ML20083F360

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Rev 1 to Test Procedure WVNS-TP-028 a, Procedure for Development of Process Control Parameters for Cement Solidification of Sludge Wash Liquids
ML20083F360
Person / Time
Site: West Valley Demonstration Project
Issue date: 07/16/1991
From:
WEST VALLEY NUCLEAR SERVICES CO., INC.
To:
Shared Package
ML20079E011 List:
References
REF-PROJ-M-32 WVNS-TP-028-A, WVNS-TP-28-A, NUDOCS 9110040221
Download: ML20083F360 (24)


Text

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1 Doc. Number WVNS-TP-028 A West Valley Re ,1,1,,R m e, ,

Demonstration Project Revision Date Om6w Engineering Telease #2076 =

Per ECN i 429 TES1 PROCEDURE PROCEDURE FOR DEVELOPMENT OF PROCESS CONTROL P ARAMETERS FOR CEMENT SOLIDIFICATION OF SLUDGE WASH LIQUIDS PREPARED BY b O L. E. Michnik Cogniza er APPROVED BY e- D. C . Me es s Cognizant System Design Manager APPROVED BY , er/ I'I U/ r-/m .:.- -

'D. L. Shugars Quality , Assurance Manager APPROVED BY 6M /7ft MJ'/daf D. J. Harward Radiation and Saf ety ManaEer APPROVED BY 67%vh- M [CC, J. C. Cwynar Process ControlvEngtheering West Valley Nuclear Services Co., Inc.

P.O. Box 191 KMJ0020:3RM West Valley, NY 141714191 WV.1816, Rev.1 911994o271 c11001 Eq{ PROJ p

"VHS-TP 02SA

.. Rev. 1 RECORD OF REVISION- i PROCEDURE If there are changes to the procedure, the revision number increases by one.

These changes are indicated in the left margin of the body by an arrow (>) at the beginning of the paragraph that contains a change.

Example:

> The strow in the margin indicates a change.

Revision On Rev No. Description of Changes Page(s) Dated 0 Original Issue as WNS-TP-028 All 05/01/91 1 Per ECN #4429 All 07/16/91 (Issued as WNS TP 028A)

W-1807, Rev. 1 - 1 MIB0900:3RM

M.fM3iII WN S - TP . 02 8 A

, Rev. 1

. RSCORD OF L4 VISION (CONTINUATION SHEET) l Rev. No. Description of Changes Revision)on Page(s Dated W 1807, Rev. 1 11 MIB0900:3RM

unvwen m.o.wat m e _.m-VVNS TP 028A Rev. 1 TABLE OF CONTENTS Section Description Page 1.0 SC0PE........................................ ... ....., . 1 2.0 DEFINITIONS AND ABBREVIATIONS .. , ,.,,.,, .... ..,,,,, 2 3.0 QUALITY ASSURANCE........, .... ........ .... ., ,,, , . 3 4,0 TOOLS , EQUIPMENT, COMPONENTS , AND REFERENCES , , . ..... 4 5.0 GENERAL INFORMATION......................... ..... ... ... 6 6.0 PROCEDURE...................... ...... ......., ,,,,. .... 7 7.0 DATA ACQUISITION ..........,, ......, ...... .. , .., , 14 TABLE 1: BASE SOLUTION.............. ............., ,,, . ... . 15 .

TABLE 2: TWENTY-EIGHT-RUN PLACKETT BUR,".AN SCREENING DESIGN... . 16 TABLE 3: VARIABLE CUBE PARAMETERS. ..,,,...,,,. ,,, . . .,, 17 ATTACHMENT A - MULT1-VARIANT CUBE WORKSHEET.,, ,...., . .. .. .. A-1 MIP,0900:3RM iii

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WVNS TP.028A Rev. 1 VVNS TP 028A PROCEDURE FOR DEVELOPMENT OF PROCESS CONTROL PARAMETERS FOR CEMENT SOLIDIFICATION OF SLUDGE WASH LIQUICS j 1

l Rev. 1 4

i l.0 SCOPE

, l 1.1 This Test Procedure is being written in partial fulfillment of WVNS-TRQ-028 and VVNJ TPL 70-11. The completion of VVNS-TRQ 028 1

will be fulfilled under UVNS-TP 0288. The objective of this overall l testing criteria is to establish windows for full scale production I i

i of the sludge wash cement waste form within which an acceptable j product can be made. Thia is based upon the requirements stated in appendix A, section VI, of the NRC Technical Position on Waste Form, .

Rev. 1, dated January 1991. These windows include variances in the

major chemical components of the simulated sludge wash liquid, the cement recipe enhancers as well as physical parameters. Laboratory specimens, 2-inch square cubes, will be used in evaluate these windows, 1.2 The work will include the formation of a series of 28 solutions j representing variations in the liquid waste chemical components and cement recipe enhancer which will produce 28 individual 2-inch by 2-inch cubes.

1 These 28 cubes will be used to screen the degree of interactions

l. between 13 individual components and will be based upon the cube's compressive strength via a Plackett Burman Screening Design test.

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1.4 The 13 individual components will include variation in the chemical

[ constituents of sulfate, nitrate: nitrite ratio, organics, aluminum, pH, phosphate , and borate . Also to be varied will be the physical parameters of total solids, mixtime, water: cement ratio, and the cement recipe enhancers of calcium, antifoam, and sodium silicate.

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. L'VNS TP . 02 8 A Rev. 1 1.5 After an appropriate curing period, per section 5.1, the laboratory specimens will be subjected to compressive strength testing as per section 6.3. This testing will provide data on the influence of variations of the chemical composition of the sludge wash liquid and the recipe enhancers on the compressive strength of the cement waste form.

1.6 The gel time, free liquid volume, pH of the free liquid and penetration resistance will be measured and recorded for each cube _.

as part of ACM 4801, 2.0 DEFINITIONS AND ABBREVIATIONS 2.1 Definitions 2.1.1 Cement-Dry Portland Type I cement in accordance with ASTM Standard C-150-85.

2.1.2 Antifoam General Electric AF9020 emulsion of 5 percent dimethlysilicone in nanopure water. This is used as a cement recipe enhancer to prevent air entrapment in the cement matrix durin8 high speed mixing.

2.1.3 Sodium silicate - is used as a recipe enhancer in the gelling of the cement waste form ar.d preve.ntion of excess bleed water.

2.1.4 Calcium nitrate tetra-hydrate - is used as a recipe enhancer in the setting of the cement vaste form.

2.1.5 Cube --2x2x2 inch mold used to make laboratory specimens.

MIB0900:3RM 2

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, WVNS-TP 028A Rav. 1 2.2 Abbreviations, ACM Analytical Chemistry Method ASTM American Society for Testing and Materials NRC Nucicar Regulatory Commission 3.0 QUALITY ASSURANCE l l

I 3.1 Analytical and Process Chemistry (A&PC) will be responsible for the

]

preparation and testing of the laboratory specimens in accordance with this test procedure and the applicable steps in the appropriate i Analytical Chemistry Methods (ACM). A6PC shall verbally notify cognizant Quality Engineer and Quality Service Manager 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> prior to commencement of work. ,

3.2 Quality Assurance Responsibilities 3.2.1 Quality Assurance shall verify all chemical used in testing l

having the correct chemical formula on container as is  !

1 required for this test procedure.

1 I

3.2.2- Quality Assurance shall provide independent verification of I 1

all chemical processing, measurin5, mixing, and other {

processes required to produce the first five cubes, Quality )

1

  • Assurance may perform the above activities on remaining l 1

23 cubes. l l

i 3.3 All WVNS personnel are responsible for documenting nonconformances j on cube recipes and/or cube preparation. Nonconformances shall be documented using Nonconformance Report Form, WV-9202. Any cube rejected shall be reported and rejected cube documented with data from other cubes.

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MIB0900:3RM 3 l

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. VVNS-TP 028A Rev. 1 3.4 A&PC shall maintain material control by labeling all containers used in tasting. A bond laboratory notebook sill be used to record solution contents and testing observation along with attachment A.

4.0 TOOLS, EQUIPMENT. COMPONENTS, AND REFERENCES 4.1 Tools and Equipment

- Ligntnin Lab Mixer, Model No. TS 1515 with high shear impeller or equivalent

- 2x2x2-inch plastic American Cube Molds 100 milliliter (mL) plastic or glass graduated cylinder with 1 mL divisions

- 500 mL polypropylene plastic bottles -

- Corning hot plate or equivalent 10 mL glass volumetric flask

- 20 mL plastic scintillation vials magnetic stirring plate and magnetic stir bar

- stopwatch or timer accurate to 1 second top loading balance readable to + 0.01 grams (g)

Blue M Oven Model No. C 2630-Q or Despatch Environmental Chamber Model No. 16301 Gilson Penetrometer Model No. CT 421 fine sand or emery paper 4.2 Reagents Portland Type I cement Calcium Nitrate tetra-hydrate, reagent grade Aluminum Nitrate, reagent grade Citric Acid Monohydrate, reagent grade MIB0900:3RM 4

VVNS-TP-028A Rov. 1

- Oxalic Acid Dihydrate, reagent grade

- d-Tartaric Acid, reagent grade

- Sodium Silicate, 38 weight percent in a water base, technical grade

- Antifoam General Electric AF9020*

Aluminum Nitrate . 9 H2 0, reagent grade

- Sodium Phosphate Mono hydrate, reagent grade

- Sodium Tetraborate Decahydrate, reagent grade

- Sodium Nitrate, reagent grade Sodium Nitrate, reagent grade

- Sodium Carbonate, reagent grade -

Potassium Nitrate, reagent grade

- Sodium Hydroxide, reagent grade

- Sodium Chromate tetra-hydrate, reagent grade

- Sodium Chloride, reagent grade

- Sodium Molybdate Dihydrate, reagent grade

- nanopure or ASTM Type I water

  • supplied by IRTS operations 4,3 References

- NRC Technical Position on Waste Form (Revision 1), January 1991

- ASTM C 150-85 " Specifications for Portland Cement"

- ASTM C 109-86 " Compressive Strength of Hy/re lic Cement and Mortars (Using 2-in or 50 mm Cube Specimetu F

- WVNS-TPL-70 ll " Test Plan of the Waste Form Oualification Program for Cement Solidification of Studge Wash Lir,oid" WVNS-TRQ-028 " Test Request for Development of the Process Control Parameters for Cement Solidification of Sludge Wash Liquids" MIB0900:3RM S

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i < -~

k'VNS TP-028A Rev. 1 f

ACM 4701 " Destructive Test of 2 inch Cement Cubes" ACM 4801 " Cement Test Cube Preparation Method"

- ACM 2401 " Density"-

ACM 2502 " Total Solids" (Microwave)

ACM 2601 apH" (Electrode) 5.0 C_ENERAL INFORMATION g

4 l-5.1 The compressive strength tests on cement waste form specimens will be used to evaluate the process control parameters and is considered j- an acceptable criteria for the overall performance of the product as j' indicated in appendix A, section VI of the NRC Technical Position on Waste Form, Rev.1, January 1991. Although cement products -

nominally achieve 75 percent of their strength in approximately l 28 days, it-has been decided by convention that a curing period of 4=

7 days for. laboratory specimens will allow the specimens to gather j.-

1 sufficient strength in order to be evaluated. This curing process for process control parameter cement specimens requires they be 4

placed -in an oven or environmental chamber and sealed individually or in a group in plastic-bags for.90 1 8 hours9.259259e-5 days <br />0.00222 hours <br />1.322751e-5 weeks <br />3.044e-6 months <br />.at 79 1 2 C and then

. a penetrometer test is performed on each specimen to see if.the cement-has: set and must be-greatar than 700 psi. During the remaining time period, for-a total of'7 days 1 8 hours9.259259e-5 days <br />0.00222 hours <br />1.322751e-5 weeks <br />3.044e-6 months <br />,-the specimens will be cure a t 20 15 C. At this-point the specimen will-be. testing for compressive strength by the applicable steps of ACM-4701.

The results from this testing will provide a-basis for the effects of variances which could be experienced in the full-scale process.

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  • ,a. - ~ , . - - -
  • YNS

Rev. 1 i

6.0 PROCEDURE Oven or environmental chamber should be set at proper temperature as defined in section 5.1. Temperature sensing and recording instrumentation shall be calibrated according to ACP ?.1, Rev. 2.

Balances shall be calibrated according to ACP 7.1.

- Safety procedures should be reviewed in ACP 7.2.

6.1 Prepare 4 liter of a base solution from the recipe presented in table 1. This will be a base solution for the preparation of four 1 11ter stock solutions.

6.2 The first stock solution will contain high sulfate and high nitrate: nitrite ratio. Add 208.8 g sodium sulfate, 420.2 g sodium nitrate, and 163.1 g sodium nitrite to 1000 mL of a bs solution.

The amoun, of sodium sulfate, sodium nitrate, and sodium nitrite will be added to the stock solution slowly; one component at a time while mixing on a stir plate. The individual component shall be allowed to go into solution before the next component is added and low heating may be applied to accelerate the dissolution process.

After this stock is made it will be used to produce cubes 2, 7, 8, 9, 19, 23, and 26 as presented in table 2. The additional component variations for each cube will be added on an individual basis. The variation amounts are presented in table 3. and the variable combination sequence for each cube is presented in table 2.

6.3 The addition of the chemical components of organics, aluminum, phosphate, and boron will be added to each cube solution based upon 100 mL being generated. These chemicals will be added one at a time while mixing on a stir plate, and each will be allowed to go into solution before the next one is added. At this point, the pH of MIB0900:3RM 7

UVNS TP 028A Rev. 1 each cube solution will be measured and adjusted according to  !

ACM 2601 with 10N sodium hydroxide and the amount recorde4 on attachment A. The total solid content for each solution will be measured according to ACM 2502. At this point, adjustments to the total solid content can be made if necessary by the addition of demineralized water to the solution or evaporation of water from the solution by heating. The final density measurement will be performed according to ACM 2401, the total solids measurement according to ACM 2502 and recorded on attachment A.

4 4

, 6.4 once the cube solution has been generated; it should be labeled with

, the cube number. All the cube solutions in each stock set will be prepared and then those solutions will be made into cement cubes.

The water to cement ratio will be calculated based on the equation -

presented in section 6.26, The proper amount of simulant will be added to the appropriate amount of cement blend, sodium silicate, and antifoam based upon that cube's variable combination presented in table.2 and the amounted presented in table 3. The cube will be made accordin5 to the procedure started with section 6.8 and the gel time, free volume liquid, pH of liquid, penetration resistance, and compressive strength will be recorded on WV-2301 from ACM 4801.

6.5 The second stock solution will contain low sulfate and low

. nitrate: nitrite ratio. Add 51.0 g sodium sulfate, 74.4 g sodium nitrate, and 163.1 g sodium nitrite to 1 liter of the base solution. Allow the chemicals to go into the solution as stated in section 6.2. This stock will be used to make cubes 4, 5, 6, 11, 13, 16, and 28.as presented in table 2, The additional component variations for each cube will be added on a individual basis. The variation amounts are presented in table 3 and the variable combination sequence for sach cube is presented in table 2. The solutions will be made according the sections 6.2 through 6.3 and 1

the simulate waste cement prepared according to section 6.4 MIB0900:3RM 8

?

  • k'VNS-TP 028A

, Rav. 1 6.6 The third stock solution will contain low sulfate and high nitrate: nitrite ratio. Add 51.0 g sod ~.um sulfate, 420.2 g sodium nitrate, and 163.1 g sodium nitrite to 1 liter of the base solution. Allow the chemicals to go into solution as stated in section 6.2.2. This stock will be used to make cubes 3, 10, 15, 18, 20, 24, and 27 as presented in table 2. The additional component variations for each cube will be added on an individual basis. The variation amounts are presented in table 3 and the variable combination sequence for each cube is presented in table 2. The solutions will be made according to sections 6.2 through 6.3 and

-simulate waste cement prepared according to section 6.4 6.7 The fourth stock solution will contain high sulfate and low nitrate: nitrite ratio. Add 203.8 g sodium sulfate, 74.4 g sodium ,

nitrate, and 163.1 g sodium nitrite to 1 iter of the base -

solution. Allow the chemicair to go into solution as stated in section 6.2.2. This stock will be used to make cubes 1. 12, 14, 17, 21, 22, and 25 as presented in table 2. The additional component variations for each cube will be added-on an individual basis. The variation amounts are presented in table 3 and the variable coubination sequence for each cube is presented in table 2. The solutions will be made according to sections 6.2 through 6.3 and simulant vaste cement prepared according to section 6.4, 6.8 Make a 5 percent antifoam solution. Wei6 ht 5.00 + 0.05 g of well mixed AF9020 in a 100 mL 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.

6.9 Prepare 2000 g 2.85 percent calcium nitrate tetra-hydrate / cement mixture by added in 57.0 g calcium nitrate tetra hydrate to 1943 g Portland Type I cement in a 5000 mL beaker and mix the dry MIB0900:3RM 9

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WVNS TP 028A Rev. 1 ingredient thorou5hly.

i Also prepara 2000 g 11.4 percent calcium l l

nitrate tetra hydrate / cement mixture by adding 228 g calcium nitrate tetra-hydrate to 1772 g Portland Tyre I cement in a 5000 mL beaker and mix the dry ingredient thoroughly.

I 6.10 Use a 500 mL plastic bottle to make a mixing vessel by evenly cutting off the tip and producing an open ended cylinder. '

6.11 Similarly cut the top off a 250 mL plastic bottle. This container will be used to add the ceaent/ calcium nitrate mixture to the liquid waste, 6.12 Tare the cutoff 250 mL bottle and add the appropriate amount  ;

cement / calcium nitrate blend based upon the cube sequence -

variation. Record weight on the appropriate form WV-2301 and attachment A. )

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6.13 Place the cut empty 500 mL mixing vessel prepared in step 6.3.2 under' impeller and set mixer speed to 1000 rpm.

6.14- Calculate the amount of simulant necessary to produce the water to cement ratio desired based on the density and total solids information in section 6.3 and the calculation in sect. ion 6.26.

Dispense the amount by the use of a graduated-cylinder.

E i

6.15 Pour the appropriate amount of simulant into the 500 mL mixing i

vessel. Rinse the graduated cylinder'after each use with nanopure l

water.

6.16 To the simulant, use an Eppendorff pipet and transfer 0.09 + 0.006 mL of the 5 percent antifoam mixture from step 6.3.1

, for low antifoam variation and 0.6 + 0.003 mL from step 6.3.1 for high antifoam variation work. Record on form WV 2301 and attachment-A.

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WVNS TP 028A Rev. 1

  • 6.17 Tare a 10 mL disposable plastic cup and add to it approximately 5.5 + 0.5 g sodium silicate for low sodium silicate variation and 22.0 + 0.5 g sodium silicate for high sodium silicate variation.

The exact amount transferred will be found to reweighing the cup after the material is poured into the sludge wash.- Record the.

weight on form WV 2301 and attachment A.

6.18 Support the mixer on a Imb stand solthat the impeller blade is 1/4 to 1/8 inch from the bottom of the 500 nL plastic bottle. Use a -

vide-mouth clamp to support the 500 mL plastic bottle without crushing the side. Set a timer for 4 minutes if doing low mixtime variation and 16 minutes for high mixtime variation. Record on '

attachmunt A. .

6.19 'Begin the mixing at 1000 rpm and start the timer. Add the dry cement / calcium nitrate mixture to the waste appropriate for your cube preparation presented in table 2 within the first 30 seconds, After 45 seconds, slowly add the sodium silicate within an additional 45 seconds. Continue to mix for the appropriate time.

6.20 After the transfer of the sodium silicate, reweigh the cup and calculate the amount'added by difference, record on form WV 2301 and attachment A, While mixing, mark a cube mold with a permanent

-marker with the date, sample type, numerical. identification sequence i number, and then weigh the cube mold, record the weight on form WV-2301.

-6.21 After completion of the mix, stop the mixer and transfer the

-contents to a plastic 2 inch cube mold. Fill to the top and tr nsfer the remaining to a 20 mL plastic scintillation vial and seal. After weighing the cube,. tare the ccale to zero and reweigh the cube with the cement in it. Record the weight on i

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WVNS-TP u28A

, Rev. 1 form VV 2301. Determine the wet density of the material by the formula below.

Vet Density - Total weight of cube (g) tare weight (R) 131 mL Record on form WV 2301. After completing this step, place the cube in a zip-lock plastic bag.

6.22 Clean the impeller with water immediately after pouring.

6.23 Visually check for gelation of the cement in the 20 mL scintillation vial. Check every 5 minutes and do not disturb between these time intervals. Record the time it takes the cement to gel. Gelation is a subjective determination, however gelled cement is indicated when the 20 mL scintillation vial can be tipped slowly to a 90 degree position, parallel to the horizon. The cement should not deform, flow, and will retain a line of form perpendicular to the horizon.

Bleedwater may be present; do not interpret as a sign of uncompleted gelation.

6.24 Transfer the cube to a drying oven with the temperature set at 79 1 2 celsius within 2 hours2.314815e-5 days <br />5.555556e-4 hours <br />3.306878e-6 weeks <br />7.61e-7 months <br /> of preparation and allow to cure in the oven for 90 1 8 hours9.259259e-5 days <br />0.00222 hours <br />1.322751e-5 weeks <br />3.044e-6 months <br />. Record on form WV-2301 time, date the cube was made and the time it was placed in the oven and also the start temperature.

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

record it on form WV-2301.

3 MIB0900:3RM 12

VVNS TP 028A j Rev. I l

l 6.26 Calculate the water to cement ratio by weight using formula below.

R - (A) (B) (1-C)

(D) (1 E)

R - Cement to water ratio A - Volume in milliliters of sample B - Density valus in grans/ milliliters of sample C - Total Solids value in decimal form D - Weight of cement used in grams E - Percent calcium nitrate in the cement blend in decimal form 6.27 After 90 hours0.00104 days <br />0.025 hours <br />1.488095e-4 weeks <br />3.4245e-5 months <br /> + 8 hours9.259259e-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 do the penetration resistance analysis (see section 6.3.22) and record the ,

time, date, and temperature of the cube removal and also the penetration resistance on form WV-2301.

6.28 CAUTION: DO NOT REMOVE THE CUBE IROM THE MOLD EVR THE PENETRATION TEST AND ONLY WHEN READY TO CRUSH.

6.29 Usin5 the concrete penetrometer model CT 421; perform the penetration resistance test by removing the cube from the bag and placing the penetrometer plunger in the center of the exposed side of the cube. Make sure the red indicator ring has been set back to the zero mark on the penetrometer. With a steady vertical force push the penetrometer against the cube until the red indicator ring is all the way down the scale when the penetrometer shaft will not penetrate the cement any further.

6.30 On the handle of the penetrometer, read the value on the red indicator ring and record the number on form WV-2301. If the red indicator ring is all the way to the end of the scale, a value of

>700 psi shall be recorded.

MIB0900:3RM 13

WNS-TP 028A Roy. 1 6.31 k'han the sample cube is cured for a total of 7 days 18 hours2.083333e-4 days <br />0.005 hours <br />2.97619e-5 weeks <br />6.849e-6 months <br />, determine the dry density by the formula below, Dry Density - Total weight of dry cube (g) - tare weight (g) 131 mL Record on form W-2301, 6.32 Crush the cube according to ACM-4'01.

7.0 DATA ACQUISITION 7.1 Two inch cubo preparation and compressive strength information will be recorded on form W 2301, Rev. 1.

7.2 The cube sequence variations presented in table 2 will be recorded on attachment A.

7.3 Simulant preparation will be performed in acccrdance with ACP 7.1.

7.4 A brief test summary and records transfer to the MRC, documenting results of the testing shall be issusd by the cognizant A&PC scientist per EP il-003.

MIB0900:3RM 14

WNS - TP- 02 8 A Rev. 1 TABLE 1: BASE SOLUTICN Constituent Formula Grams / Liter Potassium Nitrate KNO 3 10.73 Sodium Carbonate Na2CO 3 29.03 Sodium Chromate, Tetra hydrate Na2C r04 4H 2O 2.610 Sodium Chloride Nacl 1.730 7

Sodium Tetraborate, Decahydrate Na2 4B 0 10H 2O 0.161 Water HO 2 1000.00 grams MIB0900:3RM 15

' WNS 'TP-028A Rev. 1 .

TABLE 2: BJENTY-EIGHT-RUN PIACKETT-BURHAN SCREENING DESIGN Note: Before running tests, the order shall be randornized Variable Ntusbe' 6 7 8 9 10 11 12 13 Trial 1 2 3 4 5

+ - - + - -

1 + - + + + - -

- - + +

2 + + - + + + - - -

+ 4 - - + - -

3 - + + + -

+ + + + - - + -

i 4 - - - + -

- + + - + + + + - - -

5 - -

+

+ + + + - + -

- +

6 - - -

+ - + - - + -

7 + + + - - -

+ - - + + - + - - +

'8 + + -

+ + - + - -

+

+

9 + - -

+ + + - +

+ - + - -

10 - - -

+ +

+ - +

+ - -

11 - - + - -

+ + - + -

12 + - - - + - - -

+ + - + +

13 - - + - + - - -

- 4 + - - + + - -

14 + - - -

+ - - + + +

15 - + - + - - -

+ - + +

+ - + - + -

16 - - -

+ +

+ - - + + -

17 + - - - -

+ + -

l 18 - + - - + - + - - -

+ +

+ + + - + + - + + -

19 -

+ - + + - + + - +

20 - + + +

+ + + - + + +

21 + - + - + -

- +

+ + + + - + - + - -

22 -

- - +

+ + + + - -

23 + + - -

+ - -

+ + + - + - + - -

24 -

+ + -

+ + + - +

25 + - + + -

+ + + + + -

26 + + - + + - -

+ + + + + + + -

27 - + + -

28 - - -

16 HIB0900:3RH

WNS TP 028A Rev. 1 TABLE 3: VARIABLE CUBE PARAMETERS Factors High (+) Low (-) Nominal Chemical Variable Components per 100 mL Phosphate (g PO4 /g C1') 1.09 g 0.0015 g 0.08 g (Sodium Phosphate, Dibasic)

Boron (g B/g C1') 0.134 g 0.0009 g 0.0018 g (Sodium Tetraborate, Decahydrate)

Aluminum (g A1/g C1 ) 4.05 g 0.00 g 0.00 g (Aluminum Nitrate.9H 2O)

Organics Citric Acid, Monohydrate 0.096 g 0.012 g 0.024 g 0xalic Acid, Dihydrate 0.095 g 0 012 g 0.024 g D-Tirtaric Acid 0.095 g .s.012 g 0.024 g ,

pH 13.0 11.0 12.0 (10N Sodium Hydroxide)

Physical Variable Components Total Solids (%) 37 25 33 Water to Cement Ratio 0.8 0.. 0.61 Mixtime (mins) 16.0 4.0 8.0 Cement Recipe Enhancers Components Percent Calcium Nitrate 11.4 2.85 5.7 Antifoam (mL) 0.6 0.09 0.3 Sodium Silicate (g) 22.0 5.5 11.0 MIB0900:3RM 17

. VVNS TP 028A Rev. 1 ATTACRMENT A MULTI VARIENT CUBE WORKSHEET Date: Laboratory ID:

Cube No.: Stock Solution:

Component Variance (+/-) Amount Chemical component Variables

1. Phosphate ( ) g (Sodium Phosphate, Monobasic)
2. Boron ( ) x (Sodium Tetraborate, Decahydrate)
3. Aluminum ( ) g (Aluminum Nitrate 9 H 2O) ,

4 Citric Acid, Monohydrate ( ) g

5. Oxalic Acid, Dihydrate ( ) _g 6.

D-Tartaric Acid ( ) g

7. pH ( ) S.U.

Amount of 10 N Sodium Hydroxide Added mL Physical Component Variables

8. Total Solids ( ) ____%
9. Water to Cement ratio ( ) _
10. Mixtime ( ) mins Cement Recipe Enhancers
11. Calcium Nitrate ( )  %
12. 5 Percent Antifoam Solution ( ) mL l

l 13. . Sodium Silicate ( ) g-Analyst: Date:

Approved: Date:

MIB0900:3RM A1 1

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' 4-4 VEST VALLEY NUCLEAR SERVICES COMPANY DOCUMENT RELEASE FORM Document No.: _ WNS -TP- 034

Title:

Test Procedure for Confirmatory Cube Revision: 0  !

l Date: 08/13/91 '

Special Instructions:

- Distribution:

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