.429 -1.9% NP6-13 SO3 0.366 0.440 -0.074

NP6-13 SrO 0.088 0.090 -0.002

NP6-13 ZrO2 0.597 0.580 0.017


NP6-14 CaO 2.924 2.980 -0.056

NP6-14 Cr2O3 0.737 0.810 -0.073

NP6-14 F 0.198 0.260 -0.062

NP6-14 Fe2O3 2.581 2.060 0.521

NP6-14 Li2O 3.859 4.100 -0.241

NP6-14 MgO < 0.166 0.100 0.066

NP6-14 MnO 0.993 1.050 -0.057

NP6-14 Na2O 11.357 11.350 0.007 0.1% NP6-14 NiO < 0.127 0.090 0.037

NP6-14 P2O5 0.542 0.760 -0.218

NP6-14 PbO 0.053 0.050 0.003

NP6-14 RuO2 < 0.066 0.030 0.036

NP6-14 SiO2 25.030 25.300 -0.270 -1.1% NP6-14 SO3 0.228 0.240 -0.013

NP6-14 SrO < 0.059 0.050 0.009

NP6-14 ZrO2 0.208 0.310 -0.102


NP6-15 CaO 4.680 4.470 0.210

NP6-15 Cr2O3 1.849 1.940 -0.091

NP6-15 F 0.353 0.620 -0.267


Appendix A A.7


Glass ID

Oxide

BDL (<)

Measured (wt %)

Targeted (wt %)


Targeted


Targeted NP6-15 Fe2O3 4.743 4.510 0.233

NP6-15 Li2O 3.380 3.470 -0.090

NP6-15 MgO 0.263 0.250 0.013

NP6-15 MnO 2.469 2.510 -0.041

NP6-15 Na2O 8.476 8.770 -0.294 -3.4% NP6-15 NiO < 0.127 0.230 -0.103

NP6-15 P2O5 1.572 1.820 -0.248

NP6-15 PbO 0.107 0.110 -0.003

NP6-15 RuO2 < 0.066 0.070 -0.004

NP6-15 SiO2 23.104 22.770 0.334 1.5% NP6-15 SO3 0.466 0.570 -0.104

NP6-15 SrO 0.108 0.110 -0.002

NP6-15 ZrO2 0.571 0.750 -0.179


NP6-16 CaO < 0.070 0.210 -0.140

NP6-16 Cr2O3 1.739 1.820 -0.081

NP6-16 F 0.446 0.580 -0.135

NP6-16 Fe2O3 2.716 2.300 0.416

NP6-16 Li2O 5.398 5.850 -0.452 -7.7% NP6-16 MgO 0.222 0.230 -0.008

NP6-16 MnO 2.305 2.360 -0.055

NP6-16 Na2O 9.170 9.530 -0.360 -3.8% NP6-16 NiO < 0.127 0.210 -0.083

NP6-16 P2O5 1.373 1.710 -0.338

NP6-16 PbO 0.094 0.110 -0.016

NP6-16 RuO2 < 0.066 0.070 -0.004

NP6-16 SiO2 25.779 25.850 -0.071 -0.3% NP6-16 SO3 0.442 0.540 -0.098

NP6-16 SrO 0.111 0.110 0.001

NP6-16 ZrO2 0.532 0.700 -0.168


NP6-17 CaO 4.439 4.380 0.059

NP6-17 Cr2O3 1.886 2.040 -0.155

NP6-17 F 0.457 0.660 -0.203

NP6-17 Fe2O3 3.056 2.680 0.376

NP6-17 Li2O 0.234 0.300 -0.066

NP6-17 MgO 0.290 0.260 0.030

NP6-17 MnO 2.482 2.640 -0.158

NP6-17 Na2O 14.120 14.830 -0.710 -4.8% NP6-17 NiO < 0.127 0.240 -0.113

NP6-17 P2O5 1.382 1.920 -0.538

NP6-17 PbO 0.119 0.120 -0.001

NP6-17 RuO2 < 0.066 0.080 -0.014

NP6-17 SiO2 26.206 26.690 -0.484 -1.8%


Appendix A A.8


Glass ID

Oxide

BDL (<)

Measured (wt %)

Targeted (wt %)


Targeted


Targeted

NP6-17 SO3 0.487 0.600 -0.113

NP6-17 SrO 0.116 0.120 -0.004

NP6-17 ZrO2 0.320 0.780 -0.460


NP6-18 CaO 5.331 5.000 0.331 6.6% NP6-18 Cr2O3 1.750 1.790 -0.040

NP6-18 F 0.438 0.570 -0.132

NP6-18 Fe2O3 4.193 3.750 0.443

NP6-18 Li2O 3.111 3.200 -0.089

NP6-18 MgO 0.248 0.230 0.018

NP6-18 MnO 2.256 2.320 -0.064

NP6-18 Na2O 9.911 10.160 -0.249 -2.4% NP6-18 NiO < 0.127 0.210 -0.083

NP6-18 P2O5 1.394 1.680 -0.286

NP6-18 PbO 0.100 0.110 -0.010

NP6-18 RuO2 < 0.066 0.070 -0.004

NP6-18 SiO2 27.811 27.780 0.031 0.1% NP6-18 SO3 0.449 0.530 -0.081

NP6-18 SrO 0.102 0.100 0.002

NP6-18 ZrO2 0.653 0.690 -0.037


NP6-19 CaO 3.613 3.560 0.053

NP6-19 Cr2O3 0.671 0.710 -0.040

NP6-19 F 0.134 0.230 -0.097

NP6-19 Fe2O3 3.960 3.620 0.340

NP6-19 Li2O 0.367 0.430 -0.064

NP6-19 MgO < 0.166 0.090 0.076

NP6-19 MnO 0.863 0.920 -0.057

NP6-19 Na2O 14.727 15.420 -0.693 -4.5% NP6-19 NiO < 0.127 0.080 0.047

NP6-19 P2O5 0.454 0.670 -0.216

NP6-19 PbO 0.039 0.040 -0.001

NP6-19 RuO2 < 0.066 0.030 0.036

NP6-19 SiO2 23.104 23.750 -0.646 -2.7% NP6-19 SO3 0.166 0.210 -0.045

NP6-19 SrO < 0.059 0.040 0.019

NP6-19 ZrO2 0.304 0.270 0.034


NP6-20 CaO < 0.093 0.350 -0.257

NP6-20 Cr2O3 1.999 2.190 -0.191

NP6-20 F 0.515 0.700 -0.185


Appendix A A.9


Glass ID

Oxide

BDL (<)

Measured (wt %)

Targeted (wt %)


Targeted


Targeted

NP6-20 Fe2O3 2.677 2.360 0.317

NP6-20 Li2O 3.402 3.590 -0.188

NP6-20 MgO 0.289 0.280 0.009

NP6-20 MnO 2.683 2.840 -0.158

NP6-20 Na2O 13.322 13.550 -0.228 -1.7% NP6-20 NiO < 0.127 0.260 -0.133

NP6-20 P2O5 1.456 2.060 -0.604

NP6-20 PbO 0.131 0.130 0.001

NP6-20 RuO2 < 0.066 0.080 -0.014

NP6-20 SiO2 31.020 31.420 -0.400 -1.3% NP6-20 SO3 0.600 0.650 -0.050

NP6-20 SrO 0.124 0.130 -0.006

NP6-20 ZrO2 0.390 0.840 -0.450

NP6-20 Sum 96.075 100.000 -3.926 -3.9%


Appendix B B.1

Appendix B – X-Ray Diffraction Data

This appendix contains the data obtained from measurement of quenched and post-canister centerline cooling (CCC) glasses by X-ray diffraction (XRD).

B.1 XRD of Quenched Glasses

Figure B.1. XRD data for NP6-01-Q

01-075-3306 (*) - Chromite - (Fe.6Mg.4)Cr2O4 - Y: 42.08 % - a 8.35770 - b 8.35770 - c 8.35770 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 4.3

01-070-8070 (*) - Zinc Oxide - ZnO - Y: 101.59 % - a 3.24890 - b 3.24890 - c 5.20490 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63mc (186) - I/Ic PDF 5.4

Operations: Background 1.000,1.000 | Strip kAlpha2 0.500 | Import

NP6-01-Q-XRD - File: NP6-01-Q-XRD.raw - Type: Locked Coupled - Start: 5.000 ° - End: 74.995 ° - Step: 0.015 ° - Step time: 106.2 s - Temp.: 25 °C (Room) - Time Started: 14 s - 2-Theta: 5.000 ° - Theta: 2

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Appendix B B.2


01-070-6386 (*) - Chromite - (Fe0.52Mg0.48)(Cr0.72Al0.28)2O4 - Y: 75.73 % - a 8.30740 - b 8.30740 - c 8.30740 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 3.5


Operations: Strip kAlpha2 0.500 | Background 0.380,1.000 | Import

NP6-02-Q-XRD - File: NP6-02-Q-XRD1.raw - Type: Locked Coupled - Start: 5.000 ° - End: 74.995 ° - Step: 0.015 ° - Step time: 106.2 s - Temp.: 25 °C (Room) - Time Started: 14 s - 2-Theta: 5.000 ° - Theta:

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Appendix B B.3


00-052-1079 (I) - Iron Nickel Aluminum Oxide - Fe0.99Ni0.60Al1.10O4 - Y: 23.42 % - a 8.16000 - b 8.16000 - c 8.16000 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - F (0) -




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Appendix B B.4


01-075-3304 (*) - Chromite - (Mg.67Fe.33)Cr2O4 - Y: 47.60 % - a 8.34900 - b 8.34900 - c 8.34900 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 3.9




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Appendix B B.5


00-045-0229 (Q) - Lithium Zirconium Phosphate - Li2Zr4(PO4)6 - Y: 14.49 % -

01-086-1362 (*) - Magnetite - Fe2.929O4 - Y: 104.27 % - a 8.39690 - b 8.39690 - c 8.39690 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 4.9




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Appendix B B.6


01-073-2159 (I) - Magnesium Iron Aluminum Oxide - MgFeAlO4 - Y: 41.96 % - a 8.22400 - b 8.22400 - c 8.22400 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 2.8




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Appendix B B.7


NP6-07-Q-XRD

01-071-3850 (I) - Trevorite, syn - NiFe2O4 - Y: 16.12 % - a 8.35700 - b 8.35700 - c 8.35700 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 5.




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Appendix B B.8


NP6-08-Q-XRD

01-071-3850 (I) - Trevorite, syn - NiFe2O4 - Y: 20.36 % - a 8.35700 - b 8.35700 - c 8.35700 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 5.




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Appendix B B.9


NP6-09-Q-XRD

01-074-6507 (I) - Iron Nickel Oxide - FeNi2O4 - Y: 24.65 % - a 8.28800 - b 8.28800 - c 8.28800 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 4.7




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Appendix B B.10


NP6-10-Q-XRD

00-052-1079 (I) - Iron Nickel Aluminum Oxide - Fe0.99Ni0.60Al1.10O4 - Y: 21.29 % - a 8.16000 - b 8.16000 - c 8.16000 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - F (0) - 01-070-8070 (*) - Zinc Oxide - ZnO - Y: 95.49 % - a 3.24890 - b 3.24890 - c 5.20490 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63mc (186) - I/Ic PDF 5.4

Operations: Background 1.000,1.000 | Strip kAlpha2 0.500 | ImportNP6-10-Q-XRD - File: NP6-10-Q-XRD.raw - Type: Locked Coupled - Start: 5.000 ° - End: 74.995 ° - Step: 0.015 ° - Step time: 106.2 s - Temp.: 25 °C (Room) - Time Started: 14 s - 2-Theta: 5.000 ° - Theta: 2

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Appendix B B.11


NP6-11-Q-XRD

01-075-3304 (*) - Chromite - (Mg.67Fe.33)Cr2O4 - Y: 40.47 % - a 8.34900 - b 8.34900 - c 8.34900 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 3.9




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Appendix B B.12


NP6-12-Q-XRD

01-072-9809 (C) - Lithium Iron Manganese Oxide - (Li0.399Fe0.601)((Li0.225Fe0.825Mn0.95)O4) - Y: 37.72 % - a 8.31680 - b 8.31680 - c 8.31680 - alpha 90.000 - beta 90.000 - gamma 90.000 - Primitive -




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Appendix B B.13


NP6-13-Q-XRD

01-075-3305 (*) - Chromite - (Mg.63Fe.37)Cr2O4 - Y: 99.40 % - a 8.34650 - b 8.34650 - c 8.34650 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 4.

01-070-8070 (*) - Zinc Oxide - ZnO - Y: 95.03 % - a 3.24890 - b 3.24890 - c 5.20490 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63mc (186) - I/Ic PDF 5.4Operations: Background 1.000,1.000 | Strip kAlpha2 0.500 | Import


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Appendix B B.14


NP6-14-Q-XRD





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Appendix B B.15


NP6-15-Q-XRD

01-073-0212 (I) - Lithium Iron Chromium Oxide - LiFe3Cr2O8 - Y: 101.09 % - a 8.27700 - b 8.27700 - c 8.27700 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 3.9




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Appendix B B.16


NP6-16-Q-XRD


01-070-8070 (*) - Zinc Oxide - ZnO - Y: 87.34 % - a 3.24890 - b 3.24890 - c 5.20490 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63mc (186) - I/Ic PDF 5.4Operations: Background 1.000,1.000 | Strip kAlpha2 0.500 | ImportNP6-16-Q-XRD - File: NP6-16-Q-XRD.raw - Type: Locked Coupled - Start: 5.000 ° - End: 74.995 ° - Step: 0.015 ° - Step time: 106.2 s - Temp.: 25 °C (Room) - Time Started: 15 s - 2-Theta: 5.000 ° - Theta: 2

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Appendix B B.17


NP6-17-Q-XRD

01-086-1338 (*) - Iron Oxide - Fe2.910O4 - Y: 84.02 % - a 8.38740 - b 8.38740 - c 8.38740 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 5.




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Appendix B B.18


NP6-18-Q-XRD

01-072-9809 (C) - Lithium Iron Manganese Oxide - (Li0.399Fe0.601)((Li0.225Fe0.825Mn0.95)O4) - Y: 38.84 % - a 8.31680 - b 8.31680 - c 8.31680 - alpha 90.000 - beta 90.000 - gamma 90.000 - Primitive -




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Appendix B B.19


NP6-19-Q-XRD

00-012-0254 (I) - Lithium Oxide - Li2O - Y: 9.42 % - a 4.61140 - b 4.61140 - c 4.61140 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fm-3m (225) -




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Appendix B B.20


01-089-6228 (*) - Iron Silicon Oxide - (Fe0.769Si0.231)(Fe0.975Si0.025)2O4 - Y: 87.94 % - a 8.37400 - b 8.37400 - c 8.37400 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/


Operations: Background 1.000,1.000 | Strip kAlpha2 0.500 | ImportNP6-20-Q-XRD - File: NP6-20-Q-XRD.raw - Type: Locked Coupled - Start: 5.000 ° - End: 74.995 ° - Step: 0.015 ° - Step time: 106.2 s - Temp.: 25 °C (Room) - Time Started: 15 s - 2-Theta: 5.000 ° - Theta: 2

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Appendix B B.21

B.2 XRD Data for Post-CCC Glasses

Figure B.21. XRD data for NP6-01-CCC

01-071-2273 (*) - Ruthenium Oxide - RuO2 - Y: 2.11 % - a 4.49190 - b 4.49190 - c 3.10660 - alpha 90.000 - beta 90.000 - gamma 90.000 - Primitive - P42/mnm (136) - I/Ic PDF 8.5

01-086-1344 (*) - Magntite - Fe2.946O4 - Y: 74.73 % - a 8.39250 - b 8.39250 - c 8.39250 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 5.



NP6-01-CCC-XRD-1 - File: NP6-01-CCC-XRD-1.raw - Type: Locked Coupled - Start: 5.000 ° - End: 74.995 ° - Step: 0.015 ° - Step time: 106.2 s - Temp.: 25 °C (Room) - Time Started: 14 s - 2-Theta: 5.000 °

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Appendix B B.22



01-075-0526 (I) - Magnesium Manganese Aluminum Oxide - Mg.3125Mn2.0625Al.625O4 - Y: 86.67 % - a 8.34000 - b 8.34000 - c 8.34000 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd




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Appendix B B.23


NP6-03-CCC-XRD-1

01-071-6111 (*) - Spinel, aluminian, syn - (Mg0.527Al0.473)(Al1.758Mg0.126)O4 - Y: 5.31 % - a 8.02300 - b 8.02300 - c 8.02300 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227)

01-071-2273 (*) - Ruthenium Oxide - RuO2 - Y: 2.27 % - a 4.49190 - b 4.49190 - c 3.10660 - alpha 90.000 - beta 90.000 - gamma 90.000 - Primitive - P42/mnm (136) - I/Ic PDF 8.501-071-6104 (*) - Magnesium Aluminum Oxide - (Mg0.383Al0.617)(Al1.785Mg0.013)O4 - Y: 13.78 % - a 7.97900 - b 7.97900 - c 7.97900 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3

01-089-8339 (*) - Sodium Silicate - Na2(Si2O5) - Y: 11.50 % - a 8.39300 - b 12.08300 - c 4.84300 - alpha 90.000 - beta 90.370 - gamma 90.000 - Primitive - P21/n (14) - I/Ic PDF 1.3

01-079-1159 (*) - Lithium Aluminum Silicate - Li(AlSiO4) - Y: 7.81 % - a 8.22800 - b 5.03200 - c 8.27400 - alpha 90.000 - beta 107.460 - gamma 90.000 - Primitive - Pa (7) - I/Ic PDF 1.101-070-8070 (*) - Zinc Oxide - ZnO - Y: 81.03 % - a 3.24890 - b 3.24890 - c 5.20490 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63mc (186) - I/Ic PDF 5.4

Operations: Strip kAlpha2 0.500 | Background 2.138,1.000 | ImportNP6-03-CCC-XRD-1 - File: NP6-03-CCC-XRD-1.raw - Type: Locked Coupled - Start: 5.000 ° - End: 74.995 ° - Step: 0.015 ° - Step time: 106.2 s - Temp.: 25 °C (Room) - Time Started: 15 s - 2-Theta: 5.000 °

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Appendix B B.24



01-079-0991 (N) - Nepheline, syn - Na7.11(Al7.2Si8.8O32) - Y: 18.49 % - a 9.95800 - b 9.95800 - c 8.34100 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63 (173) - I/Ic PDF 0.8

01-071-6021 (I) - Iron Nickel Manganese Oxide - Fe(NiMn)O4 - Y: 51.91 % - a 8.37500 - b 8.37500 - c 8.37500 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 4.6




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Appendix B B.25


NP6-05-CCC-XRD-1


01-075-3194 (*) - Lithium Manganese Iron Oxide - (Li0.286Mn1.286Fe1.429)O4 - Y: 70.56 % - a 8.43702 - b 8.43702 - c 8.43702 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227)




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Appendix B B.26



01-085-1565 (*) - Galaxite - (Mg0.117Al0.016Mn0.663Fe0.203)(Mg0.025Fe0.067Al1.757Mn0.152)O4 - Y: 14.58 % - a 8.22260 - b 8.22260 - c 8.22260 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-c01-070-8070 (*) - Zinc Oxide - ZnO - Y: 88.75 % - a 3.24890 - b 3.24890 - c 5.20490 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63mc (186) - I/Ic PDF 5.4


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Appendix B B.27


NP6-07-CCC-XRD-1

01-070-7947 (*) - Lithium Iron Manganese Oxide - (Li0.37Fe0.50Mn0.12)(Li0.06Fe0.73Mn1.19)O4 - Y: 19.43 % - a 8.38884 - b 8.38884 - c 8.38884 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-cent


01-079-0994 (N) - Nepheline, silicious, syn - Na6.8(Al6.3Si9.7O32) - Y: 12.11 % - a 9.95900 - b 9.95900 - c 8.34400 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63 (173) - I/Ic PDF 0.8




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Appendix B B.28


01-070-8129 (*) - Magnetite, magnesian, syn - (Fe0.92Mg0.08)(Fe1.08Ni0.2Mg0.72)O4 - Y: 30.87 % - a 8.35500 - b 8.35500 - c 8.35500 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3

01-075-2934 (N) - Na-Nepheline - Na7.2(Al7.2Si8.8O32) - Y: 77.79 % - a 9.97020 - b 9.97020 - c 8.34780 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63 (173) - I/Ic PDF 0.801-070-8070 (*) - Zinc Oxide - ZnO - Y: 52.96 % - a 3.24890 - b 3.24890 - c 5.20490 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63mc (186) - I/Ic PDF 5.4



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Appendix B B.29


NP6-09-CCC-XRD-1

01-075-4393 (*) - Spinel - MgAl.47Fe1.52O4 - Y: 41.58 % - a 8.32520 - b 8.32520 - c 8.32520 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 3.5




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Appendix B B.30


NP6-10-CCC-XRD-1

01-079-2422 (*) - Gehlenite, magnesian, syn - Ca2(Mg0.25Al0.75)(Si1.25Al0.75O7) - Y: 9.12 % - a 7.71150 - b 7.71150 - c 5.04980 - alpha 90.000 - beta 90.000 - gamma 90.000 - Primitive - P-421m (113) -

01-074-2082 (I) - Nickel Iron Manganese Oxide - NiFe1.95Mn.05O4 - Y: 8.66 % - a 8.34150 - b 8.34150 - c 8.34150 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 4.

01-074-0730 (N) - Nickel Aluminum Silicate - Ni3Al2SiO8 - Y: 6.64 % - a 5.66500 - b 28.64600 - c 8.09100 - alpha 90.000 - beta 90.000 - gamma 90.000 - Body-centered - Imma (74) - I/Ic PDF 1.1

00-034-0412 (I) - Iron Chromium Oxide - (Fe0.6Cr0.4)2O3 - Y: 12.92 % - a 5.01700 - b 5.01700 - c 13.64300 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - R (0) -

01-075-2935 (N) - Na-Nepheline - Na6.41(Al6.41Si9.59O32) - Y: 17.47 % - a 9.97000 - b 9.97000 - c 8.34180 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63 (173) - I/Ic PDF 0.8




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Appendix B B.31



01-070-7949 (*) - Lithium Iron Manganese Oxide - (Li0.33Fe0.59Mn0.07)(Li0.21Fe0.86Mn0.95)O4 - Y: 35.69 % - a 8.36576 - b 8.36576 - c 8.36576 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-cent



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Appendix B B.32



01-071-1233 (I) - Magnesium Aluminum Iron Oxide - MgAl.2Fe1.8O4 - Y: 82.23 % - a 8.35900 - b 8.35900 - c 8.35900 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF




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Appendix B B.33


00-043-1027 (C) - Ruthenium Oxide - RuO2 - Y: 6.83 % - a 4.49940 - b 4.49940 - c 3.10710 - alpha 90.000 - beta 90.000 - gamma 90.000 - Primitive - P42/mnm (136) - I/Ic PDF 7.8

01-071-0854 (*) - Nickel Chromium Manganese Oxide - NiCrMnO4 - Y: 42.94 % - a 8.38000 - b 8.38000 - c 8.38000 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 4.




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Appendix B B.34


01-080-2186 (*) - Iron Oxide - Fe21.34O32 - Y: 32.13 % - a 8.34740 - b 8.34740 - c 25.04219 - alpha 90.000 - beta 90.000 - gamma 90.000 - Primitive - P41212 (92) - I/Ic PDF 3.




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Appendix B B.35


NP6-15-CCC-XRD-1

00-015-0876 (*) - Fluorapatite, syn - Ca5(PO4)3F - Y: 15.50 % - a 9.36840 - b 9.36840 - c 6.88410 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63/m (176) - I/Ic PDF 1.5


01-089-7829 (I) - Lithium Iron Manganese Oxide - Li0.67Fe1.63Mn0.698O4 - Y: 52.19 % - a 8.30591 - b 8.30591 - c 8.30591 - alpha 90.000 - beta 90.000 - gamma 90.000 - Primitive - P4332 (212) - I/Ic PDF




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Appendix B B.36


NP6-16-CCC-XRD-1

01-081-1314 (*) - Baddeleyite, syn - Zr0.944O2 - Y: 8.86 % - a 5.14948 - b 5.20211 - c 5.31975 - alpha 90.000 - beta 99.238 - gamma 90.000 - Primitive - P21/c (14) - I/Ic PDF 4.4

01-070-8070 (*) - Zinc Oxide - ZnO - Y: 97.11 % - a 3.24890 - b 3.24890 - c 5.20490 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63mc (186) - I/Ic PDF 5.401-071-1255 (I) - Magnesium Iron Chromium Oxide - MgFe.9Cr1.1O4 - Y: 56.98 % - a 8.35100 - b 8.35100 - c 8.35100 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF


NP6-16-CCC-XRD-1 - File: NP6-16-CCC-XRD-1.raw - Type: Locked Coupled - Start: 5.000 ° - End: 76.098 ° - Step: 0.015 ° - Step time: 53.1 s - Temp.: 25 °C (Room) - Time Started: 17 s - 2-Theta: 5.000 ° -

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Appendix B B.37


NP6-17-CCC-XRD-1

01-083-0556 (I) - Fluorapatite, syn - Ca5.061(P2.87O11.46)F0.89 - Y: 29.73 % - a 9.37130 - b 9.37130 - c 6.88590 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63/m (176) - I/Ic PDF 1.1

01-075-3195 (*) - Lithium Manganese Iron Oxide - (Li0.429Mn1.429Fe1.143)O4 - Y: 78.07 % - a 8.42199 - b 8.42199 - c 8.42199 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227)




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Appendix B B.38


NP6-18-CCC-XRD-1

00-015-0876 (*) - Fluorapatite, syn - Ca5(PO4)3F - Y: 24.69 % - a 9.36840 - b 9.36840 - c 6.88410 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63/m (176) - I/Ic PDF 1.5

01-071-6021 (I) - Iron Nickel Manganese Oxide - Fe(NiMn)O4 - Y: 91.88 % - a 8.37500 - b 8.37500 - c 8.37500 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 4.6


Operations: Strip kAlpha2 0.500 | Background 5.623,1.000 | ImportNP6-18-CCC-XRD-1 - File: NP6-18-CCC-XRD-1.raw - Type: Locked Coupled - Start: 5.000 ° - End: 76.098 ° - Step: 0.015 ° - Step time: 53.1 s - Temp.: 25 °C (Room) - Time Started: 15 s - 2-Theta: 5.000 ° -

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Appendix B B.39


NP6-19-CCC-PCT-1

00-033-0664 (*) - Hematite, syn - Fe2O3 - Y: 7.77 % - a 5.03560 - b 5.03560 - c 13.74890 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - R-3c (167) - I/Ic PDF 2.4

01-075-2934 (N) - Na-Nepheline - Na7.2(Al7.2Si8.8O32) - Y: 86.82 % - a 9.97020 - b 9.97020 - c 8.34780 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63 (173) - I/Ic PDF 0.801-070-8070 (*) - Zinc Oxide - ZnO - Y: 57.80 % - a 3.24890 - b 3.24890 - c 5.20490 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63mc (186) - I/Ic PDF 5.4


NP6-19-CCC-PCT-1 - File: NP6-19-CCC-PCT-1.raw - Type: Locked Coupled - Start: 5.000 ° - End: 74.995 ° - Step: 0.015 ° - Step time: 106.2 s - Temp.: 25 °C (Room) - Time Started: 14 s - 2-Theta: 5.000 °

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Appendix B B.40


NP6-20-CCC-XRD-1

00-043-1027 (C) - Ruthenium Oxide - RuO2 - Y: 14.17 % - a 4.49940 - b 4.49940 - c 3.10710 - alpha 90.000 - beta 90.000 - gamma 90.000 - Primitive - P42/mnm (136) - I/Ic PDF 7.8

01-071-0852 (*) - Nickel Manganese Oxide - NiMn2O4 - Y: 53.54 % - a 8.40000 - b 8.40000 - c 8.40000 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fd-3m (227) - I/Ic PDF 4.5

01-079-0991 (N) - Nepheline, syn - Na7.11(Al7.2Si8.8O32) - Y: 91.16 % - a 9.95800 - b 9.95800 - c 8.34100 - alpha 90.000 - beta 90.000 - gamma 120.000 - Primitive - P63 (173) - I/Ic PDF 0.8




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EWG-RPT-023 Rev 0.0

Pacific Northwest National Laboratory 902 Battelle Boulevard P.O. Box 999 Richland, WA 99354 1-888-375-PNNL (7665)

www.pnnl.gov

X-Ray Diffraction and Product Consistency Test Results for the Phase 6 … · 2020. 11. 25. ·...

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