ML20100P991

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West Valley Demonstration Project Waste Qualification Notebook
ML20100P991
Person / Time
Site: West Valley Demonstration Project
Issue date: 02/04/1992
From:
ENERGY, DEPT. OF
To:
Shared Package
ML20100P988 List:
References
REF-PROJ-M-32 NUDOCS 9202050061
Download: ML20100P991 (68)
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Text

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Demonstration Project Revision Date 11/18/91 Engineering Release #2:27 TEST PLAN CEMENT ASTE FI 'l4 QUALITICATIClI 0F SLUDCE 'a' ASH LIQUIDS PREPARED BY V'T

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, f , 4 *M J. L. Mahoney Co g;nizant Engineer NT s

APPROVED B7 -

b dd. 41CGff D. C. Meess fo5nizant S/ stem Design Manager APPROVED BY l 1b P. J. Valenti Facility Representative APPROVED BY .J//'A9Mff.J)/M-'/'/

Quality 4Wsurance Manager

% D./! L. Shugars APPROVED BY D . b M i* nN O D. J. Harvard Ra:f ajion 6 Safety Mansger a ~L h:

APPROVED BY A M P . G /m J. C. Cwynar I IRTS Process Cofitrol Engineerin6 l

1-i West Valley Nuclear Services Co., Inc.

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VVNS TPL 70-12 i TEST PLAN CEMENT WASTE FORM QUALIFICATION .,

OF SLUDGE VASH LIQUIDS 4 REV. 0 l 1.0 PURPOSE-The purpcse of this test plan is to describe the Cemenc sste Form .

Qualification of Sludge Wash Liquids. The plan specifies the to ting '

required to develop _and qualify a stable vaste form in accordance with the requirements of 10 CFR 61, Code of Federal Regulations. Title 10

" Licensing Requirements for Lard Disposal of Radioactive Waste" and the, USNRC Branch Technical Position on Waste Form. Revision 1, dated January 1991.

'2.0 APPLICABILITY This program applies to the qualification testing required to demonstrate that-the vaste form developed herein for the Sludge Wash waste stream meets the waste stability criteria of 10CFR61,56.

3.0 - GENERAL REQUIREMENTS

- 3.1 All procedures fv. corducting tests, documenting, and evaluaring test results will be preoared, reviewed, and approved in accordance with the requirements of the VVNS Policy and Procedure Manual, Engineering Procedures EP 11001, EP 11-003, and S0P 00 2.

3.2 Test ~ requirements will be as specified in-Test Requests (TRQ) 'ssued by the IRTS Engineering organization in accordance with EP 11 003 3.3 :Testin5 in response to the Test Requests shall be performed in

- accordance with the Test Procedures.(TP) issued by the Analytical & _

Process Chemistry Laboratory in accordance with EP-11-003; 3.4 operation of the Cement Solidification System (CSS) will_be-by--

qualified CSS Operations personnel in accordance with existing Standard Operating Procedures (SOP's), and authorized work orders.

'35. Lab testing wi.1 be performed by qualified Analy * . & Process Chemistry Technicians-using Analytical Chemistry Metands (ACM's),

3.6 All data collection, reporting, and hocumentation will be performed in accordance with EP.11001 and EP ll 003 as applicable.

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4,0 ECOPE The scope of the qualification program for new cement recipes for sludge wash liquids is depicted by Figure 1 and is described below. This program has become necessary because the recipe being qualified under WVMS TPL 70 11 failed to meet the immersion test requirements of the USNRC Branch Technical Position on Waste Form, Revisien 1 .ted January, 1991.

! 4.1 Immersion Qualification of Lower Waste Loadings.

This series of Test Request (VVNS-TRQ 044). Test Procedure (WVNS-TP 044), and Test Summary Report (VVSS-TSR 044) will qualify at least two cement waste form recipes at lower waste loadings. The original recipe for sludge wash liquids developed in VVNS-TP-025 __

used salt solutions concentrated to 31 + 2 wtt tota! dissolved solids (TDS).

The new recipes will qualify cement waste forms at lower salt concentrations. Immersions will be carri d out in both domineralized water and synthetic sea water as specif'ed by ANSI 16.1 - 1986. Testing will be performed on 3 iner diameter x 6 inch tall cylinders cast from cement waste mixed in the full-scale CSS mixar. Cores taken from drums produced in CSS will also be tested. A baseline cured compressive strength will be determined before immersing cores and cylinders. Thermal cycle testing of cylinders will be included as a portion of this test series.

4.2 Immersion Qualification of Alternate Recipes This series of Test Request (WVSS TRQ-XXX), Test Procedure (WVNS-TP XXX), and Test Summary Repott (WVNS-TSR XXX) will qualify at least two cement waste form recipes through modificaticns to the cement specification developed in VVNS-TP 025. Before committing to _

the tests, screening tests will be performed in the lab on small scale speciments (2" x 2" x 2" cubes) to verify general cement waste form handling (gel time, free water, etc.).

Options that may be considered include changes in the level of cement additives (calcium nitrate, sodiwn silicate), new additives, or a change in the base cement specification (ASTM Portland type I to type V). Immersion testing will be carried out in both demineralized water and synthetic sea water. Testing will be performed on 3 inch diameter x 6 inch tall cylinders cast from cement waste mixed in the full-scale CSS mixer. Cores taken from drums produced in CSS will also be tested. A baseline cured compressive strength will be determined before immersing cores and cylinders. Thermal cycle testing of cylinders will be included as a portion of this test series.

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WVMS-TPL 70 12 Rev. 0 4.3 Confirmatory Qualification of Candidato Recipe Testing on actual radioactive cement waste produced from a wash solution generated in the laboratory will be performed. This test series will again include a Test Ren,uest (VVNS-TRQ XXX), a Test Procedure (WVNS-TP XXX), and a Test Summary Report (WVNS TSR-XXX).

The radioactive wash solut.on will be produced in the laboratory i

from bench scale equipment to simulate sludge washing of the High Level Vaste. After decontamination in the laboratory to simulate STS operation, concentration to the goal TDS will be completed and at least three cement waste cubes (2" x 2" x 2")

produced. Compressive strength measurer.ent after curing, and compressive strength measurement after immersion in b<,th deminerali:ed water and synthetic sea water will be performed. __

4.4 Radioactive Qualification of Candidate Recipe Qualification of a radioactive simulant of the sludge wash cement vaste form will be performed. This test series will again include a Test Request (WVNS TRQ XXX), a Test Procedure (WVNS TP-XXX), and a Test Summary Report (WVNS TSR XXX).

Decontaminated radioactive wash solution from prior supernatant processing will be collected in the full scale STS equipment and transferred to the laboratory. Chemical adj ustments such as the increasing both the sodium sulfate and pH will be completed on the solution. Mini-cylinders (l" diameter x 3" long) will be prepared using at least one of the candidate recipes. Leach resistance of the radionuclides to both demineralized water and synthetic sea water will be performed on the cement waste forms.

4.5 Varia'ollity Testing of Candidate Recipe Variability testing of at least one candidate cement waste form recipe will be performed. This test series will again include a Test Request (WVNS TRQ XXX), a Test Procedure (VVNS-TP XXX), and a Test Summary Report (WVNS TSR-XXX).

The goal of this test series will be to define the critical process control parameters (including acceptable waste composition ranges) for at least one candidate recipe. Two of the variables that will be included in the test are the water-to cement ratio, and sulfate level in the waste.

Using sin,ulants , a multivariant experiment will be performed on cement waste forms including processing characteristics (gel time, free water, etc.), cured compressive strength, and compressive strength after immersion.

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1.0 INTRODUCTION

1.1 This work is required to demonstrate the acceptability of an actual cement product raade from radioactive sludge wash liquids. The uork will provide a dsta poir.t comparison to contrast radioactive cement against cement made with reagents simulating LWT3 concentrates. The testing shall be guided by 10 CFR 61, Code of Federal Regulations.

Title 10 " Licensing Requirements for Land Disposal of Radioactive Waste," and the USNRC Eranch Technical Position of Waste Form, Revision 1, dated January 1991.

1.2 The scops of this work is consistent with 6 etion 4.6 of VVNS TPL-70 11, ' Test Plan for the Waste Form Qualification Program for Cement Solifification of Sludge Wash Liquid."

1.3 Production of the cement cube will require the use of sludge wash solution for wash cycle al created in VVNS TP-032, and decontaminated in WVNS TP 033.

1.4 lest Procedure VVNS-TP-034, providing instructions for meeting the requests specified in this Test Request shsll be issued by the Analytical 6 Process Chemistry Cognizant Scientist per EP-11 003.

1.5 A Test Summary Report (TSR) documenting the results of this testing shall be issued by the Cognizant Teat Engineer per EP ll-003.

2.0 OBJ ECTIVES 2.1 After receipt of analytical results from test procedures VVNS-TP-032 and VVNS-IP-033, the decontaminated wash solution from wash cyclo al shall be sampled and analyzed for:

Total Dissolved Solids (TDS) Density pH gross alpha gross beta 2.2 The decontaminated wash solution shall be slowly evaporated to a nominal 31 t 2 weight percent TDS. The concentration shall be performed in a glass container. Lab personnel shall note any unusual occurrences during the evaporation (i.e., precipitation, scaling). If any solids form during the evaporation, the concentrates shall be filtered and the solids analyzed (per available quantity of solids) following the analyses listed in Section 2.3.

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WNS TRQ 034 Rev. 0 2,3 lThe resultant concentrates shall be analyzed for:

p jj NO2~ E l'04 d Ti NO3 ' ' lia SO4 *2 Ca B03 *3 TOC TIC Cr Cl F* Al U pH Total Dissolved Solids (TDS) density Total Suspet.ded Solids (TSS) alpha Pu. Cs 137 Sr 90 Tc-99 gross alpha gross beta 2.4 Approximately 96 al of the concentrates ahall be used to make a standard 2" cube per ACM-4801 using the nominal Sludge Wash Solution Cement Recipe developed in WNS TP 025, and WNS TP 026, Any remaining concentrates shall be stored in sealed containers for possible future analyses, 2,5 The 2 inch cement cube shall be cured to simulate the temperature profile documented from SIP 91 1. Following a 28-day curing period, the cube shall-be destructively tested for compre u tve strength per ACM.4701, 3.0 ' SAFETY f 3.1 Industrial hygiene practices shall be as described in the WNS Hygiene and Safety Manual, WDP 011, 3.2 Radiological work shall be performed in accordance with the WDP

-Radiological Controls Manual, WDP Ol').

3.3 Work in the Analytical 6 Process Chemistry Lab shall be performed in accordance with existing A&PC methods, supplemented by the test

~ procedure WNS-TP 034, 4.0: EQUIPMENT CONFICURATION 4,1 All lab equipment shall be set up as directed in test procedure WNS TP 034 and _the cognizant A&PC scientist.

5.0 SAMPLING FREQUENCY 5.1 Sampling frequency and volume shall-be specified in test procedure WNS TP 034 6' . 0 PERSONNEL QUALIFICATION 6,1 Testing shall be performed by qualified A&PC Technicians using ACMs per test procedure WNS-TP 034 MIB0897:3RM 2

WNS-TRQ 034 Rev. 0 6.2 c rveillance activity shall be performed by qualified Quality Assurance personnel.

7.0 REFERENCES

7.1 " Technical Position on Vaste Form," Revision 1. dated January 1991.

7.2 "Prelirninary Flow sheet -Sludge Wash with Existing 8D-2 Heel,"

EK:91:0047, J. L. Mahoney, dated 03/07/91.

7.3 " Qualification Testing of the 100 lb Order of TIE-96 Zeolite Pre pared by UOP." WNS TP 033 M

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C) West Valley o u-d" = s tr o3c Demonstration Project Revision Date 08/13/91 Engineering Release # 2163 TEST PROCEDURE o

CONFIRMATORY CUBE PREPARED BY lL.vb1 L. E. Michnik Cognizant Etiginced

( APPROVED BY  % I ((' ~/

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Cognizant Systern Design Manager D. C. Meesa s.

APPROVED BY '

GbC P. J. Valenti Cognizant Facilities Manager p -

APPROVED BY %J.I . -:wo /J% 'S' E-' '

D, L. Shugars Quality Assurant5 Manager APPROVED BY d McNsr?Jnw OMI D. J. Harvard RadlajienandSafetyManager West Valley Nuclear Services Co., Inc.

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D West Valley, NY 14171-0191 WV-1816, Rev.1

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TEST PROCEDURE FOR CONFIRMATORY CUBE VVNS TP 034 REV, 0 1,0 Scopo 1.1 This preendure is for the preparation of a 2x2x2 inch cement cube nade from actual sludge wash liquid generated from under VVNS-TP 032 and decontaminated under VVNS TP 033. The scope of this work in compliance with section 4,6 of VVNS TPL 7011 " Test Plan for the Waste Form Qualification Program for Cement Solidification of Sludge UAsh Liquid". The cube will also provide information on the reaction of the nominal recipe for cement on actual sludge wash material and determine if any unforeseen constituents are having an f* adver.se effect on the cement product.

-\

1.2 The liquid from Sludge Wash Cycle #1 created from WVNS TP 032 and decontaminated under VVNS-TP-033 will be evaporated so that the total dissolved solids in the concentrated material will have a maximus'value of 33 weight percent and a minimum value of 29, 1.3. The compressive strength data generated from this cube will be compared to data generated under UVNS TP 026, twenty eight day curing period and VVNS TSR-029A. Gel time, bleed water and penetration resistance will also be compared to the results obtained from VVNS TSR 029A, 2.0 Definitions __and Abbreviations 2,1 Definitions j-- Cement-Dry Portland Type I cement in accordance with ASTM Standard

(,,) C-150-85, DLSO460:3RM 1-

I VVNS TP 034 Rev. 0

-Antifoam General Electric AF9020 emulsion of five percent dimethyl silicone in nanopure. This is used as a cement recipe enhancer to prevent air entrapment in the cement matrix during high speed-mixing.

Sodium Silicate is used as a recipe enhancer in the gelling o'f the cement waste form and prevention of excess bleed water. It is a water. based solution of sodium silicate with 3.10 to 3.43 silicon to soda ratio, 62 percent water (nominal) .nd 11.7 pounds per gallon.

Calcium Nitrate tetra hydrate la used as a recipe enhancer in the setting of the cement waste form Cube 2x2x2 inch plastic mold used to make laboratory specimens.

2.2 Abbroviations 4

ACM Analytical Chemistry Method ASTM-American Society fer Testing and Materials 4

3.0 -Responsibilitic_s, 3.1 Analytical and Process Chemistry will be responsible for-the preparation and testing of the' laboratory specimens in accordance to i the applicable steps of the appropriate Analytical Chemistry Methods (ACMs) and VVNS TP 034, 3.2 Quality Assurance will provide surveillat.ce to ensure that the.

-requirements of this . test procedure and WVNS-TRQ 034 are satisfied and verify the final concentrate product, witnessing of the cube i- being made 4.nd also the crushing of the cube, i

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] DLSO460: 3RM 2-l

- - . - . . - , , + , . - . . . , - . - , - - - . - . . , - . ~ . . - _ . . -

WVNS TP 034 Rev. O

{

3.3 Radiation 6 Safety monitors radiation and contamination levels in the laboratory to insure work is conducted in accordance with the Rad Con Manual VVDP-010 Rev 1.

l 3.4 IRTS will be responsible for issuins the test summary report,  ;

VVNS TSR 034, in accordance with EP 11 003.

4,0 Tools, Equipment, Components and References 4.1 Tools and Equipment

-Lightnin Lab mixer Model No. TS 1515 with high shear impoller or equivalent 2x2x2 inch plastic cube molds manufactured by American Cube Mold 100 milliliter (ml) plastic or glass graduated cylinder with one al divisions 500 ml polypropylen* .lastic bottles 250 ml borosilicate beaker Corning horplate or equivalent 10 ml glass volumetric flask 20 ml plastic scintillation vials magnetic stirring plate and magnetic stir bar stopwatch or timer accurate to one second top loading balance readable to +/ 0.01 gs (grams)

DLSO460:3RM -

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VVNS-TP 034 Rev. 0 1

Blue M Oven Model No. C 2630-Q or Despatch Environmental Chamber Model No. 16307 Cilson Penetrometer, Model No. CT 421-4.2 Reagents Portland Type I ceaent Calcium Nicrate tecra-hydrate, reagent grade Nanopure water or ASTM Type I water Sodium Silicate, technical grade *-

Antifoam General Electric AP9020*

  • Supplied by IRTS operations

~

4.3 References NRC Technical Position on Waste Form (Revision 1) January 1991 ACh-4701-" Destructive Test of 2 inch Cement Cubes" ACM-2401 " Density" Rev 3 ACM 2501 " Determination of Total Solids" Rev 2

" Removal of Plutonium from West Valley High Level Liquid Waste". .

Bray, Hara, Kazmierezak, dated January, 1991 ASTM C109 86 " Compressive Strength of Hydraulic Cement Mortars (Using 2in or 50mm Cube specimens)

DLSO460: 3RM ' l l

- . - - .- ~ - - . - . - . . - - _ . - - - . , -

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

WVNS TP 034 Rev. O WVNS-TP 026 " Procedure for_ Qualification of the Nominal Recipe for

Cement Solidification of Sludge Wash Liquids", Lette r s FH:91:0088, '

3 dated June 17, 1991, to J. A. Mahoney from L. E. Michnik j TE WVNS TRQ 026 01 " Revised Salt Concentration for the " Nominal Simulant Recipe based on 128.5 inch Heel" '

VVNS+TSR 029A " Test Summary Report for Confirmatory Cube" WVNS TRQ 034 " Production of Cement Product for Actual Sludge Wesh Liquid" 32" Heel Sludge Wash Confirmatory Cube. Letter a FH:91:0073, dated May 8, 1991, to J. C. Cwynar from L. E. Michnik '

5.0 Gene ra1 ' Info rma tion 5.1 This test will be used to evaluate the nominal cement formulation recipe (see Attachment C) using actual sludge wash and supernatant 1 from tank 8D-2 based upon a nominal 130 inch supernatant heel. It will confirm the accuracy of data -and observations generated by /

laboratory simulants and determine ff any unforeseen constituent are having an undesirable ef fect on the cement product.

6.0 Procedure F

6.1 Prerequisite u

L Oven or environmental chamber should be set at proper temperature as defined in sec 6.1.20 and monitored by a calibrated thermocouple or thermometer per PRD 8,0 Rev 1 i:

Balances shall be calibrated according to ACP 7.1-j -.

Safety procedures should be reviewed in ACP 7.2 DLSO460: 3RM L- . . _ ~ . . _ , _ , _ , . _ _ _ - - . - - _ . . - - . -. - -- - -- -

l WVNS TP 034 Rev. 0

/ 6.1.1 A sufficient amount of liquid from WVNS TP 033, Sludge Wash wl shall be used to generate at least 100 milliliters of 33 percent solid sludge wash liquid, This liquid shall be placed in a 250 m1 beaker and evaporated slowly, while stirring to reduce splattering. The liquid before concentration shall-be analyzed for total dissolved solids, density,-pH, gross alpha and gross beta. The liquid shall be reduced to approximately three quarters of its initial volume. At this point the total solids 1will be determined by ACM 2401. If the total solid content is between 29 and 33 percent, the evaporation will stop and the solution allowed to cool. If the solid content is lower than-29 percent, evaporation will continue and the liquid tested periodically by ACM-2401 until the specified range of the solids is achieved. At this point the total solid content will be

, confirmed by ACM 2$01, 6.1.2 If the liquid is reduced to the point were solids are falling O out of solution due to over evaporation, the evaporation should stop and nanopure water should be added in small increments and the solution should be allowed to stir., Water and stirring shall be used to redissolve the solids. A total solid determination should be made and an appropriate amount of water added to achieve the total solids specified. _If any type of unusual occurrences are observed during evaporation, 7

t?e cognizant scientist should be notified immediately, If

-solids form during evaporation and the percent solids are within the specified range, the concentration shall'be filtered and the solids analyzed for the test parameters listed below.

O DLSO460: 3RM , __ _ , - _ - _ _ _ . _ ~ -

WNS TP 034 Rev. O T/" N The resultant- concentrates shall be analyred for:

NO2 ' K PO4 '3 .Ti

.NO3 ' Na

_ S04 ^2 Ca B03 '3 TOC TIC Cr C1' F' Al U

-pH Total Dissolved Solids (TDS) density Total Suspended Solids.(TSS) alpha Pu Cs 137 Sr 90 Tc 99

-gross alpha gross beta 6.1.3 .After the appropriate solid content has been achieved approximately 96 mis of the concentrate, the actual amount will be calculated from the equation in section 6.1.22, shall be used to make the confirmatory cube as stated in section 6.1.4 thru 6.1,27 and the remaining will be used for th'e analysis in section 6.1.2.

6.1.4- Make a 5 percent antifoam solution. L'eigh 5,00 +/ 0. 05 gs of well mixed AF9020 in a 100 mi volumetric flask and dilute to the manufacturer's mark with .nanopure water. Mix well and transfer to a beaker with a magnetic stir bar and stir continuously on a stir plate.

6.1.5 Prepare 200 gs 5.7 percent calcium nitrate tetra-hydrate / cement mixture by adding 11.4 gs calcium nitrate

' tetra hyd: ate to 188.6 gs Portland Type I cement in a 500 m1 beaker and mix the dry ingredients thoroughly.

6.1.6 Use a 500 ml plastic bottle-to make a mixing vessel by evenly

. cutting off the tip and producing an open ended cylinder.

O.

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DLSO460:3RM WNS+TP 034 Rev.=0 6.1.7 Similarly cut the top off a 250 mi plastic bottle. This

\

container will be used to add the cement / calcium nitrate mixture to the liquid waste.

6.1.8 Tare the cutoff 250 m1 bottis and add 140.5 +/ lg l cement / calcium nitrate. Record weight on the appropriate Form W-2301.

6.1.9 Place the cut 500 m1 mixing vessel prepar d in step 6.1.0 under impeller and set mixer speed to 1000 rpm.

6.1.10 Measuro 96 +/ 2 ml of 29-33 Vt concentrate from step 6.2.3 using a 100 ml graduated cylinder and record on Form W 2301.

6. L il Pour .96 mis of concentrate -into the 500 mi mixing vessel prepared in 10.2. Rinse the graduated cylinder after each use with nanopure water.

6.1.12 To the concentrate, use an Eppendorff ptpet and transfer 0.3

+/ 0.006 ml of the St antifoam mixture from step 6.3.1.

Record on Form W-2301.

6.1.13 Tare a 10 ml disposable plastic cup and add to it approximately 11.00 +/ 0.5 gs sodium silicate. The exact amount transferred will be found by reweighing the cup after the material is poured into the sludge wash. Record the weight on Form W-2301 6.1.14 Support the' mixer on a lab stand so that the impeller blade is one-quarter to one-eighth inch:from the bottom of the 500 ml plastic bottle. Use a wide mouth clamp to support the c

500 ml plastic bottle without crushing the side. See a timer for 8 minutes.

O DLSO460:3RM 8-

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WVNS TP 034 Rev. 0 6.1.15 'Begin the mixing at 1000 rpm and start the timer, Add the dry cement / calcium nitrate mixture to the waste within the first 30 seconds. After 45 seconds, slowly add the sodium

, silicate within an additional 45 seconds. Continue to mix for a total mix time of 8 minutes, 6.1.16 After the transfer of the sodium silicate reweigh the cup and calculate the amount added by difference, record on Form WV-2301. ' While miring, mark a cube mold with a permanent marker with the date, sample type, numecical identification sequence-number and then weigh the cube mold, record the weight on Form WV 2301.

6.1.17 After completion of the eight mina.e mix, stop the mixer and transfer the contents to a plastic 2" cube mold, Fill to the top and transfer the remaininb to a 20 mi plastic scintillation vial and seal. After weighing the cube tare the scale to zero and reweiSh the cube with the cement in

() it. Record.the weight on Form WV 2301.

density of the material by the formula below, Determine the wet Wet Density- Total weight of cube (g) -Tare weight of cube mold (g) 131 mis 131 mis - Volume of 2x2x2 inch cube mold Record on Form WV 2301. After completing this step place the cube in a zip lock plastic bag.

6.1.18 Clean the impeller with water immediately after pouring.

6.1.19 Visually check for gelation of the cement in the 20 m1 scintillation vial. Check every five minutes and do not disturb between these time inte rvals . Record the time it take the cement to gel. Celation is a subjective

() determination, however gelled cement is indicated when the DLSO460: 3RM - 9-

__ m.___.___ -

7.._________.___...___..

I VVNS Tp.034 {

Rev. O j i

f 20 mi scia.=4 ttion vial can be tipped slowly to a 90 degree v position, parallel to the horizon. The cement should not deform. flow, and will retain a line of form perpendicu ar to c the horizon. Bleedwater may be present, do not interpret as f a sign of uncompleted gelation.

l

! (.1.20 Transfer the cube to a drying oven with the comperature set at 79+/. 2 celsius within two hour of preparation and allow to cure in the oven for 90 +/ 8 hours9.259259e-5 days <br />0.00222 hours <br />1.322751e-5 weeks <br />3.044e-6 months <br /> in a plastic zip lock bag large enough to hold the cube and not deform the exposed cube face. Record on Form VV.2301 time, date the cube was made and_the time it was placed in the oven and also the start temperature.

6.1.21 After 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br />, determine in mis the bleedwater in the scintillation vial and also determine the pH by indicator

paper; record it on Form VV.2301. ,

6.1.12 Calculats the water to cement ratio by weight using formula below.

IA11B)(1 01  ;

(D)(0.943)

A-Volume in mis of-sample B-18ensity value in gs/mi of sample C-Total Solids value in decimal form D-Veight of _ cement used in Bs i

, i 6.1.23 -After 90 hours0.00104 days <br />0.025 hours <br />1.488095e-4 weeks <br />3.4245e-5 months <br /> +/ 8 hour9.259259e-5 days <br />0.00222 hours <br />1.322751e-5 weeks <br />3.044e-6 months <br /> take the cube out of the oven and a do the penetration resistance analysis (see section 6.3.22)

, and reeard the time, date and temperature of the cube removal ,

and also the penetration resistance on Form VV.2301.

6.1.24 Caut!on: Do not remove the cube from the mold for the #

)- penetration test and only when ready to crush.

1 DLSO460: 3RM 10 -

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W!NS.TI'.034 Fev, O i I l

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6.1.25 being the concrete penettometer model CT.421; perforts the  !

penetration resistance test by removing the cube from the bag  !

i and placing the penetrometer plungee- in the center of the

, expos 64 side of the cube. Make sure the red indicator ring has been set back to the zero mark on che penetrometer. With  ;

a steady vertical force push the penetrometer against the l cube unti? the red inoientor ring is all the way down the f scale whe1 the penetrotoeter shaf t will not penetrare the cement any further.

6.1.26 On the handle of the penettometer. read the value on the red indicator ring and record the number on Form VV.2301, if the j red indicator rint, is all the way to the end of the scale, a j value of >700 psi shall be recorded. I i

i 6.1.27 When the sample cube is cured for a total of 28 days +/ 8 i hours. Determine the dry density by the formula oelow Dry Density -Total air.ht of dry cube ( r. ) .

care _wei t h Lof cube mold (pl 131 mis 131 mis - Volume of 2x2x2 inch cube mold l

l l Record on form VV 2301 ,

i 6.1.28 Crush the cube according cu ACM;4701 by sanding the cube in j l acs~~ dance with ASTM C+109 section 10.6.2 i

, 7.0 Data Acquisition I 7.1 Two inch cube preparation and Compressive strer h information will be recorded-on Form VV 2301, Rev 1.

7.2 Total solid content will be recorded on Form VV.2306 DLSO460: 3RM 11 -  !

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t WNS .TP.034 Rev. 0 7,3 Density will be recorded on form W.2401 8.0 Attachments i

8.1 Attachment A Results from 32" Heel Studge Wash Confirmatory Cube a Dh91:0073 1 8.2 Attachment B Nominal Recipe for Sludge Wash rement l 8,3 Attachment C Nominal Cement Recipe Compressive Strength Data ,

  1. nl:91:0088 O

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- DL50460:3RM- 12 +

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I WNS TP 034 Rev. O Attachment A Table 1 Analytical Result for 32" confirmatory Cube 7 Day Curing Period A. Sludge Wash Liquid Analysis Result Density 1.23 g/ml

%TDS 29,7

h. Cube Analysis Result Cel Time 35,5 mina Slurry Density 1.76 g/mi Bleedwater None Penetration > 700 psi Compressive Strength 694 psi '

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WNS TP.034 Rev. O To: John Cwynar 1,e t te re : Fil:91:0018 Frote: Frank liara and 1.arry E. Michnik

Subject:

Cement Recipe for Sluige Vash Simulant with 33 inch l Supernatant heel Date: J anuary 24, 1990 The recipe for the laboratory scale specimen cube (2x2x2) contain the following amounts of ingredients:

1.) 140.0 grams of Portland Type I Cement with

$ 7% Calcium Nitrate 4 ilydrate 2.) 11.0 grarns Soditus Silicate 3.) 0.3 mis of 5.0 grams to 100 mis antifoam (AF 9020) 4.) 96 mis of 33.0 weight percent Sludge wash simulant This recipe will produce a product with a w ter/ cement ratio of 0.61 William F. MacKellar Manager A6PCs-P i

LO l

DLSO460
3RM B1 ,

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WVNS TP 034 Rev. O Attachment C Two Inch Cubes Laboratory ID. Drum No. Compressive Strength (psi)

Twenty eight Days 9100894 10 81433 1177 9100894 17 81298 1119 9100894 31 81439 996 Three inch by six inch cylinders Laboratory ID. Drum No, compressive Strength (psi)

Twenty.might Days 9100893 10 81433 1358 9100893 17- 81298 1500 9100893 29 81439 1464 Three Inch by Six Inch Core Not applicable 81632 1120

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Doc . Nu::.be r WN$TP.O.044

""""""='"

O west valley "

Revision Date 11/11/91 Demonstrat=on i Proj*ect Emo meerime sena.e , m o 4

TEST REQUEST VASTE FORM QUALIFICA~l ION VCPJ. FOR SLUDGE VASH LIQUIDS A

FREPARED BY . . . - - NOS , J . L. Mahoney Co5nizant Engineer APPROVED BY -

D. C. Meess Cogni: ant System Design Mapager APPROVED BY

/'

44 f'M&Ve<&>fu.L.Shugars //ffht QualitypssuranceManager APPROVED BY NN D. J. Harvard RaMion and Safety Manager APPROVED BY d< MA/ D. H, Carland Waste Management Operafi'ons Manager AFFROVED BY k- b' 7W Pr6 cess Contrdi Engineering J. C. Cvynar APFROVED BY O, - D. J. Fauth A&PC Laboratories Manager West Valley Nuclear Services Co.,Inc.

P.O. Box 191 DLSo m .R3 West Valley, NY 14171-0191 WV 1816, Rev.1

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l WNS TRQ 044

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Rev. 0 RECORD OF RIVISION i i l PROCEDt'RE [

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If there are changes to the procedure, the revision number increases by one, These  !

1 changes are indicated in the left margin of the body by an arrow.(>) at the beginning  ;

J the para 6raph that contains a change. ,

I f l Exattpig:

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> - The arrow in the margin indicates a change,-- _

Revision On

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WNS TRQ 044 {

Rev, 0 [

RECORD OF REVISION (CONTINUATION SilEET)

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VVNS TRQ 044 Rev. O V ASTE FOPJi QUALIFICATION V0PX FOR SLUDGE VASil L1 QUIDS 1.0 INTRODUCTl23 1.1 This work is required to demonstrate the acceptability of two waste form recipes using simulated sludge wash liquids. Characteristics that will be tested are required by 10 CFR 61 Code of Federal Regulations, Title 10

" Licensing Requirements for Land Disposal of Radioactive Vaste," and the paper by the Technical Branch of the Low Level Vaste Management and Decommissioning Division of the US Nuclear Regulatory Conaission " Technical Position on Vaste Form" Reviaion 1, dated January,1991.

1.2 This test request defines work that is part of the overall cement waste form qualification work identified in VVNS TPL 70 011.

l 1.3 Vork wilt be performed with a simulant represerting the actual waste liquid. The rimulant is shown in Table 1.

1.4 Vork will be performed uslag 3" diameter x 6" long cylinders cast from full scale drums processed in the Cement Solidification System (CSS) undet work order. Cores of the same physical size as the cylinders will be taken from drums processed in the CSS and tested as part of this test program.

1.5 Test f rocedure WVSS TP 046 providing specific instructions for testing in ancordance with this test requsst shall be issued by Analytical and Process Ch6mistry (A&PC) per EP 11 003.

1.6 An initial test summary transmitting the data ecords for this test series shall be issued by the A6PC Cognizant Test Scientist and the Cognizant Quality Engineer within 1; working days of the completion of the test in accordance with EP 11 003.

1. 7 Te s t Sunaary Report , VVNS TSR-044 documenting the results of this testing shall be issued by the Cognizant Engineer per EP-11 003.

2.0 OBJECTIVES The following sections apply to two cement waste recipes, one made with sludge wash simulant solution at 20 wt% total dissolved solids (TDS) and one with the simulant solution at 14 wt: TDS. The work shall be applied to each recipe.

The first two objectives below shall be completed by CSS operations, and will not be covered by Test Procedure TP 044 Coring of CSS product drums (section 2.5) will be perforraed by Vaste Management Operations and also will not be covered by Test Pr;tedure TP-044 but will be performed in accordance with work order and SOP 70 **.

2.1 Per work order, an instrumented drum shall be filled with the simulated cement waste in CSS. The instrumented drum will provide a curve of the temperature profile of the c ement waste form over several days. This temperature profile will define the curing time and temperature to be used

~

on cylinders that will be produced below.

DLS O47 9. R3 1

i VVNS TRQ 044 Rev. 0 2.2 Per work order, at least two drums shall be filled with the simulated cement vaste in CSS. During the IIlling process, at least 30 3" diameter x I 6" long cylindrical molds shall be filled with the simulated cement waste.

The molds shall be placed in a poly bag, and the bag labeled with the drum number, time and dato. Following standard procedures, the bagged samples shall be released to A&PC for transfer to the controlled temperature ,

chamber.

2.3 The cylinders shall be kept in the controlled temperature chamber at the temperature and for the duration indicated by the data from section 2.1 above. Following the high temperature curing, the cylinders shall be cured ,

er room temperature for durations as indicated below. l 2.4 A curve of compressive strength versus cure time shall be established for [

cylinders. A minimum cure time that produces a compressive strength within

  • 75 percent of the maximum shall be determined. Strength measurements shall be taken at cure times of 28, 35, and 42 days per ASTM Standard C 39 and -

Q1P 27.

2.5 After curing for a time dete* mined in section 2.4 above, but in no case less than 28 days, the three drums poured in CSS (instrumented drum t included) shall be core drilled to obtain 3" diameter X 6" long cylindrical samples. A total of 26 samples shall be obtained. Ten cores shall be [

taken from the drums within 3 days of each other for use in section 2.6 below. Cores shall be obtained from various locations in the drums (top, middle, bottom locations) to demonstrate the homogenous nature of the waste form. Locations shall be recorded on SOP 70 44, Attachment D.

2.6 A total of ten compressive strength measurements on core samples from the cement waste form drums shall be completed per ASTM Standard C 39 and QIP

27. A mean compressive strength in excess of 500 psi after 28 days is required.

2.7 Immersion testing of the cylinders shall be performed in the two.leachants; e specified in the US NRC Branch Technical Position paper. After curing for a minimum of 28 days (or as indicated by section 244 above) six cylinders shall be immersed in each of the leachants for periods of 15, 30. 45, 60, 75 and 90 de,'s . . Following immersion,. the specimens shall be visually inspected and photographed per item G. Appendix A of the US NRC Branch Technical Position paper, and subjected to compressive strength testing per .

ASTM Standard C 39 and Q1P 27. Leachant samples shall be analyzed to determine composition changes. A curve of compression strength vernus time and leachant composition versus time shall be constructed. '

2.8 Immersion testing of the cores shall-be performed in the two leachants specified-in the US NRC Branch Technical Position paper. Eight cylinders shall be immersed in each of the leachants for periods of: 90 days 3 cores, 120 days - 1 core, 150 days - I core. 180 days 3 cores.

Following immersion, the cores shall be visually inspected and photographed per_ item G. Appendix A of the US NRC Branch Technical position paper, and subjected to compressive strength testing per ASTM Standard C-39 and Q1P DLSO479.R3 2

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VVNS TRQ 044 Rev. 0

27. Leachant samples shall be analyzed to determine composition changes.

If the mean post immersion compressive strength is more than 75% of the pre immersion mean compressive strength (section 2.6 above) and greater than 500 psi, the immersion testing can be stopped. If the mean has fallen below 75% of the pre immersion strength, the test shall be continued all the way to 180 days, 1

.2.9 Thermal cycling stability of the vaste form using cylinders shall be tested j 4

in accordance with ASTM Standard B 553, and the US NRC Branch Technical '

1 Position paper, 3.0 SAFETY  ;

3.1 Industrial hygiene practices will be as described in the WVNS Hygiene &

Safety Manual, 'JVDP 011. '

3.2 Radiological work will be performed in accordance with the VVDP j Radiological Controls Manual WVDP 010.

3.3 Work in the Analytical & Process Chemistry lab will be performed in

. accordance with existing A&PC methods (ACM's) .

- 4.0 STANDARD PRACTICES [

4.1 All lab equipment shall be set up in accordance vir' l'VNS TP 044 and as directed by 'the cognizant A&PC Scientist or qualliiru A&PC !achnician.

4.2 Core-boring equipment shall be set up in accordance with 50P 70 44. I 4,3 Calibration of compressive strength testing equipment shall be in accordance with the applicable steps of- ASTM Method C 39,- C 109, and WVNS-QIP 027.

4.4 All test exceptions (form VV 1854, Rev. 1) generated durin6 this test shall be forwarded to the test requester and Quality Assurance for review and l approval.

5.0 - S AMPLING JREQUENCY f 5,1 A-total of 30 cylinders-3" diameter x 6" hi6 h will be required.

5.2 A total of 26 cores 3" diameter x 6" high will be required.

6.0 _ PERSONNEL OUALIFICATION i

6.1 Laboratory . testing shall be performed:by qualified Analytical & Process

( Chemistry Technicians in accordance with VVNS TP 044 and Analytical -

Chemistry Methods (ACM's) under the cognizance of an A&PC Scientist.

DLSO479.R3 3 l .

4 i i WNS *TTQ 0M i Rev. O l .

4 1- 6,2 Compressive strength testing e ' cylinders shall be performed by Quality l l Services personnel trained in th+ requirements of QIP 27, l

i. 1 I 6,3 Surveillance activity shall be perfortted by Quality Assurance. l b i I ' 7,0' REFERENCES l i

7.1 " Licensing Requirements for Land Disposal of Radioactive Was',e " 10 CFR f 61, code of Federal Regulations. Title 10  ;

. 7,2 " Technical Position on Vaste Form " Revision 1, Technical Branch of the Low j

Level Vaste Management and Decommiasioning Division cf the US Fuelear l Regulatory Comtnission, dated January, 1991,

! 8.0 EXPERIMENTAL AND DEVELOPMENTAL TEST ACCEP,D NCE SHEEI l 8,1 The acceptance criteria is provided as Attachment A.  !

l

+

l i

Le P

i

}

E ,

t 1

2 h

l f

l O ,!

DLSO479,R3- 4 ,

t Lw, -e--..--. ww w r. eewwew..---ww--*- u e.w mee r w - +wy e e __ .. m-g aev _ . . - _ . _ _ g-vam -mm-w w e,ven-grow w w e rerw ee-y eWVf'eur

W!iS TRQ 044 Rev. O Table 1 Siinulant Recipe for itLV Sludge Wash Solution laji NANO, 28.6

!JaNO, 27.2 N a,00, 17.0 K!!O, 1.8 Na,CO, 4.8 EfS'd NaC1 131 Na,llp0, 95

!1a,Mo0, . 211,0 22.6 Na,B,0. 1011,0 12.2 Citric acid (anhydrous) 16.5 0xalic Acid (4stthydrous) 12.9 Tartaric Acid (anhydrous) 18.0 N o,C r,0, . 211,0 159 Na0ll

  • 1.B S

'The modiwn hydroxide shall be added in approxirnate 0.2 lb

  • increinents to arrive at a pli of 12.0 12.4.

NOTE: At 20 vtt TDS recipe makes approximately 40 gallons At 14 wt1 TDS recipe reakes approxirnately 60 r,allons i

DLSO479.R3 $

W!?S .TRQ . 0t.4 Rev. O ATTACILME!iT A EX P E R I MlilALEthE'lLLOl3El{I,_ILEI_ACff1'INKIJ11CEI TRQ TP Page _1_ nf _1_

PREPARED BY:

COC TRQ E!iCR: / _ Ql'ALITY E!!Gl!4EER: / ,

DATE DATE CRITERIA FOR ACCEPTMICE OF DATA RESULTS/ COMME!iTS

1) All Tent Exceptions issued ht.ve been completed and EC!i issue .
2) All requested analyses have been completed.
3) All A&pC analytical forms, photographs, sample logs, sample preparations, raw data, calculations and laboratory s.otebook entries shall be copied and forwarded to test requester.
4) A6PC has issued a brief test summary and record transfer to MRC within 15 working days of the completion of test.

aCCEPTF.D BY:

COG TRQ EliGR; / QUALITY E!!CR: /

DATE DATE W 1891, Rev. O DLSO479. R3 A1

i WNS *TRQ.044 l Rev, 0- -l sTTACibtENT B proposed Disposition of Cyliners & Cores cylinders Quantity Test 28- Day Compressive Strength 4 35 . Day _ compressive Strength 3 42 Day Compressive Strength -3 15 - Day innersion + demin water - 1 30 Day intnersion domin water 1 J

45 Day immersion + domin water 1 i 60 Day immersion demin water 1 l

75 Day immersion. demin water 1 1$ Day 1.nersion . sea water

. 1  ;

30 Day immersicn sea water- 1 45- Day immersion . sea water .

1 60 Day immersion sea water 1  ;

75 -Day immersion sea water 1 90 Day immersion _a demin water 1 90 --Day Amersion sea water 1 Thermal Cycle 4 i' Spare 4

_ Total 30 t

-Cores  :

Test _

Quantity 42 _ Day Compressive Strength 5 43 Day' Compressive' Strength 5 90 Day. immersion demin veter 3_

90_ Day-imersion . sea water 3 120 Day immersion demin water _ 1 1

120 Day immersion sea water 1

.150- Day immersion demin-. water 1 150 - Day immersion sea water 1 180 Day immetsion demin water 3 180 Day immersion sea water 3- ,

Total 26  :

9 e

DLSO4 79.R3 - 11 - 1

, . - . - , + . - - - . . + . - . . , . . ~ . - . . = . - - . .a.,._,,- _ _ .-.-,- - ,- . - -

Doc . Itur.be r '."a45 TP 044 west Valley uviuon 0 O Demonstration Pro;ect "v t "aa "" > ""$'"

Engineering Release #2228 TEST PROCEDURE PROCEDURE POR VASTE IVPM QUALIFICATION V0PJt POR SLUDGE VAstl LIQUIDS PREPARED BY ado L. E. Michnik Cognizant SEEU n st APPROVED BY__ f 2 D. J . Pauth y,tficaVLaboratories Kanager APPROVED BY C. Meess Cognizutt System Design Kanager 1

j APPROVED BY p' D ')) ,,:_-l44/ 'l/

+ 4*

D. L. Shugars

.( Quality Assurance Kanager APPROVED BY # +. sb.J. Harvard kadiatiofand Safety % nager APPP.0VED BY_ 2 a* D. H. Carland Vasco Management Operations Manager APPROVED BY 4'/MM M J . C. Cvynar Process Controf Engineering West Valley Nuclear SerMees Co., Inc.

12.0. Box 191 SAJ0119.R3 West Valley, NY 141714191 WW1818, Rev.1 ,

1 m

l WNS TP.044 Rev. O O

PFJD OF REVELQ3 112CIEAE If there are ch nges to the procedure, the revision number increases by one. These changes are indicated in the lef t margin of the body by an arrow (>) at the beginning of the paragraph that contains a change.

Exarrole :

> The arrow in the margin indicates a change.

Revision On Rev. No. Description cf Changes Page(s) Dated 0 original Issue All 11/18/91 O

W.1807, Rev. 1 SAJ0119. R3 i

l WNS TP 044 Rev. 0

(

RECOP.D OF REVISION (CONTINUATION SHEET)

Revision on Rev No. Description of changes Page(s) Dated O

[ W-1807 Rev. 1 SM0119.R3 11

VVNS TT.044 Rev. O PROCEDURE FOR VASTL FORM QUALIFICATION VORY

( FOR SLUDCF. WASH LIQUIDS 1.0 dCOPE

. 1.1 This work is required to demonstrate the stability of three vaste form recipes. Characteristics which will be tested are required by 10 CFR 61, Code of Federal Regulations Title 10, ' Licensing Requirements for Land Disposal of Radioactive Vaste,' and the US NP.C Branch Technical Position on Vaste Form, revision 1, dated January,1991. This work is part of VVNS TPL 7012, cement Vasta Fora Qualification of Sludge Vash Liquids.'

1.2 Vork will be performed with two simulants representing the actual waste liquid. The simulants will be processed at 141 Total . 4 solved Solids (TDS) and 201 TDS. Also a batch of Heat Cement will be run (01 TDS).

1.3 The full scale waste form shall be fabricated in the CSS using simulated waste in accordance with V0f 913540, 1.4 Work will be performed using cylinders (3' diameter x 6' long) cast from full scale drums processed in the Cement Solidification System (CSS).

1.5 A curve of compressive strength versus cure time will be established for cylinders and will be measured at 2 8, 35, and 4 2 day s . Cylinder corspressive strength tests shall be conducted in accordance with Q1P 027 O

i and ASTM C 39, 1,6 After curing reaches 75% of maximum compressive strength and a minimum of 28 days curing per section 1.5 above, thermal cycling stability of the waste form will be tested on full-scale cylinders in accordance with ASTM Standard B 553.

1.7 Af ter curing reaches 75% of maximua compressive strength and a minimum of 28 days curing per section 1.5 above, the following tests shall be pe rformed:

1.7.1 A baselina compressive strength test shall be performed on at least (10) cylinders and (10) cores and its mean results should be above 500 peig. The 3' K 6' cores shall be obtained from the full-scale waste form by coring in accordance with S0P 70 44. SOP 70 44 also ensures that mixing is homogeneous by coring at dif ferent locations of the drum to remet requirements of the NRC Branch Technical Position on Vaste Form, Appendix A, section II 1.

1.7.2 At least three (3) cores shall be immersed for a period of 90 days, followed by compressive strength testing. The mean post immersion compressive strength should not be less than 75 percent of the mean baseline compressive strength (psragraph s 1.7.1 above) or below 500 psig.

J S AJ 0119.R3 1

WN S .TP . 044 Rev 0 ,

1.7.3 If the testing in section 1.7.2 above f ails, immersion testing O shall be carried out to 120 ,150. , and 180. days of immersion followed by coepressive strength testing. The results of this testing should have a mean compressive strength result of 500

, psig or greater and prove that the vaste form will stay abov. '

this limit over time.

1.8 Irradiation testing per the NRC Branch Technical Position on Vaste Form, appendix A, section 110, does not need to be performed because there is no ion exchange resins or substantial organic material in the vaste i stream. Also the cement waste form will not be subjected to greater than 10E+9 Rads.

1.9 Biodegradation per 10 CFR 61.56(b)(1) and the NRC Branch Technical Position on Vaste form, appendix A, section II E, is not required due to the extremely trace amounts of organic -material in the vaste atteam, and past performance of the supernatant wasta streu, 1.10 Free standing liquids-shall be observed and documented each time a cylinder is detnolded, or a core is removed from a drum to meet requitetsents of the Branch Technical Position on Vaste Form, Appendix A, section H. Any free liquid shall be checked for pH by pH paper or meter.

2.0 DEFINITIONS AND ABBR,l/IATIONS 2.1 Definitions Cement - Dry Portland Type I cement in accordance with ASTM Standard C-150 85 Cement Blend A homogenous mixture of Portland Type I cement with 5.7 1.7 percent technical grade flake or granular form calcium nitrate with NO ammonium nitrate, i Cast . A cube or cylinder specimen produced in the mixer, then scooped into the sold Core - A 3* diameter X 6' long right cylinder obtained from a full scale drum af ter a minimum of 28 days of curing.

Cylinder - A cast specimen 3* diameter x 6* long produced in the full scale mixer.

Domineralized Vater - unter having a conductivicy less than 5 microsho/cm at 25_ degrees Celsius and a total organic carbon content tuss than 3

parts /million.

O SAJ0119.R3 2

-,-s."e==w'v-,

WNS.TP 044 Rev. O Nest Cement Standard ASTM C.150 Portland Type I cement mixed with O

water only (no waste) .

Synthetic Seawater . a combination of various inor6anic compounds as follows:

Sodium Chloride 23.497 grams Magnostwa Chloride 4.981 graras Sodius Sulfate 3.917 grams Calcium chloride 1.102 grams Potassium Chloride 0.664 grams Sodium Carbonate 0.192 grams Potassium Bromide 0.096 grams Demitwralized Vater 965.551 al This fonsulation in from the International Organization for Standardization IOS 1691 1982(E).

2.2 Abbreviations ACM Analytical Chemistry Method A&PC . Analytical & Process Chemistry ACP . Analytical Chemistry Procedure ANSI /ANS - American Nuclear Standard Institute /American Nuclear Socie ty American Society for Testing and Materials O ASTM CSS Cement Solidification System DAS . ilata Acquisition System IVP - Industrial Work Pernit IRTS Integrated Radwante Treataant System 1,VTS Liquid Vaste Treatment System PCE - Process Control Engineering QA . Quality .cssurance QIP . Quality inspection Precedure R&S Radiation and Safety SOP Standard Operating Procedure TDS Total Dissolved Solids 3.0 RESP t1S1311.1* IES 3.1 (ntey sated Radvsste Treatment System (IRTS) Operations personnel operate r cement solidification System (CSS) in accordance with V0f 913540 a4d WNS.PCP.001 to produce the full scale drums of solidified simulant iasta required for this test procedure. Process Control En6ineering shall provide technical support when necessary.

3.2 IRTS Enr*m ming shall provida technical direction, and compares the test de 4 ec '.he Test Request requirements.

O SM0119.R3 3 l

l

WNS TP.044 Rev. 0 3.3 Quality Services provides surveillance to ensure that She requirements  !

of this test procedure are satisfied, and verifies that portions of the test (where independent verification is coquired) were performed.

Quality Services also performs compressive strength testing of cylinders and cores in accordance with QIP.027.

3.4 Analytical & Process Chemistry performs the followingi c) collection of all data b) perform thermal cycling test  !

c) perform immersion test l 3.5 Radiation and Safety (R/S) monitors rediation and contamination levels, Radiological work will be performed in accordance with WHS Radiological control Manual, WDP.010. '

3.6 Vaste Operations will be responsible for core boring the drums in accordance with SOP-70 44, 3.7 Industrial Hygiene practices are describad in the WNS Hygiene and Safety Manual. WDP.011.

4.0 TOOLS, EQUIPMENT, COMPONENTS, AND REFERENCES 4.1 Tools and Equipment 3" diameter x 6' long cylinder molds per ASTM Standard C 470 poly bags ,

solid sample (s) transport container (s) 5.ga11on high density polyethylene pails with tids 20 Licers ASTM Type ! Vater or Domineralized Water 20 Liters Synthetic Seawater recording thermometer readable to i 0.5 degree Celsius 4.2 Ccuponents 4.2.1 CSS equipment fully operational 4.2.2 Despatch Series 16000 Environmental Chamber fully operational 4.2.3 Forney Model IT 40.DR Compressive Strength Testing Unit fully operational 4.2.4 Core boring and compressive strength test equipment located in the Upper Warm Aisle /Vastr Reduction and Package Area.

SAJ0119.R3 4

_ , ~ _ _ _ _ _ - _ . _ . _. . . _ . . . _ . . . _. _ - _ ._ _ _ - _ _ - -_. . _ _

WNS.TP 044 +

Rev. 0

- 4.3 References 4.3.1 CSS (Systers 70) Standard Operating Prncedures 5

4.3.2 EP.11 001, Test control

, t 4.3.3 F.P.11 003, Development Test Control 4.3.4 WNS.TPl. 70 012, Cement Vaste form Qualification Sludge Vash 1.1 quids 4.3.5 WNS.TRQ.044, Vaste Fora Qualification Vort. for 31udge Wash 1.1 quids 4.3.6 WDP.010. WNS Radiation Controls Mouual 4.3.7 WDP.011 WHS Industrial Hygiene & Safety Manual 4.3.8 US NRC Branch Technical Posittor, on Vaste Form. Revision 1 dated January, 1991 4.3.6 ASTM C.39 Standard Test Methr d for compressive Strength of Cylindrical concrete Specimens r 4.3.10 ASTM B.$$3 Standard Test Fathod for Thermal Cycling of Electroplated Plastics 4.3.11 ANSI /ANS 16.1 American N4.tional Standard Measurement of the 1Aachability of Solidified tov.imvel Radioactive Vaates by a ,

short.tcru Procedure i 4.3.12 Wof 913540, making drums; making cylinders 4.3.13 WOf9103520, ' Additional CSS Testing (Instrumented Drums) 4.3.14 Wof 9103525,

  • Development of 201 and 141 Total Dissolved Solids Recipe for Sludge Wash Cament" 4.3.15 U0f 9103488, ' Development of Neat CSS Recipes for Sludg* Vash Cement' 4.3.16 QIP 027 Quality inapection Procedure for Comprassive Strength >

Testing of Coment Cylinders ,

4.3,17 ACP 7.2, Administrative Control Procedure for 1.aboratory- .

Safety 4.3.18 ACM 6200. Analytical Chemistry Method for operation of

Despatch Environmental Chamber i

O SAJ0119.13 5

WNS TP.044 Rev. 0 4.3.19 ACM 6400 Analytical Chemistry Method for 1snersion Testing of 0 '

Cessent Specimens 4.3.20 CED T1L St. 88 34 88, "Sulfste Resistance of Morters Hade Using Portisnd Cement and Blends of Portland Cement and Portolan or Slag.

5.0 CENERAL. INFORMATION ,

5.1 Results of this testing vill tw compared to the results obtained under  !

W FTRQ.025. WNS.TRQ.026. VVHS.TRQ.028, and WNS.TRQ+030.

5.2 All compression test results shall be reported as a mean compressive strength and standard deviation.

5,3 Quality Assurance shall be notified prior to the start of this work.

5.4 OPERATORS SHOULD PERTORM IllEQUENT CHECKS ON SYSTEMS THAT ARE TURNED ON ,

OR SHUT DOWN TO ASSURE THAT DtE SYST!X DOES VHAT IS EXPECTED,1.E. ,

VATER FLOVS, PRESSURE RISES, ETC. IF THE REQUIPS.D ACTION DtAT IS SUPPOSED-To HAPPEN DOES NOT HAPPEN, (1) STOP DO NOT PERFORM THE NEXT STEP, (2) SECURE THE SYSTEM IN A SAFE MODE

-(3) NOTIFY THE COGNIZANT A&PC SCIENTIST OR COGN12 ANT ENCINEER IMMEDIATELY.

5.5 The following is the scheduled disposition of each sample and totals.

Per Racing Iqtgl Gylindars v 28. day compression 3 9

  1. 35. day compression 3 9 v' 42. day compression 3 9 2

v' Addition 7 for baseline 7 21 e Thermal Cyc1*ng 4 12 v 15. day Immersion (domin) 1 3 V 15. day Immersion (see) 1 3 V 30 day Immersion (demin) 1 3 V 30 day Immersion (sea) 1 3 V 45. day Immersion (demin) 1 3 V 45. day Immersion (sea) 1 3 V 60. day lasersion(domin) 1 3 ,

Y 6 0. day Ismeetston(sea) 1 3

75. day Immersion (domin) 1 3
75. day Immersion (sea) 1 3
90. day laneersion(domin) 1 3
90. day Immersion (sea) 1 3 SM0119.R3 - 6

\

l l

WNS.TP.044 s Rev. O r

CRIAA O t' Baseline 90 day Immersion (unin) 10 3

30 9

90. day Immersion (sea) 3 9 120. day Immersion (deotn) 1 3 120. day Immersion (sea) 1 3 150 day Isanersion(domin) 1 3 150 day Immersion (sea) 1 3 180. day Immersion (domin) 3 9 180 day Immersion (wa) 3 9 ,

26 73 5.6 All samples shall be labelled as 'TP.44.XK1' wtsere XXX is a three digit number. The 141 Recipe three digit number shall start with 100, the 201 Recipe shall start with 200 and the 01 Recipe shall start with 300.

5.7 All samples will be kept in sealed containers and/or poly bags during curing and storage, as discussed in the Branch Technical Position, appendix A.III.C. This is intended to simulate the environment in a sealed drum.

5.8 A controlled laboratory notebook shall be used to document the history of the testing and any observation and data associated to the experbsent. References should be included to surveillance Reports, attachments to SOPS. etc. in the notebook.

All recipes are being developed ini.ependently, there is no test where 5.9 data should be analyzed across recipes, unless it is a comparison between the recipes. .

6.0 EMERCENCY RESPONSE 6.1 Tor er:argencies in the A&PC Lab, responses will be as direc:ed by ACP 7.2 and WDP 010.

6.2 For emergencies elsewhere in the plant, responses will be as directed by WDP.010.

7.0 COMPRESSIVE STRENCTH VERSUS TIME 7.1 Cylinders produced per Wof 913540 shall be placed in an environmental ,

chamber and cured for a cure time and camperature established by Wod9103520. After the established cure cias, the cylinders shall be -

ramped down to room tamperature by turning off the environmental chamber and allowing cylinders and cubes to cure at reen temperature. The rossining room camp curins for the cylinders shall be accomplished in A&IC 14bs, 1

O 1 7 SAJ0119.R3 l

~_ ~ - . ,_m---.-~,,~..m - ,-----.-s._ - ,_ _._ _ _ _. - - - .w, . . . , . . - , - - , , . . - ,,,m,,-,,,r ,,.e.

WNS TP 044 Rev. O s 7.2 To ertablish the compression straagth curve, three cylinders per recipe shall be destructively tested at the 28. day. 35. day, and 42. day pointa, As soon as the data indic .tes that the cement has reached 7$1 of maximum strength, the baseline compression testing shall start. These cylinders shall be tested per QIP.027.

8.0 BASELINE COMPRESFIVE STRENGTH TESTING 8.1 Three drums per recipe shall be cored in accordance with SOP 70 44 A total of tventy samples vill be obtained per recipe, locations of coring should be random from dnus to drum and from core to core within a drum. Locations shall be recorded on 50P 70 44 attachment D. Ten cores shall in obtained for each instrumented drums created under Vol 9103520 used for baseline compressive strength and 8 cores each from the drums produced under V0f 913540 shall be und for Immersion Testing. When section 7.2 has been satisfied, baseline compressive testing shall be conducted.

8.2 Mean baseline compression strength testing for cores, and cylinders per recipe should (11 be above 500 psig.

9.0 THERMAL CYCLING 9.1 The heating / cooling c,. amber shall conforts to the description given in AS'IM Standard B.553. The thermal cycling test shall be perforned in accordance with ACM.6200. The chamber will be equipped with a calibrated thernometer, and continuous temperature recorder.

9.2 Because ASTM Standard B 553 addresses thermal cycling of electroplated plastics, some modifications to the test method are required. Testing vill be performed on ' bare * (i.e.. not in a container) cylinders.

9.3 At or after baseline wapression testing, the unbagged cylinders shall be placed in the test chamber, and a series of thermal cycles shall be carried out in accordance with sections 5.4.1 through 5.4.4 of ASTM Standard 8 553, with the additional provision that the specimens should be allowed to come to thermal equilibrium at the high (>60 degrees C) and low (<-40 degress C) temperature limits.

9.4 Thermal equilibrium shall be confirund by chart recorder measurements of the centerline temperature (via thermocouple) of at least one (1) specimen per test group.

9.5 If thermal equilibrium of the centerline temperature is not at the temperature limits, the limits set on the environmental chamber shall be adjusted accordingly.

9.6 Three (3) cylinders per recipe shall be subjected to the thermal cycling tests.

O SAJ0119.R3 8

WHS .TP.044 Rev. O 10.7 Af ter 90 days oi imersion, 3 cores per leechant per recipe shall be O compression tested per Q1P.027. Results are required to h* 8 tester then 75% of the baseline compressive stren6th and be above 500 psig to qualify the recipe at the 90 day point. If 75% is not achieved, the following steps of section 10.0 are required.

10.8 After 120 days of inersion,1 core per loschant per recipe shall be compression tested per QIP.027.

10.9 Af ter 150 days of imersion,1 core per teachant per recipe shall be compression tested per QIP 027, 10.10 Af ter 180 days of imersion, 3 core per teachant per recipe shall be compression tested per Q1P 027.

10.11 At the 180 day point, the data shall be evaluated to assure that the waste form is not further weakened and that it is above 500 psig per the NRC Branch Technical Position requirements.

11.0 REPORTING RESULTS 11.1 All data sheets associated with this Test Procedure shall be forwarded to the Cognizant Scientist for collection and eventual inclusion into the 15 day Summary Report required by EP 11 003.

11.2 All data shall be reported with units, tolerance, and standard deviation where applicable.

O SAJ 0119. R3 14 l

Doc, Number WNS TRO.045 O v' ast valley

. Revision Number 0 L amonstration Project Fevision Date 12/06/91 Engiu,aring Release #2236 TEST REQUEST MULTIVARIANT TESTING OF LEMENT WASTE FORMS USING SIMULATED SLUDGE VASH SOLUTIONS PREPARED BY __

.g C'? /9 e J. L. Mahoney Co izanc Enginesq APPROVED BY / a er ( Ivo D. C. Meess a Cost (izant'Sydtem Dr. sign Manager

,. t  ;.

/

i --

v id I, / ',I' : ' "I ~ ' "

  • APPROVED BY D. L. Shugars Quality {nsuranceManager APPROVED BY D S,(( M f G,' k !H D. J. Harvard P a; .,,t f e i Safety Manager APPROVED BY b b-W J. C. Cwynar Pr sas Cont $ol Engineering Mana5er APPROVED BY _ !.

- D. J. Fauch Lab' oratories Manager f/

v West Valley Nuclear Services Co., Inc.

P.O. Box 191 O

d DLSO484.R3 West Ve!!ey, NY 14171-0191 W W1818,Rev.1

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

l l

WVNS TRQ.045 Rev. O RECORD OF REVISION PROCEDURE If there are changes to the procedure, the revision number increases by one. These changes are indicated in the Icft margin of the body by an arrow (>) at the beginning of the paragraph that contains a change.

Examole:

> The atrow in the margin indicases a change.

Revision On Rev. No. Description of Changes Page(s) Dated 0 Original Issue All 12/06/91 O

o Q- W 1807. Rev. 1 DLSO484.R3 i

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

WNS TRQ 045 O Rev, 0 RECORD OF REVISION (CONT 1NUATION SHEET)

Revision i*n Rev. No. Description of Changes Page(s'- Dated 4

O W-1807, Rev, 1 DLS0484.R3 11

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

1 i

)

VVNS TRQ 045 )

Rev. O <

MULTIVARIANT TESTING OF CEMENT VASTE FORMS USIN0 SIMULATED SLUDCE WASH SOLUTIONS

1.0 INTRODUCTION

1.1 This lab scale work will research the effect of sulfate, water-to cement ratio, total dissolved solidt (TDS), nitrate-to nitrite ratio, and cement additive calcium nitrate on the immersion degradation of cement waste forms. Work will be perfermed with laboratory chemicals to simulate typical sludge wash solutions.

1.2 This test request defines work that is part of the overall cement waste form qualification work identified in WVNS-TPL 7012.

1.3 All work contained in this document shall be completed by the WVNS Analytical & Process Chemistry (A6PC) Lab.

1.4 Test Procedure WVNS TP 045, providing instructions for meeting the requests specified in this Test Request shall be issued by the A6PC Cognizant Scientist per EP 11 003.

1.5 An initial test summary transmitting all records of this test series shall be issued by the Cognizant A6PC Test Scient.lst and Cognizant Quality Engineer within 15 working days of the completion of the test in accordance with EP ll.003.

1.6 Test Summary Report, WVNS-TSR 045, documenting the results of this testing shall be is. sued by the Cognizant Test Engineer per EP 11003, 2.0 OBJECTIVES 2.1 Prepare eleven 2" x 2" x 2" cubes for each of the 46 individual cement waste form recipes depicted in Table 1. The variables to be investigated are:

L variable I sulfate variable 2 nitrate: nitrite ratio variable 3 water: cement ratio l variable 4 total dissolved solids (TDS) variable 5 Ca(NO3 )2 4H 2O l The symbols "-1", "0", and "+1" represent settings for the variables i

below the nominal, at the nominal, and above the nominal respectively.

The exact range of the variations are:

l O

DLSO484.R3 1 I

i 1_ _ _ _ -.

WVNS TRQ 045 Rev. 0

-1 0 +1 low nominal high sulfate 9,9 14.1 18.3% of TDS nitrate: nitrite 1.14 1.21 1,28 ratio water: cement 0.50 0.61 0.72 ratio TDS 16.0 20.0 24.0 wtX Ca(NO3 ): -

4H2O 3.0 6.0 9.0 wtX of cement The levels of waste form components shall be set to values provided in Table 2 unless adjusted to produce one of the variations for the 46 cubes.

2.2 Gel time, bleedwater, pH of bleedwater, and penetration resistance shall be measured for each cube.

2.3 Using a temperature controlled chamber, the cubes shall be cured at 88 i 2'c for 70 -0/+8 hours.

2.4 The cubes shall be allowed to complete the curing process at room temperature for a total cure time of approximately 28 days.

l 2.5 Compressive strength of three of the cubes shall be measured as a l

/ baseline reference.

l \.

2.6 Immersion containers shall be set up with demineralized water for 90 day, l 120-day, 150-day, and 180-day immersions. After curing, three cubes L shall be placed into the 90-day container, one in the 120 day, one in the ISO day, and three in the 180 day containers, 2.7 Every 30' days, the cubes shall be inspected and photographed per item III. G. Appendix A of the US NRC Branch Technical position paper.

L 2.8 Following imLLrsion, the cubes shall be subjected to compressive strength l testing.

j 3.0 SQL*G 3.1 Industrial hygiene practices shall be as described in the VVNS Hygieno

! and Safety Manual, WVDP 011.

'3.2 Work in the Analytical & Process Chemistry. Lab shall be performed in accordance with existing A&PC methods, supplemented by test procedure

! WVHS-TP 045.

1 4.0 EOUIPMENT CONFIGURATION i

es l

l

( )- 4.1 All lab equipment shall be set up as directed in test procedure WVNS-TP-045 and per the A&PC Cognizant Scientist.

DLS0464.R3 2

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1 WNS TRQ 045 Rev. 0 5.0 $AMPLING FREOUENCY 5.1 Sampling frequency shall be identified in procedure WNS TP 045, 6.0 PERSONNEL OUALIFICATION 6.1 Testing shall be performed by qualified A&PC Technicians using ACMs per test procedure WNS TP 045.

6.2 Surveillance activity shall be performed by qualified Quality Assurance personnel.

7.0 REFERENCES

7.1 " Cement Waste Form Qualification of Sludge Wash Liquids," WNS-TPL 7012 7.2 " Technical Position on Waste Form," Revision 1 Technical Branch of the Low Level Vasta Management and Decommissioning Division of the US Nuclear Regulatory Commission, dated January,1991.

8.0 EXPERIMENTAL AND DEVELOPMENT TEST ACCEPTANCE SHEET 8.1 The acceptance criteria is provided as Attachment A.

O DLSO484.R3 3

O O ~O

'l WNS-TRQ-045 Rev. O Table 1 WO-SET, F1VE-VARIABII BOX-BEHNKEN TEST DESIGN Note: Before preparing the cubes, the order of manufacture in each set shall be randomized, but the sets shall not be mixed.

SET 1 SET 2 Variable Nunber Variable Number Trial 1 2 3 4 -5 Trial 1 2 3- 4 5 1 +1 +1 0 0 0 24 0 +1 +1 0 0 2 +1 -1 0 0 0 25 0 +1 -1 0 0 3 -1 +1 0 0 0 26 0 -1 +1 0 0 4 -1 -1 0 0 0 27 0 -1 -1 0 0 5 0 0 +1 +1 0 28 +1 0 0 +1 0 6 0 0 +1 -1 0 29 +1 0 0 -1 0 7 0 0 -1 +1 0 30 -1 0 0 41 0 8 0 0 -1 -1 0 31 -1 0 0 -1. 0 9 0 +1 0 0 +1 32 0 +1 0 0 +1 10 0 +1 0 0 -1 33 0 +1 0 0 -1 11 0 -1 0 0 +1 34 0 -1 0 0 +1 12 0 -1 0 0 -1 35 0 -1 0 0 -1 13 +1 0 0 0 0 36 +1 0 0 0 +1 14 +1 0 0 0 0 37 +1 0 0 0 -1 15 -1 0 0 0 0 38 -1 0 0 0 +1 16 -1 0 0 0 0 39 -1 0 0 0 -1 17 0 0 0 0 0 40 0 +1 0 +1 0 18 0 0 0 0 0 41 0 +1 0 -1 0 19 0 0 0 0 0 42 0 -1 0 +1 0 20 0 0 0 0 0 43 0 -1 0 -1 0 21 0 0 0 0 0 44 0 0 0 0 0 22 'O O O O O 45 0 0 0 0 0 23 0 0 0 0 0 46 0 0 0 0 0 l

i DLSO484.R3 4

VVNS TRQ 045 Rev. O Table 2 Nominal Cement Waste Form Specification Simulated HLW Sludge Wash Solution:

wt1 of TDS NANO, 35.1 NANO, 33.4 Na SO, 20.9 1 KNO, 2.2 Na.CO, 5.9 Nacl 0.35 Na,HPO, 0.26 Na, Moo. 2H,0 0.061 Na,B,0,,10H,0 0.033 Citric acid (anhydrous) 0.045 g Oxalic Acid (anhydrous) 0.035 l Tartarie Acid (anhydrous) 0.049 Na.C r,0,,2 H,0 0.43 pH 12 3

. Cement:

ASTM Portland Type. I Antifoam - 0.11 al per kg cement l Sodium Silicate - 0.075 gm of 38 wt1 solution per sm' cement Ca(NO3 ):

4H2C 6 wt% of cement l'

l l

l l O ,

- DLSO484. R3 5

. - - - - -. -_ . J

WVNS-TRQ.045 Rev. O

_ ATTACitMENT A EXPERIMENTAL AND_ DEVELOPMENT TEST ACCEPTANCE SHEET TRQ TP Page 1 of

' PREPARED BY:

COG TRQ ENGR: / QUALITY ENGINEER: /

DATE DATE CRITERIA FOR ACCEPTANCE OF DATA RESULTS/ COMMENTS

1) All Test Exceptions issued have been completed and ECN issued.
2) All requested analyses have been completed.
3) All A&PC analytical forms, s_j) photographs, sample logs, sample preparations,-raw data,

. calculations and laboratory notebook entries shall be copied and forwarded to test requeeter.

4) .A&PC has issued a brief test summary and ' record transfer en MRC withing 15 working days of the completion of test.

ACCEPTED BY; COG TRQ. ENGR: / QUALITY ENCR:. /

DATE DATE l.

l WV-1891, Rev. O l

i DLSO484.R3 A-1 o

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