ML17349A371

Rev 10 to Procedure PT-51-WS, Solidification Process Control Procedure.

ML17349A371
Person / Time
Site:	Turkey Point
Issue date:	05/21/1992
From:	Atchley P, Caughman G, Hill M PACIFIC NUCLEAR SYSTEMS, INC.
To:
Shared Package
ML17349A369	List: ML17349A368 ML17349A370 ML17349A371
References
PT-51-WS, NUDOCS 9209090181
Download: ML17349A371 (146)

Text

CONTROLLED 3h-~7>c%-tI" SOLXDXFXCATXON PROCESS CONTROL PROCEDURE PT-51-WS c~~P/ICIFIC NUCLEfIR, Revision:~

Sffective Date: I!: Jl uments The following related Pacific Nuclear/Waste Services Document(s) contain operations or information essential to performance of.instructions herein and must be issued in conjunction

~ith this document: 1.0-0 3.2.5.6.Prepare By C Date Engineeringg Customer Serv ce Date Date 2l Z-ality Ass ance gl g Ot r Q.Q4v~Document Control Date Date Date 9209090181 920821 PDR*DOCK 05000250 R PDR+>s~<StfvlcRs Qfyile p,

t r~(PT-51-MS 5/2l/92)//>>):TITLE: Solidification Process Control Procedure RECORD OF REVISIONS:REV: OESCRIPTIOM PAGE(S): OATE: SIGNATURE AFFE TEO 7.Added sign-offs on Adden-: Annotated:

dums, added addendum H...by vertical~revised addendum G,>u>><line in: volumes l.ight margi.n Z-Io-88:.9: Revised to add the use of: cenent and to put in NSDI~procedure format.Q c: 10: Revised to add PCP require-ments and to change to Waste Services Group (HSG)procedure-number f ormat.All LIST GF EFFECTIVE PAGES Paoe No.~~Rev:: Paoe No.Rev:: Pace No.Rev I'Ell, t 1[

May 21, 1992 TABLE OF CONTENTS 1.0 PURPOSE AND SCOPE

2.0 REFERENCES

3.0 DEFINITIONS

-PROCESS DESCRIPTION

'4.0 RESPONSIBILITIES 5.0 PRECAUTIONS/PREREQUISITES 6.0 PROCEDURE 6.1 System Operation 6.2 Sample Verification 6.3 Full Scale Solidification Calculations 7.0 ADDENDA A.B.C.D.E.F.G.H.LINER DATA SHEETS SOLIDIFICATION OF CITROX AND BEAD RESINS SOLIDIFICATION OF AP&BEAD RESINS OR 1004 CATION BEAD RESINS SOLIDIFICATION OF OIL SOLIDIFICATION OF BEAD RESINS AND BORIC ACID OR CLASS A GRANULAR ACTIVATED CARBON AND BORIC ACID SOLIDIFICATION OF BORIC ACID SOLIDIFICATION OF BEAD RESINS OR CLASS A GRANULAR ACTIVATED CARBON SOLIDIFICATION OF POWDERED RESINS I A'II I I 0 PT-51-WS, Rev.10 May 21, 1992 1.0 PURPOSE AND SCOPE;~~gay~4>>+5~4<er~i l This document contains the Process Control Procedures for the solidification of various types of waste using the Pacific Nuclear Solidification System and Envirostone or Portland Type I or II Cement.Control of the process parameters involves the solidification of a laboratory sample of each separate type of waste product to be solidified, calculation of the chemical volumes to be added in the specific waste container to be used and logging of the solidification details, while following the solidification operating procedures.

Log sheets for each of these three separate tasks are included in this document.

2.0 REFERENCES

2.1 United States Gypsum's Topical Report on Envirostone 2.2 10 CFR 61 2.3 NRC Branch Technical Position on Waste Form 2.4 WSG System Operating Procedure, OM-104 2.5 Pacific Nuclear Quality.Assurance Program 2.6 NRC Branch Technical Report, May 1983, Rev.0 3.0 DEFINITIONS

-PROCESS DESCRIPTION The Pacific Nuclear Solidification System is specifically designed to facilitate solidification of various forms and mixtures of radioactive waste in large scale liners.The waste is effectively immobilized using the specified type of cement which is thoroughly mixed with the waste using the system in-container

.mixing blades.The final product has proven to be a homogeneously mixed, free standing monolith with no free standing water.4.0 RESPONSIBILITIES"Not Applicable" 5.0 PRECAUTIONS/PREREQUISITES Waste can be solidified using the PNSI solidification Unit and either Envirostone or Portland Type I or II Cement in accordance with the formulas listed in this PCP.Specific waste conditioners are required for some waste forms before solidification.

The procedures for solidification of various wastes are included as separate addendums to this procedure.

44ll.t+C e PT-51-WS, Rev.10 Nay 21, 1992 If the laboratory analysis of the waste solidification shows that the waste setup time will be less than desired, Red Top Retarder can be added in small amounts to extend the setup time to long enough to ensure that the full volume of cement can be thoroughly blended with the waste to form a homogeneous mixture.If the waste/cement mixture exhibits a long setup time, as indicated by laboratory testing, accelerator (Alum or equivalent) can be added to the mixture.The exact amount, of retarder or accelerator will be determined during the laboratory solidification and then will be applied in the same proportion in the full scale solidification (within+24).6.0 PROCEDURE 6.1 System Operation The Pacific Nuclear Solidification System is operated in accordance with the approved procedures, which ensure reproducibility of the waste product from liner to liner.The process parameters and chemical ratios used in each solidification are specifically calculated for each waste batch and a sample verification satisfactorily performed before attempting a full scale solidification.

6.2 Sample Verification 6.2.1 6 2'Prior to full scale solidification of each liner of waste product, a representative sample of each waste product shall be test solidified in the laboratory.

Detailed procedures for test solidification for each waste type are attached as addenda to this procedure.

A, portion of the sample shall be isotopically analyzed to determine the waste class.This test solidification confirms the correct process chemistry ratios to be used in the full scale solidifications of the same.waste batch.The sample solidification should verify that the solidified waste product will be a uniform, dry, free-standing monolith.The waste end product shall resist penetration when probed with a firm object.The operator will number each solidified sample and record the contents of each test solidification on a Sample Verification Worksheet.

A Solidification Worksheet will then be prepared for each liner prior to solidification.

An Operations Logsheet will be prepared for each liner during solidification.

The liner serial number will be recorded on the Operations Logsheet.

PT-51-NS, Rev.10 May 21, 1992 6.2.3 6.2.4 The waste batch will be sampled and a PCP performed per the following schedule: a.Initial samp'le.b..After, additional waste is added to the holdup tanks.c.After every seven days.d.After every tenth batch or 5000 gallons of batch waste, whichever is more frequent.PCP Failure 6.2.F 1 6.2.4.2 6.2.4'If any test specimen fails to verify SOLIDIFICATION, the SOLIDIFICATION of the batch under test shall be suspended until such time as additional test specimens can be obtained.Alternative SOLIDIFI-CATION parameters can be determined in accordance with the PROCESS CONTROL PROGRAM, and a subsequent test verifies SOLIDIFICATION.

SOLIDIFICATION of the batch may then be resumed using the alternative SOLIDIFICATION parameters determined by the PROCESS CONTROL PROGRAM.If the initial test specimen from a batch of waste fails to verify SOLIDIFICATION, the PROCESS CONTROL PROGRAM shall provide for the collection and testing of representative test specimens from each consecutive batch of the sametype of wet waste until at least three consecutive initial test specimens demonstrate SOLIDIFI-CATION.The PROCESS CONTROL PROGRAM shall be modified as required to assure SOLIDIFICATION of subsequent batches of waste.If the installed equipment is declared inoperable, restore the equipment to OPERABLE status.

F" PT-51-NS, Rev.10 May 21, 1992 6'Full Scale Solidification Calculations After a laboratory sample has been solidified and it has been confirmed that the waste product will meet the requirements for a satisfactorily solidified end product, the calculations can be made for solidification of the waste form in large containers.

Calculations will be made and recorded on the Solidification Norksheet included in each addendum.7.0 ADDENDA A.B~Liner Data Sheets Solidification of CITROX and Bead Resins'C.Solidification of AP and Bead Resins or 1004 Cation Bead Resins D-Solidification of Oil E.Solidification of Bead Resins and Boric Acid or Class A Granular Activated Carbon and Boric Acid Solidification of'oric Acid G.Solidification of Bead Resins or Class A Granular Activated Carbon H.Solidification of Powdered Resins.

PT-51-WS, Rev.10 (Addendum A)May 21, 1992 ADDENDUM A LINER DATA SHEETS 1 of 5 41't I 0 PT-51-WS, Rev.10 (Addendum A)LINER DATA, SHEET-.50 CUBIC FOOT SOLIDIFICATION LINER May 21, 1992 Burial Volume: 52.0 cubic feet Usable Internal Volume: 46.8 CF (with 2" of free space in top)Empty Weight: 600 lbs Solidified Weight: (Envirostone) 51.00~8.75 F 7 Oil: 4150 lbs Resin: 4500 lbs Concentrates:

4850 lbs Solidification Data: 4 47.00 i l I 47.25 40>o 45 50 55 60 65 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 100 36~1>o 40.6 45.1 49.6 54.1 58.7 63 2 74.1 65.0 65'66'67.7 68 6 69.5 70.4 71'72 2 73.1 74.0 74 9 75.8 76 7 90 2 18-7 CF 21.0 23.4 25.7 28.0 30.4 32.7 33.2 33.6 34.1 34.6 35.0 35.5 36.0 36.4 36.9 37.4 37.8 38.3 38.8 39.2 39.7 46.8 18.7 21.0 23.4 25.7 28.0 30.4 32 7 33'33.6 34.1 34.6 35.0 35.5 36.0 36.4 36.9 37.4 37 8 38.3 38 8 39 2 39.7 46.8 in Vo'd ace 30;1 in 27.2'5.4 23.0 20.7 18'16.0 15.6 15 F 1 14.6 14.2 13'13 2 12'12'11.8 11 4 10.9 10.4 10 0 9 5 9'2 0 Solidification Efficiency

=(Waste Volume/Solidified Vol)X 1004 Packaging Efficiency

=(Waste Volume/Burial Volume)x 1004 Waste Height (E)and Void Space (F)dimensions are prior to solidification and.are.used to set.the bubble tube level indicator.

2 of 5 gN 9ll 0 PT-51-WS, Rev.10 (Addendum A)LINER DATA SHEET-142 CUBIC FOOT SOLIDIFICATION LINER May 21, 1992 Burial Volume: 128.3 cubic feet Usable Internal Volume: 118.6 CF (with 2" of free space in top)Empty Weight: 1100 lbs Solidified Weight: (Envirostone)

Oil: 10,125 lbs Resin: 11,000 lbs Concentrates:

11,900 lbs Solidification Data: 69.75 6.(.2.5 E 63.25 i I 63.5 40>o 45 50 55 60 65 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 100 35.14 39.5 43.9 48.3 ,52.6 57'61.4 62.3 63.2 64.0 64 9 65.8 66.7 67.6 68.4 69'70.2 71-1 71 9 72.8 73 7 74.6 87'Waste Vo 47.5 CF 53.4 59.3 65.3 71.2 77-1 83.1 84.2 85.4 86.6 87.8 89.0 90.2 91.4 92.5 93.7 94.9 96.1 97.3 98'99.7 100.8 118.6 W ste t 26.1 in 29.4 32.6 35.9 39.2 42.4 45.7 46.3 47.0 47.6 48.3 48 9 49.6 50.2 50.9 51.5 52.2 52.9 53.5 54.2 54.8 55.5'5'V'Sae 39.2 in 35.9 32.7 29.4 26'22'19.6 19.0 18.3 17'17.0 16.4 15 7 15'14'.4 13.8 13 1 12 4 11'llew 1 10.5 9 8 2~0 Solidification Efficiency

=(Waste Volume/Solidified Vol)X 1004 Packaging Efficiency

=(Waste Volume/Burial Volume)x 1004'aste Height (E)and Void Space (F)dimensions are prior to solidification and are used to set the bubble tube level indicator.

3 of 5 A Iil, 0 PT-51-WS, Rev.10 (Addendum A)LINER DATA SHEET 190 CUBIC FOOT SOLIDIFICATION LINER May 21, 1992 Burial Volume: 170.2 cubic feet Usable Internal Volume: 158.4 CF (with 2" of free space in top)Empty Weight: 1285 lbs Solidified Weight: (Envirostone)

Oil: 13,350 lbs Resin: 14,500 lbs Concentrates:

15,700 lbs Solidification Data: 71.0 68.75 7.2.25 72..50 F i I 40>o 45 50 55 60 65 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 100 37.35o'2.0 46.7 51.3 56.0 60.6 65.3.66.2 67'68.1 69.0 70.0 70.9 71'72.8 73.7 74'75.6 76'77'78'=79.3 93.3 Waste Vo 63.3 CF 71.3-79.2 87.1 95.0 103.0 110.9 112.5 114.0 115.6 117.2 118.8 120.4 122.0 123.6 125.1 126.7 128.3 129.9 131.5 133 0 134.0 158.4 26.7 in 30.0 33.4 36.7 40.0 43.4 46.7 47.4 48.1 48.7 49.4 50.1 50.7 51.4 52.1 52.7 53.4 54.1 54.7 55.4 56.1 56.7'6.8 40.1 in 38.8 35'32'28.8 25'22 1 21'20 7 20 1 19.4 18'18.1 17'16.7 16.1 15.4 14'14 1 13.4 12 7 12'2.0 Solidification Efficiency

=(Waste Volume/Solidified Vol)X 100%Packaging Efficiency

=(Waste Volume/Burial Volume)x 1004 Waste Height (E)and Void Space (F)dimensions are prior to solidification

'and are used to set the bubble tube level indicator.

4 of 5 0

PT-51-WS, Rev.10 (Addendum A)LINER DATA SHEET 210 CUBIC FOOT SOL'IDIFICATION LINER May 21, 1992 Burial Volume: 199.4 cubic feet Usable Internal Volume: 185.5 CF (with 2" of free space in top)Empty Weight: 1400 lbs Solidified Weight: (Envirostone)

Oil: 15,500 lbs Resin: 16,850 lbs Concentrates:

18,300 lbs Solidification Data:/8.25 75.75 (4.5"0 i 404 45 50 55 60 65 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 100" t1IIILMS 37.3>o 42.0 46.7 51.3 56.0 60.6 65.3 66.2 67.2 68.1 69.0 70'70'71 8 72 8 73'74.6 75'76'77 4 78.4 79 3 93.3 W ste Vo 74.2 CF 83.5 92.8 102.0 111.'3 120.6 129.9 131'133.6 135.4 137.3 139.1 141.0 142.8 144.7 146.5 148.4 150.3 152;1 154.0 155.8 157.7 185.5 W ste t 29.5 in 33.2 36'40.6 44.3 47.9 51'52.4 53.1 53'54.6 55'56.1 56'57.5 58.3 59.0 59 7 60.5 61.2 62.0 62 7 73.7 V S c F 46.3 in 42.6 38.9 35'31.5 27.8 24.1 23 4 22.6 21.9 21.2 20'19'19'18'17'16.7 16.0 15.3 14.5 13.8 13.1 2.0 Solidification Efficiency

=(Waste Volume/Solidified Vol)X 100%Packaging Efficiency

=(Waste Volume/Burial Volume)x 1004 Waste Height (E)and Void Space (F)dimensions are prior to solidification and are used to set the bubble tube level indicator.

5 of 5

PT-51-WS, Rev.10 (Addendum B)May 21, 1992 ADDENDUM B PROCESS CONTROL PROGRAM FOR SOLIDIFICATION OF CITROX AND BEAD RESINS 1 of 10 V

PT-51-WS, Rev.10 (Addendum B)May 21, 1992 1 0 PREREQUISITES 1.1 A sample solidification shall be performed before attempting to perform a full scale liner solidification.

1.2 The WSG operator shall ensure that a Radiological Work Permit has been issued for the performance of the sample verification activity and that adequate personnel monitoring and radiation detection equipment is on hand.1.3 The WSG operator shall ensure that all necessary materials and equipment are on hand prior to beginning the sample verification.

Suggested equipment and materials for the test are as listed below: NOTE: 6-300 to 500 ml plastic beakers 6-mixing spatulas 1-500 gram capacity scale 20 g-PNS waste conditioner WC-785 50 g-Calcium Hydroxide 1000 g-Envirostone or Portland Type I or II Cement 100 g-Anhydrous Sodium Metsosilicate (Metso)The waste and chemicals used to solidify the sample waste must be from the same containers or lot numbers to be used in the full scale solidification.

1.4 A one-liter sample shall be taken for solidification in the laboratory for each separate batch of waste to be processed.

The operator may choose to take the samples from the storage tanks to be solidified in the liner, or may take the sample from the liner directly, after the waste has been transferred to the liner.Due to the importance of obtaining a representative sample for use in the verification procedure, the operator shall confirm that the contents of the waste form to be solidified have been adequately mixed and that the sample is a part of a homogeneously mixed waste batch.2 0 SAMPLE VERIFICATION 2.1 Record the information obtained during sample verifica-tion on the Sample Verification Worksheet.

2.2 Provide a waste sample (size to be specified by the plant)to the plant staff for isotopic analysis.2.3 Place a sample of the waste in the beaker so that the resins are at the.200 ml level.-with the-liquid solution just covering the resins.This may necessitate pouring off some of the liquid solution.2 of 10 k'N l7,.II 4 PT-51-WS, Rev.10 (Addendum B)May 21, 1992 2.4 Record the initial-pH, radiation level and temperature of the waste sample.2.5 Add Slacked Lime (Calcium Hydroxide) to the waste sample in the quantity as per Table I and mix the sample thoroughly for ten minutes.Record the pH of the sample.2.6 Add PNS WC-785 to the waste sample in the quantity as per Table I and mix the sample thoroughly for ten minutes.Record the pH of the sample.2.7 Add Envirostone or Portland Type I or II Cement to the waste sample in the quantity as listed in Table I and mix the sample until the mixture begins to thicken.Record the time from the start of adding the appropriate cement to the time that the mixture thickens such that mixing is no longer required (mix time)and the time from the start of adding the appropriate cement to the time that the waste is firm to the touch (setup time).Additional cement can be added if necessary to achieve a satis-factory end product;However, if additional cement must be added, the waste solidification efficiency must be redetermined and the solidification liner waste volume adjusted.CITROX/Cation Grams Grams Grams Grams~me~eteo~WC-7 5~Ce e t 1004 CITROX 75%CITROX/254 Cation 50%CITROX/504 Cation 254 CITROX/754 Cation 4.0 3.0 2'1.0 25 25 25 25 1.5 1'0.8 0.4 103 104 105 107 NOTE: 2.8 Metso is Anhydrous Sodium Metsosilicate used in conjunction with Portland Type Cement.Continue to mix samples until a satisfactory waste pro-duct is produced.The waste setup time should be at least 30 minutes for 50 ft'iners, 60 minutes for 142 ft'iners, and 90 minutes for larger liners.If the setup time is shorter than specified for.the liner to be solidified, add a lesser amount of WC-785 and continue to perform sample testing to verify the setup time.If the setup time is greater than 150 minutes, add a greater amount of WC-785 to the waste sample and continue to per-form sample testing until a satisfactory sample is obtained which will set up in less than 150 minutes.If a satisfactory sample cannot be obtained by adjusting the amount of WC-785, the operator can adjust the amount of lime added to the waste sample and continue to test.If a satisfactory sample cannot be obtained, the operator shall refer to Section 6.2.4 and contact the Customer Service Manager before proceeding.

3 of 10 Ar PT-51-WS, Rev.10 (Addendum B)Hay 21, 1992 2.9 Remove the solidified sample from the sample container and visually examine it for evidence of soft, porous oi unsolidified areas.The solidified samples should be hard, homogeneous and of uniform coloration.

2.10 Set sample(s)aside for future disposal.3.0 FULL SCALE SOLIDIFICATION 3.1 After a satisfactory sample solidification has been performed, determine the appropriate amount of waste conditioners and cement to be added to the full scale liner solidification using the Solidification Worksheet.

3.2 After determining the appropriate volumes of additives and cement to be added to the Liner, the full scale solidification should be performed using the system operating procedure (Reference 2.4), and the Solidification Operations Logsheet should be filled out.4 of 10 t<

PT-51-WS, Rev.10 (Addendum B)May 21, 1992 SAMPLE VERIFICATION WORKSHEET FOR SOLXDXFXCATION OF CXTROX AND BEAD RESXNS Operator: Utility/Location:

Waste Type: Waste Sample From/By: Waste Temperature:

Date: F Waste pH: Page 1 of 2 No.: Sample Rad Level: Physical Characteristics (viscosity, color, sedimentation, clarity, etc.): Sample Proportions:

Waste Sample CITROX/Cation Resin Ratio Slacked Lime CA (OH), pH after Lime Addition WC-785 pH After WC-785 Chemical Additives ml ml H H Final pH Envirostone Portland Blend the required volume of cement into the waste and record the time th'e addition starts: Record the time when the mixture viscosity increases to the point when the mixer is secured: (1)Record the time when the mixture is firm to the touch: (2)5 of 10 4i PT-51-NS, Rev.10 (Addendum B)May 21, 1992 SAMPLE VERIFICATION'ORKSHEET'"'='-==-'

--=-"-FOR SOLIDXFICATXON OF CITROX AND BEAD RESXNS Sample Resul'ts: Mix time (1): Setup time (2): minutes minutes Page 2 of 2 Free Nater, if any: Relative set (soft, firm, very hard): Observations:

Sample proportions and solidification results acceptable for calculation of large scale solidification ratios: yes no Isotopic results of sample: Solidification Efficiency (Haste Volume/Solidified Volume): Op'erator Signature:

Date: Utility Representative Signature:

, Title: Date: 6 of 10 11 z Jl ,f'I N PT-51-WS, Rev.10 (Addendum B)May 21, 1992 SOLIDIFICATION WORKSHEET:-...

FOR SOLIDIFICATION OF CITROX AND BEAD RESINS Page 1 of 3 Operator: Utility/Location:

Waste Type: Date: No.: Satisfactory Sample Verification No: Solidification Efficiency:

Container Model: Date: SEE THE LINER DATA SHEET FOR THE LINER BEING USED Usable Liner Volume (with 2" safety margin): Waste Volume: Waste Height: (Waste Full/Level Bubble Tube to be set at this height)cf cf in Weight of Lime to be Added to the Liner (Use the values determined from the Sample Verification Worksheet):

gms of lime in sample/ml of waste in sample x 62.38 lbs of lime to be added to the liner Actual cf of waste in liner lbs of lime to be added to the liner.Weight of WC-785 to be Added to the Liner (use the values deter-mined from the Sample Verification Worksheet):

gms of WC-785 in sample/ml of waste in sample x 62.38=lbs of WC-.,785/cf of waste Actual cf of waste in liner lbs of WC-785 to be added to the liner.7 of 10 PT-51-WS, Rev.10 (Addendum B)May 21, 1992 SOLIDIFICATION WORKSHEET FOR SOLIDIFICATION OF CITROX AND BEAD RESINS Page 2 of 3 DRY CHEMICAL ADDITIVES Chemical Additive: Weight of Chemical to be added to the liner (use the values from the Sample Verification Worksheet):

gms chemical in sample/gms cement in sample lbs cement to be added to the liner'lbs Chemical Additive Chemical Additive: Height of Chemical to be added to the liner (use the values from the Sample Verification Worksheet):

gms chemical in sample/gms cement in sample lbs cement to be added to the liner lbs Chemical Additive WET, CHEMICAL ADDITIVES Chemical Additive: Volume of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

ml chemical in sample/ml waste in sample cf waste to be added to the liner x 7.48 gallons Chemical Additive Chemical Additive: Volume of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

ml chemical in sample/ml waste in sample cf waste to be added to the liner x 7.48=gallons Chemical Additive 8 of 10 f4' ta S PT-51-WS, Rev.10 (Addendum B)t May 21, 1992 SOLIDIFICATION WORKSHEET FOR SOLIDIFICATION OF CITROX AND BEAD RESINS Page 3 of 3 Weight of cement to be added to the liner (use the values determined from the Sample Verification Worksheet):

gms of cement in sample/ml of Waste in Sample x 62.38=lbs of cement/cf of waste'Actual cf of waste in liner lbs of cement.to be added to the liner.NOTE Cement weight may be rounded up to the next 100 pound increment thus allowing full 100 pound bags of cement to be added to container.

Calculate and record the weight percent of CITROX to resin in the liner: Operator Signature:

Date: Utility Representative Signature:

Title: Date:~a i.~l,-,>>(:-~*~9 of 10 W~0

.,PT-51-WS, Rev.10 (Addendum B)SOLIDIFICATION OPERATIONS LOGSHEET May 21, 1992 Operator: Utility/Location:

Liner Serial No.: Date No.Waste Type: Waste From: Sol idif ication Worksheet No: Waste Volume Added: Height of Waste: 'ime Mixer Started: Wet Chemicals Added (List): gal gal Dry Chemicals Added (List): lbs lbs cf: Time Completed:

time completed time completed time completed time completed Inches From Inside Bottom of Liner Hydraulic Press: Cement Added: lbs Time Started: Complete: Mixer Hydraulic Pressure PSI Time Time Mixer Secured: Waste Setup Time: Time Pillhead Removed: Time Liner Capped: Only Cap Liner With Utility Representative's Approval: Comments and Observations:

Date Liner Shipped/Shipment Number: Operator Signature:

Utility Representative Signature:

Title: Date: Date: 10 of 10

PT-51-WS, Rev.10 (Addendum C)May 21, 1992 ADDENDUM C PROCESS CONTROL PROGRAM FOR SOLIDIFICATION OF AP AND BEAD RESINS OR 100%CATION BEAD RESINS 1 of 9 C=

May 21, 1992 1.0 PREREQUISITES 1.1 A sample solidification shall be performed before attempting to perform a full scale liner solidification.

1.2 1.3 The WSG operator shall ensure that a Radiological Work Permit has been issued for the performance of the sample verification activity and that adequate personnel monitoring and radiation detection equipment is on hand.The NSG operator shall ensure that all necessary materials and equipment are on hand prior to beginning the sample'verification.

Suggested equipment and materials for the test are as listed below: NOTE: 6-300 to 500 mL plastic beakers 6-mixing spatulas 1-500 gram capacity scale 10 g-Red Top Retarder or equivalent (if required)100 g-Anhydrous Sodium Metsosilicate (Metso)1000 g-Envirostone 20 g-Accelerator, Alum or equivalent (if required)1000 g-Portland Type I or II Cement The waste and chemicals used to solidify the sample waste must be from the same containers or lot numbers to be used in the full scale solidification.

1.4 A one-liter sample shall be taken for solidification in the laboratory for each separate batch of waste to be processed.

The operator may choose to take the samples from the storage tanks to be solidified in the liner, or may take the sample from the liner directly, after the waste has been transferred to the liner.Due to the importance of obtaining a representative sample for use in the verification procedure, the operator shalJ.confirm that the contents of the waste form to be solidified have been adequately mixed and that the sample is a part of a homogeneously mixed waste batch.2.0 SAMPLE VERIFICATION 2.1 Record the information obtained during sample verifica-tion on the Sample Verification Worksheet.

2.2 Provide a waste sample (size to be specified by the plant)to the plant staff for isotopic analysis.2 of 9

~4 t V.0 PT-51-WS, Rev.10 (Addendum C)May 21, 1992 2.3 2.4 NOTE 2.5 2.6 Place a sample of the waste in the beaker so that the resins are at the 200 ml level with the liquid solution just covering the resins.This may necessitate pouring off some of the liquid solution.Record the initial pH, radiation level and temperature of the waste sample.Step 2.5 applies only if Portland Cement is used.If Envirostone Cement is , skip to Step 2.6~~'.Yp'dd 25 g of Anhydrous Sodium Metsosilxcate to the 200 ml waste sample, and mix until dissolved.

Add 108 g of cement to the 200 ml waste sample and mix the sample until the mixture begins to thicken.Record the time from the start of adding the cement to the time that the mixture thickens such that mixing is no longer required (mix time)and the time from the start of adding the cement to the time that the waste is firm to the touch (setup time).Additional cement can be added if necessary to achieve a satisfactory end product.However, if additional cement must be added, the waste solidifi-cation efficiency must be redetermined and the waste volume to be added to the solidification liner may have to be adjusted.NOTE: Step 2.7 applies only if Envirostone is the type of cement used.2.7 2.8 2.9 If the waste setup time is less than 30 minutes if a 50 cubic foot liner is being used, is less than 60 minutes if a 142 cu ft liner is being used, or is less than 90 minutes if a larger liner is being used, add Red Top Retarder to the 200 ml waste sample at a rate of Retarder Wt=0.054 of Envirostone Wt to adjust the waste setup time to the minimum time requirement for the liner size being used.Increase the amount of retarder added to the sample until the desired setup time is achieved.If the waste setup time is longer than operationally desired, add accelerator to the 200 ml waste sample at a rate of Accelerator Wt=1.04 of Envirostone Wt to adjust the waste setup time to the maximum time.Increase the amount of accelerator to the sample until the desired setup time is achieved.Continue to*mix samples until a satisfactory waste product is produced.If a satisfactory sample cannot be obtained, the operator shall refer to Section 6.2.4 and contact the Customer Service Manager before proceeding.

3 of 9 4 4y l PT-51-WS, Rev.10 (Addendum C)May 21, 1992 2.10 Remove the solidified sample from the sample container and visually examine it for evidence of soft, porous or unsolidified areas.The solidified sample should be hard, homogeneous and of uniform coloration.

2.11 Set sample(s)aside for future disposal.3.0 FULL SCALE SOLIDIFICATION 3.1 After a satisfactory sample solidification has been performed, determine the appropriate amount of Additives and'ement to be added to the full scale liner solidification using the Solidification Worksheet.

3.2 After determining the appropriate volumes to be added to the Liner, the full scale solidification should be performed using the system operating procedure (Reference 2.4)and the Solidification Operations Logsheet should be filled out.4 of 9 1)C PT-51-WS, Rev.10 (Addendum C)May 21, 1992 SAMPLE VERIFICATION WORKSHEET--

--=-.*-FOR SOLIDIFICATION OF AP AND BEAD RESINS OR 1004'ATION BEAD RESINS Page 1 of 2 Operator: Utility/Location:

Waste Type: Waste Sample From/By: Waste Temperature:

Date: F Waste pH: No.: Sample Rad Level: Physical Characteristics (viscosity, color, sedimentation, clarity, etc.'): Sample Proportions:

Waste Sample AP/Cation Resin Ratio pH Chemical Additives (if required)ml/ml ml H Cement Accelerator (if required)Blend the required chemical additives (if any)thoroughly into the waste before adding the cement.Blend the required volume of cement into the waste and record the time the addition starts: Record the time when the mixture viscosity increases to the point when the mixer is secured: (1)Record the time when the mixture is firm to the touch: (2)5of9 I 0 PT-51-WS, Rev.10{Addendum C)SAMPLE VERIFICATION WORKSHEET.FOR SOLIDIFICATION OF AP AND BEAD RESINS OR 1004 CATION BEAD RESINS May 21, 1992 Page 2 of 2 Sample Results: Mix time (1): Setup time (2): minutes minutes Free Water, if any: Relative set (soft, firm, very hard): Observations:

Sample proportions and solidification results acceptable for calculation of large scale solidification ratios: yes no Isotopic results of sample: Solidification Efficiency (Waste Volume/Solidified Volume): Operator Signature:

Date: Utility Representative Signature:

Title: Date: 6 of 9 4f PT-51-WS, Rev.10 (Addendum C)SOLIDIFICATION-WORKSHEET

• .FOR SOLIDIFICATION OF AP AND BEAD RESINS OR 1004 CATION BEAD RESINS May 21, 1992 Page 1 of 2 Operator: Utility/Location:

Waste Type: Date: No.: Satisfactory Sample Verification No: Solidification Efficiency:

Container Model: Date: SEE THE LINER DATA SHEET FOR THE LINER BEING USED Usable Liner Volume (with 2" safety margin): Waste Volume: Waste Height in Liner: (Waste Full/Level Bubble Tube to be set at this height)cf in Weight of cement to be added to the liner (Use the values determined from the Sample Verification Worksheet):

gms of cement in sample/ml of waste in sample x 62.38 lbs of cement/cf of Waste cf of waste to be added to the liner lbs of cement to be added to the liner.NOTE: Cement weight may be rounded up to the next 100 pound increment thus allowing full 100 pound bags of cement to be added to container.

DRY CHEMICAL ADDITIVES'Chemical Additive: Weight of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

gms chemical in sample/gms cement in sample lbs'cement to be added to'<he liner lbs Chemical Additive 7 of 9 II I PT-51-WS, Rev.10 (Addendum C)SOLXDXFICATION WORKSHEET.

FOR SOLIDIFICATION OF AP AND BEAD RESINS OR 1004 CATXON BEAD RESINS May 21, 1992 Page 2 of 2 Chemical Additive: Weight of Chemical to be added to the liner (use the values from the Sample Verification Worksheet):

gms chemical, in sample/'ms cement in sample lbs cement to be added to the liner lbs Chemical Additive WET CHEMICAL ADDXTIVES Chemical Additive: Volume of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

ml chemical in sample/ml waste in sample x 7'8 cf waste to be added to the liner gallons Chemical Additive Chemical Additive: Volume of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

ml chemical in sample/ml waste in sample x 7.48 cf waste to be added to the liner gallons Chemical Additive Operator Signature:

Date: Utility Representative-.Signature:-

Title: Date: 8 of 9 f g4 I PT-51-WS, Rev.10 (Addendum C)SOLIDIFICATION OPERATIONS LOGSHEET Hay 21, 1992 Operator: Utility/Location:

Liner Serial No.: Date: No.: Waste Type: Waste From: Solidification Worksheet No: Waste Volume Added: Height of Waste: Time Mixer Started: Wet Chemical Added (List): gal gal Dry Chemicals Added (List): lbs lbs cf: Time Completed:

time completed time completed time completed time completed Inches From Inside Bottom of Liner Hydraulic Press: Waste Conditioner Added: Cement Added: lbs: Mixer Hydraulic Pressure Type: Time Started: PSI Time: Complete: Time Time Mixer Secured: Waste Setup Time: Time Fillhead Removed: Time Liner Capped: Only Cap Liner With Utility Representative's Approval: Comments and Observations:

Date Liner Shipped/Shipment Number: Operator Signature:

Utility Representative Signature:

Title: Date: Date: 9 of 9

Ãk PT-51-NS, Rev.10 (Addendum D)May 21, 1992 ADDENDUM D PROCESS CONTROL PROGRAM FOR SOLIDIFICATION OF OIL--1 of 9 l

PT-51-WS, Rev., 10{Addendum D)..May 21, 1992 1.0 PREREQUISITES 1.1 A sample solidification shall be performed before attempting to perform a full scale liner-solidification.

1.2 The WSG operator shall ensure that a Radiological Work Permit has been issued for the performance of the sample verification activity and that adequate personnel monitoring and radiation detection equipment is on hand.1.3 The WSG operator shall ensure that all necessary materials and equipment are on hand prior to beginning the sample verification.

Suggested equipment and materials for the test are as listed below: NOTE 6-300 to 500 mL plastic beakers 6-mixing spatulas 1-500 gram capacity scale 50 ml-Envirostone Emulsifier 10 g-Envirostone Accelerator or Alum (if required)10 g-Red Top Retarder or equivalent (if required)100 g-Anhydrous Sodium Metsosilicate (Metso)1000 g-Envirostone 50 g-Calcium Hydroxide (Lime)50 g-Boric Acid 1000 g-Portland Type I or II Cement The waste and chemicals used to solidify the sample waste must be from the same"containers or lot numbers to be used in the full scale solidification.

1.4 A one-liter sample shall be taken f or sol idif ication in the laboratory for each separate batch of oil to be.processed.

The operator may choose to take the samples from the storage drums to be solidified in the liner, or may take the sample from the liner directly, after the oil has been transferred to the liner.If the sample is taken from the drums prior to transferring the oil to the liner, the operator will take a sample from each drum and mix the samples together in the same ratio that will be mixed in the liner.The sample will consist of 126.6 ml of oil.[This will produce a total sample size of 200 ml after 59.6 ml of water (or Boric Acid concentrations up to 24 wt4)and 13.8 ml of Emulsifier has been added.]The operator may also choose to transfer the appropriate volume of waste oil, water (or Boric Acid concentrations up to 24 wt4)and Emulsifier to the liner, thoroughly emulsify the waste, then take a 200 ml sample of the waste mixture for sample solidification.

This should be done only after it has been established that the oil will solidify using the standard formulas.1~A=S~i-~a V~Wr WV'OTE: Emulsifier is added only if Envirostone is the type solidification agent used.2 of 9 I II 1'C'4l' PT-51-WS, r, Rev.'10 (Addendum D)May 21, 1992 2.0 SAMPLE VERIFICATION 2.1 After the materials and equipment, as listed in the prerequisites to this procedure, are verified available, a sample of the waste will be taken.The operator shall take the sample, as described above.When the operator chooses to take the sample directly f rom the liner, the liner should be filled, to the normal level for solidification of oil (see the appropriate Liner Data Sheet)and the oil mixed for five minutes before sampling.The sample can then be drawn directly from the liner.After the operator has confirmed that the waste oil will solidify in accordance with the normal formulas, the water (or Boric Acid)and emulsifier (if applicable) can be added to the waste oil in the liner and mixed prior to taking the sample for solidification verification.

The waste oil and the chemicals used to solidify the waste oil must be from the same batches as will be used in the full scale solidification.

Record the information obtained during sample verification on the Sample Verification Worksheet.

2.2 2.3 2.4 2.5 Provide a waste sample (size to be specified by the plant)to the plant staff for isotopic analysis.If the oil, water (or Boric Acid), and emulsifier (if applicable) have already been blended together, obtain a 200 ml sample of the mixture and skip to Step 2.7.Obtain a 126.6 ml sample of the oil to be solidified.

Add 59.6 ml of tap water{or Boric Acid)to the waste oil.If Boric Acid is used, it may be necessary to adjust the pH using calcium hydroxide (lime)such that the pH is between 2 and 6.Allow approximately 10 to 15 minutes for reaction time before further additions.

NOTE: Step 2.6 applies only if Envirostone is used as the solidification agent.Skip to Step 2.7 if Portland Cement is to be used.2.6 Add 13.8 ml of'emulsifier to the waste/water (or Boric Acid)mixture and mix until emulsified as indicated by uniform coloration without streaking.

2.7 Add.125 grams of cement to the waste mixture and.mix with a small spatula until the waste begins to thicken.Record the time that mixing was required (mix time)and the time from the addition of the cement until the waste becomes firm to the touch (setup time).Additional cement can be added if necessary to achieve a satisfactory end product.However, if additional cement must be added, the waste solidification efficiency, must be..redetermined and the waste volume to be added to the solidification liner may have to be adjusted.3 of 9 I CAp H'J PT-51-WS, Rev.10 (Addendum D)l May 21, 1992 NOTE 2.8 2.9 2.10 Steps 2.8 and 2.9 apply only if Envirostone is the solidification agent to be used.If Portland Cement is to be used, skip to Step 2.10.If the setup time is less than desireB,-add 0.05 grams of Red Top Retarder to the 200 ml emulsified waste mixture, to adjust the waste setup time to at least 30 minutes for solidification in 50 cubic foot liners.The setup time should be adjusted to at least 60 minutes for 142 cubic foot liner solidifications and to at least 90 minutes for larger liners.Adjust the weight of retarder added to the sample and continue to perform sample solidifications until the desired setup time is obtained.If the=waste setup time is longer than is operationally desired, the operator may add Envirostone Accelerator or Alum in quantities up to 2.0%of the weight of the Envirostone added.The Accelerator or Alum should be added after the waste mixture and Envirostone have been thoroughly blended for a minimum of 5 minutes.Remove the solidified sample from the sample container and visually examine it for evidence of soft, porous or unsolidified areas.The solidified samples should be hard, homogeneous and of uniform coloration.

2.11,Set sample(s)aside for future disposal.2.12 2'3 If a satisfactory sample solidification cannot be obtained using the waste oil/water(or Boric Acid)/emulsi-fier/cement mixture for 504 solidification efficiency, as listed in Steps 2.4 through 2.7 above, repeat the sample.solidification using the formulas for 454 solidification efficiency as listed below: 114 ml of oil 59.6 ml of water (or Boric Acid)12.7 ml of emulsifier 146 gms of cement If a satisfactory.sample solidification cannot be obtained, the operator shall refer to Section 6.2.4 and contact the Customer Service Manager before proceeding.

3-0 PULL SCALE SOLIDIFXCATXONS 3.1 3.2 After a satisfactory sample solidification has been performed, determine the appropriate amount of Retarder (if applicable) and cement to be added to the full scale liner solidification using the Solidification Worksheet.

After determining the appropriate volumes of chemicals and cement to be added to the Liner, the full scale solidification should be performed..using the.system operating procedure (Reference 2.4), and the Solidification Operations Logsheet should be filled out.4 of 9

~,

)PT-51-WS, Rev.10 (Addendum D)SAMPLE VERIFICATION MORKSHEET FOR SOLIDIFICATION OF OIL May 21, 1992 Page 1 of 2 Operator: Utility/Location:

Date: No.: Waste Type: Waste Sample From/By: Waste Temperature:

F Waste pH: Sample Rad Level: Physical Characteristics (viscosity, color, sedimentation, clarity, etc.): 0'ample Proportions:

Waste Oil Sample Water (or Boric Acid concentrations up to 24 wt4)Added to Sample Emulsifier Added to Sample Chemical Additives mL mL Cement If applicable, blend the oil, water (or Boric Acid)and emulsifier together thoroughly before adding cement.Retarder and other chemical Additives should be added, if needed, and thoroughly blended in before adding cement.Accelerator, if needed, should be added after the waste and cement have been thoroughly mixed for a minimum of 5 minutes.Blend the required volume of cement into the waste and record the time the addition starts: Record the time when the mixture viscosity increases to the point when the mixer is secured: (1)Record the time when the mixture is firm to the touch: (2)5 of 9

R May 21, 1992 PT-51-WS, Rev.10 (Addendum D)SAMPLE VERIFICATION WORKSHEET FOR SOLIDIFICATION OF OIL Page 2 of 2 Sample Results: Mix time (1): Setup time (2): Free Water (or Boric Acid), if any: Relative set (soft, firm, very hard): Observations:

minutes minutes Sample proportions and solidification results acceptable for cal-culation of large scale solidification ratios: yes no Isotopic results of sample: Solidification Efficiency (Waste Volume/Solidified Volume: Operator Signature:

Date: Utility Representative Signature:

Title: Date: 6 of 9

PT-51-WS, Rev.10-(Addendum D)SOLIDIFICATION-WORKSHEET FOR SOLIDIFICATION OF OIL May 21,.1992."-'-Page 1 of 2 Operator: Utility/Location:

Waste Type: Date: No.: Satisfactory Sample Verification No: Solidification Efficiency:

Date: Container Model: SEE THE LINER DATA SHEET FOR THE LINER BEING USED Usable Liner Volume (with 2" safety margin): Oil Volume to be Added to Liner: Oil Height in liner: cf cf Water (Boric Acid)to be added to the Liner (Use the values determined from the Sample Verification Worksheet):

ml of water (or Boric Acid)in sample/ml of oil in sample inches of oil to be added to the liner inches of Water (or Boric Acid)to be added to the Liner.Oil Height in.-.Inches of Water (or Boric Acid)in.in.Hgt of Water (and Oil)in Liner (Water Level aetpoint)Emulsifier to be Added to the Liner (use the values determined from the Sample Verification Worksheet) ml of Emulsifier in Sample/ml of Oil in Sample cf of oil to be Added to the Liner x 7.48 Gallons of Emulsifier to be added to the Liner DRY CHEMICAL ADDITIVES Chemical Additive: Weight of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

gms chemical in sample/gms cement in sample lbs cement to be added to the liner=Additive lbs Chemical 7 of 9

PT-51-WS, Rev.10 (Addendum D)SOLIDIFICATION WORKSHEET FOR SOLIDIFICATION OF OIL Hay 21 1992"*Page 2 of 2 Chemical Additive: Weight of Chemical to be added to the liner.(use the values from the Sample Verification Worksheet):

gms chemical in sample/gms cement in sample lbs cement to be added to the liner lbs Chemical Additive WET CHEMICAL ADDITIVES Chemical Additive: Volume of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

ml chemical in sample/ml waste in sample x 7.48=cf waste to be added to the liner gallons Chemical Additive Chemical Additive: Volume of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

I ml chemical in sample/ml waste in sample cf waste to be added to the liner x 7.48=gallons Chemical Additive Weight of cement to be Added to the Liner: gms of cement in sample/ml of Oil in sample x 8.34=lbs of cement/gallon of Oil gallons of Oil to be added to the Liner lbs of cement to be added to the Liner NOTE: Cement weight may be rounded up to the next 100 pound increment, thus allowing full 100 pound bags of cement, to be added to container.

8 of 9

PT-51-WS, Rev.10 (Addendum D)SOLIDIFICATION OPERATXONS LOGSHEET OIL SOLIDXFXCATION May 21, 1992 Operator: Utility/Location:

Waste Type: Waste From: Solidification Worksheet No: Date: No.: Oil Volume Added to Liner: Time Completed:

Height of Oil: Inches from Inside Bottom of Liner Water (or Boric Acid)Volume Added to Liner: Time Completed:

Height of Water (or Boric Acid)and Oil: Inside Bottom of Liner A Emulsifier Volume Added to Liner: Time Mixer Started: Inches from Time Completed:

RPM: Wet Chemicals Added (List): gal gal Dry Chemicals Added (List): lbs lbs time completed time completed time completed time completed Cement Added: Accelerator Added: lbs: Time Added: Complete: lbs: Time Added: Mixer Hydraulic Pressure: PSI Time Time Mixer Secured: Waste Setup Time: Time Fillhead Removed: Time Liner Capped: Only Cap Liner With Utility Representative's Approval: Comments and Observations:

Date Liner Shipped/Shipment Number: Operator Signature:

Utility Representative Signature:

Title: Date: Date: 9 of 9

PT-51-WS, Rev.10 (Addendum E)May 21, 1992 ADDENDUM E PROCESS CONTROL PROGRAM FOR SOLIDIFICATION OF BEAD RESINS AND BORIC ACID OR CLASS A GRAKJLAR ACTIVATED CARBON AND BORIC ACID 1 of 9

PT-51-WS, Rev.10 (Addendum E)1.0 PREREQUISITES May 21, 1992 1.1 A sample solidification shall be performed before attempting to perform a full=scale.-:liner:solidification-;

1.2 The WSG operator shall ensure that a Radiological Work Permit has been issued for the performance of the sample verification activity and that adequate personnel monitoring and radiation detection equipment is on hand.1.3 The WSG operator shall ensure that all necessary materials and equipment are on hand prior to beginning the sample verification.

Suggested equipment and materials for the test are as listed below: NOTE: 6-300 to 500 mL plastic beakers 6-mixing spatulas 1-500 gram capacity scale 50 g-pH Adjustment Additive (Example: Boric Acid, Calcium Hydroxide, etc.)100 g-Anhydrous Sodium Metsosilicate (Metso)10 g-Red Top Retarder or equivalent 1000 g-Envirostone 20 g-Accelerator, Alum or equivalent (if required)1000 g-Portland Type I or II Cement The waste and chemicals used to solidify the sample waste must be from the same containers or lot numbers to be used in the full scale solidification.

1.4 A one-liter sample shall be taken for solidification in the laboratory from the bead resin tank and from the boric acid tank.Due to the importance of obtaining a representative sample for use in the verification procedure, the operator shall confirm that the contents of the waste form to be solidified have been adequately mixed and that the sample is a part of a homogeneously mixed waste batch.2.0 SAMPLE VERIFICATION 2.1 Record the initial pH, radiation level and temperature of the waste samples.2.2 Provide a waste sample (size to be specified by the plant)to the plant staff for isotopic analysis.2.3 Place a 200 ml sample of dewatered bead resins or gran-ular activated carbon in the beaker.NOTE: If the ratio of Boric Acid to bead resin or carbon is to be increased;-

calculate'the proper ratios on the work sheet included in this addendum.2 of 9

PT-51-WS, Rev.10 (Addendum E)Hay 21, 1992 2.4 Add 24 wt4 (max.)boric acid at 180 F until the liquid level is at oi'lightly above the resin or activated carbon level.2.5 Add the appropriate chemical additive, if required, to adjust the pH to between 2 and 6.2.6 Add 0.1 grams retarder (Red Top), if reguired.2.7 Thoroughly blend the waste and record the time when finished.2.8 2.9 NOTE: 2.10 2'1 2.12 Add 25 g of Anhydrous Sodium Metsosilicate to the waste'sample and mix until dissolved.

Add 117 g of cement to the 200 ml waste sample and mix the sample until the mixture begins to thicken.Record the time from the start of adding the cement to the.time that the mixture thickens such that mixing is no longer required (mix time)and the time from the start of adding the cement to the time that the waste is firm to the touch (setup time).Additional cement can be added if necessary to achieve a satisfactory end product.However, if additional cement must be added, the waste solidification efficiency must be redetermined and the waste volume to'be added to the solidification liner may have to be adjusted.Steps 2.10 and 2.11 apply only if Envirostone cement is the solidification agent used.If Portland Cement is used, skip to Step 2.12.If the waste setup time is less than 30 minutes if a 50 cubic foot liner is being used, is less than 60 minutes if a 142 cu ft liner is being used, or is less than 90 minutes if a larger liner is being used, add 0.05 g of Red Top Retarder to the 200 ml waste sample to adjust the waste setup time.Vary the amount of retarder added to the sample until the desired setup time is achieved.If the waste setup time is longer than operationally desired, add accelerator to the 200 ml waste sample at a rate of Accelerator Wt=1.04 of Envirostone Wt to adjust the waste setup time to the maximum time.Increase the amount of accelerator to the sample until the desired setup time is achieved.Remove the solidified sample from the sample container and visually examine it for evidence of soft, porous or unsolidified areas.The solidified samples should be hard, homogeneous and of uniform coloration.

3 of 9 L

PT-51-WS, Rev.10-(Addendum E)May 21, 1992 2.13 Set sample(s)as'ide"for future disposal.2.14 3.0 FULL Continue to mix samples until a satisfactory waste product is produced.If a satisfactory sample cannot be obtained, the operator shall refer to Section 6.2.4 and contact the Customer Service Manager before proceeding.

SCALE SOLXDXPXCATXONS 3.1 3.2 After a satisfactory sample solidification has been performed, determine the appropriate amount of additives and cement to be added to the full scale liner solidification using the Solidification Worksheet.

After determining the appropriate volumes to be added to the Liner, the full scale solidification should be performed using the system operating procedure (Reference 2.4), and the Solidification Operations Logsheet should be filled out.4 of 9

,"~4 0 5-~v'5pyX~~$4' May 21;1992 PT-51-WS, Rev.10 (Addendum E)SAMPLE VERIFICATION WORKSHEET FOR SOLIDIFICATION OF BORICACID AND BEAD RESINS Operator: Utility/Location:

Date: Page 1 of 2 No.: Waste Type: Waste Sample From/By: Waste Temperature:

F Waste pH: Sample Rad Level: Physical Characteristics (viscosity, color, sedimentation, clarity, etc.): Sample Proportions:

Bead Resin or Granular Activated Carbon-Dewatered Boric Acid-24 wt 4 Chemical Additives Final pH Cement Accelerator (if required)Blend the waste thoroughly (with pH adjustment additives, retarder, or conditioners, if required)and record the time when finished: Blend the required volume of cement into the waste and recor'd the time when finished: Record the time when the mixture viscosity increases to the point when the mixer is secured: (1)Record the time when the mixture is firm to the touch: (2)5 of 9 at A Irlt 9' PT-51-WS, Rev.10 (Addendum E)May 21, 1992 SAMPLE VERIFICATION WORKSHEET FOR SOLIDIFICATION OF BORIC ACID AND BEAD RESINS Page 2 of 2 Sample Results: Mix time (1): Setup time (2): minutes minutes Free Water, if any: Relative set (soft, firm, very hard): Observations:

Sample proportions and solidification results acceptable for calculation of large scale solidification ratios: yes no Isotopic results of sample: Solidification Efficiency (Waste Volume/Solidified Volume): Operator Signature:

Date: Utility Representative Signature:

Title: Date: 6 of 9 I l ,4" PT-51-WS, Rev.10 (Addendum E)P~y 21, 1992 SOLIDIFICATION WORKSHEET FOR SOLIDXFICATION OF BORIC ACXD AND BEAD RESXN--Page 1 of 2 Operator: Utility/Location:

Waste Type: Date: No.: Satisfactory Sample Verification No.: Solidification Efficiency:

Container Model: Date: SEE THE LINER DATA SHEET FOR THE LXNER BEING USED Usable Liner Volume (with 2" safety margin): Volume-Bead Resin or Activated Carbon: Volume-Boric Acid (43~Bead Vol.): Waste Height in Liner: Total Waste Volume added to Liner: (Bead Resin Volume&Boric Acid Volume)cf cf cf in cf Weight of cement to be Added to the Liner (Use the values deter-mined from the Sample Verification Worksheet):

gms of cement in sample/ml of waste in sample x 62.38 lbs of cement/cf of Waste cf of waste to be Added to the Liner lbs of cement to be added to the liner.NOTE: Cement weight may be rounded up to the next 100 pound increment thus allowing full 100 pound bags of cement to be added to container.

DRY CHEMICAL ADDITIVES Chemical Additive: Weight of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

gms chemical in sample/gms cement in sample lbs cement to be added to the liner lbs Chemical Additive 7of9 P;j 0 May 21, 1992 PT-51-WS, Rev.10 (Addendum E)SOLIDIFICATION.

WORKSHEET FOR SOLIDIFICATION OF BORIC ACID AND BEAD RESIN Page 2 of 2 Chemical Additive: Weight of Chemical to be added to the liner (use the values from the Sample Verification Worksheet):

gms chemical in sample/gms cement in sample lbs cement to be added to the liner lbs Chemical Additive WET CHEMICAL ADDITIVES Chemical Additive: Volume of chemical to be added to the liner (use the values from the Sample Verif ication Worksheet):

ml chemical in sample/ml waste in sample cf waste to be added to the liner x 7.48=gallons Chemical Additive Chemical Additive: Volume of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

ml chemical in sample/-ml waste in sample cf waste to be added to the liner x 7.48=gallons Chemical Additive Operator Signature:

Date: Utility Representative Signature:

Title: Date: 8 of 9 0

..PT-51-ÃS, Rev.10 (Addendum E)SOLIDIFICATION OPERATIONS LOGSHEET May 21, 1992 Operator: Utility/Location:

Liner Serial No.: I Waste Type: Waste From: Solidification Worksheet No: Waste Volume Added: cf: Date: No.: Time Completed:

Height of Waste:-Time Mixer Started: Wet Chemicals Added (List): gal gal Dry Chemicals Added (List): lbs lbs In.From Inside Bottom of Liner Hydraulic Press: time completed time completed time completed time completed Waste Conditioner Added: Type: lbs: Time: Cement Added: lbs: Time Started: Complete: Mixer Hydraulic Pressure PSI Time Time Mixer Secured: Waste Setup Time: Time Fillhead Removed: Time Liner Capped: Only Cap Liner With Utility Representative's Approval: Comments and Observations:

Date Liner Shipped/Shipment Number: Operator Signature:

Utility,representative Signature:

Title: Date: Date: 9 of 9

PT-51-WS, Rev.10 (Addendum F)May 21, 1992 ADDENDUM F PROCESS CONTROL PROGRAM FOR SOLIDIFICATION OF BORIC ACID 1of 9

~IP<<1, tL PT-51-WS, Rev.10 (Addendum F)May 21, 1992 1.0 PREREQUISITES 1.1 A sample solidification shall be performed before attempting to perform a full-scale liner solidification.

1.2 The WSG operator shall ensure that a Radiological Work Permit has been issued for the performance of the sample verification activity and that adequate personnel monitoring and radiation detection equipment is on hand.1.3 The WSG operator shall ensure that all necessary materials and equipment are on hand prior to beginning the sample verification.

Suggested equipment and materials for the test are as listed below: NOTE: 6-300 to 500 mL plastic beakers 6-mixing spatulas 1-500 gram capacity scale 50 g-pH Adjustment Additive (Example: Boric Acid, Calcium Hydroxide, etc.)100 g-Anhydrous Sodium Metsosilicate (Metso)'10 g-Red Top Retarder or equivalent 1000 g-Envirostone 20 g-Accelerator, Alum or equivalent (if required)1000 g-Portland Type I or II Cement The waste and chemicals used to solidify the sample waste must be from the same containers or lot numbers to be used in the full scale solidification.

1.4 A one-liter sample shall be taken for solidification in the laboratory from the boric acid tank.Due to the importance of obtaining a representative sample for use in the verification procedure, the operator shall confirm that the contents of the waste form to be solidified have been adequately mixed and that the sample is a part of a=homogeneously mixed waste batch.2.0 SAMPLE VERIFICATION 2.1 2.2 Record the initial pH, radiatio'n level and temperature of the waste samples.-Provide a waste sample (size to be specified by the plant)to the plant staff for isotopic analysis.2.3 Place a 200 ml sample of 24 wt4 (max.)boric acid at 180 F in the beaker.2.4 Add the appropriate chemical additive, if required, to adjust the pH to between 2 and 6.2 of 9

PT-Sa-WS, Rev.10 (Addendum F)Hay 21, 1992 2.5 2.6 Add 0.1 grams retarder, (Red,Top), if required.Thoroughly blend the waste and record the time when finished.2.7 NOTE: 2.8 2.9 2'0 Add 162 g of cement to the 200 ml waste sample and mix the sample until the mixture begins to thicken.Record the time from the start of adding the cement to the time that the mixture thickens such that mixing is no longer required (mix time)and the time from the start of adding the cement to the time that the waste is firm to the touch (setup time).Additional cement can be added if necessary to achieve a satisfactory end product.However, if additional, cement must be added, the waste solidification efficiency must be redetermined and the waste volume to be added to the solidification liner may have to be adjusted.Steps 2.8 and 2.9 apply only if Envirostone cement is used as the solidification agent.If Portland cement is used, skip to Step 2.10.If the waste setup time is less than 30 minutes if a 50 cubic foot liner is being used, is less than 60 minutes if a 142 cu ft liner is being used, or is less than 90 minutes if a larger liner is being used, add 0.05 g of Red Top Retarder to the 200 ml waste sample to adjust the waste setup time to the minimum time requirement for the liner size being used.Vary the amount of retarder added to the sample until the desired setup time is achieved.If the waste setup time is longer than operationally desired, add accelerator to the 200 ml waste sample at a rate of Accelerator Wt=1.04 of Envirostone Nt to adjust the waste setup time to the maximum time.Increase the amount of accelerator to the sample until the desired setup time is achieved.Remove the solidified sample from the sample container and visually examine it for evidence of soft, porous or unsolidified areas.The solidified samples should be hard, homogeneous and of uniform coloration.

2.11 Set sample(s)aside for future disposal.2.12 Continue to mix samples until a satisfactory waste product is produced.If a satisfactory sample cannot be obtained, the operator shall refer to Section 6.2.4 and contact the Customer Service Manager before proceeding.

3 of 9 e PT-51-WS, Rev.10 (Addendum F)May 21, 1992 3.0 PULL SCALE SOLIDIPICATIONS 3.1 After a satisfactory sample solidification has been performed, determine the appropriate amount of additives and cement to be added to the full scale liner solidification using the Solidification Worksheet.

3.2 After determining the appropriate volumes of additives and cement to be added to the Liner, the full scale solidification should be performed using the system operating procedure (Reference 2.4), and the Solidification Operations Logsheet should be filled out.4 of 9 0,

PT-51-WS, Rev.10 (Addendum F)SAMPLE VERIFICATION FORESHEET FOR SOLIDIFICATION OF BORIC ACID May 21, 1992 Page 1 of 2 Operator: Utility/Location:

Waste Type: Waste Sample From/By: Date: No.: Waste Temperature:

F Waste pH: Sample Rad Level: Physical Characteristics (viscosity, color, sedimentation, clarity, etc.): Sample Proportions:

Boric Acid-24 wt 4 Chemical Additives Final pH Cement Accelerator (if required)Blend the waste thoroughly (with pH adjustment additives, retarder, or conditioners, if required)and record the time when finished: Blend the required volume of cement into the waste and record the time when finished: Record the time when the mixture viscosity increases to the point when the mixer is secured: (1)Record the time when the mixture is firm to the touch: (2)5 of 9 Jtl a Vl~i PT-51-WS, Rev.10 (Addendum F)May 21, 1992 SAMPLE VERIFICATION WORKSHEET FOR SOLIDIFICATION OF BORIC ACID Sample Results: Mix time (1): Setup time (2): minutes minutes Page 2 of 2 Free Water, if any: Relative set (soft, firm, very hard): Observations:

Sample proportions and solidification results acceptable for calculation of large scale solidification ratios:~es no Isotopic results of sample: Solidification Efficiency (Waste Volume/Solidified Volume): Operator Signature:

Date: Utility Representative Signature:

Title: Date: 6 of 9 I'P 0 PT-51-WS, Rev.10{Addendum F)SOLIDXFICATXON WORKSHEET FOR SOLIDIFICATION OF BORIC ACID May 21, 1992-'-'"-'Page 1 of 2 Operator: Utility/Location:

Waste Type: Date: No.: Satisfactory Sample Verification No.: Solidification Efficiency:

Container Model: Date: SEE THE LINER DATA SHEET FOR THE LXNER BEING USED Usable Liner Volume{with 2" safety margin): Waste Volume: cf cf Waste Height in Liner: Weight of cement to be Added to the Liner (Use the values deter-mined from the Sample Verification Worksheet):

gms of cement in sample/ml of waste in sample x 62.38 lbs of cement/cf of Waste cf of waste to be added to the liner lbs of cement to be added to the liner.NOTE.Cement weight may be rounded up to the next 100 pound increment thus allowing full 100 pound bags of cement to be added to container.

DRY CEGMECAL ADDITIVES Chemical Additive: Weight of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

gms chemical in sample/gms cement in sample lbs cement to be added to the liner lbs Chemical Additive 7 of 9 Cs1 e s May 21, 1992 PT-51-WS, Rev.10 (Addendum F)~..SOLIDIFICATION,WORKSHEET FOR SOLIDIFICATION OF BORIC ACID Page 2 of 2 Chemical Additive: Weight of Chemical to be added to the liner (use the values from the Sample Verification Worksheet}:

gms chemical in sample/gms cement in sample lbs cement to be added to the liner lbs Chemical Additive WET CHEMICAL ADDITIVES Chemical Additive: Volume of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

ml chemical in sample/ml waste in sample x 7.48 cf waste to be added to the liner gallons Chemical Additive Chemical Additive: Volume of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

ml chemical in sample/ml waste in sample x cf waste to be added to the liner x 7.48 gallons Chemical Additive Operator Signature:

Date: Utility Representative Signature:

Title: Date: 8 of 9 I*'FIC T-51-WS, Rev.10 (Addendum F)SOLIDIFICATION OPERATIONS LOGSHEET Hay', 1992 Operator: Utility/Location:

Liner Serial No.: Waste Type: Waste From: Solidification Worksheet No: Waste Volume Added: cf: Date: No.: Time Completed:

Height of Waste: Time Mixer Started: Wet Chemicals Added (List): gal gal Dry Chemicals Added (List): lbs lbs In.Prom Inside Bottom of Liner Hydraulic Press: time completed time completed time completed time completed Cement Added: lbs: Time Started: Complete: Mixer Hydraulic Pressure PSI Time Time Mixer Secured: Waste Setup Time: Time Pillhead Removed: Time Liner Capped: Only Cap Liner With Utility Representative's Approval: Comments and Observations:

Date Liner Shipped/Shipment Number: Operator Signature:

Date: Utility Representative Signature:

Title: Date: 9 of 9

PT-51-WS, Rev.10 (Addendum G)May 21, 1992 ADDENDUM G PROCESS CONTROL PROGEQA FOR SOLIDIFICATION OF BEAD RESINS OR CLASS A GRANULAR ACTIVATED CARBON 0'

t PT-51-WS, Rev.10 (Addendum G)1.0 PREREQUISITES May 21, 1992 1.1 A sample solidification shall be performed before attempting to perform a full scale liner solidification.

1.2 The WSG operator shall ensure that a Radiological Work Permit, has been issued for the performance of the sample verification activity and that adequate personnel monitoring.and radiation detection equipment is on hand.1.3 The WSG operator shall ensure that all necessary materials and equipment are on hand prior to beginning the sample verification.

" Suggested equipment and materials for the test are as listed below: NOTE: 6-300 to 500 mL plastic beakers 6-mixing spatulas 1-500 gram capacity scale 50 g-pH Adjustment Additive (Example: Boric Acid, Calcium Hydroxide, etc.)100 g-Anhydrous Sodium Metsosil'icate (Metso)10 g-Red Top Retarder or equivalent (if required)1000 g-Envirostone 20 g-Accelerator, Alum or equivalent (if required)1000 g-Portland Type I or II Cement The waste and chemicals used to solidify the sample waste must be from the same containers or lot numbers to be used in the full scale solidification.

1.4 A one-liter sample shall be taken for solidification in the laboratory from the storage tank or solidification liner.Due to the importance of obtaining a represen-tative sample for use in the verification procedure, the operator shall confirm that the contents of the waste form to be solidified have been adequately mixed and that the sample is a part of a homogeneously mixed waste batch.2-0 SAMPLE VERIFICATION 2.1 Record the initial pH, radiation"level and temperature of the waste samples.2.2 Provide a waste sample (size to be specified by the plant)to the plant staff for isotopic analysis.2.3..Place a 200-ml sample of dewatered bead.resins or granular activated carbon in the beaker.--.

2 of 9 l,l PT-51-WS, Rev.10 (Addendum G)May 21, 1992 2.4 Add water until the liquid level is at or slightly above the resin or activated carbon level.2'Add the appropriate chemical additive, if required, to adjust the pH to between 2 and 6.2.6 Add 0.1 grams retarder (Red Top), if required.2.7 Add 25 g of Anhydrous Sodium Metsosilicate, if required.2.8 Thoroughly blend the waste and record the time when finished.2.9 NOTE 2'0 2'1 2'2 Add 117 g of cement to the 200 ml waste sample and mix the sample until the mixture begins to thicken.Record the time from the start of adding the cement to the time that the mixture thickens such that mixing is no"longer required (mix time)and the time from the start of adding the cement to the time that, the waste is firm to the touch (setup time).Additional cement can be added if necessary to achieve a satisfactory end product.However, if additional cement must be added, the waste solidification efficiency must be redetermined and the waste volume to be added to the solidification liner may have to be adjusted.Steps 2.10 and 2.11 apply only if Envirostone is the solidification agent used.If Portland Cement is used, skip to Step 2.12.If the waste setup time is less than 30 minutes if a 50 cubic foot liner is being used, is less than 60 minutes if a 142 cu ft liner is used, or is less than 90 minutes if a larger liner is being used, add 0.05 g of Red Top Retarder to the 200 ml waste sample to adjust the waste setup time to the minimum time requirement for the liner size being used.Vary the amount of retarder added to the sample until the desired setup time is achieved.If the waste setup time is longer than operationally desired, add accelerator to the 200 ml waste sample at a rate of Accelerator Wt=1.04 of Envirostone Nt to adjust the waste setup time to the maximum time.Increase the amount of accelerator to the sample until the desired setup time is achieved.Remove the solidified sample from the sample container and visually examine it for evidence of soft, porous or unsolidified areas.The solidified samples should be hard, homogeneous and of uniform coloration.

2.13 Set sample(s)aside for future disposal.3 of 9

PT-51-WS, Rev.10 (Addendum G)May 21, 1992 Vi 2.14 Continue to mix samples-until" a"satisfactory waste product is produced.If a satisfactory sample cannot be obtained, the operator shall refer to Section 6.2.4 and contact the Customer Service Manager before proceeding.

3.0 FULL SCALE SOLIDIFICATIONS 3.1 After a satisfactory sample solidification has been performed, determine the appropriate amount of additives and cement to be added to the full scale liner solidification using the Solidification Worksheet.

3.2 After determining the appropriate volumes of additives and cement to be added to the Liner, the full scale solidification should be performed using the system operating procedure (Reference 2.4), and the Solidification Operations Logsheet should be filled out.

PT-51-WS, Rev.10 (Addendum G)SAMPLE VERIFICATION WORKSHEET FOR SOLIDIFICATION OF BEAD RESINS OR GEVQ4ULAR ACTIVATED CARBON May 21, 1992 Page 1 of 2 Operator: Utility/Location:

Waste Type: Waste Sample From/By: Date: No.: Waste Temperature:

F Waste pH: Sample Rad Level: Physical Characteristics (viscosity, coloi, sedimentation, clarity, etc.): Sample Proportions:

Bead, Resin or Activated Carbon Chemical Additives Final pH Cement Accelerator (if required)Blend the waste thoroughly (with pH adjustment additives, retarder, or conditioners, if required)and record the time when finished: Record the time when the mixture viscosity increases to the point when the mixer is secured: (1)Record the time when the mixture is firm to the touch: (2)Blend the required volume of cement into the waste and record the time when finished: 5of 9

~I~I l: 0 PT-51-WS, Rev.10 (Addendum G)SAMPLE VERIFICATION'ORKSHEET FOR SOLIDIFICATION OF BEAD RESINS OR GRANULAR ACTIVATED CARBON Hay 21, 1992 Sample Results: Mix time (1): Setup time (2): Free Water, if any: Relative set (soft, firm, very hard): Observations:

minutes minutes Page 2 of 2 Sample proportions and solidification results acceptable for calculation of large scale solidification ra ios:~es no Isotopic results of sample: Solidification Efficiency (Waste Volume/Solidified Volume): Operator Signature:

Date: Utility Representative Signature:

Title: Date: lA 4hk-" h~~e th A W 6 of 9

4 PT-51-WS, Rev.10 (Addendum G)SOLIDIFICATION"'WORKSHEET FOR SOLIDIFICATION OF BEAD RESINS OR GR2QGJLAR ACTIVATED CARBON May 21, 1992 Page 1 of 2 Operator: Utility/Location:

Waste Type: Date: No.: Satisfactory Sample Verification No.: Solidification Efficiency:

Container Model: Date: SEE THE LINER DATA SHEET FOR THE LINER BEING USED Usable Liner Volume (with 2" safety margin): Waste Volume Beads or Carbon: Waste Height in Liner: cf cf in Weight of cement to be Added to the Liner (Use the values deter-mined from the Sample Verification Worksheet):

gms of cement in sample/ml of waste in sample x 62.38 lbs of cement/cf of Waste cf of waste to be added to the liner lbs of cement to be added to the liner.NOTE: Cement weight may be rounded up to the next 100 pound increment thus allowing full 100 pound bags of cement to be added to container.

DRY CHEMICAL ADDITIVES Chemical Additive: Weight of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

gms chemical in sample/gms cement in sample lbs'cement to be added to the liner lbs Chemical Additive 7 of 9 I.~9 II PT-51-WS, Rev=10"(Addendum G)May 21, 1992)SOLIDIFICATION WORKSHEET FOR SOLIDIFICATION OF BEAD RESINS OR GR2QAJLAR.

ACTIVATED CARBON Page 2 of 2 Chemical Additive: weight of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

gms chemical in sample/gms cement in sample lbs cement to be added to the liner lbs Chemical Additive WET CHEMICAL ADDITIVES Chemical Additive: Volume of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

ml chemical in sample/ml waste in sample x 7.48 cf waste to be added to the liner gallons Chemical Additive Chemical Additive: Volume of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

ml chemical in sample/ml waste in sample x 7.48 cf waste to be added to the liner gallons Chemical Additive Operator Signature:

Date: Utility Representative Signature:

Title: Date: 8 of 9

)PT-51-WS, Rev.10 (Addendum G)SOLIDIFICATION OPERATIONS LOGSHEET May 21, 1992 Operator: Utility/Location:

Liner Serial No.: Date: mo.: Waste Type: Waste From: Solidification Worksheet No: Waste Volume Added: cf: Time Completed:

Height of Waste: Time Mixer Started: Wet Chemicals Added (List): gal gal Dry Chemicals Added (List): lbs lbs In.From Inside Bottom of Liner Hydraulic Press: time completed time completed time completed time completed Cement Added: lbs: Time Started: Complete: Mixer Hydraulic Pressure PSI Time Time Mixer Secured: Waste Setup Time: Time Fillhead Removed: Time Liner Capped: Only Cap Liner With Utility Representative's Approval: 'omments and Observations:

Date Liner Shipped/Shipment Number: Operator Signature:

Date: Utility Representative Signature:

Title: Date: 9 of 9 PT-51-WS, Rev.10 (Addendum H)May 21, 1992 ADDENDUM H PROCESS CONTROL PROGRAM FOR SOLIDIFICATION OF POWDERED RESINS 1 of 9

PT-51-WS, Rev.10 (Addendum H)May 21, 1992 1.0 PREREQUXSXTES A sample solzdxfxcatxon shall be performed before attempting to perform a full scale liner solidification.

1.2 The WSG operator shall ensure that a Radiological Work Permit has been issued for the performance of the sample verification activity and that adequate personnel monitoring and radiation detection equipme:;t is on hand.1.3 The WSG operator shall ensure that all necessary materials and equipment are on hand prior to beginning the sample verification.

Suggested equipment and materials for the test are as listed below: NOTE: 6-300 to 500 mL plastic beakers 6-mixing spatulas 1-500 gram capacity scale 100 g-Anhydrous Sodium Metsosilicate (Metso)10 g-Red Top Retarder or equivalent (if required)1000 g-Envirostone 20 g-Accelerator, Alum or equivalent (if required)1000 g-Portland Type I or II Cement The waste and chemicals used to solidify the sample waste must be from the same containers or lot numbers to be used in the full scale solidification.

1.4 A one-liter sample shall be taken for solidification in the laboratory for each separate batch of waste to be processed.

The operator may choose to take the samples from the storage tanks to be solidified in the liner, or may take the sample from the liner directly, after the waste has been transferred to the liner.Due to the importance of obtaining a representative sample for use in the verification procedure, the operator shall confirm that the contents of the waste form to be solidified'have been adequately mixed and that the sample is a part of a homogeneously mixed waste batch.2.0 SAMPLE VERIFICATION 2.1 Record the information obtained during sample verifica-tion on the Sample Verification Worksheet.

2.2 Provide a waste sample (size to be specified by the plant)to the plant staff for isotopic analysis.2 of 9

PT-51-WS,.Rev.10 (Addendum H)May 21, 1992 2~3 2.4 2.5 2.6 2.7 Place a 200 ml sample of waste in a the beaker so that the resins are at the 200 ml level with the liquid solution just covering the resins.This will necessitate allowing the resins to settle, then pouring off some of the liquid solution.Record the initial pH, radiation level and temperature of the waste sample.Add tap water in order to bring the waste sample volume up to 253 ml.Add 25 g of Anhydrous Sodium Metsosilicate and mix until dissolved, if Portland Cement is to be used as the solidification agent.Add 93 g of cement to the 253 ml waste sample and mix the sample until the mixture begins to thicken.Record the time from the start of adding the cement to the time that the mixture thickens such that mixing is no longer required{mix time)and the time from the start of adding the cement to the time that the waste is firm to the touch (setup time).Additional cement can be added if necessary to achieve a satisfactory end product.However, if additional cement must be added, the waste solidification efficiency must be redetermined and the waste volume to be added to the solidification liner may have to be adjusted.NOTE: Steps 2.8 and 2.9 apply only if Envirostone Cement is used.If Portland Cement is used, skip to Step 2.10 2.8 2'If.the waste setup time is less than 30 minutes if a 50 cubic foot liner is being used, is less than 60 minutes if a 142 cu ft liner is being used, or is less than 90 minutes if a larger liner is being used,.add Red Top Retarder to the 200 ml waste sample at a rate of Retarder Wt=0.054 of Envirostone Wt to adjust the waste setup time to the minimum time requirement for the liner sire being used.Increase the amount of retarder added to the sample until the desired setup time is achieved.If the waste setup time is longer than operationally desired, add accelerator to the 200 ml waste sample at a rate of Accelerator Wt=1.04 of Envirostone Wt to adjust the waste setup time to the maximum time.Increase the amount of accelerator to the sample until the desired setup time is achieved.3 of 9 l'

PT-51-NS, Rev.10 (Addendum H)May 21, 1992 2.10 Continue to mix samples until a satisfactory waste product is produced.If a satisfactory sample cannot be obtained, the operator shall refer to Section 6.2.4 and contact the Customer Service Manager before proceeding.

2.11 Remove the solidified sample from the sample container and visually examine it for evidence of soft, porous or unsolidified areas.The solidified sample should be hard, homogeneous and of uniform coloration.

2.12 Set sample(s)aside for future disposal.3.0 FULL SCALE SOLIDIFICATION 3.1 After a satisfactory sample solidification has been performed, determine the appropriate amount of additives and cement to be added to the full scale liner solidification using the Solidification Worksheet.

3.2 After determining the appropriate volumes of additive and cement to be added to the Liner, the full scale solidification should be performed using the system operating procedure (Reference 2.4), and the Solidification Operations Logsheet should be filled out.4 of 9 PT-51-WS, Rev.10 (Addendum H)May 21, 1992 SAMPLE VERIFICATION WORKSHEET FOR SOLIDIFICATION OF PONDERED RESINS Page 1 of 2 Operator: Utility/Location:

Waste Type: Waste Sample From/By: Date: No.: Waste Temperature:

F Waste pH: Sample Rad Level: Physical Characteristics (viscosity, color, sedimentation, clarity, etc.): Sample Proportions:

Powdered Resin (Dewatered)

Volume with water added Chemical Additives Final pH Cement Accelerator'(if required)Blend the water added and any Chemical Additives thoroughly into the waste before adding the cement.Blend the required volume of cement into the waste and record the time the addition starts: Record the time when the mixture viscosity increases to the point when the mixer is secured: (1)Record the time when the mixture is firm to the touch: (2)5 of 9

PT-51-WS, Rev.10 (Addendum H)May 21, 1992 SAMPLE VERIFICATION WORKSHEET FOR SOLIDIFICATION OF POWDERED RESINS Page 2 of 2 Sample Results: Mix time (1): Setup time (2): Free Water, if any: Relative set (soft, firm, very hard): Observations:

minutes minutes Sample proportions and solidification results acceptable for calculation of lazge scale solidification ratios:~es no Isotopic results of sample: Solidification Efficiency (Waste Volume/Solidified Volume): Operator Signature:

Date: Utility Representative Signature:

Title: Date: en s Aw~6 of 9 PT-51-WS, Rev.10 (Addendum H), Nay 21,, 1992 SOLIDIFICATION WORKSHEET.-*FOR SOLIDIFICATION OF POWDERED RESINS Page 1 of 2 Operator: Utility/Location:

Waste Type: Date: No.: Satisfactory Sample Verification No.: Solidification Efficiency:

Container Model: Date: SEE THE LINER DATA SHEET FOR THE LINER BEING USED Usable Liner Volume (with 2" safety margin): Waste Volume: Waste Height in Liner: (Waste Full/Level Bubbler Tube to be set at this height)cf in Maximum Waste and Water Added Height in Liner: in (Waste&Water Added Level Bubbler Tube to be set at this Height)Weight of cement to be added to liner (Use the values determined from the Sample Verification Worksheet):

gms of cement in sample/ml of waste in sample x 62.38 lbs of cement/cf of Waste cf of waste (resin only)to be added to the liner lbs of cement to be added to the liner.NOTE: Cement weight may be rounded up to the next 100 pound increment thus allowing full 100 pound bags of cement to be added to container.

DRY C5&KKCAL ADDITIVES Chemical Additive: Weight of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

gms chemical in sample/gms cement in sample lbs cement to be added to the liner lbs Chemical Additive 7 of 9

'-61-WS, Rev.10: i,Addendum H}Hay 21, 1992 SOLIDIFICATION WORKSHEET FOR SOLIDIFICATION OF POWDERED RESINS Page 2 of 2 Chemical Additive: Weight of Chemical to be added to the liner (use the values from the Sample Verification Worksheet):

gms chemical in sample/gms cement in sample lbs cement to be added to the liner lbs Chemical Additive WET CHEMICAL ADDITIVES Chemical Additive: Volume of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

ml chemical in sample/ml waste in sample x 7.48 cf waste to.be added to the liner gallons Chemical Additive Chemical Additive: Volume of chemical to be added to the liner (use the values from the Sample Verification Worksheet):

ml chemical in sample/ml waste in sample x cf waste tc be added tc the liner x 7.48=gallons Chemical Additive Operator Signature:

Date: Utility Representative Signature:

l Title: Date: 8 of 9

PT-51-WS, Rev.10 (Addendum H)May 21, 1992 SOLIDIFICATION OPERATIONS LOGSHEET Operator: Utility/Location:

Liner Serial No.: Date: No.: Waste Type: Waste From: Solidification Worksheet No: Waste Volume Added: Height of Waste: Height of Waste&Water Added: Inside Bottom of Liner Time Mixer Started: Wet Chemicals Added (List): gal gal Dry Chemicals Added (List): lbs lbs cf: Time Completed:

In.From Inside Bottom of Liner Inches From Hydraulic Press: time completed time completed time completed time completed Cement Added: lbs: Mixer Hydraulic Pressure Time Started: PSI Complete: Time Time Mixer Secured: Time Pillhead Removed: Waste Setup Time: Time Liner Capped: Only Cap Liner With Utility Representative's Approval: Comments and Observations:

Date Liner Shipped/Shipment.

Number: Operator Signature:

Date: Utility Representative Signature:

Title: Date: 9 of 9