ML20246M793

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Rev 11 to Operating Procedure 1104-28I, Waste Solidification Process Control Program
ML20246M793
Person / Time
Site: Three Mile Island Constellation icon.png
Issue date: 03/09/1989
From: Mehler B
GENERAL PUBLIC UTILITIES CORP.
To:
Shared Package
ML20246M712 List:
References
1104-28I, NUDOCS 8909070251
Download: ML20246M793 (54)


Text

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l [. Nuclear ,,,_, Number

Operating Procedure 1104-28I l

Title Revision No. Waste Solidification Process Control Program 11 l

                                         ,                   Table of Contents Section                                                          Page 1.0 DISCUSSION                                                     4.0

2.0 REFERENCES

4.0 3.0 LIMITS AND PRECAUTIONS 5.0 4.0 TEST SOLIDIFICATION OF 4 TO 10 WT% BORIC ACID 6.0 (CONCENTRATED WASTE) 4.1 Prerequisites 6.0 4.2 Procedure 7.0 5.0 TEST SOLIDIFICATION OF > 10 TO 20 WT% BORIC ACID 9.0 (CONCENTRATED WASTE) 5.1 Prerequisites 9.0 5.2 Procedure 10.0 6.0 TEST SOLIDIFICATION OF WASTE OIL 13.0 6.1 Prerequisites 13.0 6.2 Procedure 13.0 7.0 TEST SOLIDIFICATION OF USED PREC0AT 15.0 7.1 Prerequisites 15.0 7.2 Precedures 16.0 8.0 TEST SOLIDIFICATION OF BEAD RESIN 18.0 8.1 Prerequisites 18.0 8.2 Procedure 19.0 9.0 ALTERNATE TEST SOLIDIFICATION PROGRAMS 22.0 9.1 Prerequisites 22.0 9.2 Procedure 22.0 2.0 1372c

             .                Nuclear                             TM1-i Operating Procedure            1104-28I
                                                ~

Title Revision No. Waste Solidification Process Control Program ') 8 s-Table of Contents (Cont'd) Section Pace 10.0 ACCEPTANCE CRITERIA 22.0 ATTACHMENT 1 Class A Unstable and Stable, Class B and C Test El-1 Solidification Data Sheet for 4 to 10 wt% Boric Acid ATTACHMENT 2 Solidification Calculation Sheet for 4 to 10 wt% E2-1 Bo-ic Acid ATTACHMENT 3 Class A Unstable and Stable Class B and C Test E3-1 Solidification Data Sheet for > 10 to 20 wt % Boric Acid , ATTACHMENT 4 Solidification Calculation Sheet for > 10 to E4-1 20 wt % Boric Acid ATTACHMENT 5 Class A Unstable and Stable, Class B and C Test E5-1 Solidification Data Sheet for Waste Oil ATTACHMENT 6 Solidification Calculation Sheet for Waste Oil E6-1 ATTACHMENT 7 Class A Stable Class B and C Test Solidification E7-1 Calculation Sheet for Used Precoat ATTACHMENT 8 Solidification Calculation Sheet for Used Precoat E8-1 ATTACHMENT 9 Class A Stable, Class B and C Test Solidification E9-1 Data Sheet for Bead Resin ATTACHMENT 10 Solidification Calculation Sheet for Bead Resin E10-1 ATTACHMENT 11 Test Solidification using Westinghouse - Hittman E11-1 Procedure FIGURE 1 Percent Solids of pH Adjusted Waste vs. Water / E12-1 Cement Ratio I i 3.0 1372c

t i ' Number Nuclear I ' L . THI-i Operating Procedure 1104-28I Title Revision No. Waste Solidification Process Control Program 8 1.0 DISCUSSION The purpose of the Process Control Program (PCP) for incontainer solidification l 1s to provide a program which will assure a solidified product with no free l standing liquid prior to transportation for disposal and which meets the re-quirements of 10 CFR 61.56. Haste Characteristics. The PCP's for each waste stream included in this procedure are based on labora-tory testing, the results of which are included in " Topical Report Cement Solidified Waste to Meet the Stability Requirements of 10 CFR 61" prepared by l Westinghouse - Hittman. These PCP's are valid for all liner types using elet-tric or hydraulic mixing heads provided by Hittman. The appropriate portions of this document shall be considered complete only when used with the operating procedures (OP 1104-28A for borated and oily wastes or OP 1104-28C for resini for full scale solidification. This document describes the methodology for determining the acceptable ratio of waste, cement and ^ additive that will result in an acceptable product for transportation and ultimately burial. The Solidification Data / Calculation Sheets convert these ratios into the recommended quantity of cement and additive that should be mixed with Class A unstable waste and the recommended quantity of cement and additive which must be mixed with Class A Stable and Class B or C wastes.

2.0 REFERENCES

2.1 Westinghouse - Hittman F421-P-004, Process Control Program for Incontainer Solidification of 4 to 20 wtt Boric Acid 2.2 Westinghouse - Hittman STD-P-05-002, Process Control Program for Incon-tainer Solidification of Oily Waste 2.3 Westinghouse - Hittman F421-P-006, Process Control Program for Incontainer Solidification of Powdered Resins 2.4 Westinghouse - Hittman F421-P-005, Process Control Program for Incontainer Solidification of Class A Unstable or Stable, Class B and C Resin at Maximum Packaging Efficiency 2.5 Westinghouse - Hittman STD-R-05-007 Topical Report Cement Solidified Waste to Meet the Stability Requirements of 10 CFR 61 2.6 Westinghouse - Hittman STD-R-05-Oll, Topical Report Mobile Incontainer Dewatering and Solidification System (MDSS) 2.7 NRC Letter from Charles E. Rossi, Assistant Director, Division of PWR Licensing-A to R.J. Leduc, Director of Engineering Westinghouse Hittman -

                             " Acceptance of Referencing of Licensing Topical Report STD-R-05-Oli.

Hittman Mobile Incontainer Dewatering and Solidification System (MDSS)", Dated Oct 31, 1986. 4.0 1372c

4UCl88r TMI-l Operating Procedure 1104-281 Title Revision No. Waste Solidification Process Control Program 8 2.8 Tech. Spec. Section 3.22.3, Solid Radioactive Watte 2.9 GPUN Radiation Protection Plan 3.0 LIMITS AND PRECAUTIONS 3.1 As required by Tech Spec 4.22.3.1.2, the PCP shall be used to verify the l solidification of at least one representative test specimen from at least every tenti batch of each type of wet radioactive waste (e.g., evaporator bottoms, o'ly waste, resin and precoat sludge). 3.2 For the purpose of the PCP a batch is defined as that quantity of waste required to fill a disposable liner to the appropriate level on the waste level indicator. 3.3 If any test specimen fails to solidify, solidification of the batch under test shall be suspended until such time as additional test specimens can be obtained, alternative solidification parameters can be determined in accordance with the Process Control Program, and a subsequent test veri-fles solidifi, cation Solidification of the batch may then be resumed using the alternate solidification parameters determined. I 3.4 If the initial test specimen from a batch of waste fatis to verify solidi-fication then representative test specimens shall be collected from each consecutive batch of the same type of waste until the three (3) consecu-tive initial test specimens demonstrate solidification. The Process Control Program shall be modified as required to assure solidification of i subsequent batches of waste. l l 3.5 For high activity wastes, such as spent resin or used precoat, where handling of samples could result in personnel radiation exposures which are inconsistent with the ALARA principle, representative non-radioactive samples will be tested. These samplef should be as close to the actual waste physical and chemical properties as possible. Typical expended mixed bed resin shall be used to simulate the spent bead resin and the appropriate mix of anion to cation powdered resin shall be used to simu-late used precoat. l 3.6 All Chemicals used to condition or solidify waste or simulated waste in solidification tests shall be the actual chemicals used in full scale solidification. 3.7 A Test Solidification Data Sheet will be maintained for each test sample solidified. Each Data Sheet will contain pertinent information of the test sample and the liner numbers solidified based on the test sample. 5.0 1372:

MUCIS8r THI-l Number Operatino Procedure 1104_281 Title Revision No. Waste Solidification Process Control Program 11 3.8 Samples should be drawn at least six hours prior to the planned full scale l- waste solidification to allow adequate time to complete the required testing and verification of solidification for Class A unstable waste. 28 i i hours should be allowed, if practical, for Class A stable, Class B and C wastes. 3.9 The tank containing the waste to be solidified should be mixed by recircu_ lating the tank contents for at least three volume changes prior to sampilng to assure a representative sample. 3.10 An RWP must be obtained and used for performing test solidification of radioactive samples. 4.0 TEST SOLIDIFICATION OF 4 TO 10 WT% BORIC ACID (CONCENTRATED WASTE)

                                                                                                                                    ~

4.1 Prerequisites NOTE: This PCP Test Solidification Procedure is applicable to Class A Unstable, Class A Stable, Class B and C Waste Forms. 4.1.1 A sufficient size sample of concentrated waste (approx. I liter) has been drawn and the following parameters analyzed for by Plant Chemistry:

  • Boron e pH
  • Total Solids a Gamma Scan NOTE: The total solids and gamma scan are used for information purposes only to track waste characteristics *nd are not to be used in the Process Control Program calculations.

4.1.2 The Ops Quality Assurance Group has been contacted to inform them of the pending Test Solidification to see if they care to witness the test. OQA Monitor Contacted Name / Date / Time 6.0 1372c

4 Nuclear ,,,_, number Operating Procedure 1104 28I Title Revision No. Waste Solidification Process Control Program 11 4.1'. 3 The appropriate portions of Attachment I have been completed including waste classificotton, chemistry information, balance calibration data and the sequential sample number. 4.2 Procedure NOTE: Tare weights of waste, cement, additives, etc. should be obtained during performance of the following procedure. Round off to the nearest gram. 4.2.1 Calculate the weight percent of Boric Acid on Attachment 1. 4.2.2 MEASURE 500 gms of untreated concentrated waste into a container. 4.2.3 RECORD the weight and volume on Attachment 1. 4.2.4 ADD 50 wt% sodium hydroxide (NaOH) to raise the pH between 8 to 8.5 for Class A unstable, Class A stable, B and C solidifica. tion. If pH is >8.5 then reduce to a range of 8 and 8.5 with l sulfuric acid. ' 4.2.5 RECORD the weight of NaOH Used and the adjusted pH on Attachment 1. 4.2.6 If large (i.e., foam causing) quantities of detergents are present TREAT the sample with an anti-foaming agent until the foam disappears. 4.2.7 RECORD the weight of anti foaming agent used on Attachment 1. 4.2.8 Determine if oil is present by looking for an oil film on the surface of the sample. If oil is present perform the following: ml (011) t ml (total sample) x 100  % 0.1

a. If oil is present in stable waste in a quantity greater i than 1% by volune, reduce the quantity of oil to less than 1% by skimming.
b. For unstable waste if oil is present and the volume is i between 3 and 12% of the volume of waste, TREAT with an emulsifying agent such as Maysol 776 (20% of the volume of oil). Oil in concentrations > 12% by volume may not be solidified by this procedure. (Refer to Section 6.0 Test Solidification of Waste 011).

7.0 1372c

                   $UCl$$7                                              TMI.1 Number
                                                          . Operating Procedure                1104 281 Title                                                                               Revision No.                      1 Waste Solidification Process Control Program                                              11
                                                                                                                            )
            .....>.__.. _____ _.._______... __..........._....__..___-______ ___..___....                                   l NOTE:                 The density of Maysol 776 is 1.0 g/ml; the volume in mi is                        i equal to the weight in grams.

4.2.9 RECORD the % oil and the quantity of any emulsifying agent used on Attachment 1. 4.2.10 Record the volume and calculate the weight of the treated Sample on Attachment 1. 4.2.11 Calculate the percent solids in the sample by completing items (9), (10), (11) and (12) in Section II of Attachment 1. 4.2.12 For the test solidification of the concentrated waste, measure into a mixing vessel 400 ml of pretreated waste. NOTE: Test solidification should be conducted using a 1,000 mi disposable beaker or similar size container. 4.2.13 RECORD the volume AND weight of the treated semple on Attachment 1. 4.2.14 Calculate the water in the tample by completing items (15), (16) and (17) in Section III of Attachment 1. 4.2.15 Using figure 1 and the percent solids from the Test Solidifica-tion Data Sheet, Item (12), DETERMINE the water / cement ratio then CALCULATE and WEIGH out the required quantity of Portland ! Type I cement. 4.2.16 RECORD the weight of cement on Attachment 1. 4.2.17 CALCULATE and WEIGH out the required quantity of metso beads, l 1.e., anhydrous sodium metas11tcate (ASMS), into a separate vessel. 4.2.18 RECORD the weight of ASMS on Attachment 1. 4.2.19 Slowly ADD the cement to the test sample while it is being mixed. NOTE: Mixing should be accomplished by stirring with an electric mixing motor with blade or manually with a rigid stirrer until a homogeneous mixture is obtained, approximately one minute. i 8.0 1372c O______-_-__-_-_-_-- _ _ _ -- -_ _- - - _ _ - - - - -

L UCl88r Number THI-l Operatino Procedure 1104_28I Title Revision No. Waste Solidification Process Control Program ,11-4.3.20 After all the cement is added, slowly ADD the ASMS to the test sample while it is being mixed. 4.2.21 After sufficient mixing (2 minutes after all the ASMS is added) so that a homogeneous mixture is obtained. SEAL the sample and CURE at 120 1 5'F for 24 hours for Class A Stable, Class B or C or at room temperature for Class A unstable. NOTE: If at any time during the 24 hour cure, the sample meets the acceptance criteria, the liner solidification may proceed. However, no test solidification shall be disqualified without at least 24 hours of cure. 4.2.22 Verify the Acceptance Criteria (Section 10) has been met and sign and date Attachment 1. ~ 4.2.23 When the Acceptance Criteria has been met per Section 10 calculate the required quantitles of cement and additives for the full scale solidification using a liner type applicable for this waste type (as determined by Radwaste Operations Engineer _ ing) and the Solidification Calculation Sheet for 4 to 10 wt% Boric Acid (Attachment 2). NOTE: The liner shall be solidified using OP 1104-28A, Radio active Waste Solidification Hittman. 4.2.24 Complete Section VII of Attachment 2 upon completion of the solidification if cement remains in the hopper. 5.0 TEST SOLIDIFICATION OF > 10 TO 20 wt1 BORIC ACID (CONCENTRATED WASTE) 5.1 Prerequisites NOTE: This PCP Test Solidification Procedure is applicable to Class A Unstable, Class A Stable, Class B and C Waste Forms. 9.0 1372c

kUCl$$7 , Number l TMI_1 1 Operatino Procedure 1104 28I Title Revision No. Haste Solidification Process Control Program 11

5. P.1 A sufficient size sample of concentrated wkste (approx. I liter) (

has been drawn and the following parameters analyzed for by Plant Chemistry: e Boron e pH

                                                                                             +     Total Solids
  • Gamma Scan NOTE: The total solids and gamma scan are used for information purposes orvly to track waste characteristics and are not .

to be used in the Process Control Program calculations. 5.1.2 The Ops Quality Assurance Group has been contacted to inform them of the pending Test Solidification to see if they care to witness the test. OQA Monitor Contacted Name / Date / Time 5.1.3 The appropriate portions of Attachment 3 have been completed including waste classification :hemistry information, balance calibration data and the sequential sample number. 5.2 Procedure

                                                   ...__________....__________________ ._____________._________________ ._____                                    i' NOTE:                                Tare weights of waste, cement, additives, etc. should be obtained during performance of the following procedure.

Round off to the nearest gram. 5.2.1 Calculate the weight percent of Boric Acid on Attachment 3. , I 5.2.2 MEASURE 500 gas of untreated concentrated waste into a container. j 5.2.3 RECORD the weight and volume on Attachment 3. 5.2.4 ADD 50 wt1 sodium hydroxide (NaOH) to raise the the pH between 12 and 12.5. If pH is > 12.5 then reduce to a range of 12 and 12.5 with sulfuric acid. 10.0 1372c j l _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ __ _ _ _ _ _ _ _ _ _ _ _ _ _ __ __ _ _ _ _ l

1 L l hCl$M ' TMI.1 Number l , Operating Procedure 1104 28I j Revision No. Title Waste Solidification Process Control Program 11 5.2.5 RECORD the weight of NaOH used and the adjusted pH on Attachment 3. 5.2.6 If large (i.e., foam causing) quantitles of detergents are i present, TREAT the sample with an anti. foaming agent. 5.2.7 RECORD the weight of anti-foaming agent used on Attachment 3. 5.2.8 Determine if oli is present by looking for an oil film on the surface of the sample. If oil is present perform the following: ml (011) *

                                                                           .m1 (total sample) x 100 -            % 0.1
a. If oli is present in stable waste in a quantity greater I than 1% by volume, reduce the quantity of oil to less than 1% by skimming,
b. For unstable waste if oil is present and the volume is i totween 3 and 12% of the volume of waste TREAT with an emaisifying agent such as Maysol 776 (20% of the volume of oil). Oil in concentrations > 12% by volume may not ta solicified by this procedure. (Refer to Section 6.0 Test Solidification of Waste 011).

NOTE: The density of Maysol 776 is 1.0 g/ml; the volume in m1 is equal to the weight in grams. 5.2.9 RECORD the % oil and the quantity of any emulsifying agent used on Attachment 3. 5.2.10 Record the volume and calculate the weight of the treated sample on Attachment 3. 5.2.11 Calculate the percent solids in the sample by completing items (9), (10), (11) and (12) in Section II of Attachment 3. 5.2.12 For the test solidification of the concentrated waste, measure into a mixing vessel 400 ml of treated waste. NOTE: Test solidification should be conducted using a 1,000 ml disposable beaker or similar size container. 5.2.13 RECORD the volume AND weight of the Fample on Attachment 3. 11.0 1372c

\

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MUCl88r TMI-l Number l Operating Procedure 1104-281 Title Revision No, Waste Solidification Process Control Program 11 i 5.2.14 Calculate the water in the sample by completing items (15), (16) and (17) in Section III of Attachment 3. 5.2.15 Using Figure I and the percent solids from the Test Solidifica. tion Data Sheet. Item (12), DETERMINE the water / cement ratio then CALCULATE and WEIGH out the required quantity of Portland Type I cement. 5.2.16 RECORD the weight of cement on Attachment 3. l 5.2.17 CALCULATE and WEIGH out the required quantity of anhydrous sodium metasilicate (ASMS) into a separate vessel. 5.2.18 RECORD the weight of ASMS on Attachment 3. 5.2.19 Slowly ADD the cement to the test sample while it is being m'ixed. NQl[: Mixing should be accomplished by stirring with an electric mixing motor with bladt or manually with a rigid stirrer until a homogeneous mixture is obtained, approximately one l PA nute . , 5.2.20 After all the cement is added, slowly ADD the ASMS to the test sample while it is being mixed. 5.2.21 After sufficient mlving (2 minutes after all the ASMS is added) so that a homogeneous mixture is obtained, SEAL the sample and CURE at 120 + 5'F for 24 hours for Class A Stable, Class B or C or at room temperature for Class A Unstable. NOTE: If at any time during the 24 hour cure, the sample meets the acceptance criteria, the liner solidification may proceed. .However, no test solidification shall be dis-qualified without at least 24 hours of cure. 5.2.22 Verify the Acceptance Criteria (Section 10.0) has been met and sign and date Attachment 3, 5.2.23 When the Acceptance Criteria has been met per Section 10, calculate the required quantitles of cement and additives for the full scale solidification using a liner type applicable for this waste type (as determined by Radwaste Operations Engineer-ing) and the Solidification Calculation Sheet for > 10 to 20 wt% Boric Acid (Attachment 4). 12.0 1372c j i

                              ; ENuclear                                          ,_,

number Operating Procedure 1104-281 Title Revision No. Waste Solidification Process Control Program 11 __.. 2_..__.__.___. .___.__..._______________ _______ __.________._ _-_____._ NOTE: The liner shall be solidified using OP 1104-28A, Radioactive Waste Solidification - Hittman. 5.2.24 Complete Section VII of Attachment 4 upon completion of the solidification if cement remains in the hopper. 6.0 TEST SOLIDIFICATION OF WASTE OIL (12 - 40% 011) 6.1 Prerequisites NOTE: This PCP Test Solidification Procedure is applicable to Class A Unstable, Class A Stable, Class B and C waste forms.. ________..______.____ __..._..n__..________-_____....____________ .__.-____ .. 5.1.1 A sufficient size sample (approx. 500 ml.) each of pH adjusted concentrated waste and waste oli have been drawn. l NOTE: The pH of the concentrated waste will be adjusted in the I tank before the test solidification. l 6.1.2 The Ops Quality Assurance Group has bsen contacted to inform them of the pending Test Solidification to see if they care to witness the test. 00A Monitor Contacted Name / Date / Time __ 6.1.3 A sequential sample number has been assigned to the test and included on Attachment 5. 6.1.4 A determination has been made as to the waste class of the pending full scale solidification by Radwaste Ops. EngU. sering. 6.1.5 The balance calibration data has been included on Attachment 5. 6.2 Procedure NOTE: Tare weights of waste, cement, additives, etc. should be obtained during performance of the following procedure. Round off to the nearest gram. 13.0 1372c

        ~

MUCIS8r THI-1 Number Operating Procedure 1104-281 Title Revision No. Waste Solidification Process Control Program 11 6.2.1 Measure into a mixing vessel 210 ml of concentrated waste and 140 ml oil.

                                           -------------------==                        -----------------------------------------------------

NOTE: Test solidification should be conducted using a 1000 ml disposable beaker or similar size container. 6.2.2 Record the waste volumes added and calculate the percent oil by volume on Attachment 5. 6.2.3 MEASURE out 28.0 ml (28.0 gms) of Maysol 776. 6.2.4 RECORD the quantity of the emulsifier on Attachment 5. 6.2.5 ADD the Maysol 776 to the waste and mix until a homogeneous mixture is obtained, at least five (5) minutes.

                                            '            NOTE:         Mixinr3 should be accomplished by stirring with an electric mixer with binde or manually with a rigid stirrer. Ary sigr,s of pure oil may be an indication that tha amui d cr.

is breaking down. Shovid this occur, contact Radw6ste Ops, Engineering for forther instructions.

                                           - - - - - - - - - . - - . . - - - . - - - - - ~ - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

6.2.6 if large (i.t., foam causing) quantitles 6f detergents are present, treat, the st:aple with anti-foaming agent u4til the foam disappears. 6.2.7 Record the amount ci anti-foaming agent used on Attachment 5. 6.2.8 MEASURE out 447.3 gms of Portland Type I cement and 51.8 gms of anhydrous sodium metasilicate (ASMS). 6.2.9 RECORD the quantities of cement and ASMS on Attachment 5. 6.2.10 Slowly ADD the cement to the test sample while it is being mixed and mix until a homogeneous mixture is obtained but in no case l 1ess than one (1) minute. l 6.2.11 After all the cement is added, slowly ADD the ASMS to the test sample while it is being mixed. 6.2.12 MIX for two (2) minutes after all the ASMS is added and homo-geneous mixture is obtained. 14.0 1372c L---__--- - _ _ - - - - - - - - - - - - -- -. - -

o UCl$$7 Number Opera'tino Procedure 1104-281 11tle Revision No. Haste Solidification Process Control Program 11 6.2.I'! Seal the sample and cure at 120 1 5'F for 24 hours for Class A Stable, Class B or C or at room temperature for Class A Unstable. NOTE: If at anytime during the 24-hour cure time, the sample meets the acceptance criteria, the liner solidification may proceed. However, no test solidification shall be disquallfled without at least 24 hours of cure. 6.2.14 Verify the Acceptance Criteria (Section 10.0) has been met and sign and date Attachment 5. 6.2.15 When the Acceptance Criteria has been met per Section 10, calculate the requiied quantities of cement and additives for. the full scale solidification using a liner type applicable for this waste type (as determined by Radwaste Operations Engineer _ ing) and the Solidification Calculation Sheet for Waste Oil (Attachment 6).

               ..........................._..~......-................................:..........

NOTE: The liner shai! be solidified using OP 1104_28A, Radioactive haste Solidification - Hittman. < 7.0 TEST SOLiO!FICATION OF USED PREC0AT 7.1 Prerequisites NOTE: This PCP Test Solidification Procedure is applicable to Class A Stable. Class B and C Waste Forms.

               ............. _ ..____ ........ ~..................................... ......

7.1.1 A sufficient size sample of used precoat (approx. 500 ml) has been drawn and the following parameters analyzed for by Plant Chemistry: l e pH (of sluice water) I e Gamma Scan NOTE. Where high activity waste could pose personnel radiation 1 exposure problems when performing the test solidification, l expended powdex with an appropriate anton/ cation ratio shall { 4 be substituted. The ratto shall be determined by Radwaste Operations Engin&ering. A small sample of use precoat (= 20 mis) shall be taken for isotopic analysis. 15.0 1372c

l l l[JHC)lllWll[' Number TMI 1 Operatino Procedure 1104-281 Title Revision No. Haste Solidification Process Control Program 11 ,,

                                                 .._-    1.........._...............--........_----............._.........___..._

NOTE: The gamma scan is to be used for information purposes only to track waste characteristics and is not to be used in the PCP calculations. l 7.1.2 The sample has set to verify 1 1% oli by volume. l 7.1.3 The Ops Quality Assurance Group has been contacted to inform them of the pending Test Solidification to see if they are to witness the test. 00A Monitor Contacted Name / Date / Time 7.1.4 The appropriate portions of Attachment 7 have been completed including the balance calibration data and the sequential sample number. l 7.2 Procedure NOTE. Tare weights of waste, ceeent, additives, etc. shocfd be obtained during performance of the following procedure. Round off to the nearest gram. 7.2.' MEASURE out 381.1 gms of dewatered powdeced resin and 151.5 gms of water and placa into separate containers. NOTE: Test solidification should be conducted using a 1,000 ml disposable beaker or similar size container. 7.2.2 RECORD the volume and weight of the powered resin on Attachment 7. 7.2.3 ADD the water to the powered resin and RECORD the weight of water added and the total volur.e of waste slurry (water plus resin) on Attachment 7. 7.2.4 If any foam is present, TREAT the sample with an anti-foaming agent. 7.2.5 RECORD the quantity of anti-foaming agent used on Attachment 7. 16.0 1372c

Muclear ,,_, nueer

        ~

Operating Procedere 1104 281 Title Revision No. Waste Solidificat!on Process Control Program 11 7.2.6 Determine if oil is present by looking ior an oil film on the surface of the sample. If oil is present perform the following: ml (011)

  • ml (total sample) x 100 -  % 0.1
a. If ot) is present and the volume is between 3 and 12% of i the volume of waste, TREAT with an emulsifying agent such as Maysol 776 (20% of the volume of oil). Oil in concentrations > 12% by volume may not be solidified by this procedure. Contact Radwaste Operations Engineering for guidance.

NOTE: The density of Maysol 776 is 1.0 gm/ml; the volume in mi is equal to the weight in gms. 7.2.7 RECORD the quantity of oil present and the amount of Maysol added to the sample on Attachment 7. 7,2.6 RECORD the initial pH of the sample on Attachment 7. 7.2.9 MEASURE out approximately 10 grams of calcium hydroxide Ca(CP)2, also known as hydrated lime. 7.2.10 Slowly ADD the ulcium hydroxtris to the powdered resin slurry, two (2) grams at a time. HIX for three (3) minutes between

                                          ~1dditions butil tSe pH is &t leatt 11 5. ADD an tdditional thrst (3) grams of calcium hydtcitide., ihls final addition M y or may not alter the pH of the slurry.

l . . . . . . . . . . , . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . l NOTE: Mixing should be arumplished by stirring with an electric l mixing motor with blade or manually with a rigid stirrer until a homogeneous mixture is obtained approximately one (1) minute. 1 1 7.2.11 RECORD the quantity of calcium hydroxide added to the slurry and the final pH on Attachment 7. 7.2.12 MEASURE out 444 gms of Portland Type 1 cement. 7.2.13 RECORD the amount of cement on Attachment 7. 7.2.14 Slowly ADD the rement to the test sample while it is being mixed. 17.0 1372c o

GUCIS8r 7,3 Number Operatino Procedure 1104-281 ___ Title Revision No. Waste Solidification Process Control Program 'll ._- 7.2.15 MIX for two (2) minutes after all the cement is added to obtain a homogeneous mixture. 7.2.16 RECORD the final sample volume on Attachment 7. 7.2.17 Seal and allow the sample to CURE for 24 hours at 120 1 5'F. NOTE: If at anytime during the C4-hour cure time. the sample meets the acceptance criteria, the liner solidification may proceed. However, no test solidification shall be dis-qualified without at least 24 hours of cure. 7.2.18 Verify the acceptance criteria (Section 10.0) has been met, sign and date Attachment 7. 7,2.19 When the Acceptance Criteria has been met per Section 10, calculate the required quantities of cement and additives using a liner type applicable for this waste type (as determined by Radwaste Operations Engineering) and the Solidification Calcula-tion Sheet for Used Precoat (Attachment 8). NOTE: The liner shall be solidified using OP 1104-28C, Primary Resin and Precoat Processing - Hittman. 8.0 TEST SOLIDIFICATION OF BEAD RESIN 8.1 Prerequisites NOTE: This PCP Test Solidification Procedure is appitcable to Class A Stable, Class 8 and C Waste forms. 8.1.1 A sufficient size sample of bead resin (approx. 500 mi) has been drawn and the following parameters analyzed for by Plant <Chemis-try: e pH (of slutte water) l e Gamma Scan l l 18.0 1372c

MUCl88r Tm_i

                                                                                           " "* b "

Operating Procedure 1104-251 litle Revision No. Haste Solidification Process Control Procram 9 ,, NOTE: Where high activity waste could pose personnel radiation exposure problems when performing the test solidification, expended non-radioactive resin shall be substituted. The source of this resin shall be determined by Radwaste Operations Engineering. A small sample of spent resin (= 20 mis) shall be taken for isotopic analysis. NOTE: The gamma scan is to be used for information purposes only to track waste characteristics and is not to be used in the PCP calculations. 1 8.1.2 The sample has set to verify < li oil by volume. . 8.1.3 Tne Ops Quality Assurance Group has been contacted to inform - them of the pending Test Solidification to see if they care t3 witriess the test. OQA Monitor Contacted Name / Date / lime 8.1.4 The appropriate portions of Attachment 9 have been completed i including the balance calibration data and sequential sample number. j 8.2 Procedure NOTE: Tare weights of haste, cement, addliives, etc. should be obtained during performance of the following procedure. Round off to the nearest gram. 8.2.1 MEASURE into a mixing vessel 240 gm of dewatered resin. __ .______.---._______...-_ .__-._-_________.-___.-______..... ..--_-_-_----_ { NOTE: Test solidification should be conducted using a 1,000 ml J disposable beaker or similar size container. NO.T E : Tap the beater gently to consolidate the resin prior to  ! measuring the volume. l I I t 19.0 1372c

t

                ~

Nuclear THI-I number l Operating Procedure 1104 28I d Title Revision No. Waste Solidification Process Control Program 11 I 8.f.2 RECORD the weight and volume of the sample (resin and water) on Attachment 9. I 8.2.3 HEIGH out 2.1 gms of EC_3 into a separate vessel. 8.2.4 RECORD the weight of EC_3 on Attachment 9. 8.2.5 WE!GH out 84.3 gms of water and record the weight on Attachment 9. 8.2.6 ADD the water to the vessel containing the EC-3 and mix thoroughly. 8.2.7 ADD the water /EC_3 mixture to the bead resin and mix thorougly. 8.2 8 If any foam is present, TREAT the sample with an anti-foaming agent. 8.2.9 RECORD the quantity of anti. foaming agent used on Attachment 9. 8.2.10 Determine if oil is present by looking for an oil film on the ( surface of the sample. If oil is present perform the following: 4 ml (011) ml (total sample) x 100 =  % 0.1 8

a. If oil is present and the volume is between 3 and 12% of the volume of waste, TREAT with an emulsifying agent such as Maysol 776 (20% of the volume of oil). Oil in concentrations > 12% by volume may not be solidtfled by this procedure. Contact Radwaste Operations Engineering for guidance.

NOTE: The density of Maysol 776 is 1.0 gm/ml; the volume in mi is equal to the weight in gms. 8.2.11 RECORD the quantity of oil and the volume of emulsifier used on Attachment 9. 8.2.12 RECORD the initial sample pH on Attachment 9. 8.2.13 MEASURE out approximately 11.5 gms of Calcium Hydroxide Ca(OH)2, also known as hydrated lime. 20.0 1372c L- _ _ _ .

                             @ M7 Number Operatino Procedure            1104 281 Title                                                                                         Revision No.

Haste Solidification Process Control Program 11 8.2.14 Slowly ADD the Ca(OH)2 to the resin sample two (2) grams at a time. Mix for three (3) minutes between additions until the pH of the slurry is at least 11.5. ADD three (3) additional gms of Ca(OH)2 This final additional may or may not alter the pH of the slurry. 8.2.15 RECORD the quantity of calcium hydroxide added to the slurry and the final pH on Attachment 9. 8.2.16 MEASURE out 178.2 gms of Portland Type I cement into a separate vessel. 8.2.17 RECORD the weight of the cement on Attachment 9. 8.2.18 Slowly ADD the cement to the test sample while it is being mixed. 8.2.19 MIX for two (2) minutes after all the cement is added to obtain a homogeneous mix. 8.2.20 RECORD the final sample volume on Attachment 9. 8.2.21 SEAL the sample and allow the sample to CURE for 24 hours at 120 1 5'F. NOTE: If at anytime during the 24-hour cure time, the sample meets the acceptance criteria, the liner solidification may proceed. However, no test solidification shall be dis-qualified without at least 24 hours of cure. 8.2.22 VERIFY the acceptance criteria (Section 10.0) has been met, sign and date Attachment 9. 8.2.23 When the Acceptance Criteria has been met per Section 10.0, CALCULATE the required quantities of cement and additives using a liner type applicable for this waste type (as determined by Radwaste Operations Engineering) and the Solidification Calcula. tion Sheet for 8ead Resin (Attachment 10). NOTE: The liner shall be solidified using OP 1104 28C, Primary Resin and Precoat Processing . Hittman. 21.0 1372: I i

l j < ~ 4UCl68r TMI_1 Number l Operatino Procedure 1104 281 Title Revision No. Waste Solidification Process Control Program 11 9.0 ALTERNATE TEST SOLIDIFICATION PROGRAMS NOTE: The PCP Test Solidification presented in this procedure should cover the majority of the waste processing require. ments of TMI.I. In the event a different waste stream requires processing or a waste stream covered by this procedure but not having the appropriate waste form or liner type, a PCP Test Solidification can be performed using a current procedure provided by Westinghouse - Hittman. 9.1 Prerequisites 9.1.1 A procedure is available for the particular waste stream to be processed. 9.1.2 This procedure has been verified current by the Radwaste Ops. Nanager or his designee and will be reviewed by the Radwaste Engineer prior to its use. 9.1.3 The sample required by this procedure has been cbtained and applicable chemistry parameters analyzed for by Plant Chemistry. 9.1.4 The Ops Quality Assurance Group has been contacted to inform them of the pending Test Solidification to see if they care to witness the test. OQA Monitor Contacted Name / Date / Time 9.1.5 Balance calibration data has been included on Attachment 11. 9.1.6 Attachment 11 has been completed. 9.2 Procedure 9.2.1 Performed the applicable portions of the Westinghouse . Hittman procedure. 10.0 ACCEPTANCE CRITERIA 10.1 Solidification Acceptability 10.1.1 The sample solidification is considered acceptable if there is not visual or drainable free water. 22.0 1372c

Nuclear ,,_, Nueer l Operatino Procedure 1104 281 Title Revision No. f i Waste Solidification Process Control Program 11-l 10/1.2 The sample solidification is considered acceptable if it resists penetration. NOTE: Physical examination shall be for resistance to a ten (10) pound load applied to the surface of the solidified product using a 1/2 inch diameter metal rod. The solidification shall be considered acceptable if the metal probe cannot break the surface and penetrate to the sample core. Normal denting of the surface is acceptable. The rod tolerances are as follows:

                                                                                        +1 lb Weight           10 lbs             -0 lb
                                                                                        +0       in                                                                  .

Diameter 1/2 inch 1/4 in 10.2 Solidification Unacceptability 10.2.1 If the waste fails any of the criteria set forth in Section 10.1 the solidification will be termed unacceptable and a new set of solidification parameters will need to be established under the procedures in Section 10.3. 10.2.2 If the test solidification is unacceptable then the same test procedure must be followed on each subsequent batch of the same type oi' waste until three consecutive test samples are solidt-fled. 10.3 Alternate Solidification Parameters 10.3.1 If a test sample for Class A unstable waste falls to provide acceptable solidification of waste the following procedures should be followed.

a. Mix 454.5 gms of cement and 45.5 gms of ASMS with 400 mis of water to ensure that the problem is not a bad batch of cement.
b. Add additional 50 wt.% NaOH to raise the pH above 8 but less than 9.2 for borated wastes.
c. If the waste (other than waste oil) is only partially solidified, use lower waste to cement and Metso ratios.

Using the recommended quantities of cement and Metso Beads, reduce the waste sample to 375 ml and continue reducing the sample volume by 25 ml. until the acceptability criteria of Section 10.1 are met. 23.0 1372c

OOlOOI THI-1

Operating Procedure 1104-28

Title Revision No. Weste Solidification Process Control Program 9 i d, If the waste oil mixture is only partially solidified try using lower waste to cement ratios. Reduce the quantity of waste by 25 ml. and the emulsifier by 1 ml., (This will result in a slightly higher concentration of emulsifier in the waste) and proceed with the test solidification. Continue with similar reductions until a satisfactory product is achieved. 10.3.2 For. Class A stable, Clast B and C waste test'samrles that fail to solidify, Contact Radwaste Operations Engine'ering for resolu-tion. i l 24.0 1372:

 ^

Nuclear 1WI.i Operating Procedure 1104-281 Title Revision No. Waste Solidification Process Control Program 8 , ATTACHMENT 1 Page 1 of 4 CLASS A UNSTABLE AND STABLE, CLASS '8 AND C TEST SOLIDIFICATION DATA SHEET FOR 4 TO 10 WT% BORIC ACID Chemistry Parameters Balance Cal. Info. Liner No.: Sa: Pole Date CMTE No. Sample No.: Boron ppm Serial No. Date: Total Solids ppm Cal. Due Date Waste Class pH Total Act. mci /cc - I. PRECONDITIONING: Weight Percent of Boric Acid (in decimal form): Boron (opm) x .01 ( ) x .01 1748 - 1748 = (1) Weight of Untreated Sample: gms (2) Volume of Untreated Sample: mis (3) Weight of 50% Na0?! Added to Adjust pH gms (4) within range per Section 4.2.4. pH of treated sample: Weight of Anti-foam Added: gms (S)

                                   % 0111 :                                                               %

Weight of Emulsifier Added: gms (6) Volume of treated sample: mis (7) Weight of treated sample: (2) + (4) + (5) + (6) = ( )+ ( )+ ( )+ ( )= gms (8) l El-1 1372c I

( . Nuclear

                                                             <                                                  TMI-i                                         ,

Operating Procedure 1104-281 l Title Revision No.

                                                          ' Waste Solidification Process Control Program                                          8 ATTACHMENT 1  (Cont'd)     Page 2 of 4 II. DETERMINATION OF PERCENT SOLIDS Or SAMPLE:

Weight of Boric Acid in Untreated Sample: l (2) x (1) -( ) x ( ) - gms (9) Weight of 50% NaOH: (4) x 0.5 - ( ) x 0.5 - gms (10) Weight of Solids in Treated Sample: (5) + (6) + (9) + (10) = ( )+( )+( )+( )- gms (11) Percent Solids in Treated Sample: 100 x (11) + [(8)] - 100 x ( ) + [( )] -  % (12) III. DETERMINATION OF WATER IN SAMPLE FOR SOLIDIFICATION: Volume of Treated Sample to be Solidified: ml (13) Weight of Treated Sample to be Solidified: gms (14) Weight of Water in Sample Contributed by Waste: (2) x (14) x [1 - (1)] - _( 8) . ( ) x( ) x [1 - ( )] = gms (15)

                                                                  .( )          .

Weight of Water in Sample Contributed By 50% NaOH: (4) x (14) x 0.5 - '

                                                              . (8)                .

( ) x ( ) x 0.5 - ( ) gms (16) Total Height of Water in Sample: (15) + (16) - ( )+ ( )- gms (17) El-2 1372c

                    .                                                                     Number Operatino Procedure                       1104-281               l Title                                                                 Revision No.

Waste Solidification Process Control Program 8 ATTACHMENT 1 (Cont'd) Page 3 of 4 IV. DETERMINATION OF QUANTITY OF PORTLAND TYPE I CEMENT AND METSO BEADS TO USE FOR SAMPLE SOLIDIFICATION: Using figure I, find the % solids in sample (12), and DETERMINE l the Hater / Cement Ratio: (18) l Weight of Cement to Use: 1 (17) . ( ) . y (18) ( ) gms (19) ' Weight of Metso Beads to use: (19) x 0,15 - ( ) x 0.15 - gms (20) l Test Solidification Performed By: Name Date Time V. SAMPLE INSPECTION Sample cured for: Hours Cured Temp. Cured Verified By Date Sample contains "No Free Liquid": Verified by Date Sample " Resists Penetration": Verified By Date El-3 1372c

i

i. .

L Nu21 ear " "*" r 1n1 1 Cperating Procedure 1104-281 Title Revision No. Waste Solidification Process Control Program 9 ATTACHMENT I (Cont'd) Page 4 of 4

                              -Additional batches solidified based on this sample solidification:

Liner Waste Liner Waste Liner Haste No. Vol. Date No. Vol. Date No. Vol. Date

2. S. 8.
3. 6. 9.
4. 7. 10.

FOOTNOTES:

1. Maximum allowable oil content for stable waste is 1% by volume.

VI. INDEPENDENT VERIFICATION BY GPUN MANAGEMENT Test Sample Meets Acceptance Criteria (Section 10) Name / Date / Time Test Solidification Data Sheets (Calculations) Reviewed Name / Date / Time El-4 1372c l

l l Nuclear TW1_i Operatino Procedure 1104-281 Title Revision No. Waste So11difttation Process Control Procram 8 ATTACHMENT 2 Page 1 of 3 SOLIDIFICATION CALCULATION SHEET FOR 4 TO 10 WT% B')RIC ACID Liner Type to be used I. Volume of Untreated Waste to Add to Liner 1,3: (3) Max. Treated Waste Vol.

                      ^Ti

( x from Solidification Data Tables - ( ) (. ) x - ft3 (21) Volume of Additives to Add to Liner: l II NaOH: (4) x 4.86 x (21) - ( ) x 4.86 x( )- gals (22) (3) () Anti-foam: (5) x 7.48 x (21) - ( ) x 7.48 x( )- ga'i s (23) (3) () Emulsifier: (6) x 7.48 x (21) - ( ) x 7.48 x( )- gals (24) (3) () III. Volume of Treated Waste to be Solidifiedl : (22) + (23) + (24) ( )+( )+( ) (21) + 7.48 - ( )+ 7.48 - ft3 (25) IV. Cement Quantity for Full Scale Solidification: (19) x 62.4 x (25) - ( ) x 62.4 x ( ) - lbs (26) (13) ( ) (26) + 94 - ( ) + 94 - bags 2 V. ASMS Quantity for full Scale Solidification: (26) x .15 - ( ) x .15 - Ibs (27) (27) + 100 - ( ) + 100 - bags 2 E2-1 1372c i

                           ~

Number MUCIO8r THI_i Operatino Procedure 1104_28I litle Revision No. Waste Solidification Process Control Program 9 ATTACHMENT 2 Page 2 of 3 VI. INDEP.'NDENT VERIFICATION BY GPUN MANAGEMENT SOLID 7.FICATION CALCU.ATION SHEETS' REVIEWED Name / Date / Time FOOTNOTES I The volume of treated waste to be solidified in a single liner cannot exceed the maximum treated waste volume listed on the attached Solidification Data Tables. 2 Round off up to the nearest whole bag. 3 Use the actual waste volume added to the liner in Steps / Equations 22, 23 and 24 if the waste volume added to the liner is less than the value obtained in Step / Equation 21. VII. DETERMINATION OF THE QUANTITY OF CEMENT ADDED TO WASTE: Quantity of Cement Added to Hopper: lbs (28) Quantity of Cement Left in Hopper: lbs (29) Quantity of Cement Added per ft.3 Waste: (28) _ (29) . ( )-( )= lbi cement / (25) ( ) ftJ waste NOTE: Minimum Quantity of Cement Allowable for 4 to 10 Ht. % Boric Acid Class A Unstable Waste is 62 lbs./ft.3 For Stable waste solidification all the cement must be added to the liner. Quantity of Cement Added Meets Minimum Requirements for unstable waste forms: Verified By Date The recommended minimum treated waste volume and minimum solidified waste volume meet the requirements of the Solidification Data Tables for STABLE waste forms. Verified By Date E2_2 1372c

ai .

                                                                                      ""*b" Nuclear 1MI_i Operating Procedure               1104-281 Title                                                                     Revision No.

Waste Solidification Process Control Program 7 ATTACHMENT 2 (Cont'd) Page 3 of 3 SOLIDIFICATION DATA TABLES FOR 4 TO 10 WT% BORIC ACID HN-100 HN-100 LVM Series 3 Series 31 Usable Liner Vol. (cu. ft.) 141.1 157.5 Max. Treated Waste Vol. (cu. ft.)- 104.4 116.6 Max. Solidified Waste 141.1 157.5 . Vol. (cu. ft.) Recommended Min. Treated Waste Vol. 98.1 103.8 (cu. ft)2 Min. Solidified Haste Vol. (cu. ft)2 132.6 140.2 Max. Rad. Level 12 12 R/hr Contact

1. For less than Ap quantities of LSA waste. For greater than A2 quantitles of LSA waste, the maximum treated waste volume is 112.4 cu. ft. due to weight limitations.
2. These minimums are required when shipping to Barnwell, to comply with the 15%

maximum void space criteria for liners containing solidified stable waste forms. E2-3 1372c

       .                                   Nuclear                              TsI_,

Operating Procedure 1104-281 Title Revision No. Haste Solidification Process Control Program 8 ATTACHMENT 3 Page 1 of 4 CLASS A UNSTABLE AND STABLE, CLASS B AND C TEST SOLIDIFICATION l DATA SHEET > 10 TO 20 WT% BORIC ACID Chemistry Parameters Balance Cal. Info. Liner No.: Sample Date CMTE No. Sample No.: Boron ppm Serial No. Date: Total Solids' ppm Cal. Due Date Waste Class pH

                                                                                                                    ~

Total Act, pC1/cc I. PRECONDITIONING Weight Percent of Boric Acid (in decimal form): Boron (ppm) x .01 ( ) x .01 - (1) 1748 - 1748 Weight of Untreated Sample: gms (2) Volume of Untreated Sample: mis (3) Weight of 50% NaOH Added to Adjust pH per Section 5.2.4: gms (4) pH of treated sample: Weight of Anti-foam Added: gms (5)

                              % 0111 :                                                                  %

Weight of Emulsifier Added: gms (6) Volume of treated sample: mis (7) Weight of treated sample: (2) + (4) + (5) + (6) - ( )+( )+ ( )+( )- gms (B) l E3-1 137::

i 4 Number

               .                 Nuclear                                    TM1-i Operatino Procedure        1104-28I Title                                                                 Revision No.

Waste Solidification Process Control Program 8 ATTACHMENT 3 (Cont'd) Page 2 of 4 II. DETERMINATION OF PERCENT SOLIDS OF SAMPLE

                       -Weight of Boric Acid in Untreated Sample                                               ,

(2) x (1) -( ) x ( ) - gms (9) Weight of 50% NaOH: (4) x 0.5 - ( ) x 0.5 - gms (10) Weight of Solids in Treated Sample: (5) + (6) + (9) + (10) . ( )+( )+( /+( )= gms (11)- Percent Solids in Treated Sample: 100 x (11) + [(8)) = 100 x ( ) + [( }) =  % (12) III. DETERMINATION OF WATER IN SAMPLE FOR SOLIDIFICATION: Volume of Treated Sample to be Solidified: ml (13) Weight of Treated Sample to be Solidified: gms (14) Weight of Water in Sample Contributed by Waste:

                                         ~
                           "(2)  x (14)      x [1 - (1)) -
                           ,( 8)         ,

() x( ) x [1 - ( }) . gms (15) () . Weight of Water in Sample Contributed by 50% NaOH:

                                      ~
                        "(4) x (14) x 0.5            .   '(    ) x  (  )' x 0.5   -     gms      (16)        !
                         ,( 8)        ,                  ,

( ) Total Weight of Water in Sample: l (15) + (16) = ( )+ ( )- gms (17) E3-2 1372c

1

                                   ~

Nuclear THI-i Operating Procedure 1104-281 i Title Revision No. j Waste Solidification Process Control Program l 8 j

                                                                                                                             'l ATTACHMENT 3 (Cont'd)                 Page 3 of 4 IV. DETERMINATION OF QUANTITY OF PORTLAND TYPE I CEMENT AND METSO BEADS TO USE FOR SAMPLE SOLIDIFICATION:

Using Figure I, find the % solids in sample (12), and DETERMINE the Water / Cement Ratio: (18) Weight of Cement to Use: (17) ( ) (18) - ( ) - gms (19) Weight of Metso Beads to use: (19) x 0.15 - ( ) x 0.15 - gms (20) Test Solidification Performed By: Name Date Time V. SAMPLE INSPECTION Sample cured for: Hours Cured i Temp. Cured Verified By Date Sample contains "ido Free Liquid": Verified By Date Sample " Resists Perpetration": Verified By Date E3-3 1372c

l L 1 IUCl68r

                                                                                  ""*b "
    ,                                                   TMI_i                                                                 I l                                                Operating Procedure                          1104-281 l        Title                                                                     Revision No.

Waste Solidification Process Control Program 9 i ATTACHMENT 3 (Cont'd) Page 4 of 4 l Additional batches solidified based on this sample solidification: Liner Waste Liner Waste Liner Waste No. Vol. Date No. Vol. Date No. Vol. Date

2. 5. 8.
3. 6. 9.
4. 7. 10.

FOOTNOTES:

1. Maximum allowable oil content for Stable Waste is 17. by volume.

IV. INDEPENDENT VERIFICATION BY GPUN MANAGEMENT Test Sample Meets Acceptance Criteria (Section 10) Name / Date / Time Test Solidification Data Sheets (Calculations) Reviewed _ Name / Date / Time E3-4 13 M C

Nuclear ""**" rnI., Operating Procedure 1104-281 11tle Revision No. Waste Solidification Process Control Progr.m 8 ATTACHMENT 4 Page 1 of 3 SOLIDIFICATION CALCULATION SHEET FOR > 10 TO 20 WT% BORIC ACID Liner type to be used I. Volume of Untreated Waste to Add to Liner1 ,3: (3) Max. Treated Waste Vol. (7) x from Solidification Data Tables = ( ) ( ) x - ft3 (21) II. Volume of Additives to Add to Liner: , NaOH: (4) x 4.86 x (21) = ( ) x 4.86 x( )- gals (22) (3) ( ) Anti-foam: (5) x 7.48 x (21) - ( ) x 7.48 x( )- gals (23) (3) ( ) Emulsifier: (6) x 7.48 x (21) - ( ) x 7.48 x( )= gals (24) , (3) ( ) i i III. Volume of Treated Waste to be SolidifiedI : (22) + (23) + (24) ( ) +( ) + ( ) (21) + 7.48 = ( )+ 7.48 - ft3 (25) IV. Cement Quantity for Full Scale Solidification: (19) x 62.4 x (25) - ( ) x 62.4 x ( )- lbs (26) > (13) ( ) I (26) + 94 - ( ) 94 - bags 2 V. ASMS Quantity for Full Scale Solidification: (26) x .15 - ( ) x .15 - lbs (27) (27) + 100 - ( ) 100 - bags 2 E4-1 1372c

    .                  NuIlear                               THI-l uomber Operatino Procedure                  1104-28I                ;

Title Revision No. Haste Solidification Process Control Program 9 i ATTACHMENT 4 Page 2 of 3 q SOLIDIFICATION CALCULATION SHEET FOR > 10 TO 20 WTI BORIC ACID VI. INDEPENDENT VERIFICATION BY GPUN MANAGEMENT SOLIDIFICATION CALCULATION SHEETS REVIEWED Name / Date / Time FOOTNOTES I The volume of treated waste to be solidified in a single liner cannot exceed the maximum treated waste volume listed on the attached Solidification Data Tables. 2 Round off up to the nearest whole bag. 3 Use the actual waste volume added to the liner in steps / equations 22, 23 and 24 , if the waste volume added to the liner is less than the value obtained in Step / Equation 21. I 1 VII. DETERMINATION OF THE QUANTITY OF CEMENT ADDED TO WASTE: I Quantity of Cement Added to Hopper: lbs (28) Quantity of Cement Left in Hopper: lbs (29) Quantity of Cement Added per ft.3 Waste: (28) - (29) - ( )-( ) - lbs cement / (25) ( ) ft3 waste j i NOTE: Minimum Quantity of Cement Allowable for >10 to 20 Wt.

                                      % Boric Acid Class A Unstable Waste is 60 lbs./ft.3, For STABLE waste solidification all the cement must be added to the liner.

Quantity of Cement Added Meets the Minimum Requirements for unstable waste forms: 1 Verified By Date i The recommended minimum treated waste volume and minimum solidified waste volume mset the requirements of the Solidification Data Tables for STABLE waste forms. i-Verified By Date E4-2 1372c I

Nuclear THI_i Operating Procedure 1104-28I Title Revision No-Waste Solidification Process Control Program 7 ATTACHMENT 4 (Cont'd) Page 3 of 3 SOLIDIFICATION DATA TABLES FOR > 10 TO 20 WT1 BORIC ACID HN-100 HN-100 LVM Series 3 Series 3I Usable Liner Vol. (cu. ft.) 141.1 157 5 Max. Treated Waste Vol. (cu. ft.) 101.3 113.1 Max. Solidified Waste 141.1 157.5 Vol. (cu. ft.) Recommended Min. Treated Waste Vol.. 95.2 100.7 (cu. ft)2 Min. Solidified Waste Vol. (cu. ft)2 132.6 140.2 Max. Rad. Level 12 12 R/hr Contact I- For less than A2 quantities of LSA waste. For greater than A2 quantities of LSA waste, the maximum treated waste volume is 106 cu. ft. due to weight limitations. 2- These minimums are required when shipping to Barnwell, to comply with the 15% maximum void space criteria for liners containing solidified stable waste forms. l l l E4-3 1372c l i L-______--_---

Nuclear TMI-l Nueer Operating Procedure 1104-28I Title Revision No. Waste Solidification Process Control Program 11 ATTACHMENT 5 Page 1 of 2 CLASS A UNSTABLE AND STABLE, CLASS B AND C TEST SOLIO!FICATION DATA SHEET FOR WASTE OIL Chem. Parameters (Conc. Haste) Balance Cal. Info Liner No.: Sample Date CMTE No.: Sample No.: Boron ppm Serial No.: Date: Total Solids ppm Cal. Due Date: Waste Class: pH l Total Act. pC1/cc I. SAMPLE PREPARATION Volume of 011 to be Solidified: mis (1) Volume of Concentrated Waste added to the oil: mis (2) Total Volume of Sample: mis

                            % 011 by Volume:

(1) x 100 - ( ) x 100 -  % (3) (1) + (2) ( )+( ) Height of 50 wt% NaOH added to sample to raise pH > 5 gms (4) Quantity of Emulsifier to Add to Sample: mis (5) Quantity of Anti Foam Added to Sample: mis (6) Quantity of Portland Type 1 Cement Added to Sample: gms (7) Quantity of Anhydrous Sodium Metas11tcate Added to Sample: gms (8) Test Solidification Performed By: l Name Date Time ! E5-1 1372c

               '                                                                                                       I
                                                                                       "*D
                           . $lLJllCll$34Blf"                1g1 1                                                     )

Operating Procedure 1104-281 Title Revision No. i i Waste Solidification Process Control Procram 9 j 1 i ATTACHMENT 5 (Cont'd) Page 2 of 2 II. SAMPLE INSPECTION Sample cured for: Hours Cured i 1 Temp. Cured Verified By Date Sample contains "No Free Liquid": Verified By Date Sample'" Resists Penetration": Verified By Date Additional batctes solidified cased or this sample solidification: Liner Waste Liner Waste Liner Haste No. Vol . ,, Date No. Vol. Date No. Vol. Date

2. 5. 8.
3. 6. 9.

4 7. 10. III. INDEPENDENT VERIFICATION BY GPUN MANAGEMENT Test Sample Meets Acceptance Criteria (Section 10) Name / Date / Time Test Solidification Data Sheets (Calculations) Reviewed Name / Date / lime I l E5-2 13 72 c l

Nuclear THI-i Operating Procedure 1104-231 Title Revision No. Waste Solidification Process Control' Program 8 ATTACHMENT 6 Page 1 of 3 SOLIDIFICATION CALCULATION SHEET FOR WASTE OIL Liner type to be used I. PARAMETERS FOR FULL SCALE SOLIDIFICATION Emulsifier:

                                                                           )=                                                         l (5) x 7.48 + (1) - (      ) x 7.48 + (                                        gal /      (9) ft3 Anti-foam 1                                 1 (6) x 7.48 x II) + (2) -(        ) x 7.48 x (      )+ (   )                   gal /      (10) ft3            -

Cement: 1 1 (7) x 62.43 x (1) + (2) -( ) r 62.43 x ( )+ ( ) lbs/ (11) ft3 ASMS: 1 1 (8) x 62.43 x (1) + (2) =( ) x 62.43 x ( )+( ) lbs/ (12) ft3 II. QUANTITIES TO BE ADDED FOR FULL SCALE SOLIDIFICATION Volume of untreated waste to add to liner j (Max Treated Waste Vol from Solidification j Data Tables):3 (13) i Concentrated Waste to be added: 60% x (13) x 7.48 - 0.60 x ( ) x 7.48 - gals (14) l Waste Oil to be added: 40% x (13) = 0.40 x ( )= ft3 (15) 40% x (13) x 7.48 0.40 x ( ) x 7.48 gals E6-1 1372:

4 Nuclear TMI-1 Numeer Operating Procedure 1104-281 Title Revision No. Waste Solidification Process Control Program 9 ATTACHMENT 6 (Cont'd) Page 2 of 3 Emulsifier to be added: (15) x (9) = ( )x( )= gals Anti-foam to be Added: (13) x (10) = ( )x( )= gals ASMS to be added: (13) x (12) = ( ) x( )= lbs (16) (16) + 100 - ( )+ 100 = bagsl

                                                                                                                 ~

Volume of cement to add to liner: (13) x (11) = ( ) x( )= lbs (17) (17) + 94 = ( ) + 94 = bagsl FOOTNOTES: I Round off up to the nearest whole bag. 2 Reduce the quantity of total waste in the liner by 1 ft3 for every 10 gallons of anti-foam added to the liner. No adjustment is necessary for the first 10

                                  ~ gallons.

3 Use actual waste volume added to the liner in step / equations used in Section II ' if waste volume added to the liner is less than the value obtained in Step / Equation 13. III. INDEPENDENT VERIFICATION BY GPUN MANAGEMENT SOLIDIFICATION , CALCULATION SHEETS REVIEWED l Name / Date / Time E6-2 1372c _---_u___e-mm__m __

Number

            .                      MUCl88r                              THI-i Operatino Procedure              1104-281 Title                                                               Revision No.

Haste Solidification Process Control Program 7 ATTACHMENT 6 (Cont'd) Page 3 of 3 SOLIDIFICATION DATA TABLES FOR WASTE 0;L HN-100 HN-100 Series 3 LVM Usable Liner Volume, (ft3) 141.1 157.5 Max. Haste Volume (oil and conc. waste), ft3 93.7 104.6 Max. Solidified Volume, ft3 141.1 157.5 Maximum Rad Level R/hr Contact 12 12 l I t E6-3 1372c

  ~

Nuclear THI-i ODer& ting Procedure 110a-2BI Title Revision No. Waste Solidification Process Control Program 8 ATTACMMENT 7 Page 1 of 2 CLASS A STABLE, CLASS B AND C TEST SOLIDIFICATION DATA SHEET FOR USED PREC0AT Balance Cal. Info. Chemistry Parameters Liner No.: CMTE No. pH Sample No.: Serial No. Gamma Scan mC1/ml Date: Cal. Due Date  % Oil  % Waste Class I. SAMPLE PREPARATION Weight of Dewatered Powered Resin gms (1) Volume of Dewatered Powered Resin ml (2) Weight of Water Added to P0wdered Restn: gms (3) Total of Volume of Powered Resin Slurry: ml' i4) Quantity of Anti-foam Agent Added to Sample: gms (5) Quantity of oil in Sample  % (6) Quantity of Emulsifying Agent Added to Sample: gms (7) Initial pH of Sample: (8) II. SOLIDIFICATION i l Quantity of Ca(OH)2 necessary to raise pH > 11.5: gms (9) i l Final pH of Sample: (10) i Quantity of Portland Cement Added to Sample gms (11) Final Sample Volume: mis (12) Test Solidification Performed By: 1 Name Date lime E7-1 1372c I L________________._ . _ . _ _ _ _ _ _ _ _ . _ . _ _ _ _ _ . - - _ - .

MUClear

                  ~
 ~

l inI.i Operatino Procedure 1104-251 Title Revision No. l Waste Solidification Process Control Procram 9 l ATTACHMENT 7 (Cont'd) Page 2 of 2 I CLASS A STABLE, CLASS B AND C TEST SOLIDIFICATION DATA S M ET  ! FOR USED PREC0AT t III. SAMPLE INSPECTION Sample cured for: l Hours Cured 1 Temp. Cured i l Verified By Date  ! Sanple contains "ho free Liquid"- - i Verified By Date  ! l Sample " Resists Penetration": Verifiec By Date l l Additional batches solidified based on this sample solidifttation: t I Liner Waste ' Liner Waste Liner Waste  ; No. Vol. Date No. Vol. Date No. Vol. Date l

2. 5 B.
                                                                                                                      \

l 3. 6. 9. l l

4. 7. 10. l i

l IV. INDEPENDENT VERIFICATION BY GPUN MANAGEMENT Test Semple Meets Atteptante l Criteria (Section 1D) Name / Date / lime i l Test Solidifttation Data l l Sheets (Calculations) Reviewed j hame / Date / lin j i E7-2 1372: l 1 _ _ _ . _ i

                        ~

Number Nuclear w -i Operatinc Procedure 1104-28I Title Revision No. Waste Solloification Procers Control Procram 8 ) l ATTACHMENT 8 Page 1 of 3 SOLIDIFICA1 ION CALCULATION SHEET FOR USED PREC0AT Liner Type to be used . I. PARAMETERS FOR FULL SCALE SOLIDIFICATION: Qu?.ntity of Water: (3) x 7.48 - ( ) x 7.48 gal / (13) ' (2) ( ) ft3 of vaste f Quantity of Anti-Foam Agent: ' (5) x 7.48 - ( ) x 7.48 , gall (14) (2) ( ) ft3 of waste-Quantity cf Emulsifier: (7) x 7.48 - ( ) x 7.48 _ gal / (15) (2) ( ) ft3 of waste  ! I Quantity of Ca(OH)2:  ! (9) x 62.43 - ( ) x 62.43 , lbs/ (16) 4 (24 ( ) ft3 of waste I Quantity of Portland Type 1 Cement: l (11) x 62.43 - 1_ ) x 62.43 _ lbl/ (17) i (2) ( ) ftJ of waste  ; II. QUANTITIES TO BE ADDED FOR FULL SCAL.E SOLIDIFICATION l Volume of Dewatered Powdered Resin to be Solidified: ft3 (18)  ! Quantity of Water: ' (18) x (13) - ( ) x( )- _ gal (19) f Quantity of Anti-Foam Agent: (18) x (14) - ( )x( )- gal (20)  ; i Quantity of Emulsifier: l (18) x (15) - ( ) x( ) - gal (21) ES-1 1372c

Nuclear Numeer

               ,                                                                   TMI-l Operating Procedure                  1104-281 Title                                                                         Revision No.

Waste Solidification Process Control Program 9 ATTACHMENT 8 (Cont'd) Page 2 of 3 SOLIDIFICATION CALCULATION SHEET FOR USED PREC0AT Quantity of Ca(OH)2: (18) x (16) = ( ) x( )= lbs (22) (22) + (100) = ( )+( )= bags 2 Quar.tity of Portland Type Cement: (18) x (17) = ( ) x( )= lbs (23) (23) + (94) = ( )+( )= bags 2 1 The volume of waste, to be solidified in a liner cannot exceed the maximum settled and treated waste volume listed on the Class B Waste Solidification Data Table for used precoat. 2 Round up to the nearest whole bag. III. INDEPENDENT VERIFICATION BY GPUN MANAGEMENT SOLIDIFICATION CALCULATION SHEETS REVIEWED Name / Date / Time i l E8-2 1372: j

       .e l

MUCl88r THI-1 Operating Procedure 1104-28I Title Revision No. L Waste Solidification Process Control Program 8 ATTACHMENT 8 (Cont'd) Page 3 of .! SOLIDIFICATION DATA TABLE FOR USED PREC0AT HN-600 MVS HN-200 MU Usable Liner Volume, ft3 59.3 59.4 Max. Solidified Waste Vol. ft3 59.3 59.4 Max. Dewatered Waste Vol.. ft3 33.3 33.3 Min. Haste Vol. ft3 32.9 32.0 Min. Solidified Waste Vol, ft3 58.6 57.0 Max. Radiation Level - R/hr Contact of Liner 100 800 l 1 i t i i l l ES-3 1372c l l

                 .                 Nuclear                           TsI-i Operating Procedure                    1104-281 Title                                                                    Revision No.

1 Waste Solidification Process Control Program 8 i ATTACHMENT 9 Page 1 of 2 CLASS A STABLE, CLASS B AND C TEST SOLIDIFICATION DATA SHEET FOR BEAD RESIN Balance Cal. Info. Chemistry Parameters Liner No.: CMTE No. pH Sample No.: Serial No. Gamma Scan mC1/mi Date: Cal. Due Date  % Oil 1 Waste Class: I. SAMPLE PREPARATION Sample Weight: gms (1) Sample Volume: _ ml (2) Weight of EC-3: gms (3) Weight of water: gms (4) Weight of Anti-foaming agent added to sample: gms (5) Quantity of oil in sample:  % (6) Weight of Emulsifier added to sample: gms (7) Initial pH of sample: (8) II. SAMPLE SOLIDIFICATION Weight of Ca(OH)2 added to sample to raise the pH > 11.5: gms (9) Final pH of sample: (10) Weight of Portland Type 1 cement added to sample: gms (11) Final Sample Volume: ml (12)  ! l Test Solidification Performed By: Name Date Time i E9-1 1372c

h L- - iltJtCiltBkERI' TMI_i

                                                                                                               ""*b

Operating Procedure 1104-281 Title Revision No. Haste Solidification Process Control Program 9 ATTACHMENT 9 (Cont'd) Page 2 of 2 CLASS A STABLE, CLASS B AND C TEST SOLIDIFICATION DATA SHEET FOR BEAD RESIN III. SAMPLE INSPECTION Sample cured for: Hours Cured Temp. Cured Verified By Date Sample contains "No Free Liquid": - Verified By Date Sample " Resists Penetration"- Verified By Date Additional batches solidified based on this sample solidification: Liner Waste Li r,e r Waste Liner Haste No. Vol. Date No. Vol., Date No. Vol. Date

2. S. 8.
3. 6. 9.
4. 7. 10.

IV. INDEPENDENT VERIFICATION BY GPUN MANAGEMENT Test Sampie Meets Acceptance Criteria (Section 10) Name / Date / Time Test Solidification Data Sneets (Calculations) Reviewed Name / Date / Time

                                                                                                                                   .I E9-2                                      1372c i i

Nuclear

                   .                                                           TsI-i Operatino Procedure             1104-281 Title                                                                  Revision No.

Waste Solidification Process Control Program 8 ATTACHMENT 10 Page 1 of 3 SOLIDIFICATION CALCULATION SHEET FOR BEAD RESIN Liner Type to be used: II. PARAMETERS FOR FULL SCALE SOLIDIFICATION Quantity of EC-3: (3) x 6.3 - ( ) x 6.3 gal / (13) (2) ( ) ft3 of waste Quantity of Water: (4) x 7.48 - ( ) x 7.48 gal / (14) (2) ( ) ft3 of waste Quantity of Ant.-Foam Agent: l (5) x 7.48 - ( ) x 7.48 gal / (15) t (2) ( ) ft3 of waste f Quantity of Emulsifier: (7) x 7.48 - ( ) x 7.48 , gal / (16) (2) ( ) ft3 of waste Quantity of Calcium Hydroxide Ca(OH)2: (9) x 62.43 .( ) x 62.43 , Ibs/ (17) (2) ( ) ft3 of waste Quantity of Portland Type 1 Cement: (11) x 62.43 - ( ) x 62.43 , lbs/ (18) (2) ( ) ft3 of waste II. QUANTITIES TO BE ADDED FOR FULL SCALE SOLIDIFICATION Waste Volume of to be Solicifiedl ,3: ft3 (19) Quantity of EC-3: (19) x (13) -( ) x( )- gal (20) l l E10-1 1372:

            ~

Li ENuclear. TMI-1

                                                                                                                  )

l' Operating Procedure 1104-281 Title Revision No. Waste Solidification Process Control Program 9 l ATTACHMENT 10 (Cont'd) Page 2 of 3 SOLIDIFICATION CALCULATION SHEET FOR BEAD RESIN Quantity of Water: (19) x (14) - ( )x( )= gal (21) Quantity of Anti-Foam Agent: (19) x (15) - ( ) x( )- gal (22) Quantity of Emulsifier: (19) x (16) - ( ) x( )- gal (23)

                                                                                                          ~

Quantity of Calcium Hydroxide Ca(OH)2 (19) x (17) - ( ) x( ) - Ibs (24) (24) + (100) - ( ) + 100 - bags 2 Quantity of Portland Type Cement: (19) x (18) - ( ) x( )- lbs (25) (25) + (94) - ( ) + 94 = bags 2 1 The volume of dewatered bead resin to be solidified cannot exceed the maximum treated waste volume listed on the Class A Stable, Class B and C Test Solidification Data Sheet for Bead Resin. 2 Round up to the iearest whole bag. 3 Reduce the quant',ty of waste in liner by 1 ft3 for every 10 gallons of anti-foam agent plus emulsifier added to liner. III. INDEPENDENT VERIFICATION Bf GPUN MANiGEMENT i SOLIDIFICATION CALCULATION SHEETS REVIEWED Name / Date / Time E10-2 1372:

E. - Nuclear 1MI-i Operatino Procedure L . . 1104-28I [ Title Revision No. 1 Waste Solidification Process Control Program 8 l l ATTACHMENT 10 (Cont'd) Page 3 of 3 SOLIDIFICATION DATA TABLES FOR BEAD RESIN HN-100 HN-600 HN-600 LVMU HN-200 MU LVMVG5 Usable Liner 148.8 59.4 64.0 61.7 Volume (cu. ft.) Max. Dewatered 120.0 47.9 51.6 49.8 Waste Volume (cu. ft.) Max. Solidified 148.8 59.4 64.1 61.7 Waste Volume (cu. ft.) Max. Rad. Level 12 800 100 100 - R/hr Contact Min. Recommended (I) Haste Vol (ft3) 106.9 46.0 - 47.3 Min Solidified (l) 132.6 57.0 - 58.6 (I) Grout will have to be added to the HN600 MU to increase the solidified waste volume to meet the 15% maximum void space criteria for shipment to Barnwell. E10-3 1372:

 -l                         .           Nu21 ear                           TsI-i
                                                                                                  ""*b'r Operating Procedure                 1104-281 l                           -Title                                                                 Revision No.

Waste Solidification Process Control Program 7 ATTACHMENT 11 Page 1 of 1 TEST SOLIDIFICATION USING WESTINGHOUSE - HITTMAN PROCEDURE Waste to be Processed: Westinghouse - Hittman Procedure No. Procedure - Title Current Revision Justification to use this alternate test procedure: Liner Type Waste Class Balance Cal Info. CMTE No. Serial No. Cal. Due Date I Approved By Eng. Review By NOTE: Form should be attached to valid Westinghouse - Hittman Procedure used for the Test Solidification i l l l Ell-1 1372c i

STD-P-05-OL.i am*-tol Pag 2 32 of 35 Revision 9

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