ML20082M295

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Rev 14 to Operating Procedure 1104-28I, Waste Sodification Process Control Program
ML20082M295
Person / Time
Site: Three Mile Island Constellation icon.png
Issue date: 06/27/1991
From:
GENERAL PUBLIC UTILITIES CORP.
To:
Shared Package
ML20082M290 List:
References
1104-28I, NUDOCS 9109050123
Download: ML20082M295 (27)


Text

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Ir kT1 Nuclear 1m -1 operating Procedure 1104-28I Title Revision No.

Waste So11dification Process Control Program 14 Applicability / Scope Responsib1e office TMI-1 Division Plant Ops. Dir.

This document is within QA plan scope X Yes No Effective Date Safety Reviews Required -

X Yes -

No 07/02/91 List of Effective Pages ,

Page Revision Page Revision Page Revision Page Revision 1.0 14 26.0 14 E8-3 8 2.0 14 27.0 14 E9-1 8 3.0 14 El-1 0 E9-2 12 4.0 14 El-2 8 E10-1 8 5.0 14 El-3 8 E10-2 9 6.0 14 El-4 12 E10-3 8 7.0 14 E2-1 8 E11-1 13 8.0 14 E2-2 9 E12-1 9 9.0 14 E2-3 7 10.0 14 E3-1 8 .

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Ohp N 73g.1 Operating Procedure 1104-281 Reviolon No.

Title Waste Solidification Process Control Program ,

14 Table of Contents Page Section DISCUSSION 4.0 1.0

2.0 REFERENCES

4.0

\

3.0 DEFINITIONS 5.0 4.0 REl%RTING REQUIREKKNTS 6.0 4.1 Semi Annual Effluent Report 6.0 4.2 Annual Report 7.0 4.3 Waste Solidification Mishaps 8.0 5.0 LIMITS AND P.9EC.TUTIONS 8.0 6.0 TEST SOLIDIFICATION OF 4 TO 10 m DORIC ACID 10.0 (CONCENTRATED WASTE) 6.1 Prerequisites 10.0 6.2 Procedure 10.0 7.0 TEST SOLIDIFICATION OF > 10 TO 20 m DORIC ACID 13.0 (CONCENTRATED WASTE) 7.1 Prerequisites 13.0 7.2 Procedure 14.0 8.0 TEST SOLIDIFICATION OF WASTE OIL 16.0 B.1 Prerequisites 16.0 8.2 Procedure 17.0 9.0 TEST SOLIDIFICATION OF USED PREccAT 18.0 9.1 Prerequisites 16.0 9.2 Procedures 19.0 10.0 TEST SOLIDIFICATION OF BEAD PRSIN 21.0 10.1 Prerequi sites 21.0 10 2 Procedure 22.0 2.0 1372c

[c d] Nuclear T81-1 Numb 2r 1104-281 Operating Procedure ,

Title Revision No.

r Waste Solidification Process Control Program 14 Table of Contents (Cont'd)

Section Page 11.0 ALTERNATE TEST SOLIDIFICATION PROGRAMS 25.0 11.1 Prerequisites 25.0 11.2 Procedure 25.0 12.0 ACCEPTANCE CRITERIA 26.0 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 wtt E2-1 Boric Acid ATTACHMENT 3 Class A Unstable and Stable, Class B and C Test E3-1 Solidification Data Sheet for > IC 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 011 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 EB-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 S711ds of pH Adjusted Waste vs. Water / E12-1 I

Cement Ratio l

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e UINuclear TH1-1 Operating Procedure 1104-281 Title Revision No.

Waste Solidification Process Control Program 14 1.0 DISCUSSION The purpose of the Process Control Program (PCP) for incontainer solidification is to provide a program which will assure a solidified product with no free standing liquid prior to transportation for disposal and which meets the re-quirements of 10 CFR 61.56, Waste 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 Masc the Stability Requirements of 10 CFR 61" prepared by Westinghouse. These PCP's are valid for all liner types using electric or hydraulic mixing heads provided by SEG.

The appropriate portions of this document shall be considered complete only when used with the operating procedures (OP llO4-28A for borated and oily wastes or OP 1104-28C for resin) 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 coment and additive which must be mixed with Class A Stable and Class B or C wastes.


==- _- =----------------------------------------------------------------.

NOTE: Until regulatory issues are resolved concerning Class B and C waste forms (refer to Reference 2.10), this procedure shall only be utilized to perform verification testing of Class A unstable waste forms only.

2.0 REFERENCES

2.1 Westinghouse - Hittman F421-P-004, Process Control Program for Incentainer Solidification of 4 to 20 wts Boric Acid 2.2 Westinghouse - Hittman STD-P-05-002, Process Control Program for Incon-tainer Solidification of OLly Waste 2.3 Westinghouse - Hittman F421-P-006, Process Control ?rogram for Incontainer Solidification of Powdered Resine 2.4 Westinghouse - Hittman F421-P-005, Process Control Program for Inccntainer Solidification of Class A Unstable or Stable, Clasa B and C Resin at Maximua 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. Roesi, Assistant Director, Division of PWR Licensing-A to R.J. Leduc, Director of Engineering Westinghouse Hittman -

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P UINuclear TM1 1 Operating Procedure 1104-2BI Revision No.

Title

~~ Waste Solidification Process Control Program 14

" Acceptance of Referencing of Licensing Topical Report STD-R-05-Oll, Hittman Mobile Incontainer Dewatering and Solidification System (MDSS)",

Dated Oct. 31, 1986.

2.8 GPUN Operational Quality Assurance Plan 2.9 GPUN Radiation Protection Plan 2.10 Waste Form Technical Position, Rev. 1, dated January 24, 1991 2.11 Generic Letter 91-02, Reporting Mishaps Involving LLW Torms Prepared for Disposal, dated December 28, 1990 3.0 DEFINITIONS 3.1 Process Control Program The PROCESS CONTROL PROGRAM (PCP): A document that shall contain the current formulas, sampling, analyses, test, and determinations to be made to ensure that processing and packaging of solid radioactive wastes based on demonstrated processing of actual or simulated wet solid wastes will be accomplished in such a way as to asbure compliance with 10 CTR Parts 20, 61, and 71, State regulations, burial ground requirements, and other requirements governing the disposal of solid radioactive waute.

3.2 Solidification SOLIDITICATION shall be the conversion of radioactive wastes from liquid treatment systems to a uniformly distributed, monolithic immobilized solid with definite volume and shape, bounded by a stable surface of distinct outline on all sider (free-standing).

3.3 Batch A BATCH is defined as that quantity of waste required to fill a dis. sal liner to the appropriate level on the waste level indicator.

3.4 operable The solid Radwaste System is operable when it is capable of performing its intended function within the required range of the Process Control Progrun.

The system shall be considered to have the capability when the performance requirements have been met by system operation within the previous 92 days or a vendor is under contract to perform solidification services in accordance with a Process Control Program.

3.5 Solid Radwaste System The Solid Radwaste System comprises the equipment necessary to solidify liquid or solid (i.e., resin) Radioactive Wastes in accordance with a Process Control Program. As a minimum the system includes a disposal liner, mixer head, cement feed system and ventilation. These components are housed in a solidification building adjacent to the TMI 1 Auxiliary 5.0 1372c

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Muclear Tx1 1 1

Ope, rating Procedure' 1104-28I {

Title Revision No. t Waste Solidification Proctes Control Program 14 (

Building. Separate Solid Radwaste Systems may also be used for specific purposes as long.as they comply with a valid PCP.

I 4.0 REPORTING REQUIREMMITS )

(

4.1 Semi Annual Effluent Report l I

4.1.1 Process Control Program-  !

i A. Changes to.a PCP shall be submitted to the NRC in the i Semiannual Radioactive Effluent Release Report for the i period in which the changes were made.- This submittal shall  !

g contains l l i D 1. Sufficiently detailed information to justify the_  !

changes without benefit of additional or supplemental  ;

informations

2. a determination that the changes did not reduce the overall.conformance of the solidified waste product to existing criteria for solid wastes, and -
3. documentation that the changes have been reviewed and  !

approved pursuant to T.S. 6.8.2. l B. Changes shall become effective upon review and approval BY  !

GPUNC Management.

l 4.1.2 Solid Waste Shipmente  !

A. The Radioactive Effluent Release Reports shall include the

-following information for each type of solid waste shipped ,

offsite during the report period *

1. Type of waste
a. Spent resins, filter sludges, evap. bottoms, etc.
i.  !
b. Dry compressible waste, contaminated equipment, l etc. )

i

c. Irradiated components, control rods, etc. l
d. Other  !
2. Total volume (cubic meters)
3. Total curie quantity

.l

4. Principal radionuclides (specify whether determined by ,

measurement or estimate),  :

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I'- U1 Nuclear m1 Operating Procedure 1104-281 Title Revision No.

Waste Solidification Process control Program 14

5. Disposition of Solid Waste Shipmente (i.e. , number of shipments to burial, mode of transportation, destination)
6. Disposition of Irradiated Fuel Shipments (i.e., number of shipraents, mode of transportation, destination) 4.2 Annual Report 4.2.1 Major Changes to Radioactive Waste Treatment Systems A. GPU Nuclear Corporation initiated safety related changes to the Solid radioactive waste systems
1. Shall be reported to the Commission in the Annual Report (T. S. 6.9.1B) for the period in which the evaluation was reviewed. The discussion of each change shall contains
a. A summary of the evaluation that led to the determination that the change could be mado in accordance with 10 CFR 50.59;
b. Sufficient detailed information to totally support the reason aor the change without benefit of additional or supplemental inf ormation;
c. A detailed description of the equipment, componente and processes involved and the interfaces with other plant systems;
d. An evaluation of the change which shows the predicted releases of radioactive materiale in liquid and gaseous effluente and/or quantity of solid waste that differ from those previously predicted in the license application and amendments thereto;
e. An evaluation of the change which shows the expec+.ed maximum exposures to individuals in the unrestricted area and to the general population that differ from those previously settmated in the licence application and amendmente thereto;
f. A comparison of the predicted releases of radioactive materiale, in liquid and gaseous ef flusntn and in solid waste, to the actual releases for the period prior to when the changee are to be made; 9 An estimate of the exposure to plant operating personnel as a result of the change; and
h. Docur.entation of the fact that the change was reviewed and cpproved.

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ENuclear Tm _1 operating Procedure

""*=<

1104-2BI .

Title 1 Revision No.

Waste solidification Process Control Program 14

2. Shall become ef fective upon review and approval in accordance with T. S. 6.5.1.

4.3 Waste Solidification Hishaps

1. TMI-l Licensing shall be notified within 10 working days of any mishaps _regarding solidification of Class B or C waste forms as follows:  ?

t The production of a solidified Class B or C waste form that has any [

of the following characteristics:

{

  • Contains free-liquid in quantities exceeding 0.5 percent of the  ;

volume of the waste. [

I

  • Contains waste with radionuclides in concentrations exceeding  !

those considered during waste form qualification testing .j accepted by the regulatory agency, which could lead to errors in assessment of waste class.

f

  • Contains a significantly different waste loading than that used j in qualification testing accepted by the regulatory agency.  ;
  • Contains chemical ingredients not present in qualification  !

testing accepted by the requiatory agency, and those quantities }*

l are sufficient to unacceptably degrade the waste product.

1

  • Shows instability evidenced by crumbling, cracking, spalling, {

voids, softening, disintegration, nonhomogeneity, or dimensional (

changes.

{

i. '

l-

  • Evidence of ptocessing phenomena that exceed the limiting ,

l' processing conditions _ identified in applicable topical reports  ;

on process control plans, e.g., foaming, temperature extremes, _j premature or slow hardening, and production of volatile ,

material.

l l 2. TMI-l Licensing shall review each event for determination of  ;

voluntary reporting to the NRC's Director of _ the Division of Low ,

Level Waste Management and Decommissioning within 30 days of the '

incident. l t

5.0 LIMITS AND PRECAUTIONS f i

5.1 The PCP shall be used to verify the solidification of at least one  !

representative test specimen f rom at least every tenth batch of each type l of wet radioactive waste (e.g., evaporator bottoms, oily waste, resin and i precoat sludge). j i

e l

8.0 1372c f

(UClear m1 1 Orierating Procedure 1104-281 Title Revision No.

Weste Solidification Process control Pr* ,tm __

14 5.2 If any test specimen fails tr r.. f, polidification of the betch vnder test shall be suspended untJ m a . me as additional test speciment can be obtained, alternative solidi. .gion parameters can be determined in accordance with the Proe7ss control Progrsm, and a subsequent test teri-fios solidification. Solidification of the batch may then be remumed using the alternate solidification parameters determined.

l:

5.3 If the initial test specimen from a L'atch of waste fails to verify solidi-fication then representative *ast specimens shall be collected from each

-consecutive batch of the same type of waste until the three (3) consecu-

  • tve initial test specimens demonstrate solidification. The Process

':.nttol Program shall be modified as required to assure solidification of

, deequent batches of waste.

5.4 Solid Radwaste System 5.4.1 The solid radws 'to system shall be demonstrated operable qu arterly. As defined in Section 3.4.

5.4.2 The solid radwaste system shall be used in accordance with the Process control Program (PCP) to process wet radioactive wastes to meet shipping and burial ground requirements.

a. With the provision of the PCP not satisfied, suspend shipments cf defectively processed or defectively packaged solid radioactive wastes from the site.

5.5 Fer high activity wastes, such as spent resin or used precoat, chore [

handling of semples could result in personnel radiation exposures which are inconsistent with the ALARA principle, representative non-radioactive [

samples will be tested. These samples should be as close to the actual i waste physical and chemical properties as possible. Typical expended mixed 1 bed resin shall be used to simulate the spent bead resin and.the j appropriate mix of anion to cation powdered resin shall be used to simu- j late used precoat. t 5.6 All Chemicals used to condition or solidify waste or simulated waste in i solidification tests shall be the actual chemicals used in full scale -!

an11dification. l

?

547 A Test Solidification Data ;b m will be maintained for esch test sample  !

solidified. Each Data Sheet will contain pertinent information of the tera  !

sample and the liner numbers solidified based on the test sample.  !

5.8 sr.mples should be drawn at least six hours prior to the_ planned full scale  ;

waste solidificatic.) to allow adequate time to complete the required [

testing and verification of solidification for class A unstable waste. 28 r hours should be allowed, if practical, for class A stable, Class B and C j wastes.

5.9 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 i sampling to assure a represen;ative sample, t 9.0 1372c {

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i Number e replNuclear TM1-1 Operating Procen a _ 1104-281

' Title Revision No.

Wast e solidification Process Control Program 14 5.10 An RWP .nust be obtained and used for performing test solidifications of radioactive samples.

6.0 TRST SOLIDIFICATION OF 4 TO 10 WT4 foRIC ACID (CDMCENTRATED WASTE) 6.1 Prerequisites NOTE: This PCP Test Solidification Procedure is applicable to Class A Unstable, Class A Stable, Class B and C Waste Forms.

For the interim, however, rt 'er to section 1.0.

6.1.1 A sufficient size sample of concentrated waste (approx. 1 liter) has been drawn and the following parameters analyzed for by Plant Chemistry

  • Moren
  • pH

+ Total Solids

  • Gamma Scan NOTE: The total solids and gamma scan are used for information purposes only to track waste characteristics and are not to be used in the Process Control Program calculations.

6.1.2 The Oph Quality Assurance Group has been contacted to inf orm them of the pending Test solidification to see if they care to witness the test.

OQA Monitor Contacted Name / Date / Time 6.1.3 The appropriate portions of Attachment 1 have been completed including waste classification, chemistry information, bal"=

calibration data and the sequential sample number.

6.2 Procedure l ..........__.........____............__............__..__ __......._--- ...__

NOTEt Tare weights of waste, cement, additives, etc. should.be obtained during performance of the following procedure.

Round off to the nearest gram.

6.2.1 Calculate the weight percent of Boric Acid on Attachmant 1.

6.2.2 MEASURE 500 gms of untreated concentrated waste into a container.

10.0 1372c

P dlNuclear Tsi.1 Operating Procedure 1104-201 __

Title Revision No.

Waste Solidification Process Control Program 14 6.2.3 RECORD the weight and volume on Attachment 1.

6.2.4 ADD 50 wtt sodium hydroxide (NaOH) to raise the pH between B to 8.5 for Class A unstable, Class A stable, B and C solidifica-tion. If pH is >8.5 than reduce to a range of 8 and 8.5 with sulfuric acid.

6.2.5 RECORD the weight of NaOH used and the adjusted pH on Attachment 1.

6.2.6 If large (i.e., foam causing) quantitier of detergents are present, TREAT the sample with an anti-foaming agent until the foam disappears.

6.2.7 RECORD the weight of anti-f oaming agent used on Attachment 1.

6.2.8 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 (oil),- ml (total sample) x 100 = n oil

a. If oil is present in stable waste in a quantity greater than 14 by volume, reduce the quantity of oil to less than 14 by skimming.
b. For unstable waste if oil is present and the volume is between 3 and 12% of the volume of waste, TREAT with an emulsifying agent such as Mayool 776 (20% of the volume of oil). Oil in concentrations > 124 by volume may not be solidified by this procedure. (Refer to Section 8.0 Test Solidification of Naste 011).

NOTE: The density of Maysol 776 is 1.0 g/ml; the volume in ml is equal to the weight in grams.

6.2.9 RECORD the t oil and the quantity of any emulsifying agent used on Attachment 1.

6.2.10 Recced the volume and calculate the weight of the treated Sample on Attachment 1.

6.2.11 Calculate the percent solido in the sample by completing items (9), (10), (11) and (12) in Section II of Attachment 1.

6.2.12 For the test solidification of the concentrated waste, measure l into a mixing vessel 400 ml of pretreated waste.

NOTE: Test solidifications should be conducted using a 1,000 ml disposable beaker or similar site container.

l l

11.0 1372c l

1

t

> RNuclear rx1 1 oporating Procedyre 1104-_281 Revision No.

Title ,

14 Waste Solidification Process control Program RECORD the volume AND weight of the treated sample on 6.2.13 Attachment 1.

(16)

Calculate the water in the sample by 1. completing items (15),

6.2 14 in Section III of Attachment and (17)

Solidifica-6.2.15 Using Figure 1 and the percent solids from the TestItem (12), DET tion Data Sheet, the required quantity of Portland Type I CALCULATE and WEIGH out cement.

RECORD the weight of cement on Attachment 1.

6.2.16 the required quantity of metto beads, CALCULATE and WEIGH out into a separate 6.2.17 anhydrous sodium metasilicate (ASMS),

i.e.,

vessel.

1.

RECORD the weight of ASM9 on Attachment 6.2.18 is being mixed.

6,2.19 Slowly ADD the cement to the test sample while it Mixing should be accomplished by stirring with ----............-....

an electric NOTE:

mixing motor with blade or manually with a rigid stirrerapproxi3atwly one until a homogeneous mixture is obtained, i l minute.

slowly ADD the ASMS to the test 6 20 After al the cement is added sample while it is being mixed.

After sufficient mixing (2 minutes after all the ASMS is added) 6.2.21 a homogeneous mixture is obtained, SEAL the sample so that Class B orand C

CURE at 120 + 5'T for 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> for Class A Stable, or at room temperature for Class A unstable.

................................--.................................... cure, the sample meets NUTE:

If at any time during the 24 hout the acceptance criteria, the liner solidification may proceed. However, no test solidification shall be  ;

disqualified without at least 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> of cure. ...

l i

has been met and sign 6.2.22 Verify the Acceptance Criteria (Section 12) and date Attachment 1.

per Section 12, 6.2.23 When the Acceptance Criteria has been met calculate the required quantities of cement and additives f or the full scale solidification using a liner type applicable f or this and waste type (as determined by Radwaste Jperations Engineering)for 4 to 10 the Solidification Calculation Sheet

( Attachment 2).

1372c 12.0

I'- U Nuclear T,1 1 Operating Procedure _ 1104-281 Title Revision No.

Wast e solidification Process control Program 14 NOTE: The liner shall be solidified using OP 1104-28A, Radio ,

active Waste Solidification - SEG. l

............___.... ....._...........____._........ ...............n._...__.__

6.2.24 Complete Section VII of AttacPnent 2 upon completien of the solidification if coment remains in the hopper.

7.0 TEST SOLIDIFICATION OF > 10 'IU 20 wt% DORIC ACID (CONCENTRATED WASTJR 7.1 Prerequisites NOTE: This PCP Test Solidification Procedure is applicable to class A Unstable, Class A Stable, Class B and C Waste Forms.

For the interim, however, refer to Section 1.0.

l 7.1.1 A suff'cient aire sample of concentrated waste (approx. 1 liter) has been drawn and the following parameters analyzed for by Plant Chemistry:

  • pH
  • Total Solide
  • Gamma Scan NOTE: he total solids and gamma scan are used for information

( purposes only to track waste characteristics and are not

[ to be used in the Process Control Program calculations.

l __............._..___ ........___..___.._.......................... ....._...

7.1.2 The Ops Quality Assurance Group has been contacted to inform them of the pending Test solidification to see if they care to witnese the test.

OQA Monitor Contacted 7.1.3 The appropriate portions of Attachment 3 have been completed including waste classification, chemistry information, balance calibration data and the sequential sample number.

1 13.0 1372:

P UlNuclear 1m.1

""* r Operating Procedure 1104-28I Title Revision No.

Waste Solidification Process control Program 14 7.2 Procedure NOTE: Tate weights of waste, cement, additives, etc. should be obtained during performance of the following procedure.

Round off to the nearest gram.

7.2.1 Calculate the weight percent of Boric Acid on Attachment 3.

7.2.2 MEASURE 500 gma of untreated concentrated waste into a contalner.

7.2.3 RECORD the weight and volume on Attachment 3.

7.2.4 ADD 50 wtt sodium hydroxide (NaOH) to raise 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.

7.2.5 RECORD the weight of NaOH used and the adjusted pH on Attachment 3.

7.2.6 If large (i.e., foam causing) quantities of detergents are present, TREAT the sample with an anti-foaming agent.

7.2.7 RiCORD the weight of anti-f oaming agent used on Attachment 3.

7.2.8 Determine if oil is present by looking for an oil film on the surface of the sample. If oil is present periorm the following ml (oil) -

ml (total sample) x 100 = _ g oil

a. If oil is present in stable waste in a quantity greater than 1% by volume, reduce the quantity of oil to less than 1% by skimming.
b. For unstable waste if oil is prewent 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 nay not be solidified by this procedure. (Refer to Section 8.0 Test Solidification of Waste 011).

NOTE: The density of Maysol 776 is 1.0 g/ml; the volume in ml is equal to the weight in grams.

7.2.9 RECORD the % oil and the quantity of any emulsif ying agent used on Attachment 3.

7.2.10 Record the volume and calculate the weight of the treated sample on Attachment 3.

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[r d] Nuclear ,,,.1

""* r  :

Operating Procedure 1104-281 l Title Revision No.

I waste solidification Process Contro1 Program 14 6

7.2.11 Calculate the percent solids in the sample by completing items (9), (10), (11) and (12) in Section II of Attachment 3.  ;

7.2.12 For the test solidification of the concentrated waste, measure into a mixing vessel 400 ml of treated waste.

l NOTE: Test solidifications should be conducted using a 1,000 ml disposable beaker or similar site container.

7.2.13 RECORD the volume AND weight of the sample on Attachment 3.

7.2.14 Calculate the water in the sample by completing items (15), (16) l and (17) in Section III of Attachment 3.

l l 7.2.15 Using Figure 1 and the percent solide from the Test Solidifica-tion Data Sheet, Item (12), DETERMINE the water /coment ratio then l CALCULATE and WEIGH out tb9 required quantity of Portland Type I cement.

I 7.2.16 RECORD the weight of emment on Attachment 3.

7.2.17 CALCULATE Lid WEIGH out the required quantity of anhydrous sodium metasilicate (ASMS) into a separate vessel.

7.2.18 RECORD the weight of ASMS on Attachment 3. ,

7.2.19 Slowly ADD the cement to the test sample while it is ceing mixed. ,

NOTE: Mixing should be accomplished by stirring with an electric mixing motor with blade or manually with a rigid stirrer l until a homogeneous mixture is obtained, approximately one I minute.

7.2.20 After all the cement is added, slowly ADD the ASMS to the test sample while it is being mixed.

7.2.21 After sufficient mixing (2 minutes after all the ASMS is added) l so that a homogeneous mixture is obtt._ned, SEAL the sample and l CURE at 120 + 5'T for 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> for Class A Stable, class B or C l or at room temperature for Class A Unntable.

l I

NOTE: If at any time during the 24 hour2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> cure, the sample meets

, the acceptance criteria, the liner solidifi ation may I proceed. However, no test solidification shall be dis-qualified without at leret 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> of cure.

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Nuclear ,,1 1

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l Operating Procedure 1104 281 Title j

Revision No. ,

l waste solidification Process control Program 14  !

I 7.2.22 Verify the Acceptance criteria (section 12) has been met and sign

-and date Attachment 3.

7.2.23 When the Acceptance Criteria has been met per Section 12.

calculate the required quantities of cement and additives for the  ;

full scale solidification using a liner type applicable for this  :

waste type (as determined by Radweste Operations Engineering) and f the Solidification calculation sheet for > 10 to 20 wt% Boric  !

Acid (Attachment 4). l NOTE: The liner shall be solidified using OP 1104-28A, Radioactive Waste solidification - SEO.

l f i

7.2.24 Complete Section VII of Attachment 4 upon completion of the 1 solidification if cement remains in the hopper. lI 8.0_ TEST SOLIDIFICATION OF WABTE OIL (12 - 40% Oil) )

i 8.1 Prerequisites  !

NOTE - 'This PCP Test solidification Procedure is app 11 cable to Class A Unstable, Class A stable, class B and C waste forms.

For the interim, however, refer to Section 1.0.

..........__..........___.....__.__.............__.................. ....... l  ;

8.1.1 A sufficient size sample (approx. 500 ml.) each-of pH adjusted concentraten waste and waste oil have been drawn.

NOTE: The pH of the concentrated waste will be adjusted in the tank before the test solioification.

8.1.2 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 l 8.1.3 A sequential sample nunbar has been assigned to the test and

! included on Attachment 5.

l l 8.1.4 A determination has been made as to the waste class of the l pending full scale solidification by Radwaste Ops. Engineering.

1'

[ 8.1.5 The balance calibration data has been included on Attachment S.

16.0 1372c

l'- U1 Nuclear ""**

Tm _1 Operating Procedure 1104-28I Title '

Revision No.

Waste solidification Process control Program 14 i

8.2 Procedure NOTE: Tare weights of waste, cement, additives, etc. should be obtained during performance of the following procedure.

Round off to the nearest gram.

8.2.1 Measure into a mixing vessel 210 ml of concentrated waste and 140 i

ml oil.

NOTE: Test solidifications should be conducted using a 1000 ml disposable beaker or similar site containcr.

8.2.2 Record the waste volumes added and calculate the parcent oil by volume on Attachment 5.  !

8.2.3 MEASURE out 20.0 ml (28.0 gma) of Maysol 776.

8.2.4 RECORD the quantity of the emulsifier on Attachment 5.

8.2.5 ADD the Maysol 776 to the waste and mix until a homogeneous mixture is obtained, at least five (5) minutes.

NOTE: Hixing should be accomplished by stirring with an electric mixer with blade or manually with a rigid stirrer. Any signs of pure oil may be an indication that the emulsion [

is breaking down. Should this occur, contact Radwaste ops. Engineering for further instructions.

ym&W-k .

d" 8.2.6 If large (i.e., faam causing) quantities of detergents are

\/j%fnN) s hl 'i present, treat, the sample with anti-foaming agent until the foam disappears.

\ l 8.2.7 Record the amount of anti-foaming agent used on Attachment 5.

l l 8.2.8 KEASURE out 447.3 gma of Portland Type I cement and 51.8 gms of I

anhydrous sodium metaoil.cate (ASMS).  ;

8.2.9 RECCRD the quantities of cement and ASMS on Attachment 5.

8.2.10 Slowly ADD the cement to the test sample while it is being mixed l and mix until a homogeneous mixture is obtained but in no case less than one (1) minute.

8.2.11 After all the cement is added, slowly ADD the ASMS to the test sample while it is being mixed.

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i luCl88r yR1 1 Operating Procedure 1104-28I {

Title Revision No.  ;

i Waste Solidification Process Control Program 14 {

8.2.12 MIX for two (2) minutek after all the ASHS is added and homo- -l geneous mixture is obtained.

8.2.13 Seal the sample and cure at 120 + 5'F for 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> for Class A Stable, Class B or C or at room temperature for Class A Unstable. ,

4 t

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 disqualified without at least 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> of cure.  !

..........__.........................__.__..........._____................... i 8.2.14- Verify'the Acceptance criteria (Section 12.0) has been met and -[

sign and dcte Attachment 5.  !

8.2.15 When the Acceptance Criteria has been met per section 12, j calculate the required quantities of cement and additives for the  ;

full scale solidification using a liner type applicable for-this waste type- (as determined by Radwaste Operations Engineering) and f the Solidification Calculation Sheet for Waste Oil (Attachment  :

6). l l

NOTE: The liner shall be solidified using CP 1104-28A, Radioactive  !

Waste Solidification - SEG. l t

l

-9.0 TRST SOLIDIFICATION OF USED PRBOOAT f 9.1 Prercquisites i I

NOTE: This PCP Test Solidification procedure is applicable to i Class A Stable, Class B and C Waste Forms, i For the intertm, however, refer to Section 1.0. I i

..______._............................_.....________..................__..... I l i

9.1.1 A sufficient size sample of used precoat (approx. 500 ml) has  !

been drawn and the following parameters analyzed for by Plant i Chemistry: {

i

  • pH (of sluice water) i e Gamma Scan 18.0 1372c

p I'- U1 Nuclear Tm 1 Operating Procedure 1104-28I Title Revision No.

Waste solidification Process Control Program 14 NOTE: Where high activity waste coula pose personnel radiation exposure problems when perf orming the test solidification, expended powdex with an appropriate anion / cation ratio shall be substituted. The ratio shall be determined by Radwaste Operations Engineering. A sma *t.ple of use precoat

(= 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.

9.1.2 The sample has set to veru 3 _ 6 oil by volume.

9.1.3 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.

00A Monitor Contacted Name / Dato / Time '

9.1.4 The appropriate portions of Attachment 7 have been completed including the balance calibration data and the sequential sample number.

9.2 Procedure NOTE: Tate weights of waste, cement, additives, etc. should be obtained during perf ormance of the following procedure.

Round off to the nearest gram.

9.2.1 MEASURE out 301.1 gma of dewatered rowdered resin and 151.5 gma of water and place into separate containers.

NOTE: Teet solidification ohnuld be conducted using a 1,000 ml disposable beaker or similar size container.  !

( __.______.................... ._______..............__.___..__ .____. __._. _

9.2.2 RECORD the volume and weight of the powered resin on Attachment 7.

9.2.3 ADD the water to the powered resin and RECORD the weight of water added and the total volume of waste slurry (water plus resin) on Attachment 7.

9.2.4 If any foam is present, TREAT the sample with an anti-foaming agent.

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Auclear 2.,11

""='"

l operating Procedure 1104-28I i Title- Revanica ** .

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Waste solidification Process Control Program 14 l

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9.2.5 RECORD the quantity of stati-foaming agent used on Attachment 7. (

9.2.6 Determine if oil is present by looking for an oil film on the i surface of the sample. If oil is present perferm the followings ml (011) -

ml (total sample) x 100 =  % 0.1 l i

a. If oil is present and the volume is between 3 and lik of the  !

volume of waste, TREAT with an emulsifying agent such as .

Maysol 776 (20% of the velume of oil). Oil in {

concentrations > 12% by volume may not be solidified by this  !

procedure. Contact Radwaste Operations Engineering for  !

guidance.

{

I NOTE: The density of Maysol 776 is 1.0 gm/ml; the volume in f m1 is equal to the weight in gms. j 9.2.7 RECORD the quantity et oil present and the amount of Maysol added to the sample on Att.chment 7. ,

9.2.8 RECORD the initial pH of the sample on Attachment 7.

f 9.2.9 MEASURE out approximately 10 grams of calciua hydroxide ca(oH) ,

also known as hydrated lime.

' t 9.2.10 slowly ADD the calcium hydroxide to the powdered resin slurry, j two (2) grams at a time. MIX for three (3) minutes between i additions until the pH is at least 11.5. ADD an additional three [

(3) grams of calcium hydroxide. This final addition may or may [

not alter the pH of the slurry. t I

NOTE: Mixing should be accomplished by stirring with an electric  ;

mixing motor with blade or manually with a rigid stirrer f until a homogeneous miFture is obtained approximately one (1) minute. ]l; f

9.2.11 RECORD the quantity of calcium hydroxide added to the slurry and  !

the final pH on Attachment 7.

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9.2.12 KEASURE out 444 gma of Portland Type 1 cement.

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9.2.13 . RECORD the amount of cement on Attachment 7. ,

t 9.2.14 Slowly ADD the cament to the test sample while it is being mixed.  !

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I'- U 1 Nuclear' .1 Operating Procedure 1104-2BI Revision No.

Title 14 Waste solidification Process Control Program 9.2.15 MIX for two (2) minates after all the cement is added to obtain a homogeneous mixture.

7.

9.2.16 RECORD the final sample volume on Att.achment 9.2.17 Seal and allow the sample to CURE for 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> at 120 1 5'F.

If at anytime during the 24-hour cure time, the sample NOTE:

meets the acceptance criteria, the liner solidificatton may proceed. However, no test solidification shall be dis-qualified without at least 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> of cure.

has been met, sign 9.2.18 Verify the acceptance reiteria (Section 12.0) and date Attachment 7.

9.4.19 When the Acceptance Criteria has been met per Section 12, calculate the required quantities of cement and additives using a liner type applicable f or this waste type (as determined by Radweste Operations Engineering) and the Solidification Calcula-tion Sheet for Used Precoat (Attachment 8).

NOTE: The liner shall be solidified using OP 1104-2CC, Primary l Rosin and Precoat Processing - SEG. I 10.0 TEST SOLTDIFICATION OF 9EAD RESIN 10.1 Prerequisites NOTE: This FCP Test Solidification Procedure is applicable to class A Stable, Class B and C Waste Forms.

For the interim, however, refer to Section 1.0. l 10.1.1 A suf ficient size sample of bead resin (approx. 500 ml) has been drawn and the following parameters analyzed for by Plant Chemis-try:

  • pH (of sluice water)
  • Gamma Scan 21.0 1372c

[c gjNuclear ,,,_1

""* r Operating Procedure 1104 281 Title Revision No.

Waste Solidification Process Control Program 14 NOTEI 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 mls) 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 calculatior.s.

10.1.2 The sample has set to verify $ 1% oil by volume.

10.1.3 The Ops Quality Assurance Group has been contacted to inform them of the pending Test Solidification to see J f they care to witness the test.

OQh Monitor Contacted hame / Date / Time 10.1.4 The appropriate portions of Attachment 9 have been completed including the balance calibration dats and sequential sample number.

10.2 Pro edure

! TOTE: Tare wolghts of waste, ceroent , additJves, etc. should be l obtained during performance of the following procedure.

Round off to the nearest gram.

10.2.1 MEASURE into e mixing vessel 240 gm of dowatered resin.

NOTE: Test solidification should be conducted using a 1,000 ml disposable beaker or similar size container.

NOTE: Tap the beaker gently to consolidate the resin prior to measuring the volume.

f 22.0 1372c

Ir LJ1 Nuclear ,,,-1 Operating Procedure 1104-201 Title Revistor. No.

Waste solidification Process Control Program 14 10.2.2 RECORD the weight and volume of the sample (resin and water) on Attachment 9.

10.2.3 WEIGH out 2.1 gms of EC-3 into a separate vessel.

10.2.4 RECORD the weight of EC-3 on Attachment 9.

10.2.5 WEIGH out 84.3 gms of water and record the weight on Attachment 9.

10.2.6 ACO the water to the vessel containing the EC-3 and mix tnoroughly.

10.2.7 ADD the water /EC-3 mixture to the bead resin and mix thoroughly. ,

10.2.8 If any foma is present, TREAT the sample with an anti-foaming agent.

10.2.9 RECORD the quantity of anti-foaming agent used on Attachment 9.

10.2.10 Determine if oil is present by looking for an oil film on the surface of the sample. If oil is present perform the followings ml (oil) -

ml (total sample) x 100 = ,,,.,,,t oil

a. If oil is present and the volume is betwser. o.. 12% of the ,

volume of waste, TREAT with an emulsif yi 'y s jent such as Haysol 776 (20% of the volume of oil). O!! .:

concentrations > 124 by volume may not be wA l'.'ified by this procedure. Contact Radwaste Operations Engineering fi guidance.

l l

l NOTE: The density of Haysol 776 is 1.0 gm/ml; the volume la ml l is equal to the weight in gms.

\ ------------------------- .....-----------------------------------.----------

10.2.11 RECORD the quantity of oil and the volume of emulsifier used on Attachraent 9.

10.2.12 RECORD the initial sample pH on Attachment 9.

10.2.13 MEASURE out approximately 11.5 gms of Calcium Hydroxide Ca(OH)2' also known as hydrated lime.

I l

23.0 1372c ,

luCIS8r T31 1 operating Procedure 1104-28I I Title Revision No.

Waste Solidification Process control Program 14 l 4

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10.2.14 Slowly ADD the Ca(OH), to the resin sample two (2) grams at a time. Hix for three (3) minutes between additions until the pH of the slurry is at least 11.5. ADD three (3) additional gma of ,

Ca(OH) . '.'his final additional may or may not alter the pH of  :

the slurry.

j 10.2.15 RECORD the quantity of calcium hydroxide added to the slurry and l the final pH on Attachment 9.

10.2.16 HEASURE out 178.2 gms of Portland Type I cement into a separate vessel.

10.2.17 RECORD the weight of the cement on Attachment 9. -  ;

f

~10.2.18 Slowly ADD the cement to the test sample while it is being mixed. i i

10.2.19 MIX for two (2)-minutes after all tne cement is added to obtai. a i homogeneous mix.

10.2.20 RECORD the final sample volume on Attachment 9.

10.2.21 SEAL the sample and allow tre sample to CURE for 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> at 120 ,

+ 5'F.

l t

[

NOTE: If at anytime during the 24-hour cure time, the sample l meets the acceptance criteria, the liner solidification may I proceed. However, no test solidification shall be die. [

qualified without at least 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> of cure. [

10.2.22 VERITY the acceptance criteria (Section 12) has been met, sign  ;

and date Attachment 9.

10.2.23 _ When the- Acccptance Criteria has been met per Section 12.0, ,

CALCULATE the required quantities of cement and additives using a  !

liner type applicable for this waste type (as determined by l Radwaste Operations Engineering) and the Solidification Calcula- E tion Sheet for Bead Rosin (Attachment 10). f t

NOTE _ The liner shall be solidified using OP_ 1104-28C, Primary. I Rosin and Precoat Processing - SEG.  !

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LM1Nuslear 1,1 1 operating Procedure 1104-281 Title Revision No.

Waste Solidification Process control Program 14 11.0 ALTEkMAD _ TEM SOLIDIFICATION PkOGRAMS NOTE: The PCP Test Solidification presented in this procedure should cover the majority of the waste processing require-  ;

ments of TMI-1. In the event a dif ferent 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 ptocedure provided by Westinghouse - SEG.

For the interim, any alternate procedures utilired shall be for unstable waste forms only.

l 11.1 Prerequisites 11.1.1 A procedure is available for the particular waste stream to be processed.

11.1.2 This procedure has been verified current by the Radwaste Ops.

Manager or his designee and will be reviewed by the Radwaste Engineer prior to its use.

11.1.3 The sample required by this procedure has been obtained and applicable chamistry parameters analyzed for by Plant Chemistry.

Applicable skmple results have been ir:luded or Attachment 11.

i 11.1.4 The Ops Quality Assurance Group has been contacted to inform them l of the pending Test solidification to see if thsy care to witness I

the test.

OQA Monitor Contseted__

Name / Date / Time 1

11.1.5 Balance calibration data has been included on Attachment 11.

l l 11.1.6 Attac hment 11 has been completed.

11.2 Procedure 11.2.1 Performed the applicable portions of the Westinghouse - SEG  ;

procedure.

11.2.2 Verify acceptability of the test solidification per Section 12.0.

11.2.3 GPUN management shall verify all calculations and document such on Attachment 11.

i 25.0 1372e

luCl88r ,,,.1 operatine Procedure 1104-281 Title Revision No.

Uaste solidification Process control Program 14 12.0 ACCEPTANCE CRITRAIA 12.1 solidification Acceptability 12.1.1 The sample solidification is considered acceptable if there is not visual or drainable free water.

12.1.2 The sample solidification is considere'd 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 surf ace 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 12 2 solidification Unacceptability 12.2.1 If the waste fatis any of the criteria set forth in seation 12.1 the solidification will be termed unacceptable and a new set of solidification parameters will need to be established under the procedures in Section 12.3.

12.2.2 2f the test solidification is unacceptable then the same test procedure must be followed on each subsequent batch of the came type of waste until three consecutive test samples are solidi-fled.

12.3 Alternais solidification Parameters 12.3.1 If a test sample for class A unstable waste fails to previde 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. ^J4 additional 50 wt.t NaOH to raise the pH above 8 but less than 9.2 for borated wastes.
c. If the waste (other thsn waste oil) is only partially solidified, use lower waste to cement and Metso ratios.

Using the recommended quantities of cement and Hetso Beads, 26.0 1372c

_ u . 2_ _ .-- , . _ _ _ _ _ _ _ _ . . . _ , __, _.,___._m

V L)1NUCl68Y m .z Operating Procadure 1304-201 Tit le Revision No.

Waste solidification Process control Program 14 reduce the waste sample to 375 ml and continue reducing the sample volume by 25 ml. until the acceptability criteria of Section 12.1 are met.

d. If the waste oil mixture is only partic.lly solidified try using lower waste to coment ration. Reduce the quantity of waste by 25 ml. and the emulsifier by 1 ml., (This will result in a slight 1s ;igher concentration of emulsifier in the waste) and proceed with the test solidification.

Continue with similar reductions until a satisfactory product is achieved.

12.3.2 For Class A stable, Class B end C waste test samples that fail to solidify, Contact Radwaste Operations Engineering for resolu-tion.

t 27.0 1372c

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