Text

Rev 0 to WVNS-PCP-002, Process Control Plan for Cement Solidification of Sludge Wash Liquid
	ML20096H452
Person / Time
Site:	West Valley Demonstration Project
Issue date:	05/20/1992
From:	Merritt Baker, Harward D, Meess D; WEST VALLEY NUCLEAR SERVICES CO., INC.
To:	;
Shared Package
ML20096H420	List: ML20096H418; ML20096H431; ML20096H452;
References
	REF-PROJ-M-32 WVNS-PCP-002, WVNS-PCP-2, NUDOCS 9205270230
	Download: ML20096H452 (64)
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Revision Number 0

Demonstration Project ,e,1si,n Date,,,,2 Engineering Release # 2352 PROCESS CONTROL PLAN PROCESS CONTROL PLAN FOR CEhE!C SOMDJ1 CATION OF SLUDGE WASH LIQUID PREPARED BY d Nf' M - M. N. Baker CognizantEn,4per APPROVT,D BY h7 D. C. Meess Cognizant System D sign Manager [ fL! APPROVED BYff il diation aK1 Safety Manager [.aJ. J. Harvard ~ A APPROVED BY N 4-d@d 80 f2 D. L. Shugars Qual'i t-//ssuranceMahag4r APPROVED BY ' mt# I # /r' A. J. Howell Opedat os chnical Su;f ort APPROVED BY l b 4 1 J. Paul IRTS erat APPROVED BY 6fMa c-P. S. Klanian Analytical & Process Chernistry West Valley Nuclear Services Co., Inc. PcP:0001279.RM P.O. Box 191 West Valley, NY 14171-0191 WV 1816. Rev.1 9205270230 920521 PDR PROJ M-32 PDR

i WNS PCP 002 Rev. O [_ RECORD OF REVISION F PROCEDURE If there are changes to the procedure, the revision number increases by one. These changes are indicated in the left margin of tha body by an arrow (>) at l-tre beginning of the paragraph that contains a change. Exarole: I { The arrow in the margin indicates a change. I-Rev. No. Description of Changs Page(s) Dated i i-0 Original Issue All 05/20/92 l i l t l l. b i I l l i i e 1 l p 1. j i i V;. i i 2 I a ? i I r 3-W 1807, Rev.. i l 3 - - PCP:0001279.RM i t j t i ~,. -,. _, -. _.... .- a

WN S. PC P - 00;' Rev. O RECORD OF REVISION (CONTINUATION SHEET) Revisic.n on Rev No. Description of Changes Page(s) Dated l W - 18 0 7, Rev 1 it PCP:0001279.RM

- - -. ~..-. VVNS.PCP 002 Rev, O PROCESS CONTROL PLAN FOR CEMENT SOLIDITIC47 ION OF SLUDGE VASH LIQUID Table of Contents i ~ l Entt i 1.0 SCOPE 1

2.0 REFERENCES

1 3.0 SYSTEM DESCRIPTION. 2 3.1 Process Description. 2 3.1.1 Waste-Storage and Dispensing Subsystem. 3 3.1.2 Mixer Flush Subsystem 3 3.1.3 Chemical Additive Systems 4 3.1.4 Cement Transfer and Storage subsystem 5 3.1.5 The Cement Metering Subsystem 5 3.1.6 The High Shear Mixing' Subsystem 5 L3.1.7. Drum Feed, Positioning and Transfer Subsystem 5 3.2 Process Chemistry Formulation for Decontaminated Supernatant 6 1 3.3 -Handling Flush Drums and~ Drums Suspected to be in Noncompliance 6 3.4~ Drum Fill.-... 7 -3.5-System Operation S 3.6 Process-Control System 8 -3.7 CSS-Data Acquisition System. 9 4.0 REQUIREMENTS FOR SAMPLE VERIFICATION. 13 4.1 - Laboratory Safe ty.. 13 4.2 Prerequisites, 13 4.- 3 Sample Acceptance. Criteria 14 4.4 Requirements for Sample Verification 15 5.0 - SAMPLE VERIFICATION PROCEDURE 15 6.0 FULL SCALE SOLIDIFICATION 25 6.1 Calculation of Fall Scale Formulation 25 6.2 Full Scale Formulation 25 6.3 Full Scale Formulation Control 25-g

7.0 LRECORDS. DOCUMENT CONTROL, AND QUALITY ASSURANCE.

26 8.0 FULL SCALE DRUM TESTING 27 Attachment A Cement Solidification System Run Plan A1 i ) PCP:0001279.RM 111 .a.

VVNS PCP 002 Rev. 0 PROCESS CONTROL PLAN FOR CLMENT SOLIDIFICATION OF SLUDCE VASH LIQUID 1.0 SCOPE This Process Control Plan describes the Cement Solidification Process, its controls, and product quality regrirements which will be used during solidification of the sludge wash liquid. The solidification recipe used sas developed and demonstrated to co.rply with the requirements of 10 CFR 61 Section 61.55 and 61.56 for low level waste stabilization. The recipe was further tested at West Valley to demonstrate process perfouaance and the capability tc control the recipe constituents at full scale. This Procese Control Plan describes the means of controlling the process to assure that the vaste form produced is in con?ormance with the qualified recipe. The Sludge Vash vaste liquid in Tank 8D 2 is Radioactive Mixed Vaste (RMV). RMW's contain, in one waste matrix, hazardous waste components that are subject to regulation by EPA under RCRA and, radioactive components that are subject to regulation by DOE or NRC under the Atomic Energy Act ( AEA) The hazardous characteristics of the PUREX waste are: Earium, cadmium, Chromium, Mercury, Nickel, and Selenium, listed in 40CFR268.24 The supernatant liquid as a vaste product of the PURPX process was pretreated during 1988 through 1991 to remove Cesium. The Sludge Vash trearment process began in October, 1991. The Sludge Wash process includes the addition of dilute caustic solutions, producing an elevated pH which is necessary .o suppress Plutonium and Uranium. Sludge Vash liquids are decontaminated to reduce the concentrations of Plutonium, Cesium, and Strontiu.T., resulting in a low level radioactive waste. To provide assurance that the waste / cement will perform to its qualified recipe, test cubes will be made, as a minimum for each 5000 gallons of waste to be processed. This will involve one (1) cube for tank SD-15A2 (gross capacity 5000 gallons) and two (2) cubes for tank 50-15A1 (gross capacity 10,000 gallons). The uniform nonhazardous nature of the cement waste form, below the concentration standards of 40CFR268.43A, is confirmed by VVNS TPL 009 the TCLP Test Plan. 2.0 EEFERENCES ACM 1201 Method to Analyze Cross Alpha and Gross Beta Radioactivity in Various Liquid Samples ACM 1501 Anions by Chromatography ACM-1601 Carbon Determination - I.R. Detection ACM 1801 Determination of Density with the PAAR Digital Density Meter ACM-2501 Determination of Total Solids ACM 2601 pH (Electrode Method) ACM-2701 Plutonium Separation by Solvent Extraction ACM 2702 Plutonium-2*1 by Americium-241 Engrowth ACM 3001 Camma Spectroscopy ACM 4001 Tc 99 Separation Method ACM-4901 Tritium Distillation PCP:0001279.RM 1-

l VVNS PCP 002 i Rev. 0 l ACM 5601 Calcium Nitrate in Cement ) - ACM-5704 Waste Classifica. os of Processed Decontaminated Supernatant Drums i VVDP 010 Radiological Controls Manual i VV 987 - Occurrence Investigation and Reporting VVNS TPL 009 Toxicity Characteristic leaching Procedure for Cement Vaste Form VVNS-TP 053 Test Procedure for Verification Cubes for 20% TDS Sludge Wash Cement Vaste SAR Volume IV Safety Analysis Report for the Cement Solidificatisn System SOP 00 1 Documents foe Work Instructions SOP 9 2 Solid Radioactive Vaste Handling SOP 70 1 Waste Transfer to CSS S0P 70 3 Automatic Solidification Operation SOP 70 4 CSS Menual Solidification with the Process Logic Controller Operational SOP 70 5 Cravimetric Feeder Operation SOP 70 6 Bulk Cement Transfer to Dry Bin 50P 70 7 Cement Truck Unioading SDP 70 8 Clean Drum Handling for CFS SOP 70 9' Automatic Drum Operations for Cement Solidification System [ SOP 70 12 CSS Mixer System Flush Operation SOP 70 14 01 14 Building Ventilation System SOP 7015 01 14 Building H&V Filter Change . SOP 70+16 Filter Change Room Filter Change SOP 70*17 Manual Drum Operations for CSS - SOP 7018 Alarm Procedure for CSS SOP 70-19 CSS Emergency Power Outage Shut Down SOP 70-25 Calibration of Critical CSS Equipment SOP 70 31~ CSS Drum Conveyor Alarm Responses SOP 70 32 Operation of the CSS Silo Air Dryer SOP 70 33 Data Acquisition System Operation 501 70 34' Operation of the 01 14/ CSS Pro,..ss Room 4 Ton Bridge Crane 50P-70 35 Operation-of the Maintenance 2 Ton Bridge Crane SOP 70 37 Smear Robot Operation SOP-70 40 CSS Drum Sampling Stat on Operation i 50P 70-41 CSS Preventive Maintenance Program SOP 70 45 Waste Certification 3,0 SYSTEM DESCRIPTION 3,1 Process Descriotion The Cement Solidification System (CSS) includes all piping, valves, instruments. controls, tanks,-and equipment required to solidify waste in cement, place it into drums, and remotely neve the drums onto a shielded truck for transport to the storage facility. Attachment A (the Run Plani contains a graphic. flow diagram describing che solidificatico system and its functions, controls and procedures. The CSS utilizes a high shear mixer to blend waste, coment and additives into a homogeneous slurry. The impeller located at the bottom of the mixer causes the contents to be drawn to the center of the mixer housing and . forces the fluid between the impeller and the casing. This method of mixing ensures thorough and homogeneous blending of all components. PCP:0001279.RM 1: w ..*w

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. ~. ~ l l VVNS PCP 002 Rev. O The CSS performs the following functions: ~ Vaste Solidification mixing decontaminated sludge wash waste with o Portland Type I cement and chemical additives, and packaging the resulting mixture into 269.L square drums. Process Control monitoring and controlling recipe constituent addit.un, o equipment functions and safety interlocks. o Cement Storage 4 Transfer bulk storage of dry Portland Type I cement powder blended wit nominally 5.711.7 (minimum of 4.0, maximum of 7.4) i v/o Ca(NO ): and transfer of batch quantities to the mixers. 3 Materials Handling remote handling of empty and filled drums within the o facility and loading filled drums onto vehicles for transport tu the RTS Drum Cell. The CSS is composed of the following subsystems: 3.1.1 Vaste Storage and Dispensing Subsystem I The Vaste Storage and Dispensing Subsystem is the beginning of the treatment process and is composed of the Vaste Dispensing Vessel and the Vaste Dispensing Pump. The waste liquid is collected and stored here before being mixed with cement; recirculation through the Waste Dispensing Pump maintains homogeneity of the waste while it is stored within the Vaste Dispensing Vessel. Feeds to the Vaste Dispensing Vessel are sampled at the final tank feeding the vessel (typically 5D 15A1 and 15A2 for decontaminated sludge wash solution). Other waste streams will not be added to the Waste Dispensing Vessel during sludge wash processing. The. waste feed solids concentration is controlled by the LVTS evaporator at 20 w/o total solids. The allowable range is 19 to 21 w/o. (Product Requirement) The effect of this range is a variance in water to-cement ratio-within the_allowsble ran6e of 0.64 to 0.68. If necessary, the feed can be diluted to nominally 20 w/o. The Aethod of analysis and tests performed on the samples are discussed in Section 4'.0, " Requirements for Sample Verification". 3.1.2 Mixer Flush Subsystem Whenever the CSS is shutdown for maintenance, when the buildup in the mixer reaches 22 pounds, or at the end of each operating day. the High Shear Mixers will be flushed to prevent residual cement /vaste mixture from hardening inside the mixing vessel. This process is controlled by the operator at the Ki CSS Panel. When flushing is required, 30 gallons of utility water is transferred to the mixer through a spray nozzle with the mixers shut down) the amount transferred is controlled by weight. The mixer is then started on high speed (2000 RPM) creating a highly turbulent. transient wave which provides good flushing action. After two or three minutes of agitation at high speed, the flush solution is . FCP:0001279.PM, .-w',--- e.r..w.. * ,e,-_.4%.- 2c y--.-.-..m +,y ...,. -.,c.ery.m..,.. .,m--. ..m. -r o r ,--,.e =~,c.,- ...miw---n<.,--. -www.-w.--M,--.,ymw,---r,. - -,

'JVNS-PCP 002 Rev. 0 dumped iOto a round 55 gallon drum at the fill station. The procedure is repeated with 15 gallons of utility water. The Flush Drum at the Fill Station is transferred to the Flush Drum Storage Station where the residue is allowed to settle out, the remaining liquid is decanted to on underground storage tank (7D 13) and will be processed through the existing plant radvaste system. The drum is reused until it is half full of r6.idue (-102 litres); the drum is then filled with cement. All flush drums are subjected to postsolidification testing per SOP 70 40, including a test for free liquid and penetration resistance, then transported to a storage area. It is expected that each mixer will be flushed prior to system shut down or as required based on mixer build up. Each flush drum holds multiple flushes. The decanted liquid is periodically sampled to confirm that it is nonhazardous. 3.1.3 Chemical Additive Systems (Product Requirement) Systems are provided to add chemicals to the mixers to accelerate the gelation rate of the waste and control the rate at which the cement sets to minimize buildup of solidified cement in the mixers minimizing the number of flushes required. Calcium nitrate at nominally 5.7 w/o is blended with dry, Portland Type I cement by the cement supplier as a gel accelerating component. Teating performed to date indicates that the recipe performance is insensitive to variations in calcium nitrate, and sodium silicate additive over the approved range it.?icated in the recipe sheets. The acceptance rang, in calcium nitrate in Portland Type I is 5.7 +1.7 percent. The blending operation is conducted by a vendor using approved procedures under thi UVNS quality assu'ance program. Samples are analyzed by the analytical laboratory for nitrate concentration to verify acceptable blending by the vendor. Experience has shovn that the calcium nitrate does not separate during transport or transfer i because it adheres to the cement particles. The dry cement / calcium nitrate blend is stored in the cement silo and is added to the mixers by the cement metering subsystem. Antifoam (CE AF 9020) is added to the mixers with the vaste solution to reduce air entrainment in the waste product. Sodium silicate is added to the mixers as the second component of the set enhancer. The amount of antifoam added is shown on the recipe sheets. It is added by injection directly to the mixers from a lab scale positive displacement pump. Only the sodium silicate addition is varied depending on the particular sludge wash vaste batch being processed, the remainder of the constituonts are held constant. The amount of sodium silicate added to each batch-is expected to vary only slightly, if at all, because of the decontaminated sludge wash solutions homogeneity. The amount of sodium silicate to be added is nominally 16 pounds per batch. The homogeneity of the sludge wash being processed is such that valid solidification results can be gained on a-sample of the full batch. Full scale recipes for 18.0 to 20.5 gallons of waste are contained in Tables Al-1 through Al 6. Homogeneity of the calcium nitrate cement blend is assured through the use of an approved blending procedure submitted by the supplier, PCP:0001279.RM VVNS PCP 002 } Rev. O l periodic quality assurance of the supplier's blending operation and f chemical analysis of the blend to assure homogeneity, j 3.1.4 Cement Transfer and Storage Subsystem TheCementStorageandTransferSyt a provides a bulk stor.ge capacity of 70 m (about 100 tons) iv. the dry cement / calcium nitrate blend and transfers it to tne Cement Metering Subsystem. The blend is delivered from off site by truck and transferred pneumatically to the Bulk Storage Silo. The transfer air exits the silo through a dust filter at the top. A blower is used to pneumatically transfer the blend to the Acrison day bin in the Cement Metering Subsystem on demand. The transport air is vented back to t"e Bulk Storage Silo where it vents through a dust filter. 3.1.5 The Cement Metering Subsystem _(Product Requirement) This subsystem uses a gravimetric (loss in weight) feeder to accurately dispense the Portland Type 1 dry cement / calcium nitrate blend from the Acrison day bin into the mixers. A bulk dry cement storage silo is located near the CSS to facilitate the filling of the day bin and minimite dust inside the facility, 3.1.6.The High. Shear Mixing Subsystem Batch control for the High Shear Mixer is automatic, the operator sets the pu.ial controls for the recipe to be processed and initiates the procecr The process parameters are controlled automatically by the HS CSS programmable logic controller (see Section 3.6). The waste feed, cement / calcium nitrate blend, and additives are metered into the mixer, which runs continuously during operation. The batch is. mixed to assure homogeneity and is discharged into the waste drum (typically 269L square drums)..Two (2) mixer batches are added co ~ each 269L square drum. The process is controlled to assure the recipe is followed and the container is filled to greater than 85 percent capacity. 3.1.7 Drum Feed, Positioning and Transfer Subsystem A remotely operable conveyor system is installed at CSS to: o Move-empty drums into the Process Cell, -o_ Place drums in pocition for filling, Read drum dose rates and bar code labels for drum identification, o o Manipulate filled drums.co the smear-station for surface contamination measurements and to the overpack station if

required, Install and crimp lids on filled drums, o

2 o Provide for storage of drums prior to load out from the' facility. PCP:0001279.RM -S-

p VVNS PCP 002 -Rev,'O -Transfer filled drums onto the shielded truck for transport to the o drum cell, and Periodically test drums for percent fill, tree water.and o penetration resistance', 3.2 Process Chemistry Formulation for Decontaminated Sludre Wash Portland Type I cement and waste alone do not produce an acceptable product because of.the delay in gelu ion and ultimately the set time. It is necessary to. utilize admixtures of constituents normally present in both the waste 9tream and-the Portland cement to

elerate gelation assuring proper dispersal of waste in the matrix by preventing cement particle settling and setting of the final-product in a reasonable time period following p roduc t io...

Early gelation 's required to permit timely transport of drums to the_ storage area. Prior to transferring waste from LWTS to the Waste Dispensing Vessel, the concentrates collection tank (either SD 15Al or SD 15A2) is samvivd. Sufficient sample volume is collected for radiochemical analysis and preparation of a varification sample for solidification. Due to its larger operating. volume, tank 50-15Al is sampled prior to solidification and also at_50 percent 110 percent level as an in process check. The in process check sample -(second sample) of SD 15Al is intended only to demonstrate the uniform -nature. of the waste, with no change in the !: quid density as the cans,is. emptied. ~ Only the first sample will be for presolidification testing. The purpose of these samples is to assure that the batch of waste to be-transferred _can be properly solidified using the reference qualified recipe and_to provide isotopic analysis for waste classification. The results of the isoccpic analysis can be torrelated with the waste solution composition. The requirements for sample verification are contained in Section 4.0. The process control systems and logic used to assure that the product is produced in accordance with the qualified formulation is described in Section 3.6, Process Control System. 3.3 Handline Flush Drums and Drums Suspected to be in Epncomoliance As described in-Section'3.1, mixers may-be periodically flushed to maintrin them free of excessive cement buildup. The residual flush water will be-decanted from the drums leaving behind a relatively dry cement product. The residual cement-following decanting will be capped with a cement and water mix specified in a flush recipe to provide a means of-solidifying any small amount of free water that may remain on-the surface of.the decanted cement. Since the cement remaining after decanting consists of residuals from several batches, its qualification and classification are uncertain. These _ drums will not be processed for immediate disposal, but will be transferred to a storage area where'the cement will be allowed to set. The drums will be= classified and transferred into a high-1,tegrity container (if rrcessary) prior to ultimate disposal. Those flush drums which qualify as Class A waste will be: stored for later disposal in the Class A disposal facility Even though the process is well controlled to produce a product meeting th qualified product characteris tics,' it may be possible through process upso:s to produce material which is outside the qualified region. These containers are referred to as " suspect drums" and could be "out-of-specification" as a PCP:0001279.RM 6-

WVNS PCP 002 Rev, 0 result of variations in PRODUCT REQUIREMENTS or PROCESS REQUIREMENTS. PRODUCT REQUIREMENTS will be those necessary to produce an acceptable waste form per 10CFR61, PROCESS REQUIREMENTS will be those necessary for smooth operation of the Cement Solidification System. FR0 DUCT REQUIREMENTS include: Water to cement ratio, percent solids in the vaste, sulfate percent of total solids, drum percent full, free water in the drum, verification (cube) compressive strength, and addition of recipe admixtures. PROCESS REQUIREMEN','S include : mix time, gel time of presolidification verification (cube) sample and data base updates, such as automatic data which would not be recorded in the event of a computer malfunction. In this case, the drum data would be reconstructed from manual data. All " suspect drums" resulting from process upsets will be evaluated on a case-by case basis, and documented on a Nonconformance Report. Upsets in PRODUCT REQUIREMENTS will be set aside for further evaluation, including compressive strength and leachability testing. A critique will be held to investigate the cause of the upset, and prevent rccurrence. Upsets in PROCLYS REQUIREMENTS will be set aside until a technical evaluation can be completed to determine product acceptability. Drums originally considered " suspect" that are found to be acceptable alter technical evaluation or testing will be placed in the Drum Cell stack. For upsets in PRODUCT REQUIREMENTS, the Noncanformance Report will be referenced on the drum data base, documenting the upset condition, evaluation or test results, and corrective actions (s). Those containers which a e unacceptable for disposal will be removed from storage and will be placed in high integrity containers prior to disposal. 3.4 Drum Fill (Product Requirement) Drums produced for disposal must be at least 85 percent full of qualified cement product or other suitable inert backfill which meets the 10CFR61 requirements. The drum fill is controlled through the volume of wastc, admixtures, and cement prepared for addition to the drum by each mixer and may be verified by load cell weight indication. A repr==entative sample of Tank 5D-15Al or SD-15A2 is analyzed for cesium, strontium, plutonium, and sulfate and total solids. Once this data is known, the data in tables Al 1 through Al 6 is used to determine both waste and cement addition criteria. Table usage is based on determination of total solids concentration in the vaste combined eith recipe batch size (e.g., 20 gallon batches) to achieve the desired drum fill. Vaste and cement (with calcium nitrate) additions are preprogrammed into the HSCSS and acrison control panels such that feed to the mixers is controlled and monitored. One drwn per.each process Tank 5D-15Al or 5D 15A2 is physically inspected for freeboard determination, free liquid presence and penetrometer resistance. The sludge wash solution to be processed is very homogeneous so it is unlikely that modification of the recipe wilt be required during the processing period for either tank (usually 2-4 days). The drum that is physically inspected is considered to be representative of the entire batch of drums from either 5D-15Al or 5D-15A2. PCP:0001279.RM,

VVNS PCP 002

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k Rev. O Tables Al 1 through Al 6 show the calculated range of drum fills produced, acceptable recipe variations, the amount of each con.=tituent to be added, and the' water to cement ratio. Percent fill is verified by the Data Acquisition System based on the weight of constituents added to the mixer within the acceptable fill range. 3.5 System operation-Before beginning any processing of decontaminated waste from the LVTS storage tanks, a successful ssmple verification must be completed in. acco: dance with the Sample Verification Procedure of Section 5.0. The successful sample solidification parameters are recorded on the Solidification Data Sheet. These parameters are used to verify that the reference recipe is either acceptable as specified or to specify minor changes to the recipe within the qualified region. Actual full scale solidification is then conducted in accordance with the Cement Solidification System Run Plan (attachment A). The sequence of operations is as follows: o A present volume of liquid decontaminated waste is added batchwise to the mixers from the recirculation line of the Vaste Dispensing Vesse'l using the-Vaste Dispensing Pump. o The recipe quantity ot Antifoam (CE AF 9020) is added to the mixer and the solution mixed at 2,000 rpm for 10 seconds. The mixer speed is reduced to 1,000 rpm and. cement / calcium nitrate o addition is initiated. Metering of the proper amount of dry mixture into the mixer requires between 2 and 4 minutes, o At the end of the cement feed step, sodium silicate is added in a water based solution. The feed is accomplished with the mixer continuing to run at 1,000 rpm. Mixar speed is monitored. The addition requires less than 30 seconds. A~ nixing time of 60 seconds is ' counted _ from the end of the sodium feed to *.he opening of the dump valve, which is held open for 40 seconds to discharge the batch into the drum. 3.6 Process Jontrol System The HS CSS PLC (Programmable Logic Controller) controls the automatic solidification process. Three independent subprograms exist within the' main O program, one controlling mixer No. 1, one controlling mixer No. 2, the third-controlling the fill nozzle and lid handler / turner with checks for proper drum positioning. This allows single cr 2 mixer-operation with no reduction in processing rate. The programs are arranged to permit only the correct operating sequences to occur. Events. called for must take place-in step or programs are inhibited and addition of any ingredient prevented. s The PLC controls the additions of waste. Antifoam, and sodium silicate and mix time as specified by operator-controlled settings on the control panel. PCP:0001279.RM -

VVNS PCo 002 Rev. O The DAS (Data Acquisition System) records weights at 'the direction of the PLC at appropriate program steps. The mixer programs allow repetition of waste and cement feeds in incremental amounts should the weight of the charge transferred be low, as checked by DAS for recipe correlation during the process. Valve V 2 which discharges liquid waste into the mixerr in the automatic mode has been tested and shown to provide a 99 percent confidence factor for the volume. The statistical interval was provided by a regression analysis. The HS CSS controller provides checks to maintain this accuracy. Among these checks are: o Before any V 2 operation is allowed, its position indications of "open" and " closed" are checked for nonsimultaneous location, o To allow V 2 operation, recirculation loop flow must be equal to or greater than 97 percent of expected nominal flow, o When called upon to open or close, valve response time is monitored and if not proper, the Waste Dispensing Pump is stopped and the program is terminated, o If valve V 14 is not directed to mixer 1 and 2 as called for, the program is inhibited, preventing double batching of one mixer, o Timing of valve opening is controlle* to within 0.1 second. Typical time settings are in range of 12 to 14 seconds, The cement mix time sequence is not a variable. It is set and not changed o during processing. The addition of the sodium silicate additive is controlled by an air-operated piston pump; the total volume charged to a mixer is controlled by counts of pump strokes by the PLC. Settings are made by the operators on the control panel based on the recipe requirements. The pumps have been calibrated for a specific discharge per stroke. Out-of-range charging will be alarmed by the DAS, based on mixer weight increase measured by load cells. A control logic diagram for the HS CSS control system is shovn in Figure 1. 3.7 CSS Data Accuisition System The CSS Data Acquisition System (DAS) is used to document the processing of each waste drum and of each mixer batch that went into the waste drums. The DAS accepts signals from the mixer load cells, the dry cement metering system, drum dose rate monitor, and bar code reader. The DAS also accepts digital signals from the HSCSS control sytcem to record weight readings for waste and cement at the proper tiec in the process. Note that back-up data is inanually taken as part of the WVNS Standard Operating Procedures. I PCP:0001279.RM -

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~ - _ ~ k'VNS PCP-002 Rev. 0 The Data Acquisition System'also is used to insure that each mixer batch is within acceptable limits, as determined by the qualified recipe parameters for_ min / max waste weight and min / max water to cement ratio. If any one of ~ these pa'rameters -is outside the acceptable limits for the mixer batch, the DAS will alarm and alert the vperator. At this point, mid stream manual corrections for such conditions as low waste weight or high water-to. cement ratio may be made, while maintaining automatic control, thus assuring that each mixer batch. and each waste drum conforms with the qualified recipe-. L Final drum weight _is calculated and recorded by the DAS as the sum of the recipe constituents. A real time display and printout of all major process steps and alarm conditions is generated using the DAS (an IBM Industrial AT microcomputer system). In addition, the DAS maintains files for all drums made during the course of produccion. An online display exists to allow instant display of drum / mixer weights, water-to cement ratios, overpacks and dose rates-of any drum monitored by the DAS. A weekly activity file is maintained on disk in order to identify drums made during an operational period. These ASCII formatted drum records may be copied to diskette during nonoperational periods'and placed in spreadshe'et form for further off-line analysis. The following is a brief summary of the~DAS accuracy in calculating drun weight: 1. The DAS retains the empty *2 mixer weight reading from the previously weighed batch. VARIANCE: Accuracy of mixer load cell (+/- 3 pounds). 2. The DAS first calculates the weight of the added waste. It takes the mixer reading after the waste has been added, and subtracts the empty mixer weight (from step No. 1.). VARIANCE: Accuracy of mixer load cell (+/- 3 pounds). 3. The DAS then obtains the weight of the added cement / calcium nitrate from the Aerison System (direct loss-in-weight reading from the cement day bin). VARIANCE: Accuracy of Acrison (+/- 2 pomnds). 4 The Antifoam agent is then added. The weight for this additive is not computed, as only 10 to 15 millilitres per batch is used. VARIANCE: Minor. 5. The weight of sodium silicate added is calculated from its density and the volume added as determined by HS-CSS pump stroke data. 1 R Empty mixer weight plus any remaining mix. PCP:0001279.RM - .+w. we --n-- n-ew-ner. ve-c .e p-- 7-1-two----- w wM t -wt

.~ VVNS.PCP 002 Rev. O VARIANCE: Accuracy of pump stroke. times the number of-strokes +'b of a stroke (t 1 pounds) NOTE: 0.15 litre / stroke and 5 litres required per batch. Periodic calibration of these pumps is performed as well as trending analysis. 6. After mixing is complete and the batch is dumped from the mixer to a drum, the empty *2 mixer weight is read. VARIANCE: Accuracy of mixer load cell (+/- 3 pounds). -7. DAS; calculates the batch weight as follows: BEGINdING EMPTY-MIXER WEIGHT (step 1) + TOTAL 'JASTE WEIGHT (step 2) + TOTAL CEMENT WEIGHT ~(step 3) + ADMIXTURE (step 5) (-) ENDING EMPTY MIXER WEIGHT (step 6), 8. After both batches have been added to the drum, the DAS calculates the total drum wei he as follows: S BATCH #1 WEIGHT + BATCH #2 WEIGHT + TARE DRUM WEIGHT (CONSTANT) A potential variance of 9 pounds per batch is possible: Load cell reading two. times 2x3-6 Acrison reading one time 1 - x '2 - 2 Admixture one time 1x1- -1 A potential variance of pounds per total drum weight is possible: -Two batch readings per drum 2x9-18 Variance in empty drum weight 5 Based on 20 gallons of waste / batch, average net mix vould be about 900~ pounds. Using highest drum weight variance (23 pounds). percentage of error is 2.6 percent. NOTES:l1. Mixer being read has no movement - variance of scale is +/- 3 pounds. 2. Effect of mixer 1 (mixing) on reading'of mixer 2 (no movement of mixer 2) is +/- 3 pounds. 3. Variar.ce if reading scale while mixer is mixing is +/- 4 pounds, 2 L

' Empty mixer weight plus any remaining mix.

PCP:0001279.RM.

=- e WVNS-PCP-002 Rev, 0 4 Accuracy and reliability of the dry cement metering system (Acrison feeder) and Waste Metering Valve (V-2) was experimentally determined to be > 99 percent. 5. Empty drum weight has a potential variance of +/- 5 pounds. 4.0 REOUIREMENTS FOR S AMPLE l'ERIFICATIO]i The tanks which feed.the waste dispensing vessel are sampled using an installed sampling system designed to provide a representative sample of the tanks. The samples are delivered to the Analytical Laboratory where they are analyzed for: Total dissolved solid content per ACM-2501 o Specific radionuclide analysis for waste classification, o o pH per ACM-2601 o Sulfate per ACM-1501 o Density per ACM-1801 These measurements are used to ensure that the waste to be processed at the CSS is compatible with the reference formulation. In addition to these analyses, a sample of the vcste is solidified using the reference recipe and ACM-4801, to - assure that a dry, solid final waste form can be produced it. the full-scale system. The sample solidification verification requirements and procedures used are discussed in sections 4.0 and 5.0, respectively 4.1 Laboratory Safety 4.1.1 A11 safety precautions outlined in Analytical Chemistry Procedure (ACP) 7.2 "Laboratocy Safety" must b6 followed. 4.1.2 While working with radioactive material, ACP 7.4 " Handling Radioactive Materials" must be followed. '4. 2 Prerecuisites 4.2.1 Representative samples of the decontaminated sludge wash, one samplo per nominal 5,000 gallons of waste to be processed is required. Two samples are obtained from 3D-15Al, one when the tank is full and one at half capacity, and one sample is obtained from SD 15A2 when it is full, after the tanks have been sufficiently na.a to ensure a homogeneous mixture. 4.2.2 Chemical and radiochemical analyses are performed to include the following: A. Gross alpha-and beta by ACM.1201 B. Camma scan by ACM 3101 C. Total solids (TS) by ACM-2502 D. . Density (F) by ACM-2401 E. pH by ACM-2601 F. Radiochemical analyses for nuclides listed in 10CFR61 C. Sulfate by ACM-1501 The analyses will be compared to ensure that all parameters are within the allowable ranges, and that the results are consistent with PCP:0001279.RM.

.~.. WVNS PCP 002 5._ Rev. O other related analyses. For example,- total solids will be proportional _to density. 4.2.3 Equipment' required for test specimen preparations. ^ A. Sample-curing oven, thermostatically controllable in the range of 85'c i 2*C Lequipped with a calibrated temperature sensing device (Thermocouplo). B. Calibrated Metler top loading balance sensitive to the nearest 0.01 gram. C. " Lighting Lab Mixer" equipped with variable speed. control, watt loading, automatic timer, and high-shear mixing blade. D.. ASTM certified-2-inch cube cement molds. E. Various containers and glassware as requireo. F. Calibrated compressive strength testing instrument. C. Chemicals-1. Portland Type 1 cement / calcium nitrate nixture obtained fror operations. '2. Antifoam agent CE AF 9020, 3. ' Sodium silicate solution Silica to soda ratio 3.23 i.05 lyr weight Water 62 1 3% oy weight-Na20 9.0 1 0.1% by weight SiO. 29.0 0.2% by weight 2 4.3 Cube-Acceptance Criterla_ To ensure that an acceptable solidified waste form has been produced, the ~ L technician shall verify that all acceptance criteria are met as follows: (: 4.3.1 Visual inspection of the samplo efter. pouring into the mold to look for any separation of liquid on the surface. 'If_ separation occurs. L estimate how much and when the bleedwater separated, Observe the ~ liquid and check for readsorption. If readsorbed, record when. (Product Requirement) j 4.3.2 Visual inspecticn of the 2 inch cube after the 24 hour cure period shows that a firm dry monolith has formed, and that no degradation. i {. (cracking or spalling) has occurred. 4.3.3 Compressive Strength (ASTM C-109) of the 2-inch cube exceeds TBD psi. [This value will be determined by testing.under VVNS-TP-053, and will be equal to the mean compressive strength minus 2 standard-6eviations] (Product Requirement) h PCP:0001279.RM 14-

WVNS PCP 002' Rev. 0 4.3.4 Pourability of the mixer is such that retention of product in the mixing container is minimal-(<5 percent of constituents). The weight of retained material (if any) is recorded on the data sheet. 4.3.5 Celation is controlled to occur not more than 90 minutes following the pour. (Product Requirement) This range of gel times allows a sufficient amount of gelation prior to transporting the drums of encapsulated waste to the drum cell. In the event that presolidification cannot be achieved within the _ qualified recipe range, the process will be stopped. At this point, further testing would be required prior to proceeding. 4.4 Recuirements for Samole Verification 4.4.1 Verify that all materials and equipment listed in Section 4.2.3 are ready and available to use in the Radiochemistry Laboratory. 4.4.2 Refer to Section 5.0 as applicable when conducting sample verification. Use the Solidification Data Sheet, Figure 1, for all sample solidifications. 4.4.3 Sample Requirements A. A sample shall be solidified prior to full scale solidification of L waste. B. If no additional material has been added to the hold tank (5D-15Al or -15A2) after the sample was taken, solidified test specimen is considered representative of tank contents. Note: An additional sample will be removed from 3D-15Al at 50 110 percent level anc used as an in process check for an additional cube sample verification. C. Test specimen sample solidification will be performed, thereafter. on each new hold tank batch of waste to be processed. D. The samples used for the 2 inch cube specimens are representative of the homoger.eous waste samples obtained from the sparged 5D-15Al or SD 15A2 hold tanks. 5,0 SAMPLE VERIFICATION PROCEDURE 5.1 Operations group will provide the laboratory with 150 mL representative sample of decontaminated sludge wash from either of the feed tanks SD 15A1 or 3D-15A2. 5.2 Upon receipt of sample, visually inspect saeple for precipitates, insoluble phases or nondissolved suspensions, and record observations on worksheet (figure 3). In the event that undissolved solids are found, the process will be stopped. PCP:0001279.RM, e

VVNS PCP 002: Rev. 0 - NOTE: THIS METHODOLOGY WILL BE USED UNTIL SUFFICIENT EXPERIENCE AND DATA ARE AVAILABLE TO ESTABLISH VASTE CLASSIFICATION BY KEY ISOTOPE RATIOS. - TiiE DECISION TO UTILIZE RATIOS VERSUS SPECIFIC ISOTOPIC ANALYSIS VILL BE MADE BY -THE MANAGER, ANALYTICAL AND PROCESS CHEMISTRY. 5.2.1= Measure gross alpha and beta by ACM Cross 1201 5.2.2 Measure Sb 125, Cs-137, Am 241.and Co 60 by ACM Camma 3101 5.2,3 Measure Tc 99 by ACM Tc 99-4001 5.2.4 Measure H 3 by ACM Tritittm-Dist-4901 and EM 13 5.2.5 Measurc total Alpha Plutonium by ACM 2701 5.2.6 Measure St 90 by ACM Sr-3001 5.2.7 Measure TS by ACM-2501 5.2'8 Measure. density by ACM 1801 5 2.9 Measure pH by ACM-pH 2601 5.2.10 Measure Sulfate by ACM 1501 5.2.11 Measure Pu-241 by ACM Pu 241 2702 5.3 Ratio the following radionuclides according to the best data available for -ratioing (Racios originally estabtished by Rylken, DOE /NE/44139-14 (DE87005887) "High Level Waste Characterization of West Valley", dated June 2, 1986 ) 5.3.1 I 129 ratio to Tc-99 5.3. Ni-59 and 63 ratio to Co-60 5.3.3 Cm 242 ratio Alpha Pu 5.3.4 C-14 ratio to Tc-99 5.4 Prepare a lab scale sample of sufficient size to make a two-inch cube using the cement / calcium nitrate mixture, antifoam emulsion and sodium silicate used in the plant. The lab scale recipe must be rigorously scaled down from the plant recipe for producing the wasta form. 5.5 The cement is to be prepared per ACM 4801, Cement Test Cube Preparation Method. PCP:0001279.RM, T v --w e..-.-s w--, ,u

. -. = - ~.. WVNS-PCP-002 1 UEST VALLEY DEMONSTR/.TXON PROJECT pov, O ANALYTICAL REQUEST Pas 1 of __ Sample Name: 5D-15Al# Charge No.: WH5250090 Log No.: Results Reported To: LWTS S/S, A. J. How11 /0TS Phone : 4836/4504 .O Sampled by: Date: Time: Location: o a.) WNS NYSDOH Certification: 10474 b.) NYSPDES Sample Type: j WO#: SOP #: OPDR#: Other: I. _ _ WVNS-PCP-002 l v A-. Is *.his sanple suspected to contain radioactive material? ( ) yes ( ) no B. Is the gross activity suspected to be > 5E 03 4C1/c.L? ( ) yes ( ) no C. If gross activity is suspected to be > SE 03 pCi/mL, R/S Rep. to record dose rate (mR/hr at 2 inches WC) R/S Rep.. Date: d D. Specific Hazards (ie. HF, Strong Base, Cd, etc.) ( ) yes ( ) no 3 If yes, list E. Specific requirements (circle): EPA NRC DOE N/A SPDES Other E. Process Control EPT0X Waste Classification ~ 1 E F. Discard sample upon approval of anab tical request: ( ) yes ( ) no If no, state reason and proposed aisposal date i w d G. Comments: I' -a .3 fupervisor or Manager Signature Date: To be filled in when sample delivered to laboratory personnel: 1 I Delivered: , Time: Date: Received: Time: Date-l REQUESTED DUE DATE: (Month / Day / Year): l 1, SUB-SAMPLE IDENTIFICATION a Analysis l Units l A B C D 5 l Requested i J Dose Rate mR/hr o Larra Scan j _j j j E Cs-137 uCi/mL l Lensity g/mL Total j j j j Solids wt% 24 hr Compr. _j U J _.] t Strenoth T'S T I pH 5 Gross j ,_j _j _j a Alpha uCi/mL Data Approved: Date: Time: WV.1113, Rev. 6 - --.

WNS-PCP-002 VEST FAllET DEMONSTRATION PROJECT Psev. 0 ANALYTICAL REQUEST eas _ or Sample Name: SD-15Al# Charge No.: WH5250090 Log No.: SUB-SAMPLE IDENTIFICATION Analysis Units A B C D I Requested J _.J J _.J l Gross Beta uCi/mL l Slurry d d J _J Density g /mL J J J J i Gel Tine min. Bleed YES/NO _l ,_l _j j Water if yes aty. l J ] J J J J J I t J J ._J J J J J U i J J J J d d J j l J J J U t J J J J J J Data Approved: Date: Time W - 1113. Rev 6,

7 __.__m. WNS-PCP-002 -UEST-VALLEY DEMONSTRATTON PROJECT pey, o ANALYTICAL REQUEST eage 1 o< Sample Name: SD-15Al# Charge No.: _ WH5250090 Log No.- e Results Reported To: LWTS S/S, A. J. Eksell /0TS . Phone: 4836/t.504 .1 Sampled by: Date: Timer

Location, u

o H a.) WNS NYSDOB Certification: 10474 b.) NYSPDES Sample Type: j l 1 WO#: SOP #: 71-10 OPDR#: Other: WNS-PCP-002 f 0 A. Is this sample suspec:ad to contain radioactive material? ( ) yes ( ) no B. Is the gross activity suspected to be > SE-03 pCi/mL? ( ) yes ( ) no C. If gross activity is suspected to t) > SE-03 pCi/mL, R/S Rep, te record dose rate (mR/hr at 2 inches WC) R/S Rep.. Date: D. Specific Hazards (ie. HF, Strong Base, Cd, etc,) ( ) yes ( ) no 3 If yes, list E. Specific requirements (circle): EPA NRC DOE N/A SPDES Other f-Process Control EPT0X Waste Classification ! 3 F. Discard sample upon approval of analytical request: ( ) yes ( ) no l If no, state reason and proposed disposal date j u d G. Comments: Sartple for Waste Classification l l Supervisor or Manager Signature Date: l 2 To be filled in when sample delivered to laboratory personnel: Delivered: Time: Date: Received: Time: Date: REQUESTED DUE DATE: (Month / Day / Year): i 2 i SUB-SAMPLE IDENTIFICATION Analysis Units A B C D 5 Requested Dose Rate mR/hr l b d Sb-125 uCi/mL l Cs-137 uCi/mL d d J te-241 uCi/mL d d d Co-60 uCi/mL d d d -d m I h Tc-99 uCi/mL d d d d I e ?~ H-3 uCi/mL d d d d ( i } Data Approved: Date: Time. v* W lll3, Rev. 6 i i y -e--- ~

MNS-PC: -002 ITEST VALLFT DEMONSTRATION PROJECT Rev. 0 ANALYTICAL REQUEST e.g __ o r Sample Name: SD-15Al# Charge No.: WH5250090 Log go,. SUB-SAMPLE IDENTIFICATION ,f Analysis Units A B C D Requested l l ] l _.] Alcha Pu uCi/mL J ] _] Sr-90 uCi/mL _.] -) J J Pu-241 uCi/mL J J J J I-129 uCi/mL I ] _] ] _.J Ni-59 uCi/mL __] _._l _] _] Co282 uC1/mL J ._J _) J i C-14 uCi/mL J J J J l l J J J U 1 J J J J _j _j _j -~ ~~ 1 J J J i t l I I Data Approved: Date: Time-W 1113, Rev. 6,. _ _. _.

= WVNS PCP 002 Rev, O FIGURE 3 Solidification Data Sheet Sample Log No, Time and Date Sample Taken; ank Sampled Cross alpha pCi/mL TS Gross beta pC1/mL Density g/mL Cs-137 uCi/mL pH SU Soi ug/g Decontaminated Supernatant Volume mL Weight of Cement / Calcium Nitrate mixture __ grams Antifoam Volume mL Sodium Silicate mL Water to Cement Ratio Time Sample Produced Cure Oven Temperature C Cure Time hours Solidification Results: Free Liquid Volume mL Cel Time minutes l Physical defects present: Yes No Compressive Strength - 24 hour cure psi i Obs e rva tions : (Including pourability, get time, visual inspection and others as detected.) l l Sample prepared by: Date: Results Approved: , Manager Analytical Laboratory Date: l l l l PCP:0001279.RM 21-

VVNS PCP 002 Rev. O INSERT FIGURE 4 PRESOLIDIFICATION VERIFICATION FLOWCHART SAMPLE CONCENTRATES TANKS SD-15A1/A2 ~ RC-EVAPORTATE OR DILUTE k l CUBE l RADIONUCLIDE EVALUATION GEL \\ NO g PER 10CFR61 COMPLET '\\STOP YES 24 pp 1st CUBE COMPRESSIVE (NO) _ REPEAT CUBE STRENGTH (NO) SEE ND CUDE CRITIQUE'I-aNONCONFDRMANCE YES REPORT 1P NABSORB ygg BLEEDWATER CRITIQUE TECHNICAL RECONDITIC ~ EVALUATION WASTE NO NO R S"/ YES, ESTABLISH OPERATING RECIPE / WATER-TO-CEMENT RA110/ADDI?IVES PARAMETERS GEL MAKE IME 0-90 NO[STOP 1 DRUM HINUTES PPOCESSING HONITOR ~ ~ " " CONTINUE ES PROCESSING P DATA COLLECTIONj HSCSS/DAS v [_ WASTE CERTIFICATION ER SOP 70-45 PCP:0001279.RM ~- -.. - _.--- ~ ~. - - i 'WVNS PCP 002' Rev. 0 . isTTACHMENT.6_IO S0P 70 ' Copies to: QA u, completion of campaigne CEMENTi10LIDIF7CATIOM RECIPE INPUT' DATA OSR/TR IRTS 2 Concentrates Tank (5D-15A1 or SD 15A2) Lab Analysis Log Number (attached) . Batch Size'(Gallons) ' Minimum Mixer Liquid Weight (lbs) Maximu.n Mixer Liquid Weight (1bs) l Minimum Sodium Silicate Weight (lbs) Nominal Sedium Silicate Weight-(ibs) Maximum Sodium Silicate Weight.(lbs) Percent Water In Waste-Slurry Specific Gravity Minimum Mix Time (secs.)' Minimum Water / Cement Ratio Nominal Water / Cement Ratio V 2' Timer Setting-* Acrison Set Point A'ntifoam Pump Timer Setting NaSi Pump l Set' ting (strokes) PROCESS CONTROL-ENGINEER /DATE VERIFIED BY SS/PCE If V-2 setting is ch'anged to accommodate-processing, denote new setting and initial drum affected.- e PCP:0001279.RM 23

.WVNS-PCP 002. +- Rev. 0 5.6 Place the 2 inch cube mold and sample into cure oven; record oven te=perature -and time on the solidification data. sheet. 5.7 . Cure the' sample for a minimum of 24 hours. 5.8 Visually inspect the sample after the cure period in the oven. The sample must be a firm solid cube with no physical degradation and with a compressive strength of greater than TBD psi. (This value will be determined by testing under-WNS-TP 053]. 5.9 -The CSS Shift Supervisor will be given a ccpy of the analytical request form showing the performance of the waste form to this point. which will allow ] processing of the batch of waste. 5.9.1-Shift Engineer reviews all daca it.cluding gel time, and the following 5 -Technical Requirements: a. TR IRTS-7: Cs 137 concentration less than 2.3 uCi/mL b. TR-IRTS-8: Completion of preso11dification testing to ensure compressive strength greate r than TBD psi. c. TR-IRTS-2: CSS Cement Recipe d, Total Pu: less than 0.767 pCi/ gram salt e. Sulfate 50 : less than 0.14 gram / gram salt f. TOS: 20 1 percent (by weight) 5,9.2 If satisfactory, the Shift Engineer completes the Recipe Input Data i-Sheet (SGP 70 33). NOTE: IF THE COMPRESSIVE STRENGTH OF A CUBE SAMPLE IS BELOW TBD PSI, l' HEN. VIOLATION OF WVNs TECHNICAL REQUIREMENT OSR/TR-IRTS-8 OCCURS. PROCESSING WILL MOI PROCEED, THE TEST WILL 3E REPEATED. IF THE SECOND CUBE FAILS A CRITIQUE WILL BE HELD TO INVESTICATE THE-CAUSE OF_THE LOW COMPRESSIVE STRENCTd. A NONCONFORMANCE REPORT MAY BE ISSUED. ALL DECMS FOUND TO BE OUT-OF SPECIFICATION WILL BE HANDLED IN ACCORDANCE WITH SECTION-3.3 0F THIS PROCEDURE, 5.10 The gel time of the first full-scale drum from each 121 will be vertfled by visual inspection. If the gel. time of the full-scale product'is less=:han 90 minutes, processing may proceed. If-the gel time of a full scale drum is greater than 90 minu,3s, the process -will be stopped, and an Occurrence Report will be completed per WV-987. Processing may or may not.be resumed, based on_a technical eve.luation of processing variables, including, but not limited to: water-to-cement.ra;io, source of cement /CaNO blend, CaNO content in the blend, NaSi addition, etc. 3 3 PCP 0001279 RM,

J VVNS-PCP 002 Rev. 0 6.0 FULL-SCALE SOLIDIFICATION 6.1 Calculation of Full. Scale Formulation The constituents for the full scale recipe on a unit bas' are identified in Section 6.2 for decontaminated sludge wash. The recipe is verified for each batch of waste collected following-evaporation in 5D-15Al or 15A2 as described in Section 4.0 and 5.0. The decontaminated sludge wash solution has been demonstrated to be homogeneous during preoperational testing and the need for recipe changes ~is considered unlikely. Note that the CSS Waste Dispensing Vessel (400 gallon nominal capacity) is recirculated at 80 GPM. Homogeneity is, however, verified by chemical and radiochemical analyses in conducting routine verification of solidification. Following verification in the laboratory, the Shift Engineer seleccs a full scale recipe depending on the batch size to be processed from Tables 10A through 10F. These recipes are all based on the standard recipe varying in percent of drum fill only. The recipe utill:ed is documented in the shift log and during ptocessing; process limits are controlled within the permitted variante stated in the recipe. In the event that the sample.cannot be solicified using constituents within the allowed recipe variance, full-scale processing is secured and the Operations Manager is notified. Full-scale solidification is not permitted until t' e recipe is resolved. 6.2 Epil-Scale Formulation Th. following full scale reference formula will produce a dry solid monolith capable of performing in accordance with the 10 CFR 61 requirement for stabilized LLW. The data are provided for one gallon of waste: -o Decontaminated supernatant 1.0 gallon (at 20 w/o nominal total dissolved solids) Portland Type I cement with nominally 5.7 w/o 10.1 pounds o Ca (NO )2 preblended 3 o Silicone Based Antifoam 0.17 to 1.14 mL l - additive GE AF 9020 l o Liquid-_ Sodium Silicate 0.83 pounds i (: l 6.3 Full Scale Formulation Control i Laboratory verification of the full-scale formulation 'is described for each batch of waste to be processed in Section 4.0. Calculation of the recipe based on the laboratory verification is discussed in Section 6.1 and the run plan, attachment A. Process control and full-scale recipe data recording are discussed in Section 3;6. Waste classification is based on the isotopic content of the decontaminated sludge wash as determined by the analytical methods described in Section 5.0 and the total drum weight as recorded in the Data Acquisition System (Section 3.6), i l PCP:0001279.RM ! l ~

WVNS-PCP-002 Rev. 0 7.0 RECOFDS. DOCl' MENT CONTFOL. ASD OUALITY ASSl'RANCE Sample verification is performed in the Analyticsl Laboratory using approved Analytical Procedures and Analytical Methods. Decontaminated sludge wash concentrate samples are withdrawn from either tank 5D-15Al or SD-15A2 anc are delivered to the laboratory for analysis (specific analyses are described in Section 4.0 and 5.0). The sample identificacion number is assigned by the Analytical Laboratory and is logged in according to san =ple receiving procedures. The required analyses are performed (see Sections 4.0 and 5.0) and the data recorded on Analytical Pequest Fo r.r.s for radiochemical analysis and on the Sol'd 'ication Data Sheet for sample solidification verification. All data sheets are reviewed in accordence with Analytical Chemistry Procedure, ACP-5.1. All analyses are performed in accordance with approved procedures and under the Analytical Quality Assurance Program. Copias of the Analytical Requests Forms are deliver 7d to the CSS Shift Supervicor The Shift Engineer reviews all data and calculates :he recipe to be used for the decontaminated waste batch to be processed. The Shift Engineer and CSS Shift Supervisor sign the Recipe Input Data Sheet (SOP 70-33) and attach the corresponding Analytical Request Forms prior to processing the batch. The Aralytical Sample Log number is recorded in the shift log. The recipe is calculated by the shift engineer using the calculation sheet contained in the shift log. The recipe calculation for a single tank's volume of waste will remain unchanged for a normal processing week because of the capacity of the sampled tank (about 5 - 10,000 gallons) and its homogeneity. Since the waste is homogeneous, recipe chcnges during any processing week are not anticipated, although, slight variation in the recipe within the limits provided in approved recipes (Tables 10A through 10F) is permitted. Thc recipe calculation is reviewed and approved by the Shift Suparvisor if the full-scale recipe is determined to be within the recipe variances allowed, If the recipe is calculated to be outside the allowed variance, full-scale solidification is not permitted to proceed and the Operations Manager is contacted for resolution. Periodic quality assurance surveillance of the log book sheets, solidification operations and analytical work is performed to assure that all records ar maintained in accordance with approved procedures. The Analytical Requests Forms are controlled in accordance with the Analytical Laboratory Document Control Procedures. The operating log book contains uniquely numbered pages for each day of operation. These logs are retainec in the shift office during use and are transmi.ted to Master Records Center (MRC) when completed. All records are available for retrieval if necessary. Data Acquisition System (DAS) output contains a proce sing record for each drum produced at CSS. Records are also maintained thtough the WVDP Master Records Center. Each drum produced is classified by the Waste Disposal Operations group using radiochemical analysis data as described in Section 5.0 and the drum weight as calculated by the DAS. The vaste classification methodology is controllea by ACM-5704 Classification records are retained for eech drum by he Waste Management Operations group. The DAS output is transmittea to ARC in accordance with Standard Operating Procedure 001, " Control of Work Instruction Documer t s ' Individual drum data sheets are transmitted to Was te Disposal Operations ir accordance with Standard Operating Procedure 9-2. " Solid Radioactive Waste PCP:0001279.RM _ - _ _ _ _ _ _ _ - _

- - -. -. ~. b'VNS PCP 002 + - Rev. 0 -Disposal",. A complete data package for each drum will be maintained in accordance with SOP-70 45. 8.0 FULL-SCALE DRUM TESTING -In addition to.the sample verification described in Section 4,0 and 5.0, full-scale verification of solidification is also planned. One drum per process tank (based on the observed consistency of the process) will be sampled at random'co verify predicted fill as calculated from recipe constituents (see-Tables Al Al-6) absence of any free liquid and penetration resistance following a 3 day cure. The objective of _ these tests is to confirm successful solidification in the full-scale waste form, confirming.the sample solidification results, Deficies.tes observed in the full scale waste will prompt further investigation of drums produced from a given waste batch. During production of the full-sca a vaste form, ore drum per production process tank is placed into a test fixture located in the Process Cell. The drum is allowed to cure and is inspected for fill height, free liquid and penetration resistance. An Inspection Data Shee.t is prepared in accordance with S0P 70-40 -inspection procedure and forwarded to Operations in accordance with SDP 00,1, attachment B-1. The testing will be done in accordance with the run. plan. 4 PCP:0001279.R.M WVNS PCP 002 Rev, 0 ATTACRMENT A CEMENT SOLIDIFICATION SYSTEM RUN PLAN FOR SLUDGE WASH LIQUID TABLE OF CONTENTS Page

1.0 INTRODUCTION

.A-1 2.01 O BJ ECTIVES., .A-1 '3.0 SAFETY........ .A 1 3.1 Industrial Safety, ..A 1 3.2 Radiation Safety. .A-1 3.3 OSR's..... .A-1 4.0 EQUIPMENT.,.... .A-2

5.0 REFERENCES

.A-2 6.0' WASTE TRANSFERS.. .A-4 7.0. CSS 0PERATIONS... .A-4 7.1 General System Operations. .A-4 7.2 Waste Recipe. .A 6 7.3 Mixer. Flushing and Flush Processing. .A-6 7.4 System Flushing.. .A-6 7,5 Conduct _of Operations.. .A 7 8.0 PESPONSE TO DiERGENCIES.. .A-7 8.1 Waste Transfer.... ..A 7 8.2 Waste Processing in Automatic.. .A-7 8.3 Waste Processing in Manual. .A-8 8.4 Flushing or Flush Processing.. .A 8 '8.5-Drum Smearing and Loadout. .A 8 8.6 Loss of Ventilation. .A S 8.7 Loss of Electric Power. .A-8 9.0 QUALITY ASSURANCE AND RECORDS MANAGEMENT. .A 9 9.1 Sample Verification Data Sheets. .A-9 9,2 Log Book Records... .A-9 9.3 DAS Output. .A-9 9.4 Full Scale Drum Testing. ..A-10 l i l PCP:0001279.RM A-1 i l -3.

WVNS-PCP-002 Rev. O ATTACRMENT A TABLE OF CONTENTS (continued) Page 10.0 PREVENTIVE KAINTENANCE AN'D CALIBRATIONS. .....A ll 1

i 10,.1 Preventive Maintenance..

.A 11 10.2 Calibration. .A-11 ATTACliMENT Al Reference Recipes for Sludge Wash Liquid. .Al 1 ATTACRhENT A2 Run Plan Graphic. .A2 1 PCP:0001279.RM A-il

.,. ~. WVNS PCP.002 + Rev; O ATTACHMENT A CEMENT SOLIDIFICATION SYSTEM RUN PLAN

1.0 INTRODUCTION

This Ru Plan addresses the procedures, equipment, and controls necessary for proper operation of the Cement Solidification System (CSS). 2.0 OBJECTIVES The objective of the CSS is to solidify decontaminated sludge wash solution processed by the LWTS with cement to produce a waste form meeting the requirements of 10CFR61, 3.0 SAFETY 3 ',1 - Industrial Safety Safe operation of this system is the responsibility of the CSS operating _ personnel. Control will be effected through the use of approved SOP's, 3,2' Radiation Safety _ All operations will be performt-d in_accordance with the latest revision of the VVNS Radiological Controls Manual, WVDP-010 and - operatitig procedures. 3.3 OSR's Operation will also befconducted within limits and conditions set by the Operational Safety-Requirements (OSRs); OSR's are PCP;0001279.RM A1 -e ,--,,-w

'JVNS PCP-002 Rev, O ATTACHMENT A (continued) indicated in the SOP's, shift log data sheets and the Run Plan Craphic (attachment A2) which is posted in the control room. 4.0 EOUIPMENT The following equipment shall be available in the area during CSS operations: A. Tool box with assorted hand tools B. Drum pallets C. Anti-C clothing D. Respirators 5.0 PEFERENCES A. Process Control Plan, 'JVNS-PCP-002 B. Cement Solidification System Safety Analysis Report, SAR Volume IV C. Design Criteria D. Standard Operating Procedures indicated in the fel:owing listing: SOP 70 1 'Jaste Transfer to CSS SOP 70-3 Automatic Solidification Operation SOP 70 4 CSS Manual Solidification with the Process-Logic Controller Operational 50P 70-2 Gravimetric Feeder Operation SOP 70-6 Bulk Cement Transfer to Dry Bin l l l l PCP:0001279.RM .-2 3

VVNS PCP 002 Rev. O ATTACHMENT-A'(continued) 5,0 REFERFNCES (continued) SOP 70 7 Cement Truck Unloading SOP 70 8' Clean Drum Handling for CSS -S0P'70-9 Automatic Drum Operations for Cement Solidification System SOP 70-12 CSS Mixer System Flush Operation SOP 70-14 01-14 Building Ventilation Systems 0P 70 1501 14 Building H&V Filter Change SOP 70-16 Filter Change Room Filter Change SOP 70-17 Manual Drum Operations for CSS SOP 70 18 Alarm Piocedure for CSS -SOP 70-19 CSS Emergency Procedure Power " allure SOP 70 25 Calibration of Critical CSS Equipment SOP 70 31 CSS Drum conveyor Alarm Responses SOP-70 32 Operation of the CSS Silo Air Dryer SOP 70-33 Data Acquisition System Operation SOP 70 34_ Operation-of the 01-14/ CSS Process Room 4-Ton Bridge Crane ' SOP 70 35 _ Operation of the Maintenance 2-Ton Bridge Crane SOP 70-37 Smear Robot Operation SOP 70-40-. CSS Drum Sampling Station Operation SOP 70-41 CSS Preventive Maintenance Program S0P 70-45 Waste Certification Run Plan Graphic Drawings 900D-2198, Sheets l'and 2 l l t l l i '. L_ l l l [ PCP:0001279.RM A3

= WVNS-PCP 002 Rev. O ATTACHMENT A (continued) 6.0 VASTE TRANSFERS Waste transfers to the CSS will be made es required using SOP-70 1. The batch size transferred to the Waste Dispensing Vessel will be approximately 400 gallons, which is enough to produce about ten (10) drums of solidified waste. The waste will be sampled prior to the first transfer at SD 15Al or 5D 15A2 in accordance with the Process Control Plan. The sample will be assigned a sample log number when it is received at the Analytical Laboratory and will be analyzed for its chemical and radiochemical composition in accordance with the Process Control Plan. A portion of the sample will be solidified to verify that us i of the reference recipe will result in a sclid dry monolith with appropriate compressive strength. The analysis results and Solidification Data Sheet will be sent to the CSS shift office; using the solidification sample verification data sheet, the shift engineer will select an approved. full scale recipe from attachrant Al and document the calculation in the shift log book. Full scale solidification will not be initiated without acceptable verification of solidification in the laboratory. Two (2) mixer batches will be dischargad into each drrm. Due to its larger operating volume, tank 5D-15Al is sampled prior to solidification and at 50 percent i 10 percent leve'l as an ir process check. 7.0 CSS OPERATIONS 7,1 General System Operations Prior to initiating transfers to the Waste Dispensing Vessel, verification of solidification for a sample of waste to be l transferred and recipe calculation for the full scale product must be completed. 1 l i l PCP:0001279.RM A-4 i. ,,7-.

VVNS.PCP 002 Rev. O ATTACRMENT A (continued) 7.1.1 Waste may be transferred to thi Vaste Dispensing Vessel from either Concentrates Storage Tanks 50 15Al or SD 15A2 while k the solidification process is ongoing providad that solidification verification was performed on a saaple of the vaste being transferred prior to initiating the transfer. Tranafers are made just prior to reaching the low level alarm po ir.t in the Waste Dispensing Vessel, At that point, sufficient volume remains in the Waste Dispens!ng Vessel to continue processing for 40 minutes. Three (3) or four (4) transfers will be required per shif t. Vaste transfers are i l j performed in accordance with 50P 70 1 7.1.2 Drums will be tested for surface contamination prior to release to the Drum Loadout Area. Drums released to the Drum Loadout Area must have smearable surface contamination levels 2 less than 20 dpm/100 cm Alpha and less than 200 dpm/100 ca: Beta contamination. All drums with greater amounts of removable contamination will be decontaminated. Contamination testing of packages is performed in accordance with SOP 70 37. The top, sides, and bottom will be _ested. 7.1.3 One (1) mixer will normally be used for waste p" c ;stan, discharging two (2) mixer batches into each drun per SOP 70 3. A backup mixer is available as an installed = pare. 7.1.4 Prior to any extended shutdown of the process, the mixers will be flushed to a decant dru.? using SOP 70-12. 7 1,5 As eight (8) drums are staged in the Drum Loadout Area, the drums will be loaded out by Vaste Operations and transported to the RTS Drum Cell. All drums will be labeled with an individual bar code set ial number. All drum data: production recipe, date filled, weight, dose ate, s.rface contamination I PC P : 00012'i 9. RM A5 I i

VVNS PCP 002 Rev. 0 ATTACRMENT A (continued) level, etc., will be cross referenced to this bar ecde se lal number and recorded by the Data Acquisition System (DAST. Drum production records as recorded by the DAS will be transmitted to MRC in accordance with SOP 00 1. Ir.diidual drum data sheets are transmitted to Vaste Operations in accordance with SOP 9 2. .i 7.1.6 All drum records including processing data, vaste classification data sheets, and DAS data will be compiled into a waste certification package in accordance with SOP 70 45. 7.2 Easte.Etting The decontaminated sludge wash solution will be solidified in the CSS in accordance with CSS SOP's. The approved recipes are shown in Ta' ale 1. Recipe verification is discussed in Section 6.0-As an operator aid, a graphic is included in ettachment A2 showing the process flow, process procedures, operational safety requirements, f product quality requirements and process requirements. 7.3 Mixet Flushine and Flush Processing Flush operations will be conducted using SOP 70 12. 7.4-System Flushing If necessary for maintenance, the s, stem may be flushed. 7. 4.1 - The Vaste Dispensing Vessel is sampled, flushed. and drained in accordance with individual work orders for the infrequent event. -7.4.2 The mixers are flushed in accordance with SDP 70-12. PCP:0001279.RM A 6.

VVNS PCP 002 ATTACHMENT A (continued) l 7,5 Conduct of Operationg A Shift Engineer and a CSS Shift Supervisor will be on each shift to assure safe and technically correct operation of the Cement I Solidification System. Technical direction of the work is the responsibility of the Shift En6 neer, all direction provided to the i operators or Maintenance personnel will be made through the CSS Shif t Supervisor. In the event of any casualty or emergency situation, the CSS Shift Supervisor, by virtue of training and experience, is solely 1 responsible to direct any actions necessary to stop and recover from such situations. Full recovery from any casualty or emergency situation will be performed in accordance with established emergency procedures. 8.0 RESPONSE TO EMERGENCIES Should a fire, or other emergency requiring evacuation occur dut-ing 4 processing operations, *he operating personnel should take the following steps: 8.1 -Vaste Transfer Immediately stop the operation in accordance with SOP 70 1 and follow plant emergency procedures. 8.2 Waste Proces11ne in Automatic L Allow the batch to continue in accordance with SOP 70 3. The system vill finish the batch and stop when an empty drum is not transferred i to the Fill Station. Follow plant emergency procedures. i I l l PCP:0001279.RM A7

'JVNS PCP 002 Rev. O ATTACHMENT A (continued) r 8.3 'daste Processine in Manual Discharge mixers to drum in accordance with SOP 70 4, follow plant emergency procedures. l 8.4 Flushir.2 or Flush Processing Inr-diately stop the operation in accordance with SOP 70 12 and ' ells plant emergency procedures. 8.5 Drum Smearine and Lo4dout Immediately stop the operation in accordance with SOP 70 37 and follow plant emergency procedures. Note that if the Drum Loadout Shield Door is QEEN, any drums should be indexed clear of the shield door, the truck drawbridge should be raised, and the shield door should be CLOSED. 8.6 LOSS OF VENTILATION Allow the batch to complete per S0P 70 3 (Automatic) or 50P 70 4 (Manual). Do not resume operation until ventilation has been restored in accordance with SOP 70 14. Evacuation of the CSS Control Room is not required. 8.7 LOSS OF ELECTRIC POEIR Complete the batch and' initiate flush in accordance with SOP 70-19. Evacuation of the CSS Control Room as not required. ? PCP:0001279.RM A8 i L

1 l VVNS PCP 002 Rev. O ATTACHMENT A (continued) 9.0 OUALITY ASSURANCE AND. RECORDS MANAGEMENT 9,1 garple verifhation Data Sheets 9 ample verif' cation is performed for eech tank volume SD 15A1 or SD 15A2 feeding to the CSS Vaste Dispensing Vessel to assure proper solidification of the waste using the reference recipe. Copies of the solicification sample data sheets are scnt to Process Control Engineering, Data sheets are approved in accordance with Analytical Chemistry Procedure s.CP 5.1. 9.2 Lou Book Records A daily log book, one set of uniquely numbered entry pages per day, is maintained at the CSS shift office. The log book is used fo; data recording required by procedure and for documentation of the recipe used. The log book contains the sample solidification verification log number assigned for each feed tank of waste to be processed SD 15A1 or 5015A2 by the Analytical Laboratory as a reference. Log book entries are reviewed and approved by the CSS shif t supervisor and when completed for an operating year, are submitted to the Master Record Center for retention. 9.3 Waste Certif_ication DAS output contains production data for each drum processed at CSS. The DAS weekly activity file is maintained on disk. Drum records may be copied to diskette during nonoperational periods. Manual data recorded on SOP 70-4, attachment B, and DAS Real Time Printout are reviewed by Operr.tions Technical Support and forwarded to Records Management with transmittal sheet. SOP 70 33, attachment B. I PCP:0001279.RM A9 l

VVNS PCP 002 f Rev. O ATTACllMENT A (continued) A copy of Presolidification Test Data, Analytical Request Form WV-1113, is forwarded f rom Analytical 6 Process Chemistry to Quality Assurance and Waste Management Operations. Missing data or data requiring clarification is corrected by Operations Technical Support. Revisions to the Drum Data Base are recorded and authorized on attachment C to SOP 70-33. Final drum classification, based on drum data and radiochemical analysis is co.npleted by Analytical and Process Chutistry in accordance with SOP 9 8, "Was-te Classification" and verified by Vaste Engineering. All drum data, including: drum classification and processing data, are compiled by Operations Technical Support per 50P 70 45. 9.4 Enll. seal _e Drum Testinz From each Processing Tank SD 15Al or A2, a drum is pulled at random from the production line and is placed into the drum tes: fixture located in the process room. The drum is tested to assure proper fill, proper penetration resistance and dryness with respect to free liquids as required in 50P 70 40. \\ i PCP:0001279.RM A-10 k....._.

=-.. -..._ WNS PCP 002 Rev. 0 ATTACRMENT A (continued) i 10.0 PREVENTIVE MAIN *ENANCE AND CALIJRATIONS 10,1 Preventive Maintenanu Periodic preventive maintenance required for the CSS is described in S0P 10 41, periodic preventive maintenance items are scheduled in the maintenance recall system. 10.2 Ealibrations Instruments requiring periodic calibration are identified in the appropricte maintenance recall lists. t i i PCP:0001279.RM A 11 _ _, _, _ _ _ _ _ _. -.. _, ~. ~.., _ _.._,-_. __

L'VNS PCP 002 Rev. O ATTACHMENT A (continued) Summary of CSS k'aste Stream Formulations Al 1 18.0 Gallons / Mixer Batch Al 2 18.5 Callons/ Mixer Batch Al 3 19.0 Ca11ons/ Mixer Batch j Al 4 19.5 Gallons / Mixer Catch Al 5 20.0 Gallons / Mixer Batch Al 6 20.5 Gallons / Mixer Batch Notes for Table Al 1 throuch ni 6 1. Drum volume accounts for plastic liner. 2. Calcium nitrate tetrahydrate based on 5.7 w/o nominal of cement. 3. 38% w/o sodium silicate solution addition based on 12.4 w/o of water in sludge wash solution 4. Antifoam emulsion added at 0.57 to 0.76 mL/ gallon of sludge wash solution 5. The Sur trvisor or Shif t Engineer may authorize use of any of the available recipes, basing his selection on the desired volume of waste to be processed per mixer batch. PCP:0001279.RM A 12 a. _. _. _... _.... _ _.. - ~ _ _. _.., _ _. _ _ _ _ _, _ _. _ _, _. _ _

WNS PCP 002 Rev. O TABLE A1 1 18.0 CALLONS PER MIXER BATCH PEFERENCE RECIPE FOR CEMENT SOLIDIFICATION OF SLUDGE VASH *.IQUID TDS 19% 20% 21% Sp. Cr. (g/mL) 1.154 1.16 1.166 Gallons of Vaste 18.0 18.0 18.0 Nom. Vater / Cement Ratto 0.66 0,66 0.66 Nasi (1bs) 7.2 to 7.2 to 7.2 to 28.6 28.8 28.8 Min. AF9020 3.07 mL 3.07 mL 3.07 mL Man. AF9920 20.5 mL 20.5.mL 20.5 mL

Vaste (1bs) 173 174 175 V 2 Timer (sec.)

12.6 12.6 12.6 // Cement 31end (1bs) 225.1 223.7 222.1 Min. Vaste (Ibs) 169 170 171 Mr.x. Veste (1bs) 177 178 -179 Min. Water / Cement Ratio 0.64 0.64 0.64 Max. Water / Cement Ratio 0.68 0.68 0.68 Drwn % Full 85% 85% 85% Slurry Density (gm/mL) 1.70 1.70 1.70 ( i l l I PCP:0001279.llM Al-1 l u ~,_ _ _ _.. _,. ~..,.. _

i VVNS PCP 002 Rev. O TABlZ Al 2 18.5 CALLONS PER MIXER BATCH REFERENCE RECIPE FOR CEMENT SOLIDIFICATION OF SLl'3GE VASH LIQUID TDS 19% 207 21% Sp. Gr. (g/mt) 1.154 1.16 1.166 Callans of Vaste 18.5 18.5 18.5 Nom. Water / Cement F stio 0.66 0.66 0.66 NaSf (1bs) 7.4 to 7.4 to 7.4 to 29.6 29.6 29.6 Min. AF9020 3.16 mL 3.16 mL 3.16 mL Max. AF9020 21.1 mL 21.1 mL 21.1 mL

Vaste (Ibs) 178 179 180 V+2 Timer (sec )

13.0 13.0 13.0

Cement Blend (1bs) 211.7 230.0 728.5 Min. Vaste (1bs) 174 175 176 Max. Vaste (1bs) 182 163 184 Min. Water / Cement Ratio 0.64 0 64-0.64 Max. Water / Cement Ratio 0.68 0.68 0.68
Batch /Mirer (1bs) 425.7 425.0 424.5 Drum % Full 87%

871 87% Slurry Density (gm/mt) 1.70 1 70 1.70 PCP:0001279.RM Al 2 ~. -. _. _, _. -.. - - = - -,,.. _ _.

. -. ~. , _ -. ~ i VVNS-PCP 002 Rev. O i TABLE A1 3 19.0 CALLONS PER MIXER BATCH REFERENCE RECIPE FOR CEMENT SOLIDIFICATION OF SLUDGE VASH LIQUID TDS 19% 20% 21% Sp. Cr. (g/mL) 1.154 1.16 1.166 callonsof Vaste 19.0 19.0 19.0 Nom. Water / Cement Ratio 0.66 0.66 0.66 NaSi (1bs) 7.6 to 7.6 to 7.6 to 30.4 30.4 30.4 Min. AF9020 3.25 mL 3.25 mL 3.25 mL Max. AF9020 21.7 mL 21.7 mL 21.7 mL

Vaste'(Ibs)-

183 184 185 P V 2 Timer (sec.) 13.4 13.4 13.4

Cement Blend (1bs) 238.2 236.5 234.8 Min. Vaste (1bs) 179 180 181 Max. Vaste (1bs) 187 188 189 t

Min. Vater / ement Ratio 0.62 0.62 0.62 Max. Water / Cement Ratio.. 0.70 0.70 0.70

Batch / Mixer (1bs) 437 432.5 432 Drum % Full 89%

89% 89% Slurry Density (gm/mL) 1.70 1.70 1 70 FCP:0001279.RM Al 3 ,-,,,.-,,,,..v. - - -.,,,..,.. -,~.

i Wl?S PCP.002 Rev. O TABLE Al 4 19.5 GALLONS PER MIXER BATCr. REFERENCE RECIPE FOR CEMENT SOLIDIFICATION OF SLUDGE VAEH LIQUID TDS 19% 20% 21% -Sp. Gr. (g/mL) 1.154 1.16 1.166 Callons of Vaste ~ 19.5 19,5 19.5 Nom. Water / Cement Ratio 0.66 0.66 0.66 NaSi (1bs) 7.8 to 7.8 to 7.8 to 31.2 31.2 31.2 Min. AF9020 3.33 mL 3.33 mL 3,33 mL Max. AF9020 22.2 cL 22.2 mL 22.2 mL

Waste (1bs) 188 189 190 V 2 Timer (sec.)

13.7 13.7 13.7

_ Cement Blend (1bs) 243.5 241.7 240.0-Min. Vaste (1bs) 184 185 186 Max. Vaste (1bs) 192 193 194 Min. Water / Cement Ratio 0.64 0.64 0.64 Max. Water / Cement Ratio 0.68 0.68 0.68
Batch / Mixer (1bs) 447.5 446.7 446 Drum % Full-

-91% 911 91% Slurry Density (gm/mt) 1.70

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4 VVNS PCP 002 Rev. O TABLE Al 5 20.0 GALLONS PER MIXER BATCH REFERENCE RECIPE FOR CEMENT SOLIDIFICATION OF SLUDGE WASH LIQUID TDS 19% 20% 21% Sp Cr. (g/mL) 1.154 1.16 1.166 Callons of Vaste 20.0 20.0 20.0 Nom. Vater / Cement Ratio 0.66 0.66 0.66 NaSi (1bs) 8 to 8 to 8 to 32 32 32 Min. AF9020 3.42 3L 1.42 mL 3.42 nL Max. AF?020 22.8 mL

2.8 mL 22.8 mL

Vaste (1bs) 192 193 194 V 2 Timer (mee.)

14.0 14.0 1(. 0

Cu:ent Blend (Ibs) 247.0 24J.0 245.0 Min. Vaste (1bs) 188 189 190 Max.-Vaste (1bs).

196 197 198 Min. Water / Cement Ratio 0.64 0.64 0.64 Max. Water / Cement Ratio 0.68 0.68-0.68

Batch /Hixer (ibs) 458 457 456 Drum % Full 94%

941 94% Slurry Density (gm/mL) 1.70 1.70 1.70 PCPiOOO1279.RM Al 5 b-..

] WNS PCP 002 s Rev. O TABLE Al 6

20. 5 CALLONS PER M.1XER BATCH i

REFERENCE RECIPE FOR CEMENT SOLIDIFICATION OF SLUDCE VASH LIQUID TDS 19% 20% 21% Sp. Cr. (g/mL) 1.154 1.16 1.66 Callons of Vaste -20.5 20.5 20.5 Nom. Water / Cement Ratio 0.66 0.66 0.66 t.. Si (1bs) 8.2 to 8.2 to 0.2 to 32.8 32.8 32.8 Min. AF9020 3.5 mL 3.5 mL 3.5 mL Max. AP9020 23.3 mL 23.3 mL 23.3 mL

Vaste (1bs) 197 198 199 V.2 Timer (sec.)

14.5 14.5 14.5

Cement Blend (1bs 256.4 254.5 252.6 Min. Vaste (1bs) 193 194 195 Max. Vaste (1bs) 201 202 203 Min. Vater / Cement Ratio 0.64 0.64 0.64 Max, Vater / Cement Ratio 0.68 0.68 0.68
Batch / Mixer (1bs) 469 469 468 Drum % Full 96%

96% 96% Slurry Density (gm/mL) 1,70 1.70 1.70 PCP:0001279.RM A1-6 _ _ _.. ~ _ __ -. _ - _ _ _

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ENCLOSURE 3 Properties of Cemented Low-Level Liquid Waste at West Valley
Garrett A, Smith

Presenter i
-West Valley Nuclear. Services Co., Inc. P. O.- Box 191 West Valley, New York 14171 (716) 942 4325 WORK PERFORMED UNDER CONTRACT DE-AC07-81NE44139 l l l-April 1992 To be presented at the Second Engineering and Technology Conference l on Waste Management and Environmental Restoration being held in San-l Juan, Puerto Rico, April 9, through April 12, 1992. 0023DAL.LET . - _ _.. _ _. - - _. _ _ _ _ _ _ _. -. _,.. - - _ _...,. = -. - -
- ~. 9 PROPERTIES OF CEMENTED LOW-LEVEL LIQUID WASTE AT WEST VALLEY ABSTRACT The West Valley Demonstration Project (WVDP) is an environmental remediation effort focused on demonstrating technologies to solidify liquid High Level Waste (HLW). To preparo for HLW solidification, the WVDP is actively protreating the waste by removing - liquid HLW from an underground
~~tanx, extracting radioactive cesium from the liquid using an ion-exchange system, and stabilizing the resulting Low-Level Waste (LLW) ir. an NRC endorsed cement waste form.~~
In May 1988, the tank contained 600,000 gallons of liquid high-level nuclear waste left from the - only commercial spent fuel reprocessing operation in the United States.- Since May 1988, WVDP has successfully prctreated over 420,000 gallons of high-level radioactive waste, resulting in over 10,000 Class C cement drums with-an average surf ace dose rate of 35 mR/hr. Prior-to pretreatment, WVDP has developed -an extensive process control and testing plan to ensure an acceptable waste form with respect to the NRC Branch Technical Position. Furthermore, WVDP has gone beyond that requirement by continually testing the cemented waste form. Based on testing performed at WVDP and independent private laboratories, the cemented waste form has met or exceeded all criteria developed during laboratory-scale qualification testing prior to full-scale operation. For example, results include actual compressive strength data ranging from 800 psi (a -6 month cure-time) to 1500 psi (a 3-year cure time) for cemented waste in the full scale product drums compared to the minimum required compressive strength of 186 psi. INTRODUCTION The pretreatment_of the liquid portion of the high-level waste is accomplished in an Integrated Radwaste Treatment System (IRTS)(see figure 1). The IRTS starts with a supernatant treatment system, that uses a natural zeolite ion-exchange material to remove 99.9% of the radioactive Cesium 137 from the waste stream. In the next step-of the process the decontaminated supernatant is concentrated to a nominal 39 % Total Dissolved Solids (TDS). This 39 percent-TDS concentrated waste liquid is then ready for cementation. The waste-is mixed with sodium silicate, an anti-foam emulsion, and Portland Type I cement blended wita 5 percent calcium nitrate. The 0023DAL.LET 2 i h
Figure 1 IRTS Process Flow Diagram i l Low-Levei Waste Processiiig Cycle TME BD-1 WT@fEh ' g ^ ~ p# l l l L 0-t ^ IIIIIIII1I g# di ci in. u stocmarant Cement Ligtid Waste / Soldfication c Traatment d y tu Supernatant l DStudgoI 70 TME BD-2 VITRIFICATIG1 SYSTD1 3 0023DAL.LET
resultant blend is mixed in a stainless steel high-shear mixer (like a household blender) and poured into 71-gallon square drums. These drums are then transported to an on-site remote storage facility, where they are stacked in a diamond position, awaiting final disposition. The WVDP cemented waste form in qualified to comply with the waste stabilization requirements of 10 CPR 61 and the tiuclear Regulatory Co=aission (11RC) Branch Technical Position on Waste Form. The pretreatment process is controlled in accordance with the Process Control Plan (PCP) for cement solidification. The PCP was prepared in accordance with the NRC's Guidelinas f or Preparation of a Solid Waste Process Control Program. An extensive testing program in place at WVDP ensures compliance with the waste stabilization requirements of 10 CFR 61 and the NRC Branch Technical Position on Waste Form. These tests begin when samples ~ of the concentrated decontaminated liquid waste, taken from 5000 gallon production batches, are checked for 10 CFR 61 radionuclide analysis. Then, a 2" x 2" x 2" cemented cube is made and checked f or gel time, bleed water, penetration resistance (af ter 24 hours), and compressive strength (af ter 7 days). These tests are completed as process control checks to verify waste acceptance per the PCP. Once the gel time, bleed water, and penetration resistance tests are satisf actorily completed, the liquid is released f or full-scale sol:, lif ication. To farther ensure an acceptable waste form, one full-scale gel time test is conducted for each concentrates batch that is solidified. To do this, a cample of the freshly poured cement waste form is scooped from a full drum and monitored to determine the amount of time until it gels. Additionally, one drum from each concentrates vaste batch is set aside for further testing. These tests include a full-scale tipper test to check f or free
~~liquid, drum penetration resistance, and freeboard to determine the percer.t full of the drum.~~
For this test the drum selected from the concentrates batch being processed is placed in the test fixture and allowed to cure for 72 hours. It is then tipped until its axis is 100 degrees from the vertical and held for an additional 24 hours. The drum is then uprighted, opened, and checked. For confirmatory testing, WVDP has conducts selected tests on samples which were core-bored out of actual product drums. The first set of tests, outlined in the Short Term Test Plan, provided data to demonstrate product homogeneity by showing a correlation between values obtained through testing of full-scale production drums and values obtained during laboratory qualification testing. The scope was limited to the following final product characteristics: 1. Compressive strength after an initial cure period of 40 days (Before and after leach testing); 2. Cs-137 homogeneity; and 3. Cs-137 leach testing. The tests were conducted on 3" diameter cylinders and cores obtained f rom fu3 ' -scale product drums by core boring after the required cure time. 0023DAL.LET 4
The Long-Term Test Plan provides information on long-term cement compressive strength and evaluates effects of aging over a five-year period. The testing censists of performing compressive strength and visual inspections of core bores obtained from full-scale product drums. Core boring and inspections are performed on a different drum approximately every six months over a period of five years. To date, WVDP has tested nine drums having a cure time of up to three and a half years. t SUMMAIlY OF RESULTS Pre-Solidification and In Process Testing To dato 106 pre-solidification samples have been taken from the concentrated decontaminated liquid waste before it was cemented. The saraples have been analyzed and the average compressive strength of the samples is shown in figure 2. This testing has shown an average compressive strength of 775 psi. All of the results from this testing are greater than the minimum allowable compressive strength of 186 psi defined in the Process Control Plan. Additionally, every drum tested for the full scale " tipper test" has exceeded 700 psi penetration resistance, with no reported free liquid. Furthermore, every drum tested had a fill factor greater than 85%, which is the minimum allowed. Short Term Test Plan During the Short Term Test Plan a drum was core bored after nominally 70 days cure time. A total of thirteen core bore samples were obtained from this drum; nine were subjected to compressive strength testing and four to Cs-137 leach testing. The failed fragments from the compressive strength test were analyzed for Cs-137 radionuclide distribution. The Short Term Test Plan compre u ive strength results are shown in table 1. The short term testing also indicated a homogenous mixture throughout the production drum and an acceptable leaching criteria for selected radionuclides. Long Term Test Plan To date nine drums have been cored and analyzed per the Long Term Test Plan. Three cores were taken and crushed from each of these drums (one from the middle, one from the top and one from the bottom). The average compressivo strength value of three cores from each drum is calculated and the mean compressive strength versus time is given in figure 3. This data shows that after three and a half years of testing the compressive strength of the full-scale production. drums is still increasing. j oo23DAL.LET 5 ---r,,--.-%,w----,~,,,--,,,-,-,,----w,- 3,-,,r,- ,,,,..w,,.,.-..-i. ,n, .---i,--~..
CONCLUSION All of the test data collected to date demonstrates that the waste form produced at WVDP meets the NRC 10-CFR-61 requirements for a Class C Low Level Waste. Furthermore,
~~WVDP, during the qualification of its cement waste form, has shown that this waste form has exceednd all of the requirements set in the NRC Branch Technical Posit in on Waste Forn.~~
This testing of the waste form did not stop whsa production began. Both the Long Term and Short Term confirmatory test progrrms continue to show that compressive strength and other requirements of the production drums moet or exceed all minimum requirements and demonstrate the integrity of the waste form over time. 2 ' ip 0023DAL.LET 6 m...._
Figure 2 Pre-Solidification Tc. Results Average Compressive Strength of Samples 15(X) = 50 1000 v E E B 05 Y c; Ea 500 E O U s e a 0 Sep--88 Jan-90 Sep-91 Date _._ NRC/WVNS Agreed Minimum Requirments 0023DAL.LET 7 --- -J
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2.0 REFERENCES

1.0 INTRODUCTION

5.0 REFERENCES

1.0 INTRODUCTION

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