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2. To: (ReceivingOrganization) 3. From: (Originatingorganization) 4. Re[oted EDT MO.:

Distribution .S:SO:haracterization Project/ N/A

5. Proj./Prog./DeplDivi:.: 6. Design Authority/Design Agent/Cog. 7. Purchase order No.:Engr.:

Spent Nuclear Fuel Project R.B. Baker N/A

8. OriginatorRemarks: 9. Equip./ComponentNo.:

For approval and release. N/A‘ 10. System/B(dg./Facility:

N/A

11. Receiver Remarks: 11A. Design BaselineDocument? [] Yet .[X] N.. ‘.2.”..”’:”.:.Aw” ;“::!’: !..._... ..—....-.-- ..- .. . .. .

13. Permit/P$rmitApplicationNo.:

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14. Required Response Oate:

N/A

15. DATA TRANSMITTED (F) (G) (H) (1)

IA) [c) (D] Apw.va! ReawJ” Origi- Re.eiv-Itenl B) D.x.rnent/DrawingNo. s~ ;:; D@si9.No.

(ElTtleorDescriptionofDataTransmitted “ator f., “at., e,Tra”s- Dkpo. Diwo-ndnal sitio” sitio”

1 HNF-3556 0 SAMPLING AND ANALYSIS N/A 2 1PLAN FOR SLUDGE LOCATEDON THE FLOOR AND IN THEPITS OF THE 105-K BASINS

. .. . -. ..- .-. -.

16.~,.. .

APPr.va!De$ig.at.rIFI Ream. +.xTransmittal(G) DkPOSitio”[H)& (1]

E,S,Q,DwN IA 1.APProval 4.Review 1.ADproved 4.Reviewednolcornme”t{seeWHC.CM-3.5, 2.Release 5.Post-Review 2.Ai?provedwhmme”t 5.ReviewedW/comments...12.71 3.Information6.rest.{ReceiptAcknow.Re@redl 3.Di.apwavedwlcormne.t 6.ReceiPtacknowledged

17. sIGNATuRE/DISTRIEWT!ON

ED-7400-172-2 (05/96) GEF097

.EC-74X-I72-1

j .

HNF-3556, Rev. O%

SAMPLING AND ANALYSIS PLAN FOR SLUDGELOCATED ON THE FLOOR AND IN THE PITS OFTHE 105-K BASINS

R. B. BakerDuke Engineering & Services Hanford, Inc. , Richland, WA 99352U.S. Department of Energy Contract DE-AC06-96RL13200

EDT/ECN : 620822 UC: UC 2070Org Code: 2F700 Charge Code: 105358B&R Code: EW7040000 Total Pages: 95

Key Words: K Basin, S1udge, Sampling and Analyses

Abstract: This Sampling and Analysis P1an (SAP) provides direction forthe sampling of the sludge found on the floor and in the remote pits ofthe 105-K Basins to provide: (1) basic data for the sludges that havenot been characterized to-date and (2) representative S1udge materialfor process tests to be made by the SNF Project/K Basins sludgetreatment process subproject. The sampling equipment developed willremove representative samples of the radioactive sludge from underwaterat the K Basins, depositing them in shielded containers for transport tothe Hanford Site 1aboratories. Included in the present document is thebasic background logic for selection of the samples to meet therequirements established in the Data Quality Objectives (DQO), HNF-2033,for this sampling activity. The present document also includes the1aboratory analyses, methods, procedures, and reporting that will berequired to meet the DQO.

TRADEMARKDISCLAIMER. Referenceherein to any.specificcommercialproduct, process, o! service bytrade name, trademark,manufacturer,or otherw se,does not necessarlIy constituteor ]mply itsendorsement,reconrnendation, or favoringby the Unlted States Governmentor any 8W”CY thereof orit. contractorsor subcontractors.

Printed i“ the United States of America. To obtain copies of this docunvmt, contact: DocunentCo”trot services,P.O. Box 950, Mai[stop H6-08, Richland WA 99352, Ph.ams(509) 372-2420;Fax (509) 376-4989.

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DATE :!,’..?r!:cR!3\

STA ~:,-~,~~ f ID:

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ReLease Approva[ Oate ReLease stamp

Approved for Public Release

A-6400-0T3 (01/97) GEF321

HNF-3556, Rev. O

SAMPLING AND ANALYSIS PLAN FOR SLUDGE LOCATED ON THEFLOOR AND IN THE PITS OF THE 105-K BASINS

R. B. Baker, T. L. Welsh, B. J. Makenas, and K. L. Pearce

November 199B

i

HNF-3556, Rev. O

CONTENTS

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

9.0

SAMPLING OBJECTIVES . . . . . . . . . . . . . . . . . . . . . . . .l.l PURPOSE . . . . . . . . . . . . . . . . . . . . . . . . . . . . :1.2 SAMPLING AND ANALYSIS ACTIVITY OBJECTIVE AND GOALS . . . . . . B

105-K WEST ANO 105-K EAST BASINS STATUS AND SAMPLINGINFORMATION 112.1 105-K WEiT” BiSiN”5iuiIGi ;HARiC~ERI~A+ION”S~AiU~ : : : : : : : : II2.2 105-K EAST BASIN SLUDGE CHARACTERIZATION STATUS . . . . . . . . 122.3 SAMPLING INFORMATION . . . . . . . . . . . . . . . . . . ...15

2.3.1 Sample Collection and Handling . . . . . . . . . . . . . 152.3.3 Field Sample Plan Modifications . . . . . . . . . . . . 192.3.4 Basis and Locations of Sampling . . . . . . . . . . . . 192.3.5 Sample Recovery, Final Compositing, and Preparation

at Hot Laboratory . . . . . . . . . . . . . . . . ...30

LABORATORY ANALYSIS INSTRUCTIONS . . . . . . . . . . . . . . . . . . 353.1 GENERAL . . . . . . . . . . . . . . . . . . . . . . . . . ...353.2 ANALYSES . . . . . . . . . . . . . . . . . . . . . . . . ...36

LABORATORY REPORTING REQUIREMENTS 474.1 OATA PACKAGING . . . . . . . :::: :::: :::: :::: :47

FINAL SUMMARY REPORT REQUIREMENTS 495.1 STATISTICAL ANALYSIS REQUIREMENT: : : : : : : : : : : : : : : : 49

SAFETY PLANS . . . . . . . . . . . . . . . . . . . . . . . . . ...516.1 RAOIATION/INDUSTRIAL SAFETY . . . . . . . . . . . . . . . . . . 516.2 NUCLEAR CRITICALITY SAFETY . . . . . . . . . . . . . . . . . . 51

GENERAL ALARA PLAN . . . . . . . . . . . . . . . . . . . . . . ...53

QUALITY ASSURANCE AND CONTROL PLAN . . . . . . . . . . . . . . . . . 55

REFERENCES . . . . . . . . . . . . . . . . . . . . . . . . . . ...57

APPENDIX A SUMMARY LETTER (DESH-9857199) DOCUMENTINGESTIMATED VOLUMES OF SLUDGE IN K BASINS . . . . . . . . 61

APPENDIX B SLUDGE DEPTH ESTIMATES AND SAMPLE LOCATIONSDETAIL FOR K WEST AND K EAST BASINS . . . . . . . . . . 77

1

HNF-3556, F@/. O

LIST OF FIGURES

1. S1udge Escaping Out Screened Holes in the Bottomof K East Basin Canister During Typical Move . . . . . . . . . . . . 13

2. Overview of the S1udge Core or Primary Floor SamplingEquipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

3. Overview of the Consolidated Floor Sludge Sampling Equipment . . . . 17

4. K West Basin Floor and Pit Sample Locations . . . . . . . . . . . . 26

5. KEast Basin Floor and Pit Samples . . . . . . . . . . . . . . . . . 29

6. Flow Chart of Sludge Sample Processing and Analyses . . . . . . . . 44

1.

2.

3.

4.

5.

6.

7.

8.

9.

LIST OF TABLES

General Sampling Scope Proposed by Data Qualfor Current Sampling . . . . . . . . . . . .

Floor and Pit Sludge Sampling Locations . .

ty Objectives. . . . . . . . . . . .

. . . . . . . . . . . .

Summary of K Basins Floor and Pit Sludge SamplingProjections . . . . . . . . . . . . . . . . . . . . . . . . . . . .

Overall Comparison of Proposed Targets from Data QualityObjectives to Present Sampling Projections for K Eastand KWest Floor and Pit Sludge . . . . . . . . . . . . . . . . . .

Summary of Sample Primary Uses, Sampler Used,and Compositing . . . . . . . . . . . . . . . . . . . . . . . . . .

Summary of Composite Samples . . . . . . . . . . . . . . . . . . .

Proposed Responsible Laboratory and Sample Conditionfor the Floor and Pit Sludge Samples . . . . . . . . . . . . . . . .

105-K West and K East Basins Floor and Pit Sludge Analyses . . . . .

Analytical Requirements for the 105-K West and East BasinsFloor and Pit Sludge Samples . . . . . . . . . . . . . . . . . . . .

12

20

21

22

24

25

33

37

39

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HNF-3556, Rev. O

LIST OF TERMS

ALARAANOVAAEABasin

CERCLA

CSBDESHDQODSCDSTECDEPAERDFGCGEAICICPISEIXMMain BasinMCOMDLNDTNHCPCBPHMCPNNLppbppmPQLPTFEQAQCRCRARPDSAPSARSARPSDSFBWPSNFCPsowSPSPCSVOATCTCLP

As Low As Reasonably AchievableAnalysis of VarianceAlpha Energy Analysis105-K West or East (as used in context) IrradiatedFuel Storage BasinComprehensive Environmental Response, Compensation,and Liability ActCanister Storage BuildingDuke Engineering & Services Hanford, Inc.Data Quality ObjectiveDifferential Scanning CalorimetryDouble Shel1 TankElectron Capture DetectionEnvironmental Protection AgencyEnvironmental Remediation Disposal FacilityGas ChromatographyGamma Energy AnalysisIon ChromatographyInductively Coupled PlasmaIon Specific ElectrodeIon Exchange Module (at K West Basin)105-K Irradiated Fuel Storage Basins Exclusive of Remote PitsMulti-Canister OverpackMinimum Detection LimitNondestructive TestingNumatec Hanford CompanyPolychlorinated BiphenylsProject Hanford Management ContractPacific Northwest National Laboratoriesparts per billionparts per mill ionPractical Quantitation Limitpolytetrafl uoroethyl eneQuality AssuranceQuality ControlResource Conservation Recovery Act of 1976Relative Percent Difference; [I(resultl - result2) I/mean]* 100Sampling and Analysis P1anSafety and Analysis ReportSafety and Analysis Report for PackagingSerial DilutionSand Filter Backwash PitSpent Nuclear Fuel Characterization ProjectStatement of WorkSpike AnalysisStatistical Process ControlSemivol atile Organic AnalysisTotal CarbonToxicity Characterization Leaching Procedure

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HNF-3556, Rev. O

LIST OF TERMS (Continued)

TGA Thermal Gravimetric AnalysisTIC Total Inorganic CarbonTICS Tentatively Identified CompoundsTIMS Thermal Ionization Mass SpectroscopyTLD Thermoluminescent DosimeterTOC Total Organic CarbonTSCA Toxic Substances Control ActTWRS Tank Waste Remediation SystemVOA Volatile Organic AnalysisWHC Westinghouse Hanford CompanyXRD X-Ray Oiffraction

4

HNF-3556, Rev. O

SAMPLING AND ANALYSIS PLAN FOR SLUDGE LOCATED ON THEFLOOR AND IN THE PITS OF THE 105-K BASINS

1.0 SAMPLING OBJECTIVES

MAs the present document is being completed the Spent Nuclear Fuel (SNF) projectmanagement and SNF Sludge Treatment Process subproject have just finished a review of thecost and benefits related to characterizationand process testing data supporting treatment ofK Basin sludges. The conclusions of this review are: (1) the benefits (i.e., reduced risks,design basis data, sludge material for processtesting,etc.)do not WarrantanY furthersampling or characterization of sludges in the K West Basin and (2) the additional samplingat K East Basin is warranted and should be completed. The project basis for this is theassumption the K East Basin sludge behavior conservatively bounds that of the sludges at theK West Basin. Based on these conclusions no further sampling of sludges will be attemptedfrom the floors or spent fuel storage canisters at K West Basin to support process treatmentdevelopment and confirmation.

By this noticethe reader isbeing informed that the K West samples will not be taken.In order to maintain required project schedules for the current sludge samplingactivities that are imminent, while maintaining consistent basis documentation:

●

●

●

●

The present Sampling and Analyses Plan (SAP) retains the references to theoriginal sampling planned for the K West floor sludge.

The K East Basin floor sludge samples described in the present SAP will betaken now as planned (this will maintain project schedules while beingconsistent with documentation).

During the period of time required to take the K East Basin samples, thesampling basis documentation (e.g., data quality objectives, etc.) will berevised reflecting the change of emphasis in sampling (i.e., sampfing sludgesonly at K East Basin).

Usirw the revised basis documents the present SAP will be revised asnecessary to assure the needs of the Sludge Treatment Process subproject aremet for sample material needed for process validation testing.

This latter item may require additional sludge sample material from the K East Basin floor toprovide sufficient sludge for validation tests. The equipment for sampling floor sludge at theK Basins will be maintained until the revisions of the basis documents are complete.

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HNF-3556, Rev. O

1. I PURPOSE

The data quality objectives (DQOS) for this S1udge sampling campaign areprovided in Makenas (1998a). The purpose of this sampling and analysis plan(SAP) is to define the strategy and the methods that will be used to sampleand analyze the S1udge (1) located on the floor of the main basin and pits at105-K West and (2) in selected locations in similar areas at the 105-K East8asin. The objectives for the sampling were rigorously developed by the SpentNuclear Fuel (SNF) sludge treatment process subproject over the past year andare documented in the general subproject DQO (Pearce 1998a), and the testingstrategy documents (Delegard 1998; Flament 1998a), followed by the specificsampling DQO (Makenas 1998) for this SAP. These objectives were furtherconfirmed by the independent review team for the initial sludge process flowdiagram (PFD) for treatment (Flament 1998b; Fink 1998). This team stronglyencouraged continued characterization of the sludge feed materials to clarifythe nominal and bounding cases involved.

The K West and K East 8asins floor and pit S1udge is generally expectedto be a nonhomogeneous mixture of particul ate materials containing some fuelelement corrosion products, environmental materials such as sand and insects,rack and canister corrosion products, sloughed-off concrete material, paintflakes from racks, and/or fuel element fission products. The K West BasinS1udge is expected to be somewhat similar in composition to that found to datein K East (Section 2.2 and Makenas 1996c) but with less fuel element relatedmaterials, because the canister barrels have 1ids and barrels have no S1otsor holes. K West sludges may also contain loose canister 1id seal material(e.g., Grafoil ), materials related to S1udge 1ike material from other Hanfordfacilities (e.g., many canisters in K West 8asin were sealed in N 8asin),ion-exchange-module (IXM)-related materials (differing from K East 8asin)that were spilled during basin operations, sand and unique basin material~~!~:ushed from the basin sand filter, and basin wall materials including

Sludge from a number of locations on the K East 8asin floor and in theWeasel Pit was sampled in 1995, characterized and documented (Makenas 1996c).A number of the samples in the present campaign are being taken in relatedlocations to provide both supplementary analyses and material required forS1udge chemical process treatment testing (Flament 1998a). The original floorsludge sample material taken in 1.995was not envisioned to be used to suPPorta treatment develo.pment project. Therefore, the quantity of sample taken atthat time was purposely kept close to the quantity needed only for projectedcharacterization analyses at that time (to minimize waste and returns toK 8asins). Thus, even with only initial testing for the S1udge treatmentprocess completed the available S1udge sample material from the 1995 samplingcampaign has been depleted in most cases. In addition to the samples used forsludge process development testing, samples are being taken at K East Basin inareas where potentially unique local quantities of sludge have either not beenpreviously sampled or where uncharacterized S1udge has been mixed with once-characterized S1udge inventories (e.g., Weasel Pit). While these sludges areexpected to be similar to those originally sampled in other locations atK East 8asin, the components may be different due to different historicactivities performed in those new locations (e.g., Dummy Elevator Pit,Sandfilter 8ackwash Pit, Tech View Pit).

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HNF-3556, Rev. O

Specifical lY this SAP contains (1) the PIan to acquire the sludge samplesfrom the floors and pits of the K West and K East Basins, and (2) the overal 1requirements for the analytical laboratories to subsample and analyze thesesamples.

1. Sam~le Acquisition Activities: Based on the DQO, which in turn isbased on the requirements from the subproject responsible for chemicaltreatment of the K Basins sludge (Flament 1998a; Pearce 1998a;Delegard 1998), a sampling campaign including 25 locations has beenplanned and described in this SAP. The satnpling wil 1 use two samplingmethods: (1) the system previously developed (Baker 1995a) using a“single pull” system to vacuum a sludge core sample into containersand (2) a modified sampling system for shallow areas of S1udge, thatprovides for a continuous suction of sample material and water into acontainer with the excess water exhausted through a fine filtertrapping the sludge sample; the system also allows sampling of two ormore similar physical locations into one container (“consolidated”samples). Once the samples are pulled by the single pull core samplerinto the special sample containers, they will be transported usingPAS-1 casks to the Hanford 222-S or 325 Building 1aboratories. Theselected subset of samples taken using the consol idation sampler willuse a container that is transported in a Chem-Nuclear cask to theHanford 325 Building Laboratory (by trans-shipping through the327 Building Laboratory pool facility).

2. Plan for Detailed Laboratory Anal Yses of Samples: The second purposeof this SAP is to provide the specific basic requirements for detailedhandling and analysis of the sludge samples after completion ofinitial acquisition activities noted in the previous paragraph. These1aboratory requirements form the general scope (i.e., specific1aboratory procedures, accuracies, etc.) and criteria (i.e., QualityAssurance, reporting, etc.) for the analyses of the S1udge samples.Statements of Work (SOW) will be written to the laboratories tosupplement this SAP after the samples are recovered from shippingcontainers and initial observations are complete. These SOWS willprovide specific instructions to the laboratories and confirm exactlywhich samples are to receive particular analyses and any specialhandling requirements. The final results of the laboratory analysesand their subsequent evaluation, will provide the final documenteddata satisfying the needs identified by the DQO (Makenas 1998a).

Basic to this sampling campaign are the specific requirements (or needs)the S1udge samples address. The DQO document (Makenas 1998a, Sections 2.4.2and 2.7) contains this rationale. Additional discussion of these requirementsare provided as background in Sections 1.2, 2.1, and 2.2 of this SAP.

The overall status of the past sampling campaigns is provided inSections 2.1 and 2.2 of this SAP. Additional sampling of S1udge in the fuelstorage canisters in both basins is planned to follow the floor and pit sludgesampling campaign which is the subject of the present SAP. The sampling ofcanisters in the future is primarily intended to provide prototypic materialfor development and design testing activities of the sludge chemical processtreatment system or its alternative (e.g., direct disposal of portions of thesludge, etc. ).

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HNF-3556, Rev. O

1.2 SAMPLING AND ANALYSIS ACTIVITY OBJECTIVE AND GOALS

The DQO document (Makenas 1998a) for the present activity summarizesthe objectives and logic relsting the present sampling effort to key SpentNuclear Fuel (SNF) project activities. The basic decisions requiring thesecharacterization data are related to (1) “does the previously uncharacterizedareas of S1udge preclude any of the goals of the S1udge treatment process toallow disposition of the resulting streams to the TWRS DST and EnvironmentalRemediation Disposal Facility (ERDF)?,” (2) “does the proposed sludgetreatment process work on a larger scale?, ” (3) “does fresh sludge (i.e,unoxidized S1udge materials versus the current, circa 1995, floor samples thatwere stored, and in most cases dried) influence the proposed sludge process ?,”and (4) “do anv of the areas of uncharacterized sludge provide constituents orbeha~i~r beyon~ the bounds previously established fo~ recovery, storage, andhandling methods to be used at the K 8asins to deliver the S1udge to theprocess treatment faci1ity?. ” The following enlarge on the DQO specifiedproject decisions being addressed by the present sampling campaign in thecontext

1.

of specific goals:

What are the physical properties and composition of the K West 8asinand K East Basin f1oor and pit S1udge from previOUS1y uncharacteri zedareas that COU1d impact the envisioned goals of the S1udge chemicaltreatment process?

Sam~l inc!Goals: Obtain samples of sludge from those uncharacterizedareas that are (1) feasible (physically-able) to sample and(2) contain significant volumes of S1udge. The S1udge samples willbe delivered to the Hanford Analytical Laboratories. Samples fromgeneral areas (e.g., single pit, related pit areas, etc. ) will becombined where reasonable to form “composite area” samples to maximizethe number of basin locations sampled for the amount (i.e., cost) ofchemical analyses performed. Data on highly local variations are notavailable using this approach, but this method is consistent with howthe sludge is expected to come to the treatment process. Al iquots ofthe samples wil1 be subjected to physical property testing, chemicalanalyses, and analyses for selected isotopic composition at theHanford Analytical Laboratories. These analyses wil1 provideconfirming data for design assumptions being used by the SNF sludgesubprojects. [Optionally, in addition, scoping process developmenttests, specific to the current treatment process, may be performedduring these analyses for the S1udge process treatment subproject ifneeds are identified and resources are available. ]

2. What are the physical and chemical effects on the envisioned S1udgeprocess treatment using “fresh” K 8asins S1udge samples: (1) withminimal aging (i.e., oxidation of components during drying, etc. ) ‘or(2) from basin locations where no historic (i.e., 1995) sludge samplematerial was avai1able for recently completed validation tests for theS1udge process treatment?

Samgl inq Goals: Obtain representative samples of K West 8asin andK East 8asin floor and pit S1udge (including areas previously sampledand analyzed from K East 8asin areas). The “sampling goals” as describedin the last portion of the prior paragraph follows similarly for this item.

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HNF-3556, Rev. O

3. Does the uncharacteri zed K West Basin and K East Basin f1oor and pitS1udge contain any constituents or combination of constituents thatWOU1d preclude the use of any processing or treatment alternative thatWOU1 d otherwise be considered as more desirable (i.e., cost effective,timely, ALARA, safer, etc.) than the current chemical treatmentprocess method? It is currently plannealto reassess options fortreatment to confirm the chemical treatment method for al1 S1udges isthe best choice from an engineering and cost standpoint.

Samul ina Goals: Obtain representative samples from uncharacterizedareas of the basins. Aliquots will be submitted for analyses todetermine chemical and isotopic compositions of selected constituents.Gross physical properties of sludge wil1 also be obtained from thesamples (e.g., settled density, volume, weight, settling time,behavior of selected layers, particle size, etc.). This will provideestimates of the analyte concentrations considered of importance toTWRS (e.g., Fowler 1995a, 1995b; Alderman 1997; Williams 1996) andalso provide estimates of analyte concentrations important tosuccessful handling of sludge as solid waste (Willis 1993).Additional attributes may need to be addressed if other S1udge processalternatives (e.g., grinding, direct disposal to solid waste, etc. )are “down-selected” and prove to be sensitive to parameters other thanthose of the chemical treatment process.

4. Does the currently proposed S1udge treatment process work on 1argeseale applications (hot tests using increased volume over the testingrecently completed) ? Whi1e this 1arge seale process testing is beyondscope of the present DQO and SAP, the present sampling scope doesinclude providing the required quantity of fresh “non-cani stern S1udgematerial for al1 subsequent final validation and 1arge seale hot cel1testing of the S1udge treatment process.

SamDl inq Goals: The demonstration of the current chemical processtreatment on a 1arger scale requires the quantities of non-canisterS1udge anticipated for testing by the sludge treatment processsubproject (Makenas 1998a; Delegard 1998). These sample quantitieswould include fresh S1udge from both previously (i.e., 1995) sampledareas and areas not sampled to-date. The material would be sampledfrom representative locations as defined by the DQO. The samples fromthe same general areas (e.g., within the same pit, same floor area,etc, ) would be combined to form samples representative of largerphysical areas (as suggested by the sludge process treatment develop-ment subproject staff). Al iquots of the resulting S1udge samplematerial would then be analyzed through a set of basic chemical andphysical analyses to provide the basis of their use in a processdevelopment testing matrix for 1arge scale process demonstration.Such testing would also consider similarities and differences betweenthe historic (i.e., 1995) S1udge sample material and the “fresh”sludge (currently being obtained), in order to relate the results ofprior and future testing.

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HNF-3556, Rev. O

5. Are the current choices of equipment reasonable to retrieve, handle(e.g., pump, etc. ), store, and process sludge within K Basins?

Samul inq Goals: Obtain fluid and theological properties whichcharacterize K West Basin and K East Basin sludges not previouslysampled to allow accurate development and validation of designs forS1udge handl ing equipment (i.e., transport, processing, filtering,etc.). This goal could also provide required Information fordeveloping suitable simulants for equipment development.

6. Can a nondestructive test method, such.as portable gamma scanning,provide an acceptable measure of the f1ssi1e content or of markerradionucl ides consistent with the fissi1e accountabi 1ity needs forK Basin floor and pit sludge handling and receipt? (This was notdirectly addressed in the DQO but is inferred in Table 2.4 of thatdocument under isotopes of europiurn).

Sampl inq Goals: Obtain contingent data for the potential developmentof relationships between fission product radioisotopes (measurable bygamma scan methods translatable to field applications) and plutoniumconcentration (measured by analytical 1aboratory methods) in theS1udge samples such that, if possible, one or more of the fissionproducts can be identified as a marker for P1utonium when quantifyingresidual transuranics in the S1udge. The data for europium isotopescan come from the gamma scan analyses being run for other objectivesat essential lY “no cost” and collected as a future contingent torespond to this issue.

In addition to the large-scale testing of the sludge treatment process,there wil 1 be the need for foilow-on verification related to the products ofthe treatment process being directly demonstrated as acceptable to thereceivers of the final waste streams. At this time the two receivers would be(1) TWRS double shell tanks (DSTS)-S1ated to receive the S1udge treatmentproduct stream and (2) ERDF-s1ated for the solid process waste stream.

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HNF-3556, Rev. O

2.0 105-K WEST AND 105-K EAST BASINS STATUS AND SAMPLING INFORMATION

2.1 105-K WEST BASIN SLUDGE CHARACTERIZATION STATUS

The 105-K West Basin was designed and constructed in 1950 to 1951. Thepurpose of the basin was to receive and store irradiated fuel from the K Westreactor. The basin provided the freshly irradiated fuel with cooling and a150-day period of time to allow short-1 ived isotopes to decay. The water inthe basin provided the workers with shielding from the nuclear radiationresulting from the isotope decay while they sorted and handled the fuelelements underwater.

The K West reactor stopped the irradiation of fuel in 1971. In 1976,the basins started receiving irradiated N Reactor fuel from the 105-N Basin.The fuel was stored in the basin in closed twin barreled canisters(Baker 1995a). A portion of this fuel is stil1 stored in the basin today,and some fuel elements have breached cladding such that significant corrosionof the exposed uranium fuel material may have occurred. These corrosionproducts are primarily hydrolyzed metal and deteriorated fuel compounds thatprecipitate as a flocculent sediment in the bottom of the canister barrelsand may be partially released to the basin when 1ids are removed. In additionsome canisters have 1id locking bars that have failed (broken), leaving thebarrels “closed” but not necessarily “sealed.”

Analyses of sludge in the K West Basin has occurred on (1) sludgesampled from nine selected fuel canisters, (2) smal1 samples of sludge fromthe Sandfilter Backwash Pit (i.e., North Loadout Pit), (3) subsurface S1udgeanalyzed from under cladding, and (4) trace amounts of S1udge that accompaniedfuel elements removed from canisters in 1995. Item 1 relates tocharacterization samples that received extensive analyses (Makenas 1998b).Item 2 relates to periodic cursory operations sampling made on the S1udgein the Sandfilter Backwash Pit which contains on the order of 4 m3 of sludge(depths of up to about 1 m). Item 3 relates to a series of samples of S1udgethat were in the shipping container and clung to the fuel elements examinedas part of the K Basins fuel element examinations (Makenas 1996c). Becauseof its possible impact, since it contains about 7% of the sludge at K Basins,it is noted that the appearance of the uncharacterized sludge in the K WestNorth Loadout Pit (Sandfilter Backwash Pit) appears different than othercharacter zed areas. This is described in Dodd (1995). Observed was agelatinous behavior associated with the release of large bubbles as the S1udgewas probed for depth measurements.

As part of the prior K West Basin characterization effort gas and watersamples were obtained from a number of the sealed canister barrels. Ofconcern was the gas composition related to hydrogen, cesium fission productsin the water, and the levels of corrosion inhibitor remaining in the canisterbarrel water. Corrosion inhibitor was injected into the barrels as they wereinitially closed. The DQO document for the canister sludge characterizationeffort (Makenas 1998b) provides additional background information.

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HNF-3556, Rev. O

The DQO for the present sampling campaign identifies the detailed statusof those areas in the K West Basin that have significant volumes of S1udgeand if they have been characterized. The information is summarized in Table 1which provides the base objectives of the sampling as prescribed by the DQO.The volumes of the samples address two basic requirements: (1) the need fromuncharacterized locations for chemical and physical characterization analysesand (2) the need of specific sludge sample material for use in treatmentprocess development and validation testing.

Table 1. General Sampling Scope Proposed by Data Quality Objectivesfor Current Sampling (Table 2.3 of Makenas 1998).

Number of (d~ya~~rtamsArea Locations per Sample Purposel

K East Floor 42 400 Treatment

K East Weasel Pit 2 500 Treatment

K East North Loadout Pit 2 350 Treatment

K East Dummy Elevator Pit 2 300 Character zat ion and Treatment

K East Tech View Pit 2 200 Character zat ion and Treatment

K West Floor 5 100 Character zation and Treatment

K West North Loadout Pit 53 200 Character zation and Treatment

K West Tech View Pit 23 200 Character zation and Treatment

K West Dummy Elevator Pit 1 200 Character zation and Treatment

Total 25 6400 Character zat ion and Treatment

lTreatment implies the material will be used for process studies.Characterization implies the samples address a here-to-for uncharacterizedarea of S1udge.

‘Includes one sample with intentionally 1arge concentration of resin beads.3Samples spread between main pit and transfer channel .

2.2 105-K EAST BASIN SLUDGE CHARACTERIZATION STATUS

K East Basin has a general operating history similar to that noted forK West Basin. The differences between the basins are: (1) K East Basin wasthe first of the two put into operation for N fuel storage, (2) the fuelstorage canisters have no 1ids, (3) and the fuel is in a much more degradedcondition. The canister barrels in some instances also have slotted sides andopen bottoms that can leak much of the canister sludge as they are moved inthe basin during normal handling, Figure 1. The basin itself is uncoatedconcrete, as opposed to K West Basin where the basin was drained and coated to

12

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Figure 1. Sludge Escaping Out Screened Holes in theBottom of K East Basin Canister During Typical Move.

13

HNF-3556, Rev. O

seal the concrete prior to the current storage mission. As noted in the DQOand in Appendix A, the K East Basin contains significantly more S1udge on itsfloor and in the pits than K West Basin (about 50 m3 K East versus 7 m3K West).

The K East Basin main basin floor and Weasel Pit S1udges were recentlycharacterized, based on 20 samples taken in 1995 (Makenas 1996c). In additionnine (9) samples of sludge from K East Basin fuel storage canisters weresubsequently taken in 1997 (Makenas 1996b). The nine canister samples weretaken to compare the mean property measurement values from the canister S1udgeto those of the floor/pit sludge. The K East Basin floor sludge was alsoperiodically sampled prior to 1995 (Baker 1995b). The analytical results haveindicated the floor sludge material to contain predominantly sands, ferricoxides, aluminum oxides, and uranium oxide residuals. The sludge has alsobeen found to contain trace amounts of barium, cadmium, chromium, lead, andsamariurn. Some S1udge samples from the floor, Weasel Pit, and canistersshowed the presence of polychlorinated biphenyls (PCBS). Samples from thecanisters also showed S1udge samples generated gas both in some of theshipping containers and during the settling studies. These samples containedvery high concentrations of fuel (e.g., uranium concentrations in dry canistersludge was high as 65 wt%). The gas formed in the K East canister sludge wasfound to be hydrogen with traces of fission gases and tritium. This leads tothe conclusion that unreacted uranium metal fuel could be present, however nosuch metal fuel was detected in the samples analyzed by X-Ray diffraction(XRD) . This 1ack of confirmation may result from there only being acomparatively few particles of uranium or that the particles are quicklycoated with an oxide layer masking the uranium metal from the XRD analysis.

The sludge in the 105-K East Basin Sand Filter Backwash Pit (SFBWP) andits transfer channel have been sampled periodical lY by operations to monitorfissile inventory buildup and a special sampling effort was completed in 1994related to a safety issue (Bechtold 1994; Baker 1995b).

The most recent overall set of measurements of floor S1udge depths inthe 105-K East Basin main basin were completed in 1994 and have shown that thebasin floor is covered with sludge to a depth of 5 cm to 19 cm (Baker 1995a)and that the Weasel Pit is covered with sludge up to a meter or more in depth(Makenas 1996c), see Appendix B, Figure B1. Potential local sources of sludgethat could ‘influence the floor S1udge characterization were evaluated by theSpent Nuclear Fuel Characterization Project organization (SNFCP) at that time(Baker 1995b). The local sources (besides the environmental sand, insects,etc.) considered were:

. Fuel S1udge passing through openings in canisters containingbreached fuel elements

. Corrosion of the aluminum canisters

● S1oughing of the unsealed concrete walls that form the basin

● Flaking paint off the fuel storage racks

+ Historical activities (e.g., fuel handling, IXM maintenance, etc. )affecting areas near the mouth of the pits (i.e., Weasel Pit,Tech View Pit, Dummy Elevator Pit, North Loadout Pit, and SouthLoadout Pit).

HNF-3556, Rev. O

As noted earlier, detailed sampling and analyses for the floor S1udge in theK East Basin main basin and Weasel Pit (Makenas 1996c) agreed withexpectations, with the exception of the unexpected identification of PCBS insome of the s]udge samples and the quantity of IXM beads found in certainlocations.

The DQO for the present sampling campaign identifies the detailed statusof those basin areas that have significant volumes of S1udge and have notbeen characterized in the original detailed sampling campaign in 1995. Theprimary reason these were not sampled at that time was because of physicaldebris obstructed sampling; in some cases these locations can now be sampled.Several other areas sampled in 1995 or 1994 now either have significant newsludge added to the area (i.e., Weasel Pit) or did not have a ful1 complimentof characterization analyses run on them (i.e., Sandfilter Backwash Pit).Finally, because almost al1 the S1udge samples from the prior floor and pitcharacterization campaign have been depleted during sludge treatment processtesting, more material is required for the validation tests from the generalbasin floor area and Weasel Pit. The information summarized in Table 1provides the base objectives of the sampling as prescribed by the DQO. Aswith the K West Basin sampling, the volumes of the samples in K East Basinaddress the two primary objectives: (1) the need of sludge from areas yetuncharacterized so chemical and physical characterization analyses can be madeand (2) the need of the sludge treatment process development subprojectrelated to development and validation testing.

2.3 SAMPLING INFORMATION

2.3.1 Sample Collection and Handling

The sampling at K Basins will be conducted such that the operation doesnot impact the water qual ity/air emissions. The sampl ing apparatus isdescribed in Baker (1998b and 1995c). Two similar systems wil1 be used toacquire samples. The first, the “single pull” sludge core sampler, is thesame equipment used for the 1995 K East Basin floor sampl ing campaign,Figure 2. It utilizes a metal tube (or pipe) to isolate representative coresamples of the S1udge material on the floor of the main basin and in remotepits. This core is vacuumed into a set of special 4 1iter sample bottles onthe basin grating above. The sampling team will foilow approved samplingprocedures during the collection of the samples. Detailed descriptions of thesampling apparatus and methodology will be provided in the sampling procedure(K Basins OP-43-031E [KE] and OP-43-032W [KW]) and Project Work P1an (K BasinPWP-98-001) .

The second sampling system, Figure 3, the “consolidated sampler, ” issimilar to the first except it is designed to collect sludge samples fromareas where the 1ayer of sludge is relatively shallow and does not provideenough depth for reasonable core sampling (e.g., depths less than about0.4 in.). This sampler uses a similar nozzle system, but CO1lects a sampleinto a 10 1iter, underwater container (similar to that used for canisterS1udge sampling, Makenas 1998b). The system does a continuous draw of

15

HNF-3556, Rev. O

Figure 2. Overview of the Sludge Core or Primary Floor Sampling Equipment.

m Ilfr VATER I

lt1141il !-.1 I

SXTP.ACID4

16

HNF-3556, Rev. O

Figure 3. Overview of the Consolidated Floor Sludge Sampling Equipment.

----

LAYOUT/SCHEMATIC CO NSOILDATED SAMPLER

P“n

17

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material through a fine (e.g., 5 micron) filter, exhausting the filtered waterback into the basin pool. Thus, the sampler is expected to capture mostparticles greater than 5 microns and a portion of those 5 microns or less.The prior floor and canister S1udge samplers pul1 directly into containers,retaining al1 water and material, that is no filters are used and no water ormaterial is exhausted back to basin (ie., “single pull”). This was done toassure minimal change in the physical properties of the S1udge sample pulled.For the subject shallow depth sludge samples it was judged much more importantto obtain significant volumes of material for analysis and testing than theconcern for the effects of the filter on physical properties and minor 1oss ofvery fine particles.

Each S1udge sample container will be 1abeled or marked with a uniquesample number. The SNFCP organization Test Engineer shall verify to ensurethe samples are properly identified and the sample location recorded prior tomoving the sample from the K Basins area. The SNFCP organization TestEngineer wil 1 ensure that the sample custody during transportation will betracked at al1 times by “chain-of-custody” protocol, resulting in documentedtraceabi 1ity.

After the S1udge core or “single pul1” samples have been collected intothe sample bottles, they wil1 be loaded in the PAS-1 Cask containers perK Basin procedure OP-43-016 “Load and Ship K Basin Sludge Samples in PAS-1Cask. ” For the consolidated sampler containers, similar logic will be usedbased on procedures currently being developed. The containers in this casewill be moved from K Basins to the 327 Building facility using theChem Nuclear cask (instead of the PAS-1 casks), and from there to the325 Building Laboratory using a Hanford 300 Area inter-building cask.

It is the intent of this SAP to ship the samples to the analytical1aboratory within a week of when they are CO1lected. If logistics precludeshipment within one week from the date of sampling, the SNFCP organizationProject Coordinator will evaluate the situation to provide applicable storagefor the samples. The consolidated sampler containers may be stored at theK Basins in the pool for a longer period of time (i.e., 1 month or more). Inthe basin pools these containers remain in an environment (i.e., temperature,chemistry, etc. ) similar to the sludge under general basin conditions, so thestored samples should maintain their integrity.

Once the sludge samples arrive at the 1aboratories they wil1 be storedand handled to avoid evaporation as much as possible. Because chemicalpreservation steps do not make allowance for S1urries and would adverselyaffect the sample (PH change), chemical preservation of samples wil1 not beperformed. It should be noted that since hydrogen gas generation has occurredin the canister S1udge samples, safety precautions are required in sealing anysmall containers in laboratories and hot cells.

As in the past campaigns, it is planned that the analytical 1aboratorieswill dispose of the remains of the S1udge and water samples after the analysesand sludge treatment process development tests are completed. If it is foundbeneficial, and the operations groups at K Basins concur, decanted water maybe returned to the K Basins from the laboratories.

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2.3.2 Sample Record Keeping

A vital part of the sampling activity is the assurance that al1 of theinformation and data associated with each sample are accurate and verifiable.Therefore, al1 pertinent information and data collected during the samplingsample breakdown, analyses and reporting will be recorded. The pertinent datato be CO1lected and the corresponding records will be maintained in accordancewith the requirements of the sampling procedure (K Basins OP-43-031E andOP-43-032W), and the QA at the 1aboratory doing the sample breakdown, analysisand reporting (see Section 8.0). Chain of custody (COC) forms will be used ateach step of collection and transfer by field and 1aboratory personnel (i.e.,required in K Basin Project Work P1an, etc). The SOWS for the sampling effortmay also provide additional direction on record keeping.

2.3.3 Field Sample Plan Modifications

Any modifications to the sludge sampling plan made in the field mustbe made/approved by the SNFCP organization Test Engineer and/or SNFCP ProjectCoordinator and documented. Changes affecting quality related informationwill include QA approval .

2.3.4 Basis and Locations of Sampling

Samples will be taken from locations consistent with the DQO(Makenas 1998a). In addition to the general DQO criteria, the selectionprocess also considered: (1) accessibility of the areas by the sampling crewat the basins, (2) possible disruption of the base S1udge layers by recentoperation and construction activities, and (3) current safety restrictions atthe basins. As in past sampling campaigns, a criterion was used to sample inreasonably accessible locations (i.e., sampling through grating slots--nograting removal, sampling around debris--no major debris removal , and samplingaround operation obstructions--not removing current restrictions around floordrain valves, etc.). Using these criteria were judged to have no significantimpacts on the qual ity of the samples with respect to their use. This followssince the S1udge within the areas being sampled is expected to be uniformlydeposited across these areas due to the expected dispersion of the materialthrough the pool of water.

Tables 2 and 3 define the samples and corresponding intended locations.In two 1ocations, the total number of samples taken was changed S1ightly fromthe DQO. Target versus projected S1udge volumes are noted in Table 4. Oneof the two samples to be taken in the K East Basin Tech View Pit was deletedbecause it was not possible, in the very shallow S1udge found present, to geta reasonable quantity of material that would warrant two core samples.Correspondingly, a sample was added to the K East Basin main floor area thatwil 1 be taken between the barrels of a canister with damaged fuel to provideadditional data (only one such sample was taken in 1995 campaign, “KES-O-09”).Such data are of concern to S1udge treatment process subproject for evaluatingthe alternative of recovering the K East Basin floor sludge, grouting it, andsending it directly to solid waste. One of the five samples indicated in the

19

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Table 2. Floor and Pit S1udge Sampling Locations.

SampleLocation

Location Identification Specific Sample Location Information

KW Basin

Main/EastBay K!J-(l)-Cl Deepest area of this bay (0.1 in. see SD-T1-054).

Main/CentraiBay KW-(2)-CI Deepest area in this bay (0.1 in. see SD-TI-054). ConsolidateduringsampLingwith KU-(1)-CI.

Main/West Bay-North KW-(3)-C2 Deepest area in NU corner of this bay (0.271 in. see SD-TI-054).Consolidateduring samp(ingwith KW-(5)-C2.

Main/West Bay-center KU-4 Core sample from deepest position in baylmain basin. Near center ofwest wall, 0.68 in., see SD-T1-054.

MainlWestBay-South KW-(5)-C2 Deepest area in SW corner of bay (0.4 in. see SD-TI-054). Consolidateduring sampling with KW-(3)-C2.

Worth Loadout Pit-1 KU-6 Center of Northwestopen area beyond restrictionin main pit.

North Loadout Pit-2 KU-7 Center of southwestopen area beyond restrictionin main pit.

North Loadout Pit Trs-1 KU-8 center of West haLf of transferchannel.

North Loadout Pit Trs-2 KU-9 Center of East ha1f of transferchannel.

Dummy Elevator Pit K!4-(10)-C3 Deepest area in pit, consolidateduring samfAing with KW-(12)-C3.

Tech View Pit South KE-11 Deepest area in Tech View South trans channeL, best effort.Channe(

Tech Vieu Pit Main KE-(12)-c3 Deepest area in main pit (0.11 in., see sD-TI-054). Consolidateduringsamp(ingwith KW-(10)-C3.

KE Basin

Main/East Bay KE-I Cubical 0168 South side, similar to KES-K-12 tocation.

Main/EastBay-South KE-2 Cubical 1065 North side.

MainlUest Bay-IXM KE-3 Same as KES-H-08 Location,cubicaL 6755 onty North side, deepest area.

Main/West Bay KE-4 Cubicat 6722 North side, similar to KES-I-15.

North LoadOut Pit KE-5 Middle unrestrictedarea of main pit.

North LoadOut Pit Trs KE-6 Midd(e of trmsfer chan”ei.

Olmy Etevator Pit-1 KE-7 Best effort middle of East ha~f of pit.

OlmlrlyElevator Pit-2 KE-8 Best effort midd(e of West half of pit.

WeaseL Pit-East KE-9 Midway between uhere KES-R-18 and KES-S-19 were take”.

Weasel Pit-west KE-ID Midway between where KES-P-16 and KES-Q-17 were taken.

Tech View Pit North KE-11 North channe( midway between doors, along South ual1, deepest studge.Channet

Main Basin East-lXM-2 KE-12 Second IXM main f~oor sampte, cubica~ 6756 to deepest area, simiLar toKES-H-08.

Setween Barrels KE-13 Cubica( 4573, between barrels of slotted canister ~ith damaged fue[.

Note: The KES samples are from 1995 sampling, see WHC-SP-1182.

20

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Table 3. Summary of K Basins Floor and Pit Sludge Sampling Projecti

21

ens.

HNF-3556, Rev. O

Table 4. Overall Comparison of Proposed Targets from Data Quality Objectivesto Present Sampling Projections for K East and K West Floor and Pit S1udge.

~

DQO SAP

Target Target Target CalculatedDry Total Target Total Total Calculated

Weight Dry Total As- Volume Recovered TotalNumber of per Weight Settled As- Volume S1udge Dry Number ofSample Location per Area Weight Settled As-Settled

LocationsWeight Sample

(9) (9) (9) (m!) (m!) (m!) Location!

KE F1oor 3 400 1200 2000 1538 1530 1193 4

KE Floor, 1 400 400 667 513 878 685 2IXM

KE Weasel 2 500 1000 1667 1282 1523 1188 2Pit

KE North 2 350 700 1167 897 1143 891 2Loadout Pit

KE Dummy 2 300 600 1000 769 740 577 2ElevatorPit

KE Tech 2 200 400 667 513 148 116 1View Pit

KW Floor 5 100 500 833 641 1130 882 5

KW North 5 200 1000 1667 1282 1496 1167 4Loadout Pit

KW Tech 2 200 400 667 513 356 278 2View Pit

KW Dummy 1 200 200 333 256 263 205 1ElevatorPit

Total 25 6400 10667 8205 9208 7182 25

Notes: Assumed conversion factors:Density g/ret as-settled 1.3Factor from wet to dry 0.6Recovery factor cores 0.57 (based partially on 1995, total recovery to

1aboratory)Recovery factor consolidated 0.75 Estimate

22

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DQO for the K West Basin North Loadout Pit was deleted. This was done becausesufficient volume of material could be obtained from four samples (conservingresources) and four samples was judged sufficient to characterize the 1imitedarea accessible.

To maximize the number of locations sampled within the resourcesavailable, sampling is planned at 25 locations but this material will becomposite into 12 samples prior to starting detailed analyses in thelaboratories. The DQO calls for not combining material from different pits.This was followed except for very shallow areas. Here it was judged much moreadvantageous to obtain a composite than have to ignore the area because ofresources precluding so many analyses. Further, the only such composite (fromK West Dummy Elevator Pit and Tech View Pit) is from pit areas that are inopen communication (i.e., no doors or screens in between) with the main basin.

The conversion factors and constants used throughout the present SAP forS1udge density; relsting wet and dry S1udge; and expected recovery factors forthe samples is provided in the notes of Table 4. These are based on pastexperience from sampling floor sludge in K East Basin (Makenas 1996c).

S1udge depths in Table 3 are based on the historic data (K East Basinmeasurements made in 1994 and 1995, K West Basin measurements made in 1997).Operations at K Basin may have affected S1udge depths noted here and currentactual depths could vary. As sludge samples are taken during the campaign theS1udge depths of the sampled area wil1 be confirmed using the scales providedon the outside of the isolation tubes used in the core sampler or measuredwith an auxil iary measurement scale when the consol idated sampler is used.Generally, it is intended to take samples where local area depths of sludgeare greatest (reflecting the greatest amounts of material in the basins). Itwill be an option for the SNFCP Test Engineer to move the location of a samplein a specific area if the S1udge depth appears more appropriate at a nearbylocation. Final sampling locations will be documented in the logbook andvideo taping wil 1 be performed as samples are taken. AS with prior campaigns(e.g., Makenas 1996c) the final evaluation report for these samplingactivities will document the locations and condition of the sludge in theareas sampled.

K West Basin--Twelve sample locations, Figure 4, were selected from K WestBasin, Tables 2 and 3. Six of these wil1 be taken with the primary floorS1udge sampl ing device using the isolation tubes to isolate cores of sludge(i.e., single pull core sampler). Six locations will be sampled with theconsolidated sampling equipment (because of the comparatively shallow depthof sludge in these areas). With the consolidation sampler the S1udge fromtwo similar physical locations in the basin will be drawn into a singlesampling container (i.e., they will be consolidated), see Section 2.5.1. Forthe K West Basin campaign this will result in three consolidated samplecontainers containing the material from the six K West Basin and open pitlocations. See Tables 5 and 6 for summary of which sampler is being used todraw specific samples.

Main Basin Floor: Samples wil1 be drawn from five locations,Figure 4, of the main basin floor at K West Basin. Figure B1 ofAppendix B indicates the depths involved, based on measurements made in

23

N.D

S1udge TyPe FinalSample Primary Sample Initial Process Sampling Composite

Location Container Characterization Treatment Equipment SampleLocation Identification Identification Sample? Sample? Used Identification

KW Basin

Ku Basin Hain/East Bay KU-(1 ).C1 MCI Y Y CO”,.( idatd FIJI

nclin/centml w KW(2)-C1 ml Y Y cons. [ i dated FU1

Nain/Uest 8wNorth KW-(3).C2 WC2 Y Y CO”,.( i dated F!41

Main/vest w-center W-4 ml Y Y Core FW2

Main/Mest B.y South KW(5)-C2 UC2 Y Y cons. [ i d,t ed FU1

North Loadout Pi t-1 K!+6 W82 Y Y core FU3

North Lmdo”t Pit-2 KW7 !+33 Y v core FU3

U.,th L.adout Pit 1,s.1 KM-8 WA Y Y core FW3

North L.ad.ut Pit Tw2 KU-9 m Y v c.,. FW3

Dmny Elevator Pit KW(10)-C3 UC3 Y Y CO”,. ( id, ted n14

Tech Vial Pit South Chaml W-II !436 Y Y core FU5

Tech Vie. Pit Main KI+(12)-c3 MCI Y Y Con.ohid,tf.i FU4

.KE Basin

Main/Ea,t W KE-1 EB1 N Y Co,. FE1

M.in/Ea.t Bay-South KE.2 E82 N Y core FE1

U3in{llest W-1X!4 KE-3 EB3 N Y core FEZ

Main/L!e.t W KE.6 E84 N Y core FE1

.Nmth Loach.t Pit KE-5 EB5 N Y core FE3

North Lmdo”t Pit 1,s KE-6 E86 N Y core FE3

Dumr Ekv.3tor Pit-1 KE-7 EB7 Y Y cow FE4

Dumly EIWat.? Pit.2 KE.8 EB8 ‘f Y cow w

W,.3S, I Pit-EaSt KE-9 E89 N Y core FE5

Weaset Pit-Uest KE-10 EB1O N Y core FE5

le.h Vie” Pit Ninth Chml KE.11 EB11 Y Y core FE6

Main Basin EW.1W2 KE-12 EB12 N Y core FE2

.Betueen8.,,.1s KE.13 EB13 N Y core FE7

BIa.k KBLK K81K N/A Nlh core K8LK

m

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HNF-3556, Rev. O

Table 6. Summary of Composite Samples.

Sample Primary Samples Used toSample Type Designation Make Composite Area Represented

1

Core S2udge Sampler

Normal FW2 KW-4 KW deepest floor

Research FW3 KW-6, KW-7, KW-8, KW-9 ~;a~~;~h loadout pit and

Normal FW5 KW-11 KW tech view pit

Normal FEI KE-1 , KE-2, KE-4 KE floor, general

Normal FE2 KE-3 , KE-12 KE floor, IXM beads

Research FE3 KE-5 , KE-6 KE North loadout pit andchannel

Normal FE4 KE-7 , KE-8 KE dummy elevator pit

Normal FE5 KE-9, KE-10 KE weasel pit

Normal FE6 KE-11 KE Tech view pit

Normal FE7 KE-13 KE floor between S1ottedbarrels with damaged fuel

Normal K8LK Equipment blank water KE equipment water sample

Consolidated Sludge Sampler

Normal FW1 KW-(1)-C1, KW-(2)-CI, KW floor, East bay andKW-(3)-C2, KW-(5)-C2 Center bay

Normal FW5 KW-(1O)-C3, KW-(12)-C3 KW dummy elevator pit andtech view pit

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Figure 4. K West Basin F1oor and Pit Sample Locations.

Y

26

HNF-3556, Rev. O

1997 (Maassen 1997). The consolidated sampling equipment will be used todraw two approximately 350 ml (i.e., original wet sample volume) samplesof S1udge from one location in the East Bay and one in the Central Bay,into a single sample container. These locations were selected becausethey are the deepest observed (Maassen 1997) in these bays with veryshallow S1udge depths. The West Bay was observed to have deeper areas ofsludge than the East and Central Bays. A second consol idated samplecontainer wil1 be used to draw similar quantities of S1udge from twolocations in the West Bay, one from the Northwest and one from theSouthwest areas. These samples wil1 be representative of two of thedeeper (though stil1 comparatively shallow) areas in the main basin.The consolidated sample target volumes were intentionally made largerthan required by DQO to provide for contingency during sample recoveryin the 1aboratory.

Finally, a fifth location will be sampled in the main basin using theprimary (i.e., core) sampling device, drawing a sample using the 1argestdiameter isolation tube (i.e., 4 in. diameter). This sample will betaken at the location in the West Bay where the S1udge is indicated tobe the deepest on the main floor (Maassen 1997) see Figure B1. It isintended that this sample provide any required data on S1urry rheologyproperties for the main basin floor sludge, since it will have thematerial most representative for this type characterization (versus theconsol idated sampler material that may not include a portion of thepopulation of very fine, less than 5 microns, particle sizes). Thecombination of using the consolidated sampler to provide the two 1argervolume samples from four areas (primarily to support pretreatment processdevelopment) and one core sample (to provide a base check using singlepul1 sample material) provides for the intended sampling objectives.

North Loadout (or Sandfilter Backwash) Pit: The North Loadout Pit wil 1have a total of four samples taken from it, Figure B2. Sludge in thispit has not been previously characterized? see Section 2.1, and itrepresents the greatest volume of S1udge In K West Basin, Appendix A.Sludge depth measurements, Figure B3, for this pit were reported byDodd (1995) . Routine operations have taken very smal1 dilute samples ofsludge to characterize potential fissile material inventory changes asbackfl ushes have occurred. For the present characterization campaign twosamples will be taken from the transfer channel; dividing the channelinto a front (East) half and a back (West) half then taking samples nearthe middle of these areas. Two samples wil1 be taken from the main pitarea; spanning the available open area outside the floor drain valverestricted area, (a 6 ft radius circle encompassing the floor drainvalves, see Figure B2). The primary intent is to CO1lect sufficientsludge material for S1udge treatment process development testing, sinceit is not expected that there will be significant variation in the sludgecomposition across the pit because of the way the material is backfl ushedinto the pit with 1arge volumes of water. However, it is expected thatthe S1udge composition will vary by depth. To provide some spatialvariation indicator, and since a 1imited number of sizes of isolationtubes are available, two samples are being taken in the relatively smallarea of the main pit.

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South Loadout Pit: The sludge in the South Loadout Pit was pumped tothe South Channel of the Tech View Pit in 1997, see Appendix A.

Dummy Elevator Pit and Tech View Pit: The Dummy Elevator Pit has anestimated sludge volume of only 1.4 ft3, with a maximum estimated depthof 0.3 in. (Maassen 1997). The Tech View Pit also has a relatively smallquantity of sludge, total of 2.4 ft3. It was judged it would be adequatefor these pits to use one consolidated sample including: approximately350 m! of S1udge from the deepest location in the Dummy Elevator Pit anda similar quantity from the deepest location in the main pit of the TechView Pit. While the DQO recommended that S1udge samples from differentpits not be combined, in the case of these two “open” (to the main basin)pit areas with only shallow quantities of sludge, it was judged moreimportant to obtain some information and significant material from bothareas than potential ly eliminating one due to resource constraints.Because the consolidated sampler equipment cannot be used in the SouthChannel of the Tech View Pit (area is screened off from main basin) acore sample is being taken in this shallow area. Figures B4 and B5provide the sampling locations and Figure B1 provides selected sludgedepths for reference.

Weasel Pit and Oischarqe Chute: It was judged with a maximum observeddepth of 0.1 in., Figure B], that neither of these relatively small areaswarrant sampling (Makenas 1998a).

K East Basin--In K East Basin 13 samples will be taken, Figure 5. All thesamples being taken in K East Basin will be drawn with the primary (i.e.,core) floor sludge sampler.

Main Basin Floor: Cubicle locations in two of the three bays wereselected for sampling based on sludge depth and past sampl ing locations,Figure 5. The sample locations were generally chosen from the deeperareas, Figure B6, so the sum of the samples represent the 1argestquantities of S1udge on the K East Basin floor. Similarly, generallocations to those used in prior (Figure B7) campaigns (i.e., oppositesides of the same empty cubicals sampled in 1995) were chosen in severalcases; this was done to better assure accessibility and provide some1inkage of the sludge from prior analysis results to the currentmaterial . Two samples, KE-3 and KE-12 were chosen specifically toprovide samples with a high percentage (e.g., 75%) of IXM beads, similarto sample KES-H-08 from the sampling made in 1995. These samples withbeads seek to provide the quantity identified in DQO as wel1 asproviding, on a best effort basis, some additional material for testingas identified in Oelegard (1998) as needed.

Sample KE-13 was selected, as requested by the S1udge treatment processdevelopment subproject staff, to be between the barrels of a canisterwith damaged fuel . This will provide a second data point under theseconditions (one taken in 1995, “KES-O-09”). KE-13 is being taken fromthe floor in the Center 8ay. The overal1 volume of sludge in this bay isless than the other two bays and a portion (i.e., the central area) ofthe S1udge originally located in this bay was pumped to the Weasel Pitafter 1995. Therefore, the two samples to come from the Weasel Pit inthe present campaign should include some material from this bay.

28

HNF-3556, Rev.

Figure 5. K East Basin Floor

o

and Pit Samples.

Y

29

HNF-3556, Rev. O

North Loadout Pit: A sample wil1 be drawn from the center of the non-restricted area of the main pit of the North Loadout Pit. A secondsample will be taken from the transfer channel near its center,Figures B8 and 89. These samples are primarily to provide material forthe S1udge treatment process development. Since the material in theseareas should be reasonably mixed as backflushes are made of thesandfilter, only a single sample from each general location is required.

South Loadout Pit and Discharge Chute: No significant sludge remains inthe South Loadout Pit or the Discharge Chute. The South Loadout PitS1udge was pumped to the Weasel Pit after 1995. The Discharge Chute waspumped to the Weasel Pit prior to the 1995 sampling campaign(Welsh 1995).

Dummy Elevator Pit: The Dummy Elevator Pit was not sampled during the1995 sampling campaign because there was too much debris in it to allowaccess to the floor by the sampling equipment. Some of the debris hasnow been removed and significant sludge is projected to reside in the pit(though this has not been directly measured, Appendix A). Two sampleswil 1 be taken from the Dummy Elevator Pit on a “best effort” basis (thereis still significant debris) during the present sampling campaign. Onesample wil 1 be attempted near the center of the East half of the pit andone in the West half of the pit, Figure B1O.

Weasel Pit: Since the 1995 characterization campaign the Weasel Pit hashad S1udge from the South Loadout Pit and the center area of the CenterBay added to it. Figure Bll indicates the sludge depths in 1995 andFigure B12 the sample 1ocations used in 1995. For the current samplingcampaign of the Weasel Pit two samples will be taken, Figure B13. Onesample will be taken between the location of the samples designatedKES-Q-17 and KES-P-18 in the 1995 campaign, and similarly the secondsample wil 1 be taken between the locations of the KES-S-19 and KES-R-18samples. Because harder layers were encountered at different depthsduring the 1995 sampling of this pit (Makenas 1996c), it is planned thatthe particular locations previously sampled wil1 be avoided during thecurrent sampl ing to better ensure representative core samples areobtained (i.e., from undisturbed areas).

Tech View Pit: The Tech View Pit sludge was not sampled in the 1995campaign. One sample will be drawn during the current campaign. Thiswil 1 be located, Figure B13, where the deeper area of sludge was observedpreviously in the North Channel (Baker 1995a).

2.3.5” Sample Recovery, Final Compositi ng, and Preparation at Hot Laboratory

Procedure(s) or test instructions for the recovery of the sample materialfrom the shipping containers (i.e., either 4 liter bottles or 10 liter sludgecontainers) and subsequent sample preparation and handl ing will be prepared bythe designated Hanford Laboratory. These procedures will be similar to thoseused for the K East Basin floor sludge samples (Bechtold 1994). The samplepreparation and handling procedure wil1 contain the detailed instructions

30

HNF-3556, Rev. O

necessary to safely and properly record observations, monitor, settle, decantand subsample (as needed), digest (if necessary), handle, package, and 1abeleach sample and its derivatives in the hot cell/hood. The SNFCP organizationProject Coordinator will concur with the procedures or test instructions priorto their application.

For the present floor and pit sludge sampling campaign, it is planned tocombine or composite sample material from similar basin locations (e.g., samefloor area, same pit, etc. ) prior to initiating the detailed analyses or useof the sample S1udge materials for testing. In the case of the samples comingfrom the primary (i.e., core) sampler, this means combining the S1udge samplematerials from several locations together into a single initial container(e.g., combining sludge from sample bottles from several 1ocations into agraduated cylinder) at the 1aboratory hot cel1. Then proceeding withsubsequent characterization analyses and pretreatment testing from thiscomposite sample. In the case of the consolidated sampler the sludge samplematerial wil 1 be combined as it is CO1lected from the two or three basinlocations sampled. Therefore, the material need only be removed from thesample container and transferred to laboratory container to begin analyses(e.g., settling, etc.). Tables 3, 5, and 6 show the samples that arecurrently planned for compositing, this may be revised in the SOWS if thecondition of the actual sample material recovered warrants a differentapproach.

Samples will be designated either “normal” or “research” after settling,the handl ing of the “normal” and “research” samples differ in that theresearch samples will be separated for analyses of individual 1ayers. A“normal” sample will be homogenized and analyses will be performed on theintegrated properties. The “research” samples will be separated into major“1ayers” and each 1ayer analyzed. This is necessary for meaningful rheologymeasurements and is of interest for possible impact of settled layers behavingdifferently than the mixed mass of the sample (e.g., plutonium concentration).Layers will be identified as was done for the prior K East Basin floor sludgesamples--that is a visual identification by color and/or texture of regions ofsludge material appearing as stratum after settling studies are completed.Typical ly two or three layers were found in the K East Basin S1udge samples. ”Table 5 indicate those samples initiallY selected for research samples,however, this selection could be revised in subsequent SOWS after the materialhas gone through settling studies.

Analysis of all the sludge samples by 1ayers was considered. It was?however, concluded the 1imited number of research samples would be sufficient.Factors involved in this decision (not analyzing by 1ayers in all samples)included: the sludge feed streams will be mixed during recovery and transportto the sludge treatment equipment, the difficulty in objectively determininglayers, settling differences between the evolving material in the basin versususing al1 the material at once in the analytical 1aboratory, a desire tomaintain the maximum sample quantity to minimize potential for inhomogeneitieswhen spl itting, and lack of objective data concerning the distribution of theheavier components. The research samples were chosen from the North LoadoutPit because these represent the 1argest volumes of S1udge that have not beencharacterized related to fluid properties and information on layering (such asdensities).

HNF-3556, Rev. O

Subsampl es for organics analyses and other analyses affected by either

drying or acid digestion (TIC, TOC, TC, DSC, IC, XRD, etc. ) need to be

obtained prior to sample preparation.

In some cases, as specified in subsequent SOWS, the 1iquid portion andthe wet S1udge should be sampled for the various analyses. Table 7 indicatesthe condition of the sample material for the various analyses.

It is very important that the analytical 1aboratories measure and recordthe evolving densities (i.e., volumes and weights) of the sludge samples(i.e., as-settled, centrifuged, partially dried, dried, etc.). Thesedensities will allow both comparison to past work and the state of sludge ascollected.

32

HNF-3556, Rev. O

Table 7. Proposed Responsible Laboratory and SampleCondition for the Floor and Pit Sludge Samples.

AcceptableProposed to Acid Acceptable

Analysis’ Laborat.ory2 Digest ? to Dry ? Comments

{ad-Chemistry’

!,l!:o~!%lcrn222-s Yes Yes 238PU, 23g’240Pu222-s Yes Yes

U To{al 222-s Yes YesU Isotopes 325 Yes Yes

Zssu 234U 235U 236U 238U

GEA 222-s Yes Yes V, Cs, aid Eu Isoto~esTotal Alpha 222-s Yes YesTotal Beta 237 222-s Yes Yes99Tc, 90Sr, Np 222-s Yes Yes

;eneral ChemistryICP Metals 222-s Yes YesIC Ions 222-s No NoTOC/TIC/TC 222-s No NoSVOA/PCB 325 No NopH 222-s No NoCaustic Demand 222-s No No

‘hysical Pro~ertiesSettling Rate 325 No NoAppearance 325 No NoViscosity 325 No No Report Ful1 CurvesOe:)e;y (p) 325 No No

325 No NoDry Particle 325 No NoXRD

Pyrophori c Material 325 No YesResiduals (digest) 325 No Yes

Particle Size 325 No NoParticle Shape 325 No NoZeta Potential 325 No No

“hermal PropertiesTGA/DSC 325 No No Report Ful1 Thermogram

‘recess Testinq Sam~les 325, 222-S No No

,‘Some sludge materials have PCB levels that may require a TSCA permit for furtherprocess testing.

2222-S is the Hanford 222-S Laboratory facility, 325 is the Hanford/PNNL 325 BuildingRadiochemi stry Process Development Laboratory.

3Shipping between 1aboratories may require 325 Building to run selected radiochemi stryto support sh~~ments.

4Report 236Pu, Pu, 240Pu, and Zqlpu if generatedas part of other analYses.

33

HNF-3556, Rev. O

This page intentionally left blank.

34

HNF-3556, Rev. O

3.0 LABORATORY ANALYSIS INSTRUCTIONS

3.1 GENERAL

Specific instructions on processing of each S1udge sample and compositeS1udge samples in the analytical laboratories wil 1 be provided by Statements

of Work (SOW) from the SNFCP organization prior to shipment of samples or

after the observation of the recovered samples. For shipping subsamplesbetween 1aboratories S1udge samples may be analyzed initially to ascertainproperties such as fissile and fission product content for criticality,shielding and accountability.

Each sludge shipping container (either 4 liter bottle or 10 litercontainer) wil 1 be received by the analytical 1aboratories. The S1udgesamples will then be recovered from the shipping containers and prepared forsettling studies, Section 2.3.5. Certain samples will be combined to providecomposites, either as indicated in Tables 5 and 6, or as directed bysubsequent SOWS. During the settling studies, any observations of gasgeneration from the sludge material should be immediately noted to the SNFCPorganization. If significant, an evaluation will be conducted to determine ifgas monitoring is required. High resolution video taping will be made ofsamples during settling studies and if gas generation is observed.

Selected sludge physical properties (e.g., settling rate, density, etc. )wil1 be obtained prior to any subsampl ing efforts. Other properties (suchas viscosity and particle size/shape) must be determined from aliquots takenprior to any other preparation steps. Prior to heating or acid digestion,aliquots of both the 1iquid and the solids will be obtained from theappropriate samples. These aliquots wil1 be used by the 1aboratories fororganic, TIC, TOC, XRD, DSC, TGA, and other analyses sensitive to eitherdrying or acid digestion. An aliquot of the thoroughly stirred dried sludge,of sufficient weight to minimize sample heterogeneity, wil1 then be processedthrough an acid digest procedure. An aliquot of the acid digested sludgeshall be prepared and sent to the 1aboratory. Any residual solids whichremain after the acid digestion step wil1 be analyzed by XRD. If there is asufficient quantity the residuals will also be subjected to caustic fusion andfurther ICP, radiochemistry, and XRD analyses. The acid digest (i.e., hotplate and beaker) used will be the same as that previously used for the K EastBasin canister sludge analyses (Makenas 1997) or as specified in subsequentsows . The general condition of the sample for the different analyses isprovided in Table 7.

The 1aboratory will analyze each aliquot in duplicate or as directed inSection 8.0 of the present SAP or subsequent SOWS. Each subsample taken fromthat aliquot must go through separate sample preparation, if samplepreparation is required. If a sufficient amount of dried sludge is notavailable for the acid digestion step, then analyses for that sample may be1imited to higher priority data. The laboratory should subsequently documentthe reason for not performing any of the analyses called for in the SOW in thenarrative of their data report. An alternative to not performing the analysesis to have K Basin Operations take additional samples for the “other”

35

HNF-3556, Rev. O

required analyses. The choice of not performing analyses or requesting

additional samples will be at the discretion of the SNFCP organization ProjectCoordinator.

A flowchart showing the general analysis scheme for the S1udge samples

in the 1aboratory is presented in Figure 6. The analytical tests for theanalytical laboratory work are shown in Table 8. The reason or need for eachof these analyses is defined in the DQO (Makenas 1998a). In general thesamples designated as “normal” will receive all the analyses in Table 9 withthe exception of those related to rheology measurements. The “research”samples wil 1 be split into samples of the observed layers or strata, and thesewill each in general receive all the analyses in Tables 8 and 9 includingrheology measurements (also see Sections 2.3.5 and 3.1).

Note that no analyses for waste designation are called for in the DQO(see Section 2.2 of that document). This follows directly from the assumptionmade by the SNF Project for K 8asin sludge that the waste designation wil 1 bemade based on “process knowledge. ” As discussed in the DQO document,pyrophoricity of the sludge is being assessed from the XRD measurements formetal 1ic zirconium, metal 1ic uranium, and uranium hydrides. Exothermicreactions may be evaluated by differential scanning calorimetry (DSC).

An additional objective of this sampling campaign is to providerepresentative sludge material to the K Basin S1udge treatment processdevelopment subproject testing activities. Any material not directlyused for characterization analyses will be kept as much as possible inan “as-collected” state during any storage in the hot cel1s and shippingactivities. The material should not be allowed to dry out (oxidizing somematerials and causing physical changes), be mixed with non-prototypicmaterials (e.g., de-ionized water, etc.) or subjected to extremes inenvironment (i.e, higher than room temperatures, high PH, contact withpotential ly contaminating surfaces, etc.). The disposition of the samplematerial will be the subject of a SOW after the samples are obtainedand initially observed. This SOW wil1 provide more direction on storageenvironment requirements. The actual testing and analyses related to S1udgeprocess development testing itself will be covered under separate SOWS fromthe sludge treatment process subproject. The exception to this is for scopingprocess testing done with the initial samples in direct cooperation with thesludge treatment process subproject, in order to improve the economics of theoveral 1 project.

3.2 ANALYSES

Table 9 shows the analytes, methods, and the laboratory proceduresrequired for the analysis of the samples. The table also 1ists therequirements for detection levels, precision, and accuracy of data results.Note that if di1ution factors change from what is expected based on factorsfrom the 1995 K East Basin floor S1udge sampling (Miller 1995), the detectionlevels, precision, and accuracy values shown in Table 9 will have to bere-evaluated. The SNFCP Project Coordinator will be notified of the conditionand a decision will be made and documented on how to proceed. One reagentblank will be run if required by the laboratory procedure for each analytical

36

HNF-3556, Rev. O

Table 8. 105-K West and K East Basins F1oor and Pit Sludge Analyses.

Requested Analysis Analysis Technique Constituents to be Reported

Am-Isotopic Separation and AEA 241Am 238Pu, 239/240pu , and

Pu-Isotopic243/24tCm

Sr-90 Separation and beta 9osr

counting

NP-237 Extraction and alpha237NP

counting

Total Gamma GEA241AM, 134CS , 137CS

60Co, ‘52Eu, ‘54Eu,‘55Eu, 212Bi, 2Q8T1~ 125Sb, 226Ra, 95Nb,106Ru/Rh and ‘44Ce/Pr and other gamma

emitters in 1ibrary

Gross Alpha Gas proportional Detectable alpha emitterscounting

Gross Beta Gas proportional Detectable beta emitterscounting

U Total Laser fluorescence or Total uraniurnphosphorescence

U Isotopics TIMS 233 234Uu? , 2=U, 236U 238~ibpuU $1 so reportavailable data on , 2 Pu, 24’JPU,

and 24’PU)

Metals ICP Al, Cd, Sm, B, Fe, Ba, Cr, Pb, Ag,Be, Tl, Zn, Cu, Mn, Mg, Ca, Na, K,Se, U, Zr, Bi, P, and Ni (Hf, Sn ifin current suite of analyses)

IC Analyses IC

Tc-99

pOL3”, S042-, F“, Cl‘, Br-

S01vent extraction 99Tcwith liquidscintil1ation counter

Organics SVOA Any TICS found in the analysis,

Endothermi c/Exothermic DSC/TGA (use TWRS DSC/TGA include annotated thermogramReactions (Optional ) method with nitrogen

and air cover gas)

Settling Rate Settling columns and Volume settled versus time, videovideo camera tape

37

HNF-3556, Rev. O

Table 8. 105-K West and K East Basins F1oor and Pit S1udge Analyses. (Continued)

Requested Analysis Analysis Technique Constituents to be Reported

Polychlorinated PCB as near EPA PCB concentration in indicated sol ids

Biphenyls (PCB) methods as reasonable (1 ppm) and water (0.2 ppb)

Settled Densities Gravimetric/sample Settled density, volume, and weightpreparation procedure

Residual from Digest Gravimetric/sample Weight percent of original materialpreparation procedure left after acid digest (wet and dry)

Residual Analysis XRD Qualitative analysis of anyundigestible residue

Pyrophoricity XRD Qualitative analysis of the sludgeprior to heating or digestion.Unreacted metal 1ic uranium andZr; unoxidized uranium hydride;uranium oxide; hydrates of A1205,U02+ and FeOX

Particle Size Particle size Size, distributionDistribution analyzer and sieves

Particle Shape Optical microscopy, ShapeSEM, or TEM

Particle Density Gas pycnometer/ Density dry/dens ity wetcalculation

Viscosity Viscometer Viscosity

TIC/TOC/TC Persulfate oxidation TIC (C032-),TOC, TCand COU1ometry

Zeta Potential Zeta plus instrument mV

Caustic Demand Potent iometric Buffering capacity(Optional) titration

Gas Generation from Capture measured Rate of gas volume generated (as aSettlers (Optional ) volume of gas over function of hours), composition of

specific time and gas released, and temperature ofanalyze for S1udge samplecomposition

pH pH probe pH units

Cyanide Standard methods Cyanide concentration

38

HNF-3556, Rev. O

Table 9. Analytical Requirements for the 105-K West andSamples (222-S and 325 Laboratories).

East Basins Floor and Pit Sludge(Continued)

Process Constituents Procedure Required MDL’

Separat ion, AEA

=8PU LA-953-104 8.0 #Ci/gPNL-ALO-417/496/422

239/240puLA-953-104 3.0 flCi/g

PNL-ALO-

417 J4961422

241Am LA-953-104 15.0 pCi\g2431244cm

PNL-ALO- 15.0 flCi/g

417/496/422

Phosphorescence or U total LA-925-009 10 pgJg

Fluorimetric PNL-ALO-445

Thermal Ionization ~331sotopics PNL-ALO-455 25 pgJg

Mass Spectroscopy234U, 235U

236: ‘(TIMS)

2:41 (236P;, LA-506-1O1(TIMS) Plasma Mass 239p;Spectroscopy

241puj7Pu, and (ICPMS)

(ICPMS)

GEA LA-548-121

PNL-ALO-450

‘34CS 0.20 #Ci/g

137CS 0.015 #Ci/g

60C0 0.010 flCi/g

241Am 15.0 pCi/g

152Eu 1.5 pCi/g154EU 1.5 #Ci/g

155Eu 2.0 flCi/g

2128i 10.0 flCi/g208T, 30.0 flCi/g

Precisionz lAccurac~

T7

+20% I --*2O% ISPCz*20% SPC

+20% --

*2O% --

+20%

*20% --

*2O% --

*2O% --

1Required Method Detection Limit (MDL) has been established based on expect:d concentrations and use of the data,taking into account different capabilities of the taboratorles for the equlixnent and analysis methods in use.

2Measured san@e precision determine-d by duplicate ana Lyses. The Re~ative Percent Difference (RPD) between the dupticateanalyses is uithin the specifiedbounds; e.LI.,-20% < RPD < 20%. RPD = [(resu~tl- resu(t2)/meanl*100.

3“At[ spike recoveries should be within ?25%. Alk methcd standard recoveries shouLd be nithin statistical processcontrol (SPC). A serial di(ut ion (sD) ui~( be used to eval.ate the method accuracY fOr sOme metal ana(Ytes.

4The san@e preparation procedure uitt provide the calculation used to determine the sludge sett Led density.

5Ana[yze for PCB using same methods as used for K East canister s(udge samples or as directed in LO1/SOU. A[l Aroctorcompounds shou(d be identified and quantified.

6If availab(e from routine analysis, extraordinary measures (purchase of nen equipent) not required.

7Report if data are generated as part of other requested ana[yses.

Sp--At Least one spike ana(ysis requir’ed.

39

HNF-3556, Rev. O

Table 9. Analytical Requirements for the 105-K West and East Basins Floor and Pit SludgeSamples (222-S and 325 Laboratories). (Continued)

Process Constituents Procedure Required MDL’ Precisionz Accuracy3125sb 10.0 #Ci/g +20% --

106Ru/Rh 35.0 pCi/g f20% --

144Ce/Pr 25.0 pCi/g +20% --

~ 1.0 flCi/g +20% --

226Ra 45.0 pCi/g +20% --

Gross Alpha Total a LA-508-1O1 3.0 flCi/g *20% *25% SII

PNL-ALO-420/421

Gross Beta Total 8 LA-508-101 0.50 pCi/g i20% t25% S12

PNL-ALo-430/431

ICP Metals LA-505-161PNL-ALO-211

I ,

II IAlI100 #g/g +20% HO% SD I

II Cd 15 pg/g +20% *25% SP

Sm 200 &g/g *20% +25% Sp

B 100 us/a +20% t25% SD,., .,Fe 100 pg/g *20% tlO% SD

Ba 100 fig/g f20% i25% SP

Cr 20 pg/g izcl% *25% Sp

Pb 200 pg/g +20% +25% sp

Ag 20 pg/g i20% f25% SP

II IBe I I 10 ucl/q 1+20% !+25% SD II

II IT1 I I 400 uqla

Zn 20 pgfg *20% t25% SP

Cu 20 pg/g *20% +25% SP

K 1000 #g/g +20% +25% SP

Se 200 uci/Q *20% *25% SO

1Required Method Detect ion Limit (MDL) has been estab[ i shed based on expected concent rat i ..s and use of the data,taking into account di f fere”t .apabi 1 i ties of the laboratories for the equipnemt and analysis methods in use.

2Measure.+ san@e precision determined by duplicate analyses. The Relative Percent Difference (RPD) between the d“p[icateana(yses is within the specified bounds; e.g. , -20% . RPD < 2074.

3RPD = [(resdtl - result2)lmea”l *100.

A([ spike recoveries shou(d be within *25%. Al 1 method standard recoveries shoutd be within statistical processcontro[ (sPC). A Seriat di l.tion (SD) wi I ( be used to eva[uate the method accwacy for some metal amalytes.

4The sample preparation procedure !4( 1L provide the ca (ctdat i on used to determim the sL”dge set t led density.

5Ana Lyze for PCB using same methods as used for K East canister s(udge sampLes or as directed i“ LOl/sOU. All Aroc(orcompoucds shou Ld be identified and quantified.

61f avai l.abl e from routine analysis, extraordinary measures (purchase of neu equi pent) not req”i red.

7Report i f data are generated as part of other requested ana I yses.

Sp--At ieast one spike ana Lysis required.

40

Table 9. Analytical RequirementsSamples (222-S

HNF-3556, Rev. O

For the 105-K West and East Basins Floor and Pit Sludgeand 325 Laboratories) . (Continued)

Process Constituents Procedure Required MDL1 Precisionz

Mn 20 pg/g i20%

Mg 200 pg/g +20%

Ca 200 /lg/g +20%

Na 200 &g/g 120%

Zr 20 pgfg *20%

Ni 40 ~g/g *20%

P 400 pg/g +20%

Bi 200 ,ug/g *20%6 Hf TBD6

*20%

Sn TBD 12(I%

u 1000 /.Jg/g i20%

IC Anions--F-, Cl-, LA-533-105NOzj~ N03:, P043-, PNL-ALO-212

20 pg/mt i20%

S04 , Br

Solvent Extraction 99Tc LA-438-101 0.05 .ug/g +20%with LiquidScintillationCounter

Exothermic/ DSC (with air and LA-514-114 -- +20%Endotherm c nitrogen cover PNL-ALO-508

gas)

Drained Solids Percent water LA-560-112 +20%(TWRS) (TGA) PNL-ALO-508

Hot Persulfate/ TIC (C032-) and LA-342-1OO 40 P9/9 +20%Coulometry TOC/TIC/TC PNL-ALO-381

Separation and 90Sr LA-220-101 1.0 #Ci/g +20%8eta Counting PNL-ALo-430/431

Accuracy3

+25% SP

+25% sp

+25% SP

+25% SP

*25% Sp

*25% SD

+25% SP

+25% sp

+25% SP

?c25%SP

t25% SII

*25% Sp

SPC

SPC

SPC

i25% SP

f25% SP

1Required Method Oetect i on Limit (MDL) has been estab[ i shed based on expected concentrate ions and use of the data,taking into account different capabi 1i t ies of the laboratories for the equipnent and analysis methods in use.

2Measured sample precision determined by dup( i cate ana 1yses. The ReLat ive Percent Oi f f erence (RPD ) between the d“pL icateana(yses is uithln the specified bounds; e.g. , -20% . RPD . 20%. RPD . [(resu[tl - result2) /mea”l *100.

3AL1 spike recoveries shou{d be within i25%. Alt method standard recoveries should be within statistical processcontro L (sPC). A seria[ dilution (SO) wi ( [ be used to eva Luate the method accuracy for some metal analytes.

4The samp[e preparation procedure wi L1 provide the calcu tat i on used to determine the s Ludge sett ted density.

5Ana[y.ze for PCB using same methods as used for K East canister s(udge sampLes or as directed in LO1/SOU. ALL Aroc[orcompounds shou(d be identified and quantified.

6I f avai [able from routine analysis, extraordinary measures (purchase of new equitxnent ) not requi red.

7Report i f data are generated as part of other requested anat yses.

SP- -At (east one spike ana Lysis ?equi red.

41

HNF-3556, Rev. O

Table 9. Analytical Requirements for the 105-K West and East Basins Floor and Pit SludgeSamples (222-S and 325 Laboratories). (Continued)

Process I Constituents

Extraction and 237NpAlt)haCountinq

Gravimetric Settled and dry(before and after density/volumeacid digest, etc. )

Caustic Demand Buffering[ovtional ) capacitv

KRD--Prior to U (metallic),Sample Heating and Fe hydrates,Acid Digestion Al hydrates,

U hydrides,U oxides, and Zrmetal

KRD--Digestate Any identifiableResidue compounds

(analytes) afteracid digest andcaustic fusion

Settling Rate IVO1ume settledversus time

I

‘article Size lParticle size1. Analyzer (submicron to2. Sieving 0.25 in.) and

distribution

Procedure

LA-933-141PNL-ALO-415/422

Samplepreparationprocedure4LA-519-132

LA-211-104

PNL-ALO-268

PNL-ALO-268

Samplepreparationprocedure

1. LT-5I9-1OIPNL-ALO-530

2. Testinstructionapproved bySNFCP

PNL-ALO-530

LT-519-115PNL-ALO-502

Required MDL1

5 flCi/g

N/A

O.O4 mole/kg

NIA

N/A

N/A

N/A

N/A

N/A

Precision*

k20%

N/A

*20%

N/A

N/A

N/A

N/A

N/A

N/A

—ccuracys

25% SP

N/A

SPC

N/A

N/A

N/A

N/A

N/A

N/A

1Requi red Method Detection Limit (MDL ) has been estab[ i shed based on expected concentrations and use of the data,taking into account different capabi { i ties of the laboratories for the equipnent ard analysis methods in use.

LMeesured samp(e precision determined by duplicate ana( yses. The Rekative Percent Difference (RPD) between the duplicate

ana(yses is uithin the specified bounds; e.g. , -20% . RPD . 20%. RPO = [(resu[tl res”(t2)/meanl *100.3

All spike recoveries shou[d be within ?25%. Al I method standard recoveries shou(d be within statistical processC.wrol (sPC). A serial di I.tion (SD) Ui (( be used to evaluate the method accuracy for some metal am[ytes.

4-The sample preparationprocedure wi Lt provide the calculation used to determine the sludge sett[ed demity.

‘Ana(yze for PCB “sing same methods as used for K East canister s(udge samples or as directed in LOI/sOU. All Ar.ac Lorcompo.twds shou(d be identified and quantified.

61f available f ran routine ana [ ys.is, extraordinary measures (purchase of new equiment ) not required.

7Report i f data are generated as part of other requested ana Lyses.

SP- -At least one spike analysis req”i red.

42

HNF-3556, Rev. O

Table 9. Analytical Requirements for the 105-K West and East Basins Floor and Pit SludgeSamples (222-S and 325 Laboratories). (Continued)

Process Constituents Procedure Required MDL1 Precision* Accuracy

Organics SVOA--al 1 TICS LA-523-131/406 Report TICS N/A N/APNL-ALo-120/ >10 ppm344/345

Polychlorinated PNL-ALO-3465 1 ppm (solids) --5 5--

biphenyls (PCB)5 LA-523-136 0.2 ppb (water) --5 5-.

Zeta Potential Zeta potential TWRS-95-5.6a-2, TBD TBD TBDRev. O

pH (electrode) PH LA-212-106 0.1 pH units i15% SPCPNL-ALO-225

Gas Generation Gas volume as Test plan TBD TBO TBORate (optional ) rate of data time approved by

~gi~;; hgw~) , SNFCP

temperature ofS1udge

;as Composition ‘> He$ ArJ.N?) PNL-ALO-284 TBD TBO TBO(optional) Xe, Kr, trltlum,

and any othersignificant gases

;yanide LA-695-102 LA-695-103 5 pg/g t20% t25% SPPNL-ALO-287/2B9 PNL-ALO-287/2B9

1Requi red Method Detection Limit (MDL ) has been estabL i shed based on expected concentrations and “se of the data,taking into account different capabi 1i ties of the laboratories for the equipment and ana I ysis methods in use.

zMeasur&d sarnp(e precision determined by duplicate ana(ys es. The ReLative Percent Difference (RPD) betweem the duplicateanalyses is within the specified bounds; e.g. , -21XZ < RPD < 20%. RPD . [(res”[tl resu Lt2)/meanl *100.

3ALL spike recoveries shou(d be within ?25%. AL I method standard recoveries should be within statistical processcontro( (sPC). A seria( di Lution (SD) wi LL be used to eva[uate the method accuracy for some metak ana(ytes.

4The sample preparation procedure wi (1 provide the talc.kation used to determine the s[udge settled demity.

5Ana[yze for PCB using same methods as us:d. for K East canister sludge samp[es . . as directed in Lo I/SOW. A([ Aroc[or

cc$wounds should be Identified and quantIfIed.61f availab(e from routine ana~ysis, extraordinarymeasures (purchaseof new equipment)not required.

7Report if data are generatedas part of other requestedanatyses.

SP- ‘At least one spike mat ysis req”ired.43

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Figure 6. Flow Chart of Sludge Sample Processing and Analyses.

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batch. An equipment blank from the K Basin sample collection mockup may beanalyzed for each set of new sampling equipment. At least one hot cell blank(if the hot cell is used) wil1 also be analyzed. One method control standardwil 1 be run with each batch. A matrix spike will be run per matrix, whereapplicable, as indicated in Table 9. Also see Section 8.0 on QA requirements.

General ly analyses noted in Table 9 may be performed at either the325 Building 1aboratory or the 222-S laboratory depending on S1udge treatmentprocess subproject 1ogistics and past support in the K 8asins sludge char-acterization efforts (for consistency of data), follow-on test needs, specific1aboratory capabil ities, sample quantities, schedule, and contractual andHAMTC restrictions. The SOW including the detailed analyses requirements willdefine which 1aboratory will perform which analyses. All analyses wil 1 beperformed consistent with doing work at the Hanford Site and as part of theProject Hanford Management Contract (PHMC).

Additional analyses of the 1iquid fraction of the sludge samples, beyondthose noted in Figure 6, are potential options to support (1) calculation ofmaximum theoretical leachate concentration for RCRA heavy metals, and/or(2) bench scale water/sludge processing tests. These will be addressed in theSOW to the 1aboratories if they are to be performed. It is acknowledged thatdue to the potential dose rate of these samples such analyses could requiresignificant additional preparation and costs at the 1aboratories.

As noted earlier, additional scoping characterization analyses orcombined characterization and process development tests, supporting thedevelopment and validation of treatment process may also be performed ifwarranted. If performed, these will be consistent with the OQO and the sludgeprocessing subproject objectives in order to utilize 1imited sample andmaximize the use of resources (i.e., funding, 1aboratory waste disposal, ALAR,etc.). Such analyses wil1 be documented in SOWS to the 1aboratories.

Quality assurance (QA) and quality control (QC) information wil1 conform”to those required for a “ful1” data package (as discussed in the followingsection). The QA/QC standards must conform to Table 9 and/or the applicableanalytical procedures. The control standards, spike recoveries, precisionbetween duplicates, hot cel1 blanks, and equipment blanks need to be withinthe specified requirements as noted in Table 9. If the precision betweenduplicates or the spike recoveries exceed the appropriate criteria there aretwo options; (1) make one rerun to see if acceptable results are obtained (ifacceptable results are not obtained, report the QC failure to SNFCPorganization) or (2) report QC failure and suggested actions immediately toSNFCP Program Coordinator for evaluation.

The method detection level (MDL) as used in this document is thedetection level which is expected to be achievable by the 1aboratory toanalyze a 1istealconstituent, yet is low enough to detect whether theconstituent is present in concentrations significant to resolving data qual ityobjectives (Makenas 1998a).

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Precision and accuracy requirements for laboratory analytical resultsspecified in this document are based on an assessment of achievable laboratory

capabil ities, given the complex nature of the samples to be analyzed, their

radioactive nature; and the consequent handl ing, dilution, and analysis

methods prescribed. The precision and accuracy statements calculated from the

1995 K East Basin sludge samples were also considered in determining therequirements presented in Table 9. The DQOS for the present sampling effort(Makenas 1998a) consolidate and incorporate the various analyses performed toassure that the overal 1 process wil1 produce the analytical results leading toa real ization of the sampling objectives.

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4.0 LABORATORY REPORTING REQUIREMENTS

The laboratories wil 1 be required to submit a final report within a

period defined in the SOW from SNFCP Project Coordinator to the 1aboratories.Opportunities for parallel operations wil1 be developed and schedules wil1 beprepared for laboratory work which wil1 minimize the time actually required.Samples will be processed through the 1aboratory with the priority required tomeet the completion date given in the SOW. The 1aboratory wil 1 be required tosubmit interim prel iminary data reports to the SNFCP Project Coordinator asrequested.

The final reports submitted to the SNFCP Project Coordinator fortechnical review will conform to the requirements for a “full” data package(e.g., similar to Silvers 1997; Miller 1997). If a laboratory uses its ownset of internal sample identification numbers in the data reports, a clearcross-reference of these numbers to the original sample identifications willbe provided. A narrative that summarizes the results and their quality willalso be included, as well as the signature of the individual (s) responsiblefor the report. The data package will give the duplicate results, al1 the QCdata (1aboratory method control standard results, spike recovery results, hotcell blank results, the equipment blank results), deviations from any of therequirements, chain of custody forms, and a narrative. Additional informationon the data report content is given in Sections 3.1 and 3.2.

Data related to dose rates measured on samples to be shipped between the325 Building and 222-S analytical laboratories, should be transmitted from theshipping laboratory to the receiving laboratory at least 5 working days priorto the actual shipment.

The laboratory performing the analyses of the PCB concentrations in thesludge samples will inform the SNFCP Project Coordinator as soon as definitivedata are available. This information wil1 also be transmitted to the1aboratories, in case there are any impacts on managing waste. Theinformation wil 1 also be provided to K. L. Pearce, NHC, for assessment ofimpact on sludge process treatment feed stream assumptions.

4.1 DATA PACKAGING

Analytical analysis results will be reviewed and processed on a prioritybasis by the analytical laboratories and other supporting organizations tomeet the schedules provided in the SOW.

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5.0 FINAL SUMMARY REPORT REQUIREMENTS

The completed data packages from the analytical 1 aboratories wil 1 be sent

to the SNFCP Project Coordinator who will coordinate data review and final

summary data report preparat ion. The data will be reviewed specificallyagainst the criteria set in the DQO document (Makenas 1998a). The ProjectCoordinator will ensure the data and reports become a part of the permanentProject Records.

5.1 STATISTICAL ANALYSIS REQUIREMENTS

A statistical analysis of the data will be performed as a separateactivity from the overal 1 1aboratory final data package. This analysis wil 1be reported as part of the final summary evaluation report to be completed bythe SNFCP. For each analyte, analysis of variance (ANOVA) techniques wil 1 beused to fit a statistical model to the data. This statistical model can beused to:

● Estimate the variability between samples (heterogeneity of thesamples)

● Estimate the analytical variability (precision)

● Compute confidence intervals (e.g., 95% 90%, etc. ) on the meanconcentration for each analyte consistent with the requirements ofthe DQO and sludge process treatment subproject at the time of thereport

● Compare present S1udge data to past campaigns.

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6.0 SAFETY PLANS

6.1 RADIATION/INDUSTRIAL SAFETY

An industrial safety assessment will be performed prior to the start of

these activities consistent with the requirements of each performing facility

or laboratory. The requirements of HSRCM-I, Hanford Site Radiological ControlManual shal1 be adhered to during the performance of sampling activities.— ,

6.2 NUCLEAR CRITICALITY SAFETY

A Criticality Safety Assessment will be performed in accordance withrequirements of each facil ity or 1aboratory involved [e.g., K Basin MasterWork PIan (MWP-95-TBD)], prior to the start of each activity. Therequirements determined by these assessments shall be adhered to during theperformance of the sampling activities.

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7.0 GENERAL ALARA PLAN

The sampling procedure for the activities discussed in Section 2.3.1 wil 1

take into consideration exposure reduction techniques which wil 1 minimize theradiation exposure to the sampl ing team.

ALARA considerations will be an integrated part of the design effort for

the sampling and sampling equipment to m’inimize personnel exposure. The

appl ication of the sampling equipment wil 1 be made under specific ALARA plansdeveloped and applied at the K Basins during the campaign. Each 1 aboratory

will apply its own review and ALARA P1 an consistent with operation on the

Hanford Site (e. g., the Hanford Site Radiological Control Manual, HSRCM-1).

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8.0 QUALITY ASSURANCE AND CONTROL PLAN

All sampling, sample handling, sample packaging/shipping, and analytical

process activities wil1 be performed in accordance with the requirements ofthis plan, along with the approved sampling and analysis procedures. Thecontrols identified in this P1an, along with those contained in the programplan, have been established to assure the applicable quality assurancerequirements of IOCFR830. 120 and FOH QAPD (HNF-MP-599, Rev. 2), are satisfiedduring the performance of this activity. In addition, the analytical1aboratory wil1 perform the analyses to its internal quality assurance programplans. The 222-S 1aboratory wil1 follow WHC-SD-CP-QAPP-016, Oualit~ AssuranceProgram P1an for Laboratory Analysis and Process Testinq. The 325 8uilding1aboratory wil 1 follow MCS-033, Qual it~ Assurance PIan for ActivitiesConducted by the Analytical Chemistry Laboratory.

Method specific quality control and quality assurance such ascalibrations and blanks are found in the analytical procedures notedin Table 9. Sample quality control (duplicates, spikes, and standards) areidentified in Section 3.2 or in the following paragraph. If no criteria areprovided in the current document, the performing laboratory shal1 perform toits quality assurance plan(s).

Sample groups wil 1 be assigned categories in the SOW that reflect thenumber of dupl icates and spike analyses that should be run. The categoriesare:

Cateqory1

2

Duplicate analyses wil1 be performed on al1 “first-time”characterization samples (i.e., al1 samples from K West Basin, plusthose from K East Basin containing locations KE-7, KE-8, and KE-11).There should be at least four samples receiving duplicate analysesif there is an insufficient number of samples from those indicated,the 1aboratory will select enough additional samples to provide atotal of four. One of the samples used for duplicate analyses willbe chosen by the 1aboratory for spike analyses. The balante of thesamples wil1 be handled as normal 1aboratory batches with QA as pereach laboratories internal QA plan.

For the two “research” samples the 1aboratories will run duplicateson layer analyses, no spike analyses are required.

As noted previously, duplicates are repeats of all analyses aftercompletion of settling analyses. Selection of samples within categoriesshould optimize the use of samples with larger volumes for dupl icates,allowing the maximum number of requested analyses to be performed for eachcategory.

Care should be taken with water samples processed in conjunction withthe S1udge analyses (e.g., equipment blanks, etc.), processing them onbest effort basis with criteria similar to that called out in Table 9,applicable laboratory procedures, or as called for in the final SOW.

athe

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9.0 REFERENCES

Alderman, C. J., 1997, Internal Memo to R. P. Omberg, “Request for Additional

Laboratory Tests on Archive K East Basin Floor/Pit S1udge and CanisterS1udge, ” CJA-97-001 .

Baker, R. B., 1998a, “Revised Estimates of Sludge Volumes in K East and K West

Basins, ” DESH-9857199, to K. L. Pearce, (included as Appendix A of this

SAP), Duke Engineering & Services Hanford, Inc., Richland, Washington.

Baker, R. B., 1998b, System Design Description for Sampling in K Basin FuelStorage Canisters, WHC-SD-SNF-SDD-004, Rev. OA, Westinghouse HanfordCompany, Richland, Washington.

Baker, R. B., 1996, Internal Memo to R. P. Omberg, “Recommended K West BasinCanisters for S1udge Sampling, ” Westinghouse Hanford Company, Richl and,Washington.

Baker, R. B., 1995a, Summary Status of K Basin Sludge Characterization,WHC-SD-SNF-TI-006, Rev. O, Westinghouse Hanford Company, Richland,Washington.

Baker, R. B., 1995b, Internal Memo to T. L. Welsh, Potentia7 ParametersInfluencing Floor Sludge Vo7ume or Composition at K East Basin, (Appendixin Welsh 1995), Westinghouse Hanford Company, Richland, Washington.

Baker, R. B., 1995c, System Design Description: Samp7ing Equipment forK Basin F700r S7udge, WHC-SD-SNF-SDD-O03, Rev. OA, Westinghouse HanfordCompany, Richland, Washington.

Bechtold, D. B., 1994, Report of Laboratory Test P7an for Ana7ysis of KE BasinBackwash Pit Samp7es, WHC-SD-NR-TRP-021, Rev. O, Westinghouse HanfordCompany, Richland, Washington.

Bechtold, D. B., 1993, Laboratory Test P7an for Ana7ysis of KE Basin BackwashPit Samp7es, WHC-SD-NR-TP-023, Rev. 1, Westinghouse Hanford Company,Richl and, Washington.

Bridges, A. E., 1996, Internal Memo to D. L. Edwards and K. J. Young,Instructions for C7eaning K Basin Canister Sludge Samp7e Containers,Westinghouse Hanford Company, Richland, Washington.

Delegard, C. H., et al., 1998, K Basin S7udge Materia7s Treatment TestingStrategy, HNF-1926, Rev. O, Pacific Northwest National Laboratory,Richl and, Washington.

Dodd, E. N. Jr. , 1995, 105-KW Sandfi 7ter Bac&ash Pit S7udge Vo7umeCharacterization, WHC-SD-SNF-TI-O1O, Rev. O, Westinghouse HanfordCompany, Richland, Washington.

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9.0 REFERENCES (Continued)

Fink, S. D., et al., 1998, Sludge Treatment System Project Independent ReviewTeam Report: Process F70w Review, Numatec Hanford Corporation, Richl and,Washington.

Flament, T. A., 1998a, Testing Strategy to Support the Development of K BasinsludgeTreatment Process, HNF-2574, Rev. O, Numatec Hanford Corporation,Richland, Washington.

Flament, T. A., 1998b, SNF Project S7udge Treatment System Process F70wDiagram, H-1-81170, EDT 625270, Numatec Hanford Corporation, Richland,Washington.

Fowler, K. D., 1995a, Data Qua7ity Objectives for Waste Tank FarmsCompatibi 7ity Program, WHC-SD-WM-DQO-001, Rev. 1, Westinghouse HanfordCompany, Richland, Washington.

Fowler, K. D., 1995b, Tank Farm Waste Transfer Compatibi 7ity Program,WHC-SD-WM-OCO-015, Rev. OA, Westinghouse Hanford Company, Richland,Washington.

HSRCM-1, Hanford Site Radio 70gica7 Contro7 llanua7, Westinghouse, HanfordCompany, Richland, Washington.

Maassen, D. P., and N. R. Roe, 1997, Floor S7udge Depths and Vo7ume of the105-K I/est Basin, HNF-SD-SNF-TI-054, Rev. O, Duke Engineering & ServicesHanford, Inc., Richland, Washington.

Makenas, 8. J., 1998a, Data Qua 7ity Object ives for Samp7 ing of S7udge from theK West and K East Basin F700r and from Other Basin Areas, HNF-2033,Rev. O, Duke Engineering & Services Hanford, Inc., Richland, Washington.

Makenas, B. J., et al., 1998b, Ana7ysis of S7udge from K West Basin Canisters,HNF-1728, Rev. O, Duke Engineering & Services Hanford, Inc., Richl and,Washington.

Makenas, B. J., Pearce, K. L., and Baker, R. B., 1996a, Data QualityObjectives for K I/estBasin Canister S7udge Samp7ing, WHC-SD-SNF-DQO-012,Rev. O, Westinghouse Hanford Company, Richland, Washington.

Makenas, B. J., 1996b, Canister Choices for Samp7ing of Fue7 and S7udge fromK West Basin Canisters (Second Characterization Campaign),HNF-SD-SNF-SM-006, Rev. O, Duke Engineering and Services Hanford, Inc. ,Richland, Washington.

Makenas, B. J., et al., 1996c, Ana7ysis of S7udge from the K East Basin andl/ease7 Pit, WHC-SP-1182, Westinghouse Hanford Company, Richland,Washington.

Meznarich, H. K., 1998, Quality Assurance Program P7an for Laboratory Ana7ysisand Process Testing, WHC-SD-CP-QAPP-016, Rev. 3A, Westinghouse HanfordCompany, Richland, Washington.

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9.0 REFERENCES (Continued)

Miller, G. L., 1997, Chemica 1 and Radiochemica 1 Characterizat ion of 105-K EastBasin Canister S7udge, HNF-SD-WM-DP-228, Rev. OA, Rust Federal Servicesof Hanford, Inc. , Richland, Washington.

Miller, G. L., 1996, Final Chemical and Radiochemical Analytical Report of105-K East Basin S7udge, WHC-SD-SNF-DP-004, Rev. lD, Westinghouse HanfordCompany, Richland, Washington.

Miller, G. L., 1995, Interim Chemical and Radiochemica7 Analytica7 Report of105-K East Basin S7udge, WHC-SD-SNF-DP-004, Rev. O, Westinghouse HanfordCompany, Richland, Washington.

Packer, M. J., 1998, K Basins S7udge Inventory Composition, HNF-SD-SNF-T1-053,Rev. O, Duke Engineering & Services Hanford, Inc., Richland, Washington.

Pearce, K. L., et al., 1998a, Data Quality Objectives for K Basin ConditioningSystem Laboratory Testing, HNF-1927, Rev. 1, Duke Engineering & ServicesHanford, Inc., Richland, Washington.

Pearce, K. L., et al., 1998b, 105-K Basin Nateria7 Design Basis FeedDescription for Spent Nuc7ear Fue7 Project Facilities, Vo7ume 2, S7udge,HNF-sD-SNF-TI-009, Rev. 2, Numatec Hanford Corporation, Richland,Washington.

Pitner, A. L., 1997, Visual Examinations of K West Fue7 Elements,HNF-SD-SNF-TI-046, Rev. O, Duke Engineering and Services Hanford, Inc.,Richland, Washington.

Pitner, A. L., 1996, Test Plan for K East Visua7 and Ultrasound Survey ofCandidate Canisters for Fuel and S7udge Characterization,WHC-SD-SNF-TP-024, Rev. O, Westinghouse Hanford Company, Richland,Washington.

PNL, 1991, Qua7ity Assurance P7an for Activities Conducted by the AnalyticalChemistry Laboratory (ACL), MCS-033, Rev. O, Pacific NorthwestLaboratories, Richland, Washington.

Silvers, K. L., 1997, K East Basin Canister S7udge Samp7e Ana7ysis, PacificNorthwest National Laboratory, Richland, Washington.

Silvers, K. L., 1995, K Basin S7udge Samp7e Ana7ysis, Basin F700r and Wease7Pit, Pacific Northwest National Laboratory, Richland, Washington.

Trimble, D. J., and T. L. Welsh, 1997a, Cesium-137 in K Mest Basin CanisterWater, HNF-SD-SNF-ANAL-014, Rev. O, Duke Engineering and ServicesHanford, Inc., Richland, Washington.

Trimble, D. J., Internal Memo to D. S. Takasumi, 1997b, “K West Basin CanisterSludge Inventory. ”

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9.0 REFERENCES (Continued)

Welsh, T. L., R. B. Baker, B. J. Makenas, and K. L. Pearce, 1996, Samp7ingand Ana7ysis Plan for Sludge Located in Fuel Storage Canisters of the105-K East Basin, WHC-SD-SNF-PLN-016, Rev. O, Duke Engineering andServices Hanford, Inc., Richland, Washington.

Welsh, T. L., R. B. Baker, B. J. Makenas, and K. L. Pearce, 1995, Samp7ingand Ana7ysis P7an for F700r Sludge of the 105-K East Main Basin andtiease7 Pit, WHC-SD-SNF-PLN-O06, Rev. O, Westinghouse Hanford Company,Richland, Washington.

Williams, N. H., Letter to E. D. Sellers (RL), 1996, “Sludge Disposal Plan of

Execution, ” 9656039.

Willis, N. P., 1993, Hanford Site Waste Acceptance Criteria, WHC-EP-0063-4,Westinghouse Hanford Company, Richland, Washington.

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APPENDIX A

SUMMARY LETTER (DESH-9857199) DOCUMENTINGESTIMATED VOLUMES OF SLUDGE IN K BASINS

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CORRESPONDENCE DISTRIBUTION COVERSHEET

R. B. Baker376-5109

Ns. K. L. Pearce, NHC DESH-9857199

subject: REVISED ESTIP’LATES OF SLUDGE VOLUNES IN K EAST ,4140K h’EST BASINS

DISTRIBUTION

APP?DV8( Dcte Xane Lc.czt ion WIstt

CorrespondenceControl A3-01

B&W Henford ComoznvA. G. !!estra R3-B6

Duke Fnoineerina & Services Hanford. Inc.

C. J. Alderimn x3-74

D. W. Bergmann HO-40

K. H. Bergsmann X3-55

A. E., Bridges HO-40

L. O. BruggEman HO-40

S. L. Hecht HO-40

O. P. tiaassen HO-40

B. J. F!akenas HO-40

J. Perez-Carter” HO-40

A. L. Pitner HO-40

A. N. Praga R3-86D. R. Precechtel X3-85J. A. Swenson R3-11O. J. Trimble HO-40RBB File/LS HO-40SNF Project Files R3-11

.“Pacific Northwest National Laboratory“.A. J. Schmidt K2-12

K. L. Silvers K9-oa

Num;tec Hanford CorvoratfonD. A. Dodd T6-50T. A. F1ament H7-20W. W. Rutherford H7-20

}:ASTRNN. P..Roe HO-40

x

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xxxxxxxxxxxxxxxx

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xxx

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A-600 $-S38 (OL/97) L5F039

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%%+ DE&S Hanford, Inc.

A DuleEnginteiing& SmiecsCompany

.? O. Box35oRichbrd WC 99352

August 28, 1998 DESH-9857199

Ms. K. L. PearceSpent Nuclear Fuel Project, Process DesignNumatec Hanford Corporation H7-20Post Office Box 1300Richland, k’ashington 99352-1300

Dear Ns. Pearce:

REVISED ESTINATES OF SLUDGE \TOLU14ES IN K EAST AND K i!EST BASINS

Reference: InternalI!eioo,R. B. B?ker to K. L. Pearce, “Current Estimates ofSludge Volumes in K East and K Nest Basins,” dated March 19, 1997.

In Narch 1997, a review was made of the volume estimates of sludge from theK East and K west Basins (Reference). Considered were the volumes of sludge(1) on the main basin floors, (2) in remote pits, (3) in fuel storagecanisters, and (4) that expected to be generated from washing the storagecanisters and”fuel elements prior to packaging the fuel elements in the SpentNuclear Fuel (SNF) multi-canisteroverpacks (MCOS).

Per your request,“andwith your support, we have reviewed these originalestimates and their sources. Many of them still remain the best valuesavailable. There have been, however, some changes (such as additionalmeasurements from K West Basin and improved estimates based on additionalcharacterization data) hrhichhave resu?ted in revision of some of the previousS1udge volurneestimates. The revised sludge volume estimates and those stillapplicable are summarizedherein (Attachments I and 2).

: Please contact me if you have questions or you need additional information.

. Very truly yo.;rs,

..

(@ 4524.R. B. Baker, Senior fngine~rSNF CharacterizationProject

jms

Attachments 2

.*,4,,

.64

HNF-3556, Rev. ODESH-9857199ATTACHMENT 1Page 1 of 8

K EAST AND K h’ESTBASINS REVISED SLUDGE VOLUME ESTIMATES

R. B. BakerAugust 28, 199B

1.0 SUFtiARY

The revised estimates of sludge volumes in the K Basins based on this revieware provided in Tables 1 and 2. Figures 1 through 3 provide overviews of thevolume fractions of sludge for both basins together and separately. As usedthroughout the Spent Nuclear Fuel (SNF) Project, the physical definition ofsludge used herein was particulatematerials in K Basins (i.e., sand, fuel,corrosion products, cladding, IXM beads, insects, etc.) with no pieces greaterthan those expected to pass through a screen with 0.25 inch (6350 microns)openings.

2.0 SUMMARIES OF SLUDGE VOLUMES MADE PREVIOUSLY THAT ARE STILL VALID

A general review was made of the previously provided K Basins sludge volumeestimates (Baker 1997). It was determined that the volume estimates forsludge reported in Baker (1997) remain unchanged for the following areas (theprimary references these data come from is also indicated):

. K East (KE) Basin main floor (Baker 199S)

● KE Basin remote pits (Baker 1995; Makenas et al. 1996)

9 KE Basin canisters (Pitner 1996)

● K West (KW) Basin North Loadout Pit (Baker 1995; Dodd 1995)

Attachment 2 of the current 1etter provides the text from Baker (1997) forreference with respect to the assumptions made for these areas. The KW BasinNorth Loadout Pit (or Sandfi lter Backh,ash Pit) values had a minor error inBaker (1997), the sludge depths were incorrect, the S1udge volumes quoted werecorrect. In addition, for “consistencyit is suggested you refer to the more

“detailed Dodd (1995) for the sludge measurement data for this pit, as well as: Baker (1995)..”

3.0. REVISEO ESyIMATES OF SLUOGE“VOLUMESAT K BASINS

Fuel Wash Sludoe

Recent estimates of volumes of S1udge have just been completed for the‘ material generated during washing of canisters and fuel elements at both

KE and KW Basins (Pearce and Pitner, 1998a and 199Bb, respectively). Theseestimates replace prior fuel wash sludge estimates and are being revised basedon the availability of additional dat,a from laboratory evaluations of materialfrom the K Basins fuel element surface and subsurface examinations(Pitner 1997; Silvers 1998). Additionally, it was previously assumed that

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DESH-9857199ATTACHMENT 1Page 2 of 8

fuel wash sludge was generated by metal fuel pieces being granulated (crushed).inthe fuel washing machine and thus, turned into additional sludge. Thisassumption has been revised as it is now judged that the washing machine doesnot have the capability to significantly “granuJate” the fuel pieces. However,it is expected that the washing process will cause further breakage of theelements and dislodge corroded uranium pieces, zirconium cladding, and looselyadhered material (such as coatings and internal sludge). This dislodgedmaterial is referred to as the “fuel h’ashsludge” and IS assumed comprised ofthree components; pieces of coatings, fuel pieces and Internal sludge (i.e.,sludge originating directly from within the fuel elements). The fuel washsludge component volume calculationsare documented in Pearce and Pitrier(1998a and 1998b). The calculatedvolumes for the KE Basin and KW Basin fuelwash sludge components are provided in Tables 1 and 2, respectively.

K West 8asin Canister Sludoe

Volume estimates for KW Basin canister sludge made previously were based on7aboratory measurementsof KE canister S1 udge density and measured 1S7CScontent found in the tiaterof the closed canister barrels in KW Basin(Trimble 1997). These prior estimateswere revised (Pearce and Pitner 1998b)based on additional characterizationdata from KW Basin fuel storage canisters(Makenas et al. 1998). The revised volumes are provided in Table 2.

K West 8asin Remote Pits and Main Easin Floor

The volume of S1udge in the KW Basin remote pits and on the main basin”floorprovided-fn Baker (1997)were based on a quick general sur~-hese areaswith S1udge depths approximatedthrough the ful1 depth of water in the pool.A much better estimate is now available based on direct underwatermeasurements of S1udge depths in the remote pits (except for the North LoadoutPit) and on the main floor of KW Basin (Maassen and Roe 1997). After thesemeasurements were made the sludge in the South Loadout Pit was pumped to theTech View Pit South Channel. The quantity of S1udge originally“ reported1ocated in the South Loadout Pit was therefore added to the volume of S1udgereported for the Tech View Pit. The final estimates of sludge in the KW Basinremote pits and on the floor of KW Basin are provided In Table 2.

,:K East Basin and K West Basin North Loadout Pits..-

The depths and yolumes of S1udge in the North Loadout Pits (also referred toas, Sandfilter Backwash Pits) in both KE and KW Basins are based on directmeasurements made at the end of 1995 (Baker 1995; Dodd 1995). Some minorincrease in S1udge depths has 1ikely occurred because of additionalbackwashing of the sandfilters. It is judged (based on input from K Basinstaff), however, that this has had 1ittle influence on the overal1 volumes

, (i.e., within the uncertaintiesnoted). Therefore, the volumes of sludge inboth pits are still reported the same as in Baker (1997) with exception of thecomments in Section 2.0. Additional depth measurements are planned in thefuture for these pits during acquisitionof sludge characterization samples.

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DESH-9857199ATTACHMENT 1

Page 3 of 8

4.0 REFERENCES

8aker, R. 8., 1995, Summary St;tus of K Basin Sludge Characterization,MHC-5D-5NF-T1-006,Rev. O, ~estinghous.aHanford Company, Richland,Washington.

Baker, R. B., 1997, IIcurrentEstimates of Sludge volumes in K East andK Nest Basins, t’ Internal tfemo to K. L. Pearce, dated March 19, 1997,Duke .Engineering & Services Hanford Inc., Richland, Washington.

Dodd, E. N. Jr., 1995, 105-KW Sandfilter Backwash Pit Sludge Vo7umeCharacterization,WHC+D-SNF-TI-010, Rev. O, Westinghouse HanfordCompany, Richland Washington.

Lodwick, R. J., 1997, 105 K vest Basin: South Loadout Pit S7udge DepthEstimation, InternalMemo to D. W. Bergmann, dated August 1, 1997,Duke Engineering & Services Hanford, Inc., Richl and, Washington.

Maassen, D. P. and N. R. Roe, 1997, Floor Sludge Depths and Volume of the105-K blestBasin, HNF-SO-SNF-T1-054,Rev. O, Duke Engineering & ServicesHanford, Inc., Richland, Washington.

‘Makenas, B. J., et al., 1998, Analysis of Sludge from K !+JestBasin Canisters,HNF-1728, Rev. O, Duke Engineering & Services Hanford, Inc.,,Richland,Washington.

._Makenas, B. J.,”T. L. Welsh, R. B. Baker, O. .R. Hansen, and G. R. Golcar”,

1996, Ana7ysts of S7udge from Hanford K East Basin F700r and Measel Pit,WHC-SP-1182, Rev. O, htestinghouse Hanford Company, Richland, Washington.

.

Pearce, K. L., and A. L. Pitner, 1998a, K East Basin S7udge Vo7ume Estimatesfor Integrated Water Treatment System, HNF-3166, Rev. 1, Duke Engineering& Services Hanford Inc., Richland, k’ashington.

Pearce, K. L., and A. L. Pitner,.1998b, K West Basin S7udge Vo7ume Estimatesfor Integrated Water Treatment System, HNF-3165, Rev. 1, Ouke Engineering& Services Hanford Inc., Richland, Washington.

.’Pitner,“A. L.; 1997, K Basin Fue7 Subsurface Examinations and Surface CoatingSamp7ing, HNF-SD-SNF-TI-060,Rev. O, Duke Engineering & Services HanfordInc., Rich]and, Washington. . .

Pitner, A. L., 1996, K East Caniiter S7udge Survey, WHC-SD-SNF-TI-034,,Rev. O,WestinghouseHanford Company, Richland, Washington.” -

Silvers’,K. L., 1998, “K Basin Fuel Subsurface Sludge and Coating Analysis,”Letter PNNL 28964-02 to R. P. Omberg (DESH), Pacific Northwest NationalLaboratory, Richland, Washington.

Trimble, D. J., 1997, “K h’estBasin S1udge Volume Inventory,” Internal Memoto D. S. Takasumi, dated January 26, 1997, Duke Engineering & ServicesHanford, Inc., Richland, Washington.

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Table 1. Estimates of Sludge Volumes for K East Basin Floor, Pits, and Fuel Wash Components.

Sludge Upper Bound.Average S1udge Volume Positive S1udge Volume

Location or Source Depth Area(in.) (ftz) ft3 .m3 Un~S~~~?~ty ft3 m3 Reference

Tech View-North 1.0 49.4 4.0 0.1 50 6.0 0.2Channel

Baker (1995)

;~g~n~:ew-South 0.2 49.4 0.9 0.0 50 1.3 0.0 Baker (1995)

Tech View Pit 0.9 141.5 10.4 0.3 50 15.6 0.4 Baker (1995~

Ieasel Pit Channel 12.0 53.8 53.8 1.5 20 64.5 ‘“1.8 Baker (1995)Makenas (1996)

k’easelPit 32.3 112.3 302.5 B.6 20 362.9 10.3 Baker (1995)]iakenas(1996)

North Loadout Pit 33.0 66.5 183.0 5.2 20 219.6 6.2 Baker (199S)

North Loadout Channel 20.0 “23.2 38.6 1.1 20 46.4 1.3 Baker (1995)

South Loadout Pit 0.0 64.6 0.0 0.0 0 0.0 0.0 Baker (1997).

South Loadout ChanneT 0.0 230 0:0 0.0 “o 0.0.“ 0.0. Baker (1997) ,

Dummy Elevator Pit 6.0 97.0 48.5 1.4 50 72.8 2.1 Baker (1995)-

,Dischar~eChute. 0.0 316.5 0.0 0.0 0 0.0 0.0 Baker (1995)-

Main Basin Floor 1.9 4848.4+ 760.4 21.5(Open)

20 912.5 25.8 ~aker (1995)

Canisters--Empty 13.8 0.4 20 16.6 0.5 Baker “(199S)

Canisters--Fueled 106.1 3.0 147 261.4 7.4 Pitner (1996)

Subtotals“ 1522.0 43.1 1979.6 56.0

Fuel Wash Components: .Fuel Pieces NA NA 5.3 0.149 NA 1:.; :.;;; Pearce (1998a)Coating NA 2.2 0.061 NAInternal S1udqe 1: NA 18.3 0.518 NA 45:7 1:294 :

Grand Total 1547.8 43.8 2041.6 57.8

*Open area around canisters set on floor.

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Table 2. Estimates of Sludge Volumes for K h’estBasin Floor, Pits, and Fuel Wash Components.

Sludge Upper BoundAverage S1udge Volume Positive S1udqe Volume

Location or Source Depth Area +ts MS Percent(in.) (ft’) Uncertainty

ft3 /Reference

fig~n:: ew-North 0.066 49.35 0.27 0.008 4~7***1“]3 0“032 Maassen (1997)

Tech View-South 0.319 49.35 1.27 0.035 Combined**Channel**

3“76 0“]07 Maassen (1997)

Tech View Pit 0.066 141.50 0.78 0.022 417 3.24 0.092 Maassen (1997)

k!easelPit Channel 0.066 50.67 0.282 0.008 379 1.07 0.0302 14aassen(1997)-

h!easelPit 0.066 116.46 0.647 0.018 379 2.45 i3.0694Maassen (1997)

North Loadout Pit 20.7 65.2 112.3 3.18 20 134.8 3.82 Dodd (1995)

North Loadout Channel 8.8 22.7 16.2 0.46 20 19.4 0.550 Dodd (1995)

South Loadout Pit** 0.0 65.00 O.0** 0,0 NA 0.0 0.0 Maassen (1997~

South Loadout 0.0 22.30 0.o** 0.0 NA 0.0Channel**

0“0 Maassen (1997)

,OummyElevator Pit 0.16 97.10 1.31 0.0371 385 5.05 0.143 Maassen (1997)

Discharge Chute 0.052 526.30 2.28 0.0647 432 9.88 0.280‘Maassen (1997)

Main Basin Floor 0.064 5479.2* 29.0 0.822 229 66.3(Open)

1“88 Maassen”(1997)

Canisters--Fueled NA NA 35.7 1.01 77 55.8 1.58 Pearce (1998a)

Subtotals 200 5.67 303 8.58 ~~

Fuel Wash Components:Fuel Pieces WA 5.26 0.149 150Coating

13.2 0.373 Pearce (1998a). :: NA 14.3 0.406 150

Internal S1udge21.6 0.613

NA NA 18.3 0.518 150 45.7 1.294

Grand Total “o 238 6.74 383 10.9

*Open area around canisters set on floor.**The sludge measured in Maassen (1997) in the South Loadout Pit was transferred to theTech View Pit South Channel in September 1997 (Maassen 1997; Lodwick 1997). The volumeof S1udge measured in b+aassen(1997) in South Loadout Pit (1.003 ft3, 0.0263 m3) has

3, 0.00766 m3) in this table.been”added to the Tech View Pit South Channel (O.271 ftThe uncertainties used were from Maassen (1997) for Tech View-South Channel 417%,and for the South Loadout Pit sludge volume 263%.

***Uncertainties taken from Maassen (1997)were based on upper limits of the 95% confidenceinterval including,randomvariabilities and systematic measurement variability.

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HNF-3556, Rev. ODESH-9857192ATTACHMENT IPage 6 of 8

Figure I. Co~parison of Sludge Volume Fractions\IerSu~Lo~atjons or sources at K ~~Sif)S.

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Figure 2. Comparison of Sludge Volume Fractionsversus Locations or Sources at K East EaSitI.

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Figure 3. Comparison of Sludge Volume Fractionslfer~usLo~ati~n~ or s~urces at K West Basin

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HNF-3556, Rev. O

OESH-9857199

ATTACHMENT 2

Background InformationText from Reference Baker 1997

Consisting of S pages,including cover page

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73

.Uta= nanToro, Inc. HNF-3556, Rev. O........”.

A Duke Engineering & services C0rnp2ny Memo

From: Spent h’uc?e:rFuel EvacuationsPhone:

. .376-5109 HO-40

Ctte: March 19, 1997Subject: CURRENT ESTIKATES OF SLUDGE VOLUMES IN K Vs.? ANO K k’ESTEASlliS “

To: K. L. Pe:rce

cc: C. J, Alderman0. l?.BergrrtrmK. H: %rg$mns., L. HechtP. G. LEROY3. J. JMenes

References: (1)

. (2)

(3)

... .

.“. ,

(4)

(5)

(6)

““

.: (7)

R3-11

X3-85 M. J. PackerR3-85 .A. L. ?itnerW: A. }{. ?r:ga

D. R. PrecechtelR~-i~ : D. S. Takasuini.~o-fo D. J. .TrfrhleHO-40 R3J3File/L3

X3-65t+o-koR3-85X3-65xs-~j

tio-40Ho-:o

Internal Memo, A. L. ?itner to D. S. TzkaswT~, “K WestS:sin Sludge \rolumeEsttr,ztes for Integrated A’lterTreatment Systsin, 0 dzted Jzriu~ry 29, 1597. [A1so provf dedin DESH107.620777 dated Febru~ry 1S?7. ]

Internal ~mo, D: J. Trfmble to D. S. TZkZSLImi,“KhkstBasin Slydse Volume Inventory, ” dated Januw 26, 1$$7.

..”D. J. Tritnble, Cesivm-137 in K.Jt’est“3~sfn Cznfster Wter,l-MF-sD-SNF+NAL-014,Rev. 0, dated J@N.Y 24,”1997.

Internal Memo, A. L. Pitner to D. S. P=kasurni,‘K EastBasin S7udge ~oTumeEstfmates fbr Megrated FaterTreatment. System, n dated Jwwry 23, 1997. [Also providedin DESHEDT620776 dated February 1997:].

A. L. Pitner, K E&ct Cznister Sludge StirveY,h!-lC-SD-SiiF-TI-034,Rev. O, dated August 28, 1995.,.B. J. tkkenas, et al”., An.e7ysfsof Sludge from Wford.K East Bzsin Floor cnd A’eeselPit, WHC-SP-11S2,d~tedApril 19%. .

S. ‘M. She@ znd H. M. Beary; Spent h’uc7ecrFuel ProjectTechniczl Dztzbook, ~WC-SD-SNF-TI-015, Rev. 0,. dzted

. . . August 11, 1S?5 (ECN191395 Februwy 1995).. ..”. .. (8) R: i..3tker, Summry Status of”K Basin”S7udie ‘

Charzcterizction.hIiic-sR-SNF-TI-006,Rev. O, datedJmumy: 1?95. .-

.:.“. . .“

., .,.

. . ... r.” . ..”. ,.. . . . . .

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. ..

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K. L. Pzrk

. ~%h219, 1997

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,Peryou! request, a revi~w k’zs”rtdeof th? current.estimztcs for vo7unes ofsludge In the K East %sln md K h%st ~asin. Conslc!ered was the slud~e orithe main b~sin floor, in r=note pits, In fuel can~sters, =nd the potentialfor” generation of s~udge” from h’zshing storige canisters/fuel prior to tt,efuel being pzck:ged in multi-canister overwcks (~COS). ~tt~”chfients 1 ~nd 7.provide a sutmzry of these results.

Past Swa~:rfes OFS?udce Volumes

M original sum=ry o? sludge \Io7umesin the 3:sins Ws provided inRefErence 8. These wrs bzsed primarily on measurements of slud~e depthsm:de at the K %t znd K I@t Basins just prior to the report being issued(i.e., 1994). These sludge volw:s, with uncertainty estimtes, were T=t=rused both in the Spsnt !iuclew ~~el (SNF) projsct feed document znd ths SNFProject Dztzbook, Reference7.. I,? ,zznycaszs these estir,zt~sremzin thebest values availzble. How:verj there have been additiofi~l .measur=:fits.improved estimates, and Chtnges affecting sore of these sluoge estimttes.For th=ss jnstmces the improved values should be used andthese =redescribed in the follcwing sections znd att:chm:nts.

Because of.recant questions, it is re-emphasized here that the estii=tes ofsludge-cvolurw n:de in Reference 8 for the floor of the K East main besineccouni for the ~.ct thet the fuel stor~ga. canisters. slt directly on thek-%.~loor, with. the “floor sludge” bu?lt-up around. them. My sludge underthe ciiiisters is assunied insignificant or accounted fo~ fn the uncertaintyof the~sludge vo7umesprojected. :s residing in the caslsters themselves.. . . .

Revised Estimates of Sludoe \~olumesat K Btsins

Revfsed estimates of vo7umes of sludge in the fue7ed canisters in K EastBasin were made based on ultrasound measurements of s7udge depths made in aset. of selected fuel cmisttrs in 19s6; Reference 5. These represent a“muchbetter estimate of this sludge volume than that provided in Reference S,becwse there is accurate direct data as a basis rather than the secondaryobservations used in Reference E. Attachment 1 provides these revised

. values. Not.athe magnitude of the volumes provided in these revised .,..estim;tes are simi7zr to those provided in the original estinates ofReference B within the bounds:ident~f ied (e, g., Reference ,8: total volumein”fue7ed’ canisterswas about 7.5 m w>th.a bounding estimate of 1;.7 ia3$and

in Reference,5:. total vo7ume,is 3.o m bounding estimate of 7.4 m).. . . .,,

Ikesuram$ntk of sludgs volukin the fue7ed”(sealed) c~nisters in K WestBasin were also zttempted using ultr~sound equipment to nzke depthmeasurements of the sludge. However,”thess mc:surements were found to beinconsistent, zs opposed to tha valid me:suremants resulting from therkzsurem:nts in K E?st :&sin starz:e canisters. Ths prob?em h’ith the~P~lication in K.h’=st3=sia. canisters WZ”Sprobebly ceused by (1) less sludgebs]ng present .znd(2) conpl~c~ticns >rising from pieces of thafiatsrial ysed

. . . ... .“ .75--

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HNF-3556, Rev. O

K. L. PzrkPege 3Fkrch 19; 1997

to ~~al ths canister lfds ~alling b,etweErIthe fusl ilEiaElitSduring the”process of %oving the canister lids, sEe Reference 2. Given this, it was.ju@ad a bettar estiz?te of s.ludgzvolums w possible~froni measured cssfumconcentrations in the water smples znalyzed from a selected ser of-sealedcanister barrels in K West Basin. This zppro+h is fully described inReference 2, and the resulting voluiaes given in Attechfient Z of the currentmemo.

The volufisof sludgs indicited in Reference 8 as contained in the Weasel Pit~t K East Basin, kas bzsed on as inference of s~uds~ d~p~~ m=m:d from theshadow of sludge observed on the screen separating the Weasel Pit from themain basin. A much batter estimate was later made zvail?ble based on

measurements fi;dein August md September 19S5. These ?re”discussed inReference 6, wjich concluded an integrated sludge volume for the pit h’as7.4 LIS(264 ft.-).Since these fiezsurefi$fitsh’=remade in 1953 at lezst th’oactivities hzva &dd*dsludge to this pit. First, the South Loadout Pit wascleaned and this slw’$e pumpedto the Weasel ?it. Second, tn ~rea of theCenter Ezy of the K East kin WEScleznsd of sludge, to support processirtgand cleaing enpty canisters, zgain the sluo’g~ w~s pumped tO the k’=~sel ?it.Estimates of the sludge moved to the k’ezsel ?~t were made based on thesludge estiti,ated in these &rees froin RefErence 8 data. These quantitieswere then added to the volufi? of sludge estiia~ted from measurements m=deinSeptember 1995 (R$f:rsnce5) for the ?JeaselPit. For the South Lo:dout ?ita volume OE3.3-n has .:ssumed.ta heve. b-mo\<ed& and for.thz.clezned. “portiori 0$ the Center B:y the estimate of tha associated volume of sludgewas O.~ m ; The 1tiw volume was subtncted from th= main”basin+ oor.value. The final estiffi~tes of sludge in the K East Basin kreaseT Fit and onthe main basin fl?or .xe shown in Attachment 1.

A quick survey h’asmade of the K west Basin rEmote pits znd main basin flooras “aresult of your request. FFom this the estimates of sludge depths weremade that ~re shownin Attachment 2. Direct physical measurement of slud~edepths on the K West main bzsin floor and in the pits (except the NorthLoadout Pit) i$ pl :nned to be completed by the Spant hhclear FuelEvaluations groupwithin the next,2 months.

,..The depths ..andvolumes of sludge in the “tlorth Lo&dout Pits (i. e., 5&ndfilterBackwash P;ts) in both K East and K west Basins zre based on directmeasurements made ~t “the end of 1995, ,Reference ‘8! Some minor increzse insludge depths has no doubt occurred due, to further beck’wshing of thesandfilters;. It is assisraedhere this has had little influence on thevolumes (i. e., within the uncertainties noted). This will be verified inthe next year when samples, are tzken fjrom.these pits for ch.w.zcterizztion.. . . . ., . .. . . . . .. .Similar to the North Lozdout Pits,,theie FjZS likely “be’ensore incre;s; insludge vo]ums on ths K East ~~in b~iin floor since 1?S5 hrhen depthm:asurernsnts h’:re m:asw+. Here again this is asswaed to be within thauncertainties. indicated.

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HNF-3556, Rev. O, ,.

.’...

$lg~.4Park

M~rch 19, 1997

To provide a coinprehmsive set of sludge. volumes; estimztes :re. alsoincluded in Attzchmart 1 for the future Washing of fuel znd cznlsters :t theK East Sasinj these estimzteswere tzken from Refermce 4. K-vest Basin wasalso reviewed to ~:ke a simi~zr estimate for fuel ,h’qshing,Rererence 1.Here it M,asestiiiittedthat”?t this time a value slfillarto the K Ezst >=Sinvalue should be used. This is reflected in Attachment 2.

Please cont=ct ma if You have qu=stfonso,

(f@ozlR. B. Baker, Fellow EngineerSpent h’ucle~r Fuel Evaluations

Jiim

Attachments 2

PEERREVIEk’:

A%2b 3/,?/97 ~~Date:A. L. PitnerSpent t4uclear Fuel Evaluations

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,.-. .

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APPENDIX B

SLUDGE DEPTH ESTIMATES AND SAMPLE LOCATIONS DETAILFOR K WEST AND K EAST BASINS

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HNF-3556, Rev. O

Figure B1. Floor S1udge Depth (in inches) at Locations Measured in1997 at K West Basin (Maassen 1997). (Prior to S1udge Being Pumped

from South Loadout Pit to Tech View South Transfer Channel. )

81

HNF-3556, Rev. O

Figure B2. K West Basin North Loadout Pit Sample Locations.

.....

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HNF-3556. Rev. O

Figure B3. Surface Fit of Sludge Depth Data in K West BasinNorth Loadout (Sandfilter Backwash) Pit in 1995.

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HNF-3556, Rev. O

Figure B4. K West Basin Weasel Pit and Tech View Pit Sample Locations.

z+—————

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HNF-3556, Rev. O

Figure B5. K West Basin Dummy Elevator Pit

I

Sample Locations.

—

z85

HNF-3556, Rev. O BEST AVAILABLE COPY

Figure B6. Fit of S1udge Depth Data in the Three Bays of K EastMain Basin in 1995. (Locations relate to Figure 4)

86

HNF-3556, Rev. O

Figure B7. Sample Locations Used in 1995 Campaign in K East Basin.

87

N

...+

105-KE Basin North Loadout Pit’s Exclusion Zone,Plywood Covering, and Sample Locations (all units

wm<

0

in inches)

HNF-3556, Rev. OBEST AVAILABLE COPY

Figure B9. Surface Fit of Sludge Depth Data in K EastBasin North Loadout (Sandfilter Backwash) Pit in 1995.

89

HNF-3556, Rev. O

Figure B1O. K East Basin Dummy Elevator

z—

Pit Sample Locations.

,,.. ....,...,f.>.....’.

90

Figure BII. S1udge Depth Data for K East Basin Weasel Pit in 1995.

COP”(

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HNF-3556, Rev. O

Figure B12. Sample Locations Used in the K EastBasin Weasel Pit for the 1995 Campaign.

—N —

K[3-R-18 {7 MI(2L3’)1 -

[86m@’-10-)]

[.591..

KS-O- 17 j760m(30-)t -

“KES-P-16 j30cm(12”)i -

Es “’””’

m ““’””

[168cm(5-6.)]

L$a4kc=’’’cm(jVII

36cm( !-2-)][t04cm!3’-5-)]

1 ‘W’”)’l L,_. f.,.’’’(,)

[185m(6’-1<)]

J

~[ :8m(0 -T;]

4

,4-)]

[36m( 1-2-)]

,-2”’)1

L-1 [135cm(4’- 5-)]~

1. SCREEN F3ETWECN WCASZLPIT AND TRANSFER CHANNELTO MAIN BASIN

2. SPECIAL ~RACKETS TOSUPPORT ISOLATION TuBES.

\ \ SLUOGE OEPTH MLWJREO

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HNF-3556, Rev. O

Figure B13. K East Basin Weasel Pit and Tech View Pit Sample Locations.

\?,.,. ,,,,...,..;.

1

[

1 m

$jN

.::.’....

z—

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Project Title/Work Order EDT No. 620822

Sampling and Analysis P1an for Sludge Located on the Floor and ECN No.

in the Pits of the 105-K Basins/HNF-3556, Rev. O

Text Text Only Attach./ EDTIECNNama MSIN With All Appendix Only

Attach. Only

Fluor Daniel Hanford, ” Inc.

E. W. Gerber R3-11R. L. McCormack R3-11M. J. Wiemers R3-11N. H. Williams R3-11

B&W Protec

T. L. Welsh T4-40

Duke Enqineerinq & Services Hanford, Inc.

C. J. Alderman x3-74R. B. Baker (2) HO-40D. W. Bergmann HO-40K. H. Bergsman X3-85A. E. Bridges HO-40R. W. Brown X3-65L. D. Bruggeman HO-40S. L. Hecht HO-40D. P. Kimbal J X3-71D. P. Maassen HO-40P. J. MacFarl an HO-40B. J. Makenas HO-40K. R. Morris X3-56J. Perez-Carter HO-40A. L. Pitner HO-40A. M. Segrest R3-11D. W. Smith R3-11J. A. Swenson R3-11C. A. Thompson X3-72D. J. Trimble HO-40SNF Project File R3-11

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Pacific Northwest National Laboratory

P. R. BredtC. H. DelegardG. R. GolcarA. J. SchmidtK. L. SilversJ. M. Tingey

A3-88 xA3-B9 x

T6-07 xT6-50 xH7-20H7-20 1S4-45 xH7-20 x

P7-25 xP7-25 xK6-24 xK2-12 xK9-08P7-25 ;

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