PNL-4955-1

MaCMaterials Characterization Center

Approved Reference andTesting Materials for Use inNuclear Waste ManagementResearch and DevelopmentProgramsG. B. MellingerI. L Daniel

December 1983

Prepared for the U.S. Department of Energyunder Contract DE-ACO6-76RLO 1830

Pacific Northwest LaboratoryOperated for the U.S. Department of Energyby Battelle Memorial Institute.

z

O3Baltelle

�)LXI

DISCLAIMER

This report was prepared as an account of work sponsored by an agency of theUnited States Government. Neither the United States Government nor anyagency thereof, nor any of their employees, makes any warranty, express orimplied, or assumes any legal liability or responsibility for the accuracy, com-pleteness, or usefulness of any information, apparatus, product, or processdisclosed, or represents that its use would not infringe privately owned rights.Reference herein to any specific commercial product, process, or service bytrade name, trademark, manufacturer, or otherwise, does not necessarilyconstitute or imply its endorsement, recommendation, or favoring by theUnited States Government or any agency thereof. The views and opinions ofauthors expressed herein do not necessarily state or reflect those of the UnitedStates Government or any agency thereof.

PACIFIC NORTHWEST LABORATORYoperated by

BATTELLEfor the

UNITED STATES DEPARTMENT OF ENERGYunder Contract DE-AC06-76RL0 1830

PNL-4955-1

MacMaterials Characterization Center

Approved Reference andTesting Materials for Use inNuclear Waste ManagementResearch and DevelopmentPrograms

G. B. MellingerJ. L. Daniel

December 1983

Prepared for the U.S. Department of Energyunder Contract DE-AC06-76RLO 1830

Pacific Northwest LaboratoryOperated for the U.S. Department of Energyby Battelle Memorial Institute

CONTENTS

I. SUMMARY ........................................................................ 1

II. INTRODUCTION .................................................................. 3The Objective of the MCC .............. ........................................ 3The Nuclear Waste Materials Characterization Organization ....................... 3This Document . ................................................................ 3Classifications of Standard Materials ............................................. 3Approved Reference Materials .................................................. 4Approved Testing Materials .............. ....................................... 4Archiving and Distribution of Standard Materials .................................. 4

III. SUMMARY OF STANDARD MATERIALS ............................................. 5Inventory of Available Standard Materials ........................................ 5Materials Policies . .............................................................. 5

IV. STANDARD MATERIALS DESCRIPTIONS ............................................ 7ARM-1; Reference Waste Glass, Nonradioactive .................................. 8ATM-1, 2,3 and 4; 76-68 Type Glass, Actinide Dopants ........................... 10ATM-5; 76-68 Type Glass, Fully Radioactive . ...................................... 12ATM-6;Barnwell Type Glass, Radioactive Dopants ............................... 14ATM-101; H. B. Robinson Spent Fuel, Typical PWR .............................. 16MCC 76-68; 76-68 Type Glass, Used for Selected Applications ...... ................ 16Planned Acquisitions; Reference Leachates, Basalt, Bentonite,

Glass ATMs, Spent Fuel ................ ........................................ 18

V. REFERENCES ..................................................................... 19

iii

r

1. SUMMARY

This document, addressed to members of the waste management research and developmentcommunity, summarizes reference and testing materials now available from the MaterialsCharacterization Center (MCC). These materials are furnished under the MCC's charter to distributereference materials essential for quantitative evaluation of nuclear waste package materials underdevelopment in the U.S.

Reference materials with known behavior in various standard waste management related tests areneeded to assure that individual testing programs are correctly performing those tests. Approvedtesting materials are provided to assist the projects in assembling a materials data base of defensibleaccuracy and precision.

This is the first issue of this publication. Future Issues will provide updates of the characterizationstatus of the materials presented In this issue, and information about new standard materials as theyare acquired.

1

I. INTRODUCTION

In this section, the objectives of the MaterialsCharacterization Center (MCC), and the structureand functions of the Nuclear Waste MaterialsCharacterization Organization (MCO), (of whichthe MCC is a part), are briefly outlined. The pur-pose for and information contained In this listingof approved reference and testing materials aredescribed. Two classifications of standard materialsavailable from the MCC are defined, and thearchiving and distribution of the materials arediscussed.

The Objective of the MCC

The objective of the MCC is to assist the DOE pro-jects for nuclear waste form production, transpor-tation and disposal to assemble a materials database of defensible precision and accuracy. A majorresponsibility of the MCC is to arrange for theformulation, acquisition and distribution of refer-ence and testing materials essential for quantitativeevaluation of nuclear waste forms and repositorysystems under development in the U.S.

The Nuclear Waste Materials CharacterizationOrganization

The MCC Is part of the Nuclear Waste MaterialsChacterization Organization (MCO). The MCO,created by the Department of Energy (DOE), coor-dinates the collection of a defensible materialsproperty data base. This data base can be used as arecognized, referenceable source of data for wastemanagement systems design, integration, andlicensing.

The MCO is coordinated by the Materials SteeringCommittee (MSC) and It consists of the MaterialsIntegration Office (MIO), the MCC, and the Mate-rials Review Board (MRB). The MCO is structurallyarranged as shown in Figure 1. The direction of theMCO is determined by means of quarterly meet-ings of the MSC In which issues affecting the over-all program objectives are addressed and resolved.The MIO functions to integrate the activities of theMCC and the MRB to assure that the test methodsand materials data needed by the waste manage-ment community are available when required.

Figure 1. The Structure of the MaterialsCharacterization Organization

This Document

The purpose of this document, which will beupdated periodically, is to Inform members of thenuclear waste management research and devel-opment community about the reference and test-ing materials available from the MCC. Thefabrication and compositions of these materials arereported. Also reported are summaries of anycompleted characterization and the intended usesfor these materials. New materials which are beingacquired or are under consideration are alsodescribed.

Classifications of Standard Materials

MCC standard materials are intended to provide abasis for comparison of data quality obtained inrepository development work by the DOE projects,and to assist In verifying the accuracy and precisionof the data obtained. For that purpose, two classifi-cations of standard materials are available from theMCC. These are Approved Reference Materials(ARMs) and Approved Testing Materials (ATMs).These two types of materials are described in thissection.

3

Approved Reference Materials

The primary use of ARMs is as a standard referenceand calibration material, similar to that of the SRMsof the United States National Bureau of Standards(NBS). The characterization of each ARM (compo-sition, homogeneity, behavior under specific MCCtest conditions) is conducted by MCC and support-ing laboratories such as NBS to a high level ofaccuracy and precision. The ARMs are intendedespecially for field calibration of MCC testmethods, and for verification by test method usersthat they are conducting the test procedure in acontrolled reproducible manner. Therefore, theprimary requirement for each ARM is a well-defined uniform composition representing a classof waste form, rather than a specific formulation.

Only one ARM is currently available. The MCC hasno present plans for other ARMs.

Approved Testing Materials

The purpose of ATMs is to serve as common test-ing materials, officially endorsed by DOE, for usein the DOE nuclear waste repository developmentprojects. ATMs represent specific formulations oftypical waste forms, or of other components ofproposed repository systems. Each ATM will becharacterized appropriately by MCC for composi-tion, homogeneity and behavior under specifiedtest conditions. Accuracy and precision of dataregarding performance under test conditions willbe determined from consensus-average dataobtained by both the MCC and DOE projects. Theprimary objective is to develop a defensible database of known accuracy and precision using thesecommonly accepted testing materials of recog-nized quality.

ATMs will be sufficiently numerous to allow con-trolled testing under all reasonable conditionsrequired by the DOE repository development pro-jects. The ATMs may be produced by the MCC orby the waste-form producer. In every case theMCC will conduct sufficient characterization tovalidate the use of the material as an ATM.

Archiving and Distribution of StandardMaterials

An important function of MCC is the maintenanceof a complete archive of all MCC reference andtesting materials used in the nuclear repositorydevelopment programs, and of the characteriza-tion documentation for those materials. Sufficientquantities of these materials will be stored by MCCat PNL to assure their future availability in reason-able quantities for additional testing or resolutionof important questions raised in scheduled testsand experiments.

The MCC will be responsive to the needs of thewaste management community for high qualityreference and testing materials. Readers interestedin obtaining any of the items listed in this docu-ment or additional materials not listed, shouldcommunicate their needs to the MCC. Addressrequests for existing or new standard materials to:

J. E. Mendel, ManagerMaterials Characterization CenterPacific Northwest LaboratoryRichland, Washington 99352

4

Ill. SUMMARY OF STANDARD MATERIALS

In this section, the materials available from theMCC are summarized in tabular form. The MCC'spolicies for acquiring, characterizing and distrib-uting the materials are outlined.

Inventory of Available Standard Materials

Table 1 provides a summary of the reference andtesting materials available from the MCC. TheMCC plans the use of its manpower and fundingcarefully to maximize the number and quality ofreference and testing materials for application tothe U.S. nuclear waste R&D programs. In addition,funding is allotted to a careful characterization ofeach material consistent with its intended use. Thischaracterization is an essential step in certifyingwith confidence that the material is suitable for useas a standard to verify test performance, or as areference point to compare materials or testconditions.

Further acquisitions are planned. Users areencouraged to communicate their needs to theMCC.

Materials Policies

The MCC acquires and distributes reference andtesting materials which are of wide use to thenuclear waste management research and devel-opment community. These materials are providedwithout charge, in reasonable amounts, to DOEprograms. Others, such as Nuclear RegulatoryCommission (NRC) users, will pay pro-rated pro-duction costs. The materials will normally besupplied in the form in which they were produced(e.g., glass will be furnished as cast bars). Somelaboratory test programs require use of the mate-rials in a special form (e.g., sized blended powders,specially shaped monoliths, unique containment),or with special characterization. Usually the MCCcan supply the materials in the form required, pro-viding there is sufficient prior notice.

The MCC will characterize all reference and test-ing materials and provide characterization resultsto the users. As a minimum, the composition andhomogeneity will be determined. Statistical

TABLE 1. MCC Reference and Testing Materials

Designation

ARM-1

Type Purpose

Waste Form Reference

QuantityFabricated

255 kgReference Waste Glass,nonradioactive

ATM-i 76-68 glass, U-dopedATM-2 76-68 glass, Am-dopedATM-3 76-68 glass, Np-dopedATM-4 76-68 glass, Pu-dopedATM-S 76-68 glass, fully

radioactiveATM-6 Barnwell glass,

radioactive dopantsATM-101 Spent Fuel, Typical PWR

MCC 76-68 76-68 glass, nonradioactive

Repository Development TestsRepository Development TestsRepository Development TestsRepository Development TestsRepository Development Tests

Repository Development Tests

Repository Development TestsSelected Applications

4kg0.45 kg0.45 kg0.45 kg3 kg

3 kg

9 pins200 kg

5

methods will be applied to sampling proceduresand evaluation of uncertainty in the analytical data.Additional characterization will generally be app-lied consistent with the material's intended use.Reference waste form materials will be subjectedto MCC leach tests to provide reference data forverification of users' test performance. Microstruc-ture and phase analyses will be conducted on solidmaterials.

Documentation reports will be available for all ref-erence and testing materials supplied by the MCC.These reports will include details of materials fabri-cation and the results of its characterization. Also

included, when available, will be a statistical analy-sis of the uniformity of the material's composition,phases, etc. These reports will be provided to therequestors of a reference or testing material, or toa program that needs to examine such a reportprior to a material request.

In order to provide materials as quickly as possible,and because of the time required for adequatecharacterization, materials are being made avail-able before all characterization has been com-pleted and compiled into a formal documentation.Reports of additional characterization will bedistributed as the information becomes available.

6

IV. STANDARD MATERIALS DESCRIPTIONS

In the following section, the presently available reference and testing materials are described. In addition toinformation on composition, the methods of fabrication, characterization and reporting of the materials areoutlined. Detailed characterization of these materials is in progress. The compositional information listed foreach material is based on nominal values or initial analyses. This. information will be updated as characteriza-tion work progresses.

The homogeneity of standard materials is of particular Importance, and at the same time is difficult toachieve with low concentrations of dopants added to bulk quantities of glass. In addition to the problem ofthorough uniform mixing of additives, some components of ATM glasses tend to segregate, precipitate orcrystallize under glass forming conditions. Characterization in progress on the ATMs includes a carefuldetermination of material homogeneity. Where such information is already available it is included here inthe narrative description of the standard material.

7

ARM-1This material represents a generic borosilicate reference waste glass.

Reference Waste Glass, It is nonradioactive. It was produced by Schott Optical Glass ofNonradioactive Duryea, PA in 1983, in the form of 6 x 7 x 50 cm bars.

Its composition is shown in Table 2, based on analyses by theNational Bureau of Standards. Flame atomic absorption spectrometryand direct-current plasma emission spectrometry were used for theanalyses. Each value is based on the analysis of ten statistically ran-dom samples of the material. Each sample was analyzed twice. Refrac-tive index measurements confirmed the high homogeneity of theglass.

Additional characterization of the glass will include analyses of theresidual strain and numbers and types of inclusions. The glass behav-ior in various MCC tests will also be determined.

Current plans call for a report to be completed by March of 1984which will cover ARM-1's fabrication, characterization and behaviorin the 28-day MCC-1 leach test. Additional test behavior informationwill be added to this document as it becomes available.

8

TABLE 2. Composition of ARM-1(a)

Oxide Wt%

A1203 5.59B203 11.3BaO 0.658CaO 2.24CeO2 1.51Cs2O 1.17LW20 5.08MoO3 1.66

Na2O 9.66Nd2O3 5.96P20, 0.65SiO2 46.5

SrOz 0.45311O2 3.21ZnO 1.46ZrO2 1.80

TOTAL 99.90

StandardDeviation

0.060.250.0080.030.040.030.130.030.110.200.030.90.0050050.030.03

(a) Based on analysis of ten random samples,each sample analyzed twice.

9

ATM-1, 2,3 and 476-68 Type Glass,Actinide Dopants

These materials represent borosilicate glasses which incorporatehigh-level wastes resulting from the reprocessing of commercialnuclear reactor fuel. Their compositions are based on 76-68 glass(Mendel, 1977). Each contains a single actinide dopant, either naturalU, Am-241, Np-237 or Pu-239; no other radioactive species are pres-ent. Glass compositions are given in Tables 3 and 4.

These glasses were prepared at PNL in 1983 from crushed MCC 76-68glass to which dopants were added. Each batch was melted in plati-num crucibles and bars were cast and annealed. The bars of ATM-lbare -2 x 2.5 x 17.5 cm and weigh -275 g each. The bars of ATM-la, 2,3 and 4 are 1.3 x 1.3 x 7.6 cm and weigh -36 g.

TABLE 3. Composition of ATM-1 (U-doped 76-68 glass)

Oxide

A12032 4 1

Amz03

B203BaOCaO

CeO2Cr203

CsaOFe2O3La203

M003Na2ONd2O3NiO23NpO2

P20129PuO

SiO2SrOTiO2

U0 2ZnOZrO2

WtO

0.5

9.00.52.3

ATM-la(a)

Standard16 Deviation

9 0.02

6 0.015 0.007 0.04

ATM-lb(b)

0.920.471.119.564.16

1.971277

1.410.23

0.80

42.000.423.08

3.98(c)5.101.89

0.010.010.060.130.05

0.031.210.020.01

0.16

0.260.010.05

0.460.04

Wt%

0.80

11.30.662.30

1.130.48

l w7(b)8.74.73

2.0512.0

1.650.24

0.70

39.90.482.79

3.754.411.98

StandardDeviation

0.02

0.250.010.01

0.120.02

0.060.02

0.010.130.010.01

0.06

0.180.000.01

0.130.060.07

(a) Prepared from MCC-76-68 glass lot 3(see Table 7); composition listed is that of the baseglass except for U0 2 .

(b) Prepared from MCC 76-68 glass lot 1 (see Table 7); composition listed is the initialanalysis of the ATM.

(c) Wt% U0 2 added to the base glass; not yet analyzed in the ATM.

10

Alpha autoradiography has been performed on cut bar sections ofATM-2, 3 and 4. The Pu in ATM-4 was fairly uniformly distributedwithin the bar. There was some layering of Np within the ATM-3. Thisappears to have occurred during bar pouring. The Am in ATM-2 isvery uniform in the center of the bar, but has a lower concentrationaround the bar's exterior surface.

Additional characterization of these glasses will include determiningthe actual compositions of ATM-la, 2, 3 and 4. Also, the crystallinity,presence of phase separation and homogeneity of ATM-1 through 4will be analyzed.

TABLE 4. Composition of ATM 2, 3 and 4 (Transuranium-doped 76-68 glass)

ATM-2(a)

StandardWt% Deviation

ATM-3(a)

StandardWt% Deviation

ATM-4(a)

Oxide

A120 324Am 2 O3

Bl03BaOCaO

CeO2CrZO3

Cs2OFe2O3

La2Os

MoO3NazONdzO3NiO2 3 7 NpOa

P,05

23Pu02

5102SrOTi1 2

U02

ZnOZrO2

0.59

9.060.552.37

0.920.471.119.564.16

1.9712.77

1.410.23

0.80

42.000.423.08

5.101.89

0.02

0.010.000.04

0.010.010.060.130.05

0.031.210.020.01

0.16

0.260.010.05

0.460.04

0.59

9.060.552.37

0.920.471.119.564.16

1.9712.771.410.23

0.31 0 (b)

0.80

42.000.423.08

5.101.89

0.02

0.010.000.04

0.010.010.060.130.05

0.031.210.020.01

0.16

0.260.010.05

0.460.04

Wt%

0.59

9.060.552.37

0.920.471.119.564.16

1.9712.77

1.410.23

0.800.062(b)

42.000.423.08

5.101.89

StandardDeviation

0.02

0.010.000.04

0.010.010.060.130.05

0.031.210.020.01

0.16

0.260.010.05

0.460.04

(a) Prepared from MCC 76-68 glass lot 3; composition listed Is that of the base glass exceptfor the transuranium oxide.

(b) Based on a single measurement In the ATM.

11

ATM-576-68 Type Glass,Fully Radioactive

This material represents a borosilicate glass which incorporates thehigh-level waste resulting from the reprocessing of commercialnuclear fuel. Its composition is based on 76-68 glass (Mendel, 1977).ATM-S is fully loaded with actual waste from the reprocessing ofcommercial nuclear fuel. This waste was generated during theNuclear Waste Vitrification Project (NWVP) at PNL (Wheelwright,1979).

ATM-5 was fabricated at PNL in 1983. The nonradioactive ingredientswere combined, melted and crushed to form a base glass. All subse-quent processing was performed in a hot cell. Dried and powderedNWVP waste was added to the base glass. The powdered waste wasmade by heating NWVP waste solution to drive off water and NOx.Oxides of Np, Pu and U were added to the batch to bring their levelsto those in the 76-68 composition. The glass was produced in theform of cast, annealed bars -2 x 2 x 18 cm, weighing -180 g.

The anticipated composition of ATM-5 is shown in Table 5. This isbased on analyses of the powdered waste and nonradioactive baseglass. The actual glass composition, crystallinity, homogeneity andphases will be determined in early 1984.

A report is presently available which covers the fabrication of ATM-S.A supplement to this report covering characterization will be pre-pared by late 1984.

12

TABLE 5. Anticipated Composition of ATM-S(a)

AnticipatedOxide Composition, wt%

Glass AdditivesB203 9.50CaO 2.00Na2O 13.01SiO 40.00T102 3.00ZnO 5.00

WasteComponentsAgO 0 .0 3 (b)

BaO 0.84CdO 0.03(b)CeO2 1.03Cr2Oj 0.54

CSu2 1.l2ib)EU203 0.07(b)FeO, 7.56GdzO3 0Q05(b)La2Os 0.54

MoO, 1.15Na2O 5.51Nd2O3 1.81NiO 0.29P20, 0.48

PdO 0 53(b)PmO3 ,04(b)Pr.On 0.53(b)Rb2O 0.13(b)RhZO3 0.18

RuO2 0.63SmO 0.33(b)SrO 0.34

Tc2O, a46(b)TeO2 0.19

YO, 0.21(b)

ZrO, 1 .7 5 (b)

Other 120(c)

Actinides

AmO) 0.16Cm2O, 0.01NpO2 0.31PuO2 0.06UO 4.17

(a) Based on analyses of batch components; analysesof ATM not yet completed.

(b) Component of NWVP Waste which has not yetbeen analyzed. Anticipated amount In ATM-5based on composition of PW-8 Waste(Mendel 1977).

(c) Minor Impurities In NWVP Waste; Al0, BO, CaO,MgO, MnO2, S102, 02, BnO.

13

ATM-6Barnwell Type Glass,Radioactive Dopants

This material represents a borosilicate glass which incorporates theanticipated high-level waste from the Barnwell Nuclear Fuel Plant(BNFP) (Anderson, 1982). The glass was requested by the Basalt WasteIsolation Project (WIP) for use in their repository interactions testingprograms. The types and levels of radioactive dopants which it con-tains were those specified by the BWIP. The composition of the glassformer mix (type 83-B-15) to which the simulated waste was addedwas developed by the Commercial Waste Treatment Program at PNL.

ATM-6 was fabricated at PNL in 1983. It was produced in a hot cell.Radioactive dopants were mixed with a pre-melted and crushed glasswhich contained the nonradioactive components. The dopants usedincluded depleted U, Cm-244, Th-232, Np-237, Pu-238, 239 and 240,Tc-99, Cs-137 and Se-75. The glass was produced as cast, annealedbars -2 x 2 x 18 cm, weighing -180 g each. A portion of this glass wascrushed into two size fractions, -60+115 and -115+250 Tyler mesh,using a motor-driven A1203 mortar and pestle. A few grams of thiscrushed material are still available.

Table 6 compares the compositions of the bar and crushed materials.It can be seen that except for Na20 nd Tc207 there is no significantdifference between them. This indicates that no impurity was intro-duced by the crushing operation, nor did any significant segregationoccur during sieving. The reason for the Na2O and Tc207difference isbeing investigated.

ATM-6 has been examined using an SEM/microprobe. Overall, thematerial was uniform in appearance and composition. No evidenceof crystallinity was seen. One small bubble, -300u in diameter wasfound in the specimens examined; flakes of Ru were found in itsinterior surface. This was the only evidence of inhomogeneity in thematerial.

Additional characterization of this material will include a crystallinitydetermination by X-ray diffraction and a homogeneity determinationbased on compositional analyses.

A report is currently available for ATM-6 which covers its fabricationand characterization. An analysis of the homogeneity of ATM-6 willbe available as a supplement in early 1984.

14

TABLE 6. Composition of ATM-6

Approximate Compositions, wt%(a)

Bars Crushed

Oxide

Glass AdditivesA1203

UZONa2O(c)Si0

Average(b)

5.649.194.38

14.449.0

StandardDeviation

0.210.410.171.32.4

-60+115

5.429.094.21

17.846.7

Tyler mesh size

-115250

5.549.364.38

17.947.8

-250

5.528724.24

14.646.1

Waste ComponentsAgzOBaOCaOCdOCeO2Cr1 03Cs2OFe 2 0O

Gd2OsMnO2MgOMoO 3Na2ONaCINa2SO4Nd 2O3

NiO

PbOPdORb2ORuO2SeO2Sm 2 03

SnO,SrOTeOz1102

ZnOZrO2

Radioactive Dopants44Cm 2 03

mNPO2

2"PuO2

23s24cpuO2"5SeO2"Tcz0,(C)u3TO332ThO3

0.40

1.060.110740.53

0.08

0.070.010.040.03

0.12 0.020.22 0.051.54 0.07

(Inciuded above)

1.62nd

27

0.290.13002

0.090.64

6.SE-53.0E-3Q358

2.5E-32.OE-2l.9E-70.1282.4

l.lE-2

0.06

0.63

0S10.11

0.55

150.351.48

1.26nd

0.29

0280.14nd

0.100.15

S.6E-S3.OE-30.3122.SE-32.OE-21.6E-70.308

0.56

0.770.11

0.66

0.150.331.50

1.27nd

0.33

0.230.12nd

0.100.15

6.4E-S3.3E-30.368

2.7E-32.2E-21.6E-70.305

0.38

0.840.10

0.48

0.120.231.42

1.44nd

0.34

0.270.13nd

0.100.15

6,3E-S31E-30.360

2.SE-32OE-213E-70.289

0.15

0.020.010.01

0.090.36

2E-63E-40.0251E-411E-36E-90.0080.1

4E-3

(a) Based on initial Incomplete analyses. Data omissions in the table Indicate that the component Is present butanalyses are not yet completed.

(b) Average of three samples taken during bar pouring.(c) Analytical discrepancy between bars and powder is under Investigation.nd - Not detected.

15

ATM-101H. B. Robinson Spent Fuel,Typical PWR

This material represents the class of spent commercial nuclear reactorfuel characterized by low burnup and high in-reactor fission gasrelease. This fuel came originally from the H.B. Robinson PWR. Thefuel's nominal burnup is 30 MWd/KgM. It was removed from thereactor in 1973. It was received by PNL from EG&G, Idaho inNovember 1983.

Prior to shipment of the rods to PNL, the rods' fission gases were ana-lyzed by EG&G, Idaho and Exxon Nuclear Idaho Company. Analysesincluded: rod void volume, gas pressure and gas composition.Results of these analyses will be received by the MCC early in 1984.The rods are undergoing additional characterization at PNL. This isexpected to include transverse and longitudinal ceramography, grossgamma scanning, inventory calculation and analytical spot-check ofinventory (selected transuranics and fission products), and a radialdistribution calculation and spot-check by SEM/microprobe or EDX.

Current scheduling calls for a report to be issued in June 1984 cover-ing material characterization and sample preparation.

MCC 76-6876-68 Type Glass, Usedfor Selected Applications

This material represents a borosilicate glass which incorporates thehigh level waste resulting from reprocessing of commercial nuclearreactor fuel. This glass is nonradioactive. Its composition is based onthat of 76-68 glass (Mendel, 1977).

MCC 76-68 was fabricated by Penberthy Electromelt of Seattle,Washington, in 1980. It was supplied in the form of cast, annealedbars, 2.5 x 2.5 x 30 cm. Three lots were produced; the composition ofthese lots, as determined by nductively Coupled Plasma spectrome-try (ICP) is given in Table 7. The observed variation in composition ofrandom specimens of this material is as much as 10% for some ele-ments. MCC recommends that use of this material be limited toapplication in which this inhomogeneity is acceptable. One use ofthis material is as a feed stock for the production of doped ATMsbased on 76-68 glass.

16

TABLE 7. Composition of MCC-76-68 Glass

Compositions, wt%(a)

Lot 1

Oxide Wt%

A1203

8203BaOCaOCdOCeO2Cr 203Cs20Dy203

Eu203Fe2O3Gd2O3KzOLa2O3MgOMnO2MoO3Na2ONd2O3NiOP20sSiO2SrO2T102ZnOZrO2

TOTAL

0.848.650.622.290.05

<0.020.501.210.010.019.080.030.09

4.890.180.062.17

11.601.650.250.56

40.330.492.864.752.33

95.50

StandardDeviation(b)

0.030.060.010.040.01

0.020.080.000.000.120.010.030.060.010.000.010.950.010.030.080.810.010.040.080.04

Lot 2

StandardWt% Deviation(b)

0.638.990.542.220.050.820.471.140.010.019.520.020.274.330.140.061.96

11.301.470.220.66

40.730.423.044.761.79

95.57

0.030.150.020.110.010.110.010.010.000.000.170.000.060.240.010.010.050.200.080.020.110.320.010.030.050.07

Lot 3

Wt%

0.599.060.552.370.050.920.471.110.010.019.560.02

<0.064.160.160.061.97

12.771.410.230.80

42.000.423.085.101.89

98.76

StandardDeviation(b)

0.020.010.000.040.010.010.010.060.000.000.130.00

0.050.010.010.031.210.020.010.160.260.010.050.460.04

(a) Based on analysis of three bars for each lot.(b) Standard deviation of a single analysis.

17

Planned Acquisitionsa) Reference Leachatesb) A27 Cast Steel,

Basalt, Bentonitec) Glass ATMsd) Spent Fuel

Additional standard materials will be acquired during 1984:

a) A series of reference leachates will be made available which willapproximate the leachates resulting from various MCC test procedures.These materials will be used to confirm that leachate analysis is beingperformed correctly.

b) The BWIP has provided the MCC with samples of the A27 cast steel,basalt and bentonite used in their testing program. These will be used asreference materials in repository interactions tests.

18

V. REFERENCES

Anderson, K. J., et al. 1982. Barnwell Nuclear Fuel Plant (BNFP) Waste Characterization and WasteTreatment. PNL-3136/Fr-O1. Pacific Northwest Laboratory, Richland, Washington.

Mendel, J. E., et al. 1977. Annual Report of the Characteristics of High-Level Waste Glasses. BNWL-2252. Battelle, Pacific Northwest Laboratory, Richland, Washington.

Wheelwright, E. J., et al. 1979 Technical Summary: Nuclear Waste Vitrification Project. PNL-3038,Pacific Northwest Laboratory, Richland, Washington.

Commercial Waste Treatment Program, Monthly Report. March 1983. Pacific Northwest Laboratory,Richland, Washington.

19

PNL-4955-1

DISTRIBUTION

No. ofCopies

OFFSITE

DOE Office of Defense Waste &Byproducts Management

Washington, DC 20545ATTN: R. D. Walton, Jr. DP123

2 DOE Office of Geologic RepositoryDeployment

Washington, DC 20545ATTN: M. W. Frei

W. K. Eister

DOE Office of Terminal WasteDisposal and Remedial Action

Washington, DC 20545ATTN: J. A. Coleman NE-25

J. A. Turi NE-25

2 DOE Chicago Operations Office9800 South Cass AvenueArgonne, IL 60439ATTN: S. A. Mann

J. C. Haugen

2 DOE Savannah River Operations OfficeP. O. Box AAiken, SC 29801ATTN: T. B. Hindman

W. I. Brumley

2 DOE Albuquerque Operations OfficeP. 0. Box 5400Albuquerque, NM 87115ATTN: M. McFadden

K. Golliher

2 DOE National Waste Program Office505 King AvenueColumbus OH 43201ATTN: R. Wunderlich

I. Neff

DOE Nevada Operations OfficeP. 0. Box 14100Las Vegas, NV 89114ATTN: D. L Vieth

2 Technical Information Center

No. ofCopies

2 National Bureau of StandardsWashington, DC 20234ATTN: H. P. R. Frederikse

W. K. Haller

3 Argonne National Laboratory9700 South Cass AvenueArgonne, IL 60439ATTN: M. ). Steindler

W. B. SeefeldtC. C. McPheeters

Brookhaven National LaboratoryUpton NY 11973ATTN: D. G. Schweitzer

4 Lawrence Livermore NationalLaboratory

P. O. Box 808Livermore, CA 94550ATTN: . Harrar

D. IsherwoodV. OversbyL. Ballou

2 Oak Ridge National LaboratoryP. O. Box YOak Ridge, TN 37830ATTN: L. R. Dole

H. Godbee

2 Sandia National LaboratoriesP. O. Box 5800Albuquerque, NM 87107ATTN: R. B. Diegel

M. A. Molecke

S E. I. duPont deNemoursSavannah River LaboratoryAiken, SC 29808ATTN: P. L Gray

M. . PlodinecJ. A. StoneG. G. WicksL J. Hennelly

3 Catholic University of AmericaVitreous State LaboratoryKeane HallWashington, DC 20064ATTN: P. B. Macedo

A. BarkattC. . Montrose

3 Nuclear Regulatory CommissionWashington, DC 20555ATTN: M. I. Bell

K. S. KimE. Wicks

Distr-1

No. ofCopies

Massachusetts Institute of TechnologyBuilding 13, Room 406277 Massachusetts AvenueCambridge, MA 02139ATTN: R. L. Coble

Pennsylvania State UniversityMaterials Research LaboratoryUniversity Park, PA 16802ATTN: W. B. White

University of ColoradoDepartment of Geological SciencesCampus Box 250Boulder, CO 80309ATTN: D. D. Runnells

2 University of FloridaDepartment of Materials Science

and EngineeringGainesville, FL 32611ATTN: L. L. Hench

D. E. Clark

University of IllinoisDepartment of Metallurgy and

Mining EngineeringUniversity of IllinoisUrbana, IL 61801ATTN: H. Birnbaum

University of MinnesotaDept. of Chemical Engrg.

Material Science141 Amundson HallMinneapolis, MN 55455ATTN: W. W. Gerberich

Alcoa LaboratoriesAlcoa Center, PA 14069ATTN: G. Mac Zura

4 Office of Nuclear Waste IsolationBattelle Project Management Div.P. O. Box 16594Columbus, OH 43216-6594ATTN: Mgr. Quality Assurance Office

D. P. MoakD. E. ClarkR. W. Cote

3 Battelle Memorial InstituteBattelle Columbus Laboratory505 King AvenueColumbus, OH 43201ATTN: N. E. Miller

D. StahlI. Means

No. ofCopies

Office of Crystalline RepositoryDevelopment

Battelle Project Management DivisionP. 0. Box 16595Columbus, OH 43216-6595ATTN: A. A. Bauer

I. E. Burke33 Forest Rd.Burnt Hills, NY 12027

4 EG&G Idaho, Inc.P. 0. Box 1625Idaho Falls, ID 83415ATTN: G. Gibson

J. HinckleyR. TallmanR. M. Nielson, Jr.

Enrico Fermi Institute5640 5. EllisChicago, IL 60647ATTN: R. Clayton

Exxon Nuclear Co., Inc.Idaho Corporation

P. O. Box 2800Idaho Falls, ID 83401ATTN: J. R. Berreth

Mound FacilityP. 0. Box 32Miamisburg, OH 43242ATTN: E. L. Lewis

Rockwell International Science Center1049 Camino Dos RiosP. 0. Box 1085Thousand Oaks, CA 91360ATTN: A. B. Harker

U. S. Steel Corporation5733 Northumberland St.Pittsburgh, PA 15217ATTN: S. K. Cobum

2 West Valley Nuclear Services, Inc.P. 0. Box 191West Valley, NY 14171-0191ATTN: . L. Knabenschuh

J. M. Pope

Distr-2

No. ofCopies

ONSITE

6 DOE Richland Operations Office

3 E. A. BrackenP. A. CraigL. OlsonH. E. Ransom

4 Rockwell Hanford Operations

W. J. AndersonM. J. SmithE. H. RandklevP. . Salter

3 Westinghouse Hanford Company

8. EinzigerR. L. KnechtJ. . McCown

No. ofCopies

27 Pacific Northwest Laboratory

W. M. BowenD. J. BradleyG. L. BryanT. D. ChikallaJ. L. DanielR. C. Liikala). E. MendelM. D. MerzJ. L. McElroyG. B. MellingerD. RaiG. R. RobinsonW. A. RossR. . SerneS. C. SlateD. M. StrachanR. G. StrickertR. P. TurcotteR. E. WestermanJ. F. Williford, Jr.Publishing CoordinationTechnical Information (2)

Distr-3