ML20081C150

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Rev M to Procedure SD-OP-003, Process Control for Chem-Nuclear Sys,Inc Cement Solidification Units
ML20081C150
Person / Time
Site: Catawba Duke Energy icon.png
Issue date: 05/20/1983
From:
CHEM-NUCLEAR SYSTEMS, INC.
To:
Shared Package
ML20081C146 List:
References
SD-OP-003, SD-OP-3, NUDOCS 8403120156
Download: ML20081C150 (20)


Text

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REV. CESCRIPTION DATE ATPROVED A Complete Reurite ' 6/24/81

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B Incorporate Changes C Complete Rewrite 9/11/81 9/29/81 h@ h  ! 0 Incorporate Chance Per Chance A7/hl./[ M d h

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V , E Incorpor:tte Changes Per Omnge Request

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G Recueet cD-Oo-003-0; 3/z(a/f D N.'$ h CHANGFM DFS GW:GE SD-OP-003-06 l 7 /3 7/VM y/gh  ; _H _OW3GES PER OWiGE RECCEST SD-OP-003-07,, J CHANGES PER OIANGE REDUEST SD-OP-003-08 [ff//FA dj/kg//pdf) K i /j /' : 2. , ;4d,7./ CHANGES PER CHANGE Rtwtsr SD-OP-003-09 y//t/ f/ 3 / 'LQfA ]v L M OIANGES PER CHANGE REQUEST SD-OP-003-10 3k/hh b [ M ,__'k _ QWEES PER OIANGE REQUEST SD-OP-003-11 ///f/JS [///T/L/ L / l I

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NOTE: THIS INFORMATION IS CONSIDERED PROPRIETARY AND IS NOT TO E E RELEASED T.'ITEOl'T WP,ITTEN PERMISSION OF CHEM-NUCLEAR SYSTE.MS, IMC. f _ ' j>: 7

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3 SHEET 1 J 8403120156 831028 cssaioansas PDR ADOCK 05000413 E PDR

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    .,. r.                                                                                                    3 TABLE OF CONTENTS t

Page 1.0 SCOPE 3

2.0 REFERENCES

3 3.0 SYSTB1 DESCRIPTION 3 4.0 REQUIRDIENTS FOR SAMPLING TESTING 6 5.0 TEST DOCUMENTATION 8 6.0 AIA!INISTRATIVE IROCEDURES 8 TABLE 1 - Equipnent Recommended For Testing Sample 9 FIGURE 1 - ICP Solidification Of Boric Acid Concentrates (N-24, Cement, Lime Sequence For PWR Waste) 10 FIGURE 1-A - ICP Solidification Of Boric Acid Concentrates (Lime, Cemen: Sevence For PWR Waste) 12 FIGURE 2 - ICP Solidification Of Particulate Wastes (Resin . Beads, Powdex And Diatonneeous Earth Slurries) 14 FIGURE 3 - ICP Solidification Of Sulfate Concentrates (BWR ( Wastes) 16 FIGURE 4 - ICP Solidification Of Miscellaneous Aqt.eous Wastes 18 FIGURE 5 - Liner And Cask thlculations 19 FIGURE 6 - ICP For Preparation Of Fluid Mixture For In-Situ Solidifications 20 l i I DOCUMENT REV. SHEET SIM)P-OO3 K 2 j CNSQ 1002/8 78

h AR T 1.0 SCUPE 3 1.1 Purpose The purpose of the Process Control Program for CNSI Cement Solid-( ification Units is to establish processing conditions assuring safe and effective solidificatiert of various low-level radio-active waste liquids and slurries including resins, concentrated

                      ,       liquids, and the various filter sludges produced by IVR and BWR utilities.

1.2 Applicability This Process Control Program shall be used by all personnel op-erating the CNSI Gement Solidification Unit. 'Ihis procedure is applicable to all liners listed on Figure 6 except the 21-300. 2.0 REFERENClS 2.1 QA-AD-OOl, Cf.SI Quality Assurance Program 2.2 CN-AD-019, CNSI ALARA lblicy 2.3 LN-AD-002, CNSI Design Control 2.4 CNSI Operating Procedures for Gement Solidification Units, as applicable 2.6 NUnEG 0472, Hadiological Effluent Technical Specifications for PWM

2. 6 NUREG 0473, P.adiological Etfluent Technical Specifications for BWR 2.7 branch Technical Position-ESTB 11-3, Design Guidance for Solid Radioactive Waste Management Systems Installed in Light-Water-Cooled Nuclear Power Reactor Plants 2.8 ANSI 199, Liquid Radioactive Waste Processing Systems for Pres-surized Water Reactor Plants 2.9 ANSI 197, Liquid Radioactive Waste Processing Systems for Boiling Water Reactor Plants 2.10 NRC Hagulatory Guide 1.143, Design Guides for Radioactive Waste Management Systems, Structures, and Components Installed in Light-Water-Cooled Nuclear Pbwer Plants
                   -2.11      Design t.nd Control of Concrete Mixtures, 12th Edition, Pbrtland Cement Association.

3.0 SYSTEM DESCRIVrION 3.1 Process Description The CNSI Cement bolidification Unit is specifically designed to -( facilitate solidification of various radioactive wastes including evaporator bottoms and ion exchange resin slurries and sludges. DOCUMENT REV. SHEET ( SD-OP-OU3 L 3 j cNSQ 1002/8 78

. .y .. . 3 Inmobilization of the waste is accmplished using readily avail-able Portland I Cement in conjunction with hydrated lime and particular process additives. Other Portland Cements, Types II and III, may be employed for specific waste handling conditions [,. requiring controlled modifications of cement activity. h e waste is solidified in a disposable liner which may already contain same of the required conditioning chetnicals. Pre-installed mixer blades permit continuous agitation until a thick cement Mste has

                    ' fomed that will set to a hard, uniform, water-free matrix. he end product is a true cement structure fomed in accord with established principles of concrete technology.

3.2 Process Parameters Portland Type I Cement combines with water through several inter-mediate reactions to fom stable hydrates from chemically ccm-bined mixtures of calciun, silicon, altnintn, and iron oxides. These reactions are exothemic (heat producing) and do not pro-gress rapidly unless a strongly alkaline pH (11-12) is main-tained. Waste streams may contain certain metallic radionuelides that are chemically bonded (and not leached) in the ~ cement struc-ture without loss of product strength. Other constituents can significantly accelerate or retard cement set, and must be con-trolled by the addition of selected chemical agents. Judicious control of total cement content maximizes waste volume efficiency and minimizes heat developnent for large voltne solidifications. Preferred waste to additive solidification ratios have been detemined by the C4SI Research and Develonnent ProgIsm, but it is reccgnized that waste stream composition and C density are variable, and that verification cf the solidification fomula is necessary for each new lot of waste liquid. Eis important consideration is detailed by waste fom in Figures 1 throtgh 4. 3.3 Solidification Unit Description 3.3.1 h e CNS! Cement Solidification Unit is a portable system containing all piping, support, control and monitoring equipnent necessary to solidify radioactive liquid waste using the cement process. 3.3.2 he unit is composed 'of several processing subsysterrs, each controlling a specific function of the cement pro-cess. Rese subsystems include waste transfer, chemical addition, cement conveyor, vent, and dewater systems. Control functions for the unit are incorporated into the pnetmatic and main control pnels. Service supplies are provided by the utility and distributed through the ser-vice air, water, and electrical distribution systems. t

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DOCuteENT REV. SHEET SD-OP-003 - G 4 L J CNSQ 1002/8-78

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                  ,                                                                                              l 1       t' 3.3.3    Most of the unit canponents are arranged on portable frameworks (skids) to provide flexibility of operations for either indoor or outdoor use. W e cement conveyor,

( control panel, punp skid, hydraulic skid and fillhead contain most of the major elements of the mobile unit. 3.3.4 A closed-circuit television system is an integral part of the unit and allows the operator to monitor the solidification process. 3.4 System Operation 3.4.1 Before beginning any waste processing with the & ment Solidification Unit, the CNSI operator shall conplete a successful sample solidification in accordance with the Sample Verification Procedure of Section 5.0. 3.4.2 he sample solidification information is recorded on a CNSI Solidification Worksheet, and is used in con,iunc-tion with Figures 1 through 5 to calculate full sca h values. 3.4.3 Actual waste solidifications shall then be conducted in accordance with the Operating Procedures (Ref. 2.4) using full scale formulas as calculated on CNSI Solidi-fication Worksheets. 3.4.4 Sequence of Operation The conditioning chemicals may be preloaded, in some cases, into the liner or added to the waste while mixing. he addition of chemicals or waste usually may

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be interrupted without ill effect. W e mixer may also be secured during waste or chemical addition with no effect on the process, but must remain in operation during those additions necessary for proper solidification. . l l 3.4.o haste-to-Cement Hatio (by voluns) The normal volune ratio of waste to solidification com ponents will be approximately 2 to 1 up to 3 to 1 for

evaporator concentrates and other liquids and 2.5 to 1 l for resins, powdex and other solids. If recairnended ratios are exceeded, cure time may. be delayed and there may be reeldual free-standing liquid in the vessel after solidification.

k DOCUMENT REV. SHEET

                    - SD-OP-003                                            G             S k                                                                                               J CNSQ 1002/8 75
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   ,                       3.4.6      Cure Tirne

( Cure time will usually be 1.! to 36 hours as shown by a continuing temperature rise. Ttle liner should be venti-l lated until tempcrature begins to decrease indicating safe completion of the solidification process. 4.0 RHJUIRBiENTS FOR SAMPLE TESTING 4.1 General Precautions 4.1.1

                                     'Ihe chemicals and cement used are considered non-toxic and safe to handle, however, care should be used to avoid breathing dust.      If a liquid caustic is used for special applications, follow the safety precautions out-lined in the appropriate operating procedure, Hef. 2.4.

NOTE: IF DIFFIGLTIES ARE ENCOUNTEED WI'Ill ANY PART OF THIS VER-IFICATION PROCEDURE OR UNEXPECIED RESULTS ARE OlsrAIhTD, CON-TACT THE SOLIDIFICATION MANAGER OR SUPERVISOR. 4.2 Radiological Precautions 4.2.1 'Ihe CNSI operator shall be subject to the applicable Health Physics and safety precautions of the facility providing the radioactive waste. f 4.2.2 laboratory gloves, face shield and an apron shall be ( worn while handling, collecting and testing of all samples. 4.2.3 'Ihe CNSI operator shall ensure that radiologically clean and contaminated zones are established in the sample process area to prevent the possible spread of contamination. 4.3 Prerequisites 4.3.1 Waste Hecirculation l 4.3.1.1 Due to the' importance of obtaining a repre-sentative sample for use in the verification procedure, the waste generating facility per-l sonnel shall confirm that the contents of the waste storage tank have either been recircu-lated for a minimum of three volume turnovers or are adequately mixed to achieve a homr>- geneous mixture. 4.3.1.2 Any number of mechanical operations of the waste storage tank may negate the effects of previous recirculation / agitation period. These operations would include the following: DOCUMENT REV. SHEET SD-OP-003 F 6 L J CNSQ 1002/8-78

  • r-3 4.3.1.2.1 Introduction of additions 1 waste into the storage tank after re-circulation has corrmenced.

4.3.1.2.2 Securing of recirculation while drawing the verification sample. 4.3.1.2.3 Shifting from a recirculation mode to a transfer mode. 4.3.1.3 If any of the situations listed above occur, it will be necessary to repeat the recircu-lation process and sample verification pro-cedure of Section 5.0 in order to re-estab-lish the solidification process parameters. 4.3.2 Waste Identification 4.3.2.1 he utility supplying waste shall provide waste composition and properties. % e CNSI operator may confirm waste density and pH as necessary. NME: WASTE CONTAINING OIL ABOVE ONE PECENT BY VOLEME SHAll NW BE SOLIDIFIED BY THIS PCP. 4.3.3 Equipment Equipnent required to use during the sample verification procedure is listed in Table 1. %e table indicates the reconnendeo quantity to begin a verification procedure. The CNSI operator shall ensure that all necessary equip-ment is available or adequate substitutes are available. The CNSI operator shall ensure that additives receivM comply with the chemical composition necessary for this process. 4.4 Sample Acceptance Criteria The sample verificstion is performed by examination of lab com positions containing actual waste material. %e tect confirms the correct process constituents. Et acceptance criteria for a good product are as follows: 4.4.1 Visual inspection of the end product af ter solidifi-cation indicates a uniform, dry, free-standing monolith. DOCUMENT R EV. SHEET SD-OP-003 F 7 L J CNSQ 1002/3 78

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4.4.2 'Ihe end product msists penetration when probed with a spatula or other firm object. 4.6 Hequirements for Sample Verification 4.5.1 Verify that all materials listed in Table 1 are avail-able and ready to use in the area selected by the util-ity for solidification testing. 4.6.2 Be prepared to complete the test procedures outlined in Figures 1 through 4, as applicable, when conducting sam-ple verifications. 4.5.3 Sample Hequirements 4.6.3.1 A sample shall be solidified prior to full scale solidification of waste. If there is no change in the chemical composition of the waste as verified by the utility, (Ref. 4.3.1) test results and full scale solidifi-cations will be consiaered reproaucible. Thereafter, a sample solidification will be conducted prior to the tenth batch solidified from the same source of waste. 4.6.3.2 'lhe CNSI operator shall ensure, much as possible, that the test sample it represen-tative (i.e; thoroughly mixed) and that the sample line has been properly purged prior to i drawing the PCP sample. 5.U TEST IX1CUMENTATION b.1 Calculate and record the required test information on the CNSI Solidification Worksheets for all waste sample verifications. 6.2 Use the appropriate figure (1 through 5) for test instructions and documentation for the various wacto forms to M solidified. l ' ! 6.0 A1111NISTHATIVE PROCEDURES 6.1 'the CNSI operator shall forward a copy of each completed CNSI Soldification Worksheet to the Manager, Solidification Services

for review following completion of liner solidification.

6.2 '1he CNSI Solidification Worksheets and related instruction sheets l are considered as proprietary information and not to be distri-buted outside of Chem-Nuclear Systems, Inc. Each CNSI operator shall maintain a controlled tile of these documents for his own reference. (.l L DOCUMENT REV. SHEET SD-UP-UU3 L 8 CNSQ 1002/8 78

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 ,,                                         ECUIPMENT RECOMMENDED FOR TESTING SAhBLE e
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250 ML Plastic beakers With Lids (12) Solidification chemicals should 600-1000 E Plastic Containers (10) be the same as used in full Wide Blade ' Spatula (2) scale operation and should be 0-2120 Fahrenheit Thennoneters (3) stored in capped containers. pH Paper: Wide Range (O To 9.0) Farrow Hange (9.0 to.13.0) 0-600 or 0-1000 gm Triple Beam Balance Hydroneters, Bange 1.000 - 1.200 and 1.200 - 1.400, or equivalent Hot Plate, Varihble Temperature Control Pyrex Beakers, 600 ML Capacity (12) httrking IVn Sample Heating Oven, Thermostatically 03ntrolled Fran 1000 F to 1800 F. (See NOTE) Graduated Cylinders, 250 ml (2) NOTE: WASTE S1IDIFIED WITH CBENT ON A SMALL SCALE AT AMBIENT TEMPERATURE WILL SET MUG M0ltE ELCWLY DUE IU RBIOVAL OF EXOTHERMIC HEAT. SAMILE CONDITIONING IN A TDIPERATURE-00ffrRQ1ED OVEN PERMITS MORE MEANINGF1L EVALUATION OF KLIDIFICATION RESILTS IN 6-24 HOURS AS SPECIFIED FG THE WASTE FORM, m AS ESTALISHED BY EXPERIENCE AT A PARTICLLAR UTILITY. k DOCUMENT R E V. SHEET L SD-OP-003 G 9 L s J CNSQ 1002/8-78

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F. 3 FIGURE 1

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PCP SCLIDIFICATION OF BORIC ACID CONCENTRATES

    .                              (N-24, CEMENT, LIME SWUENCE lOH PWR WASTE) 1.0     SAMILE VERIFICATION NorE: 'IIIE QIDlICE ADDITIVES USED FOR FCP PREPARATION SHOUE BE 'IHOSE ACrD-ALLY USED IN FILL-SCALE SCLlDIFICATI(N AND SHOUE BE SIORED IN CAPPED CONTAINERS.

1.1 Frcm past experience and the analysis supplied by the utility, deter-mine the appropriate FCP solidification formula using the table below. Note that boric acid waste that has been partly neutralized un-inten-tionally or to reduce storage temperature may require different or additional solidification agents and result in less efficient waste handling. Waste temperature must also be considered in detemining the preferred ICP fomula and full-scale material requirements. Table Bomn Content Boric Acid Waste *WT. Of CNSI *WT Of CNSI Weight Of Weight Of (ppm) Equivalent Volume Agen t N-24 Agent N-50 Cement Lime O- 6,900 0-4% 200-210 ML 5 Gi 0-5 G1 170-210 G1 60-80 GI 7,000-21,000 4-12% 210-240 hL 10 G1 0-10 Gi 130-180 G1 60-80 G1 Above 21,000 Above 12% 220-250 ML 15 G1 0-15 G1 120-170 G1 60-80 G1

  • Typical Amount Or As Required By Test Results I' 1. 2 Notify the utility that preparations for verification testing are ccm plete and that a sample is required.
1. 3 If waste sample has crystallized and is non-uniform, the entire sample must be heated to 1400 F or above until crystals have re-dissolved.

Then measure out waste volume required in 250 ml graduate and immed-iately transfer to a 600 ml pyrex beaker. 1.4 If sample is less than 1600 F, heat sample to 1600 F on the hot plate using a glass rod to occasionally stir contents. Then remove beaker from the hot plate and, when temperature is .iust 1600 F, inmediately add required weight of CNS! Agent N-24. Stir vigomusly to disperse ' powder in hot liquid, and note maximin temperature reached during the 30 seconds of stirring after addition. Record temperature on CEI Solidification Worksheet I, Item (b). If temperature does not increase by about 6-100 F, it may be necessary to add CNSI Agent N-50 to assure desired solidification. 1.5 Add inmediately the required weight of CNSI Agent N-50 and cement , and disperse thoroughly with spatula. Use minimtn cement weight in accor-- dance with experience, and add CMI Agent N-50, as necessarv. M.Un4ENT R EV. SHEE1 SD-OP-003 J 10 V J cNso icons.7s ~~

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1. 6 Proceed directly with lime _additica and using minimum weight for first lime addition, or if experience with the particular waste

( form indicates that the Irquired pH will be achieved with a quan-tity of lime different than the mininum indicated on the table, that-quantity may be used for the first lime addition. Mix with spatula and check pH with litt:ns paper to confirm a value of 11 or above. ' Add more lime if pH is low or if mix is too watery. 1.7- Transfer entire sarrple to a 250 ml container using spatula.  ! Attaen lid firmly and place sample 'in oven at 165 + 50 F.

1. 8 ' Maintain sealed. sample in oven for 6-24 hours according to past experience et that particular utility. Then remove sanple from oven and allow to cool for at least 2 hours before unsealing and evaluating solidification results according to guidelines of Paragraph 4.4.

NOTE: DIE 2-HOUR COOLING PFRIOD CAN BE DELETED IF EXPERIENCE WITH DlIS PARTICULAR WASTE STREAM INDICATES DIAT NO WATER IS

                                      ' STANDING ON DIE SAMPLE AND IT MEETS DIE RLVJIREMBrfS OF PARAGRAMI 4.4.

2.0 FU1L SCALE CAlfULATIONS 2.1 D2tennine the volume (cubic feet) of waste to be received by com-picting CNSI Solidification Worksheet II or according to past ex-perier.ce at the particular utility. { 2.2 Be sure that total solidification weight and waste radiation level is consistent with allcmable transportation regulations and

                           ' requirenents.

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DOCUSAENT = RE V. SHEET SLM)P-003 J 11 e - J CNSQ 1002/5 75

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FIGtRE 1-A ' PCP SCLIDIFICATION OF HORIC ACID CMCENTRATES (LIME, CEMENT SWUENCE M PhR %ASTE)

.        1.0     SAMILE VERIFICATION NOTE: THE OEMICAL ADDITIVES USED MR PCP IREPARATION SHOLLD BE THOSE ACT-DAILY USED IN PtLL SCALE SCLIDIFICATION Am SHOLLD BE S'KRED IN CAPPFD CONTAINERS.

1.1 Frm the waste analysis supplied by the utility, detennine the appropriate additives from the following chart and enter the amounts on CNSI Solidification Worksheet I. Use minimum amounts of cement and lime in accord with waste properties and past experience. CHART 1 Boric Acid Otlcitm *CNSI *Soditri Boron Omtent F4 uivalent Cement Lime 011oride Moderator Hydroxide Of Waste (PRI) (By Weight) (gms) (gms) (gms) S-4 (gns) (50% Solu.) 0- 3,500 0-25 190-240 10-20 3.0 10 2.5 ml" 3,500- 7,000 2-4% 180-230 20-30 3.0 10 2.5 ml" 7,000-10,000 4-6% 170-220 30-40 3.0 10 2.5 ml" 10,500-14,000 6-8% 160-210 40-50 3. 0 10 2.5 ml" 14,000-17,500 8-10% 150-200 45-60 3.0 10 2.5 n1" 17,500-21,000+ 13-12%+ 145-190 50-70 3.0 10 2.5 m1** clypical Amounts Or As Hequired, If Any, Bv Test Results.

        **0r 5 nL Of 25% Solution.

f* 1.2 Notify the utility that preparations for verification testing have been ccmpleted and request that a sample be taken.

1. 3 Freshly screen sufficient lime and cement in separate containers to avoid undispersed 1trnping in the samples.

1.4 Add calcita chloride, CNSI Moderator S-4, and lime (as indicated in Chart 1) to a 600-J000 ml container. 1.5 Ehsure that the waste sample is uniform by heating to 14qc F or more, if necessary, and then add 200 m1 to each container. Mix thomughly using wide blade spatula and then check the pH of each sample with riarrow range paper and recon 1 results on CNSI Solidifi-cation Worksheet I. The pH at this point should be at least 10.5. Continue mixing and retesting if the pH is low, and add more lime if necessary. Record weight of lime added on CNSI Solidification Work-sheet I. NOTE: -LIME AE BCRIC ACID WASTE DO Nor REACT QUICKLY 70GE'IHER. BE SURE TO MIX DIOROUGLY FOR AT LEAST 3 MINUTES BERRE DECIDING TO ADD MORE LIME BASED UPON UNFIRMING THAT DIE pH IS STILL low. 1.6 Add the aporopriate amount of cement to the container (s) while con-tinuing ntLxing with spatula. Blend mixture (s) thomtghly. DOCUMENT REv. SHEET q SD-OP-003 J 12 j cwso ioove 7s

r 1.7 Using a pipet, add the sodium hydroxide solution, if mquired, and mix thoroughly. 1.8 Transfer sample mixture (s) to 250 ml beaker (s). Fill to approxi-mately 1/4" of the top.

     .C 1.9      Place lids securely on samples and imediately transfer to oven con-trolled at 1350 F 1 50 F.         '1 hen cure for 6-24 hours, according to experience at that particular utility.

1.10 flerreve the samples from the oven, and allow to cool for at least 2 hours before mmoving the lid (s) and evaluating solidification re-sults according to guidelines of Paragraph 4.4. NOTE: DIE 2-HOUR COOLING PHlIOD CAN BE DELETED IF EXPE21IENCE WITil D11S PARTICULAR WASTE SDtEAM SHOWS DIAT IT IS NOT NECESSARY 'ID EVAIDATE DIE SAMPLE. NOTE: OBTAINING A FIRM, DRY PCP PRODUCT AT 1300 F WILL NORMALLY ASSURE DIAT A TEST FORMULA WIll Ht0 VIDE A RAPID AND ACCEPTABLE FLU -SCME SOLIDIFICATION WIDI A CLEARLY MEA 5URABIE EXGnlERM.

                                     'ID DDdONSTRATE ONLY DIE EXPECTED FINAL PRODUCT }{ARDNESS, Tile SEALED SAMPLE SHOULD BE CURED AT 170 1 50 F FOR 18-24 Il0UllS
                                     'ID CINPIETE DIE HARDENING REACTIONS.

2.0 FULL SCALE CAirULATIONS (Boric Acid Concentrates) 2.1 Detemine the volume (cubic feet) of waste to be mceived in the liner. Hefer to the table in Figum 5 for usable liner volumes and also consider past experience and allowable cask payloads. (- 2.2 '1he amounts of cement and lime mquired are determined by using the information in the table below. 'lhe ratio of cement to lime varies according to the analyzed level of boric acid in the waste (to be supplied oy the utility). Waste Aaalysis Equivalent Weight Of Lime Weight Of Cement Per FIN Boron Boron Acid Content Per Cu. Ft. Of Waste Cu. Pt. Of Waste O- 3,500 0-2% 4.0- H.O its. 59.4 - 75.0 Lhs. 3,500- 7,000 2-4% 6.4- 9.5 Lbs. 5G.2 - 71.8 Lbs. 7,000-10,500 4-6% 9.5-12.7 Lhs. 53.1 - 68.7 lbs. 10,500-14,000 6-8% 12.7-15.8 Lbs. 50.0 - 65.6 Lbs. 14,000-17,500 8-10% 14.1-19.0 lbs. 46.8 - 62.4 Lbs. 17,500-21,000+ 10-12i+ 15.8-22.1 Lbs. 45.2 - 59.2 Lbs. clime And Cement htetors Selected Are Bared On Baron Analysis, ICP Hesults, And Past Experience. 2.3 Determine the full scale forcula and level alarm settings by con-pleting CN31 Solidification Worksheet 11 for PWR wastes. 2.4 'lhe volume of caustic mquired, if any, for full scale solidificaton is dependent on a number of variables, such as waste corposition and ambient conditions. 'Ihe maximum volume of caustic is 10 gallons of 25% concentration or 5 gallons of 50% concentration. 'Ihese amounts i k! are not to be exceeded without supervisor's approval. DOCUMENT REV. SHEET i y SD-OP-003 K 13 csso toove.7s

r. FXGURE 2 3 ICp Solidification Of Particulate Wastes (Resin Heads, Powd.-x And Diatcraceous Earth Slurrie s) l.0 Sample Verification

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NOTE: 'IEE OIDdICAL ADDITIVES USED FOR PCP PREPMIATION SHOLLD BE Ti!0SE ACIUAILY USED IN FULL SCALE S(LIDIFICATION AND S110lLD BE S'KMD- IN CAPPED CONTAINERS. 1.1 Arrange with the utility to assign a special test area which cor.- tains adequate protection from the anticipated higher raditt.!cio levels of bead resins. 1.2 Notify the utility that the preparations for verification it sting have been completed and request that a saste sample be supplisd. 1.3 Transfer 100 ml of resin from the sample containt.r to a 250 ml disposable beaker and allow solids to settle. Typically, tie. s will be a layer of wuter on top of the re sin beadc. Ce n*. e1 f um (i pimies wij) show rn se p r ui..n or liqu!1 NOTE: WHEN RADIATION LEVELS ARE EXCESSIVE IN ACCORDANCE WITH THE UTILITY GUIDELINES, THE SAMRE AMOUNT MAY BE REDUCED 'IU AS LITILE AS 25 hL. BE SURE 'IO REDUCE OIllER ADDITIVFS BY THE SAME RATIO. 1.4 hieasure and record on CNSI Solidification Worksheet the waste- 141 using the wide range pH paper. Add line (01(OH)2) in 2 gm in-crements until a pH of 10.5 to 11.5 is reached by a narrow (9-13) ( range pH paper. Stir thoroughly af ter each addition of limt. and add 3 more grams after the desired pH range is reached. Record the total amount of lime added on CNSI Solidification Worksht.t.t I for particulate sustes. Alternate lethod; hhere lime is not acceptable (i.e; cannot be added to the slurry) substitute 50 percent doditm hydroxide solu-tion for lime in Step 1.4 and add in one ml increm nts until a pH of 11 to 11. 5 !s 's nehed h ' w.c tenet - I'.rm wi n .t . p. 1. .; W

                                                                                    .            .t ,

l.7. NOTE: LIME IS THE PREFERRED AGENT FUI PRE-TREA'IMENT OF ION-EXCHANGE TYPE WASTES, SINCE IT IS MORE COMPATIILE WITH CBENT REACTIONS AND FORMS A MORE STAlLE END PRCDUCT. 1.5 Add cement slowly stile stirring until a smooth homcuentous mix is obtained. 'Ihe amount addi.d for a 100 ml' wacte samph mav Lt 80 to 150 gns derroding on resitt type , quantity of line adiivi miit amount of sater jn the slurry. Record amount of centnt ad%i on the CNSI Solidification k)rksheet.

1. ti Place the lid over the ht.aker and stort the sealed nix in an ovin controlled at 120-1300 F for 18-24 hours. Then allow sample to cool for at least 2 hours before removing lid and evaltn ting solidification.

k. DOCUMENT R E V- SHEET SD-Op-OO3 f L M CNSQ 1002/8 78

r.

 .                                                                                                    3 1.7      Evaluate the sample using the guidelines of Paragraph 4.4. It the sample does not meet the acceptance criterin, contact the Supervisor,    Solidification Services for possible formula

{ modifications. 2.0 Full SCALE CALCLUTIONS (BEAD-TYPE Oft PARTICLUTE WAS33) 2.1 Determine the volume of waste material to be receivcd and the amounts of cement and lime or sodium hydroxide solution requircd by completing t!m CSSI Solidification Worksheet for bead-type or particulate wastes. Reduce the calculated amounts as necessary to comply with weight and radiation limitations imposed by waste activity and shielding requircments. l t DOCUteENT M E V. S.4EET SD-OP-003 F 15 L J cNso 1oo2/s-7s

r-3 FIGURE 3 FCP Solidification Of Sultate Concentrates (BWR Wastes) 1.0 Sample Verification NOTE: TilS CHEMICAL ADDITIVES USED FOR PCP FREPARATION SHOULD BE 'I110SE ACTUA USED IN FULL CONTAINERS. SCALE SOLIDIFICATION AND S110UID BE SIDRED E CAPPED 1.1 Notify the utility that preparations for verification testing have. been completed and request that a sample be p)ovided. 1.2 Add 15-30 gms of lime,15-25 gms of CNSI Agent M-5, and 0-2 cc.s of boric acid to a 600-ItX)O ml container. NOTE: BORIC ACID IS USED 'IO RETARD DIE OIDlICAL HEACTION WHICH DECREASES THE EXUTHERM. NORMALLY 1 GRAM OF BORIC ACID WILL BE ADDED. TRE AMOUNT OF B0itIC ACID REQUIRED WILL VARY WITH WASTE TEMPHIATURE AND pH. A HIGHER WASTE TaiPHtATURE AND A HIGHER pH WILL REQUIRE MORE DORIC ACID. AS EXPEL-IENCE WITH A PARTICULAR WASTE STRE/M 'IllE 3OltIC ACID MAY BE DELETED OR IN-OtEASED 'IU 2 GHAMS MAXIMUM. 1.3 Add 200 ml of radwaste to the container and mix thoroughly. Check the pH and record on CNSI Solidification Worksheet I. It pH is less than 11.5, add more line as necessary and re-test. 1.4 Gradually add 135-175 gms of cement over a 5 minute period while continuing mixing. Blend thoroughly until mixture is homogeneous. NOIE: HIGH DENSITY OR SOLIDS CONTENT OF THE WASTE MAY NECESSITATE A REDUCTION ( IN THE AMOUhT OF CDdENT REQUIRED 'ID ACHISVE A WORKABLE PASTE. MINIMIZE CDAENT USAGE CONSISTENT WITH OBTAINING A FIRM, DRY ACCEPTABLE MtODUCT. 1.6 Transfer (pour) sample mixture into a 250 m1 beaker, filling to within 1/4 inch of the top. 1.6 Place the lid over the container and store in an approved radio-active materials storage area in the oven provided. The sealed sample should be kept at 140-lbtP F for 18-24 hours. NUIE: UNHEATED SAMPLE MIXTURES DO NUT ATTAIN THE SOLIDIFICATION TD4PERATURES GENERATED IN THE LINER AND MAY NOT INDICATE A COMPARABLE DEGHEE OF SET j ' DURING THE SAME TIME PHtIOD. SAMPLES ALIDrrD 'IO SET WITHOUT HEATING MAY EXHIBIT MORE BLEED LIQUID AND BE LESS UNIFORM THAN THE FULI, SCALE WASTE SOLIDIFICATION PHODUCT. l 1.7 After cooling for at least 2 hours outside o'f the oven, mmove cap ano evaluate the sariple using the guidelires of luranraph 4.4. 1.h Contact the Supervisor, Solidification Services if the test svn-ple fails to mriet solidification requirements. 2.0 Ft;LL.-SCALE CAirt;LATi(b8 2.1 In determining the volume (cubic feet) of waste to bo mcei vm , (' refer to the table in Figure 5 for usable liner voltmw and also consider past experience and allowable cask pavloads. DOCUMENT REV. SHEET SD-UP-003 M 16 k J CNSQ 1002/8 78

 .r
            .                                                                                                                                                                                                                                                                               3 2.2              'lha typical amounts of solidification agents required to set 200 ml of representive waste liquid are indicated in the table below.

Variable amounts of undissolved solids in the waste necessitate modifying the cement content accordingly. Make up two (2) or ( more test mixes at the sane time to determine the best cermnt value consistent with maximizing waste volume while obtaining a uniform, firm proauct. Specific Gravity Cement Typical

  • Agent M-5 Of Waste Weight Lirn WT. Weicht 1.20 Or Above 135-155 gms 30 gms 15 gns 1.12 - 1.19 145-166 gms 25 grs 20 pris 1.04 - 1.11 160-170 gms 20 gms 20 gms Less '1han 1.(M 155-175 gms 15 grrs 25 gms /
  • VARIABLE AOCORDING 'IU WASTE pH AND SPECIFIC GIAVITY l

l 2.3 Determine the full scale formula and level alarn settings hv com-pleting the full scale CNSI Solidification Worksheet Il for H4H wastes. L i a DOCUMENT REV. SHEET SD-OP-003 M 17 L J CNSQ 1002/8 78

r FIGURE 4 ICP Solidification Of hilscellane.ous Aqutous Wastes

  .                         (Not Representing Typical BWR Or IVR Concentrates) r k       1.0   SAMILE VERIFICATION NorE: THE CHalICAL ADDITIVES USED FOR PCP TESTING SHOILD BE THOSE ACTUAILY CAPPED        USED CONTAI?ERS. IN F1LL SCALE SCLIDIFICATION AND Sif00LD BE S'IORE 1.1      Notify the waste generator tha t prepara tions for verification testing have been cotipleted and that a sample is required.

1.2 .Wasure out 200 ml of radwaste sample in a 600-1000 ml disposable container. 1.3 Add 120 to 140 grams of Ibrtland Gement and mix well with spatula.

1. Ma hil to 1m grans of lini. ami nix ell with sintola.

NOTE: ON A NEW WASTE SAMIbE, START WITil MINIMUM QUANTITIES OF CDiENT AND LIME 'IO FUBf A SM00rli MIX Nor PRCDUCING EXCESSIVE ELEED LIQUID. 1.6 Transfer (pour) sample mixture into 250 ml plastic beaker, f1111ng to within 1/4 inch of the top. 1.6 ( Press lid tightly over sample container and stort in an approvtd constant-temperattu e oven. 120-1300 F for 18-24 hours.

                                                            'Ihe sealed sample should be held at NorE: IT IS NECESSARY 'IO H(LD SAMILE MIXTURES AT ELEVATED TDI-PERATURES 'IO SIMlLATE SCLIDIFICATION CXEDITIONS OF FLLL SCALE OPERATIONS.

1.7 Hemove sample from oven and allow to cool for at least 2 hours b.fo e un valir.q. Evsltr*S mi lili rle:it ion us i t. ,,a i n.1 1 tif luragntpa 4. l. 1.8 Contact the Supervisor, Solidification Services if the test saw ple containing traximtn amounts of cement and line still falls to meet solidification requirements. A significant change in typi-cal cement to lime ratio or refomulation with an approved addi-tive may be neces wry.

2. 0 FLLL SCAll CALCLLATIONi 2.1 1)etermine the voltrnt (cubic fet t) of wastt to be receive d , et -

ferring to the table in Figure 5 for usabh liner voltnts.

2. 2 (bmpitte the CNSI Solidification horkshe et 11 for Miscellani ot. .

Aqueous hastes to determine actual chemical requirement s a n,i level control settings. (s DOCUMENT REV. SHEET 1

                                                                                                ~ P' q               SIMP-Ou3                                                   G                                  j cNso too2/s 7s

7 FIGURE 5 7 Liner and Cask Calculations ( Liner L21-300 L21-235 L14-195 L14-170 1B-120 L7-100 Ih-80 Diameter 82" 82" 76" 74" 61" 74.5" 58" Height 104.5" 79" 75.5" 69.37" 71.b' 37" 54" Tog 1 Volume, Ft 317 241 190 174 120 93 82 Usable Volume, Ft (2" Safety Factor) 311 235 190 169 116 88 79 Ft3/In. Of height 3.05 3.05 2.62 2.52 1.69 2.52 1.53 w'eight, its. 2400 1800 1650 1550 1100 1250 950 Cask Payload, Lbs.(Including 27250 27250 17700 14000 20000 13000 7500 Liner height) t M UMENT R EV. SHEET L S M P-003 J 39 l

  • J I CN501002/3 73
                                   -         . . - - _                            --~----.          _
 '.'~     ,

FIGURE 6 ' PCP FOR MlEPARATION OF FLUID MIXTUH12 FUR IN-SITU SOLIDIFICATIONS 1.0 SAMPLE V Q FICATION NOTE:

   .(                DIE OIDlICAL ADDITIVES FUI PCP PREPARATION S11001D BE DIOSE ACITAILY l' SED IN Full                                                          4CALE SOLIDIFICATIONS AND SHOUID BE S'IORED IN CAPPED CONTAINERS.                                                                                                                                                                          -
                                                                                                                                                                                                                      ^

1.1 Secure representative samples of all components to be used in the actual solidification. 1.2 To a 600-3000 ml plastic beaker, weigh in the dry materials listed In-Situand record values on CNSI Solidification Worksheet (tor Solidifications). Sodium Sulfate, Anhydrous 16.0 gm Lime, Ifydrated 40.0 gm Boric Acid, Granular 2.0 gm 1.3 h cri a graduate, add 200 ml of water to the dry ingrediants and blend thoroughly with sp'Itula. Check pH with narrow range inter to confirm that the mixture is 11.5 or greater. 1.4 Add in 190-230 grams of Portland Cement and mix well with spatula to assure uniformity. nix to a smooth, fluid consistency. Control the flow characteristi m of the NOTE: DIE REQUIRDIENT FOR IN-SITU SOLIDIFICATION IS A CDENT (IMOSI-TION TIAT CAN BE FUMPED AS A FLUID, BUT WILL SET HARD WIDI LITILE (s OR NO mRm LIQUID AFTER PLACEMBT. HIE MiOPER CDNSISTENCY IS BEST DESCRIBED AS A " HEAVY GEAM 'IU A SOFT ICE GEAM" TEX 1tRE. AllIUSI CEMENT WEIGHT AS NECESSARY 'IO OBTAIN DESIRED TEXTURE. 1.6 Af ter confirming the proper weight of cement needed to control the flow characteristics of the mix, note this value on the Solidification Worksheet (for In-Situ Solidifications). 1.6 Transfer inch of the fluid top, cement and then mixturn to lid attach a 250 firmml container to about 1/4 1v. 1.7 FPlace for 18-24 sealed hours. container in an oven controlled at about 130-1400 before unsealing. Examine Then remove the container and allow to cool product and record approximate volume of free liquid, if any, and the apparent relative hardness. NOTE: IF AN O'!EN IS Nor AVAILABLE, DIE TEST SOLIDIFICATION MAY BE COM-PLETED AT WAHM ROud TDIPERATURE (75-850 F), BUT WILL NOT NEES-SARILY GIVE TIE SAME RESbt.TS OVER DIE SAME TIME PERIOD. SMAll SAM-PLES DO NOT RETAIN DIE NORMAL EXGTHERMIC HEAT OF CEMBT HYDRATION THAT ACCELERATES HARDENING OF BUIE MIATURES. 2.0 Determine the volume of waste material to be received and the amounts of cement, lime, sodium sulfate, and boric acid required by contileting CNSI Solidification worksheet for In-Situ Solidifications. Chemical ammts may be changed with supervisor approval as necessary to comply with (' weight requirements. and radiation limite cions imposed by waste activity and shielding DOCUMENT REV. SHEET q SU-OP-OO3 K 20 J CNSO 1002/B 78 _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ . _ . _ _ _ .}}