ML20083F375

Rev 0 to Test Procedure WVNS-TP-034, Confirmatory Cube

ML20083F375
Person / Time
Site:	West Valley Demonstration Project
Issue date:	08/13/1991
From:	Michnik L WEST VALLEY NUCLEAR SERVICES CO., INC.
To:
Shared Package
ML20079E011	List: ML20079E008 ML20083F355 ML20083F360 ML20083F370 ML20083F372 ML20083F375 ML20083F377
References
REF-PROJ-M-32 WVNS-TP-034, WVNS-TP-34, NUDOCS 9110040227
Download: ML20083F375 (19)

Text

. __ - .. . _ - -_

West Valley oec . "-8 r =s tr m' Demonstration Project Revision Date 08/13/91 Engineering Release o 2163 1

l TEST PROCEDURE CONFIRMATORY CUBE PREPARED BY M [

Cognizant Erigineer Avka L. E. Michnik

[

APPROVED BY c D. C. Meess Co5nizant System Design Manager APPROVED BY /  % bib P. J. Valenti Cognizant facilities Manager APPROVED BY ' A4D 'rw,-

. '2 D. L. Shugars QualityqssuranceManager APPROVED BY d .h N w ?3rN 0 bl D. J. Harvard Rad {iajionandSafetyManager West Valley Nuclear Services Co., Inc.

DLSO460: 3RM P.O. Box 191 West Valley, NY 14171-0191 WW1816, Rev.1 911004o227 913003

- FIiR PROJ M-32 PDR l

l WNS TP-034 Rev. 0 RECORD OF REVISION 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 pa agreth that contains a change.

Example:

> The arrow in the margin indicates a change.

Revision On Rev, No. Description of Chare,es Page(s) Dated 0 Original Issue All 08/13/91-W-1807. Rev. 1 i DLSO460: 1RM

WNS TP 034 Rev, 0 RECORD OF REVISION (CONTINUATION SHEET)

Rev, No, Dascription of Changes Revision)on Page(s Dated W-1807, Rev, 1 11 DLSO460:3RM

,_ _ __ _ . _ _ _ . ~ _ _ _ __ ._

^

. 1 TEST PROCEDURE FCR CONFIRMATORI CUBE .

WVNS TP 034 REV. 0 1.0 Scope 1,1 This-procedure is for the preparation of a 2x2x2 inch cement cube *

-made'from actual sludge wash liquid generated-from under WVNS-TP 032 and decontaminated under WVNS TP 033. The scope of this work in compliance with section 4.6 of WVNS TPL 70 11 " Test Plan for the Waste' Fora Qualification Program for Cement Solidification of Sludge' ,

Wash Liquid". The cube will also provide information on-the reaction of the nominal recipe for cement on actual sludge wash matori U and determine if any unforeseen constituents are having an adverse effect on the cement product, 1.2 The-l liquid 1:om Sludge Wash Cycle #1 created from WVNS TP-032 and decontaminated under UVNS-TP-033 will be evaporated so that the total dissolved solids-in the concentrated material vill have a maximum value of 33 weight percent and a minimum value of 29.

i 1.3 The compressive strength data generated from this cube will be compared to' data generated under WVNS TP-026, rwenty-eight day curing period, and WVNS-TSR-029A, Cel time, bleed water and-penetration resistance will=also be compared'to-the results obtained '

l- from WVNS-TSR-029A.

2.0 Definitions and Abbreviations 2.1 Definitions ~

Cement-Dry Portland Type I cement in accordance with ASTM Standard C 150-85.

L LLSO460:3RM- -. . . __ _ . . _ _ - . . _ . - _ _ . . _ - - - - - . - . _.

o VVNS TP 034 I

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 of the cement vaste 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) and 11.7 pounds per gallon.

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

2.2 Abbreviations ,

ACM-Analytical Chemistry Method AST~ merican Society for Testing and Materials 3.0 Responsibilities 3.1 Analytical and Process Chemistry will be responsible for the preparation and ter.'ng of the laboratory specimens in accordance to the applicable steps of the appropclate Analytical Chemistry Methods (ACMs) and VVNS-TP-034, 3.2 Quality Assurance will provide surveillance to ensure that the requirements of this test procedure and UVNS TRQ-034 are satisfied and verify the final concentrate product, witnessing of the cube being made and also the crushing of the cube.

DLSO460:3RM

.c WNS-TP 034-Rev, O 3.3 Radiacion 6_ Safety monitors radiation and contamination levels in  ;

the laboratory co insure. work is-conducted in accordance with the.

~

Rad Con Manual WDP 010 Rev.1.

3.4 IRTS will'be~ responsible for issuing the test summary report, WNS-TSR 034, in accordt.:ce with EP 11 003.

4.0 Tools, Equipmcat, Components and References 4.1 Tools and Equipment

'Lightnin Lab mixer Model-No. TS-1515 with high shear impeller 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 al.polypropylene plastic bottles 250 ml borosilicate beaker t

Corning hotplate or equivalent 10 mi:. 16 ass ;olumetric 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 ;s (grams)

'l

- DLSO460: 3RM .: , . . . . -.-

WVNS-TP 034 Rev, 0-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 cement Calcium Nitrate tetra-hydrate, reagent grade Nanopure water or ASTM Type I water Sodium Silicate, technical grade * .

Antifoam Ceneral Electric AF9020*

• Supplied by IRTS operations 4.3 References NRC Technical Position on Waste Form (Revision 1) January 1991 ACM 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)

I 1

DLSO460:3RM )

.i '- -WVNS-TP 034

.Rev. O n.

WVNS TP-026 " Procedure for Qualification of the Nominal Recipe for

-Coment Solidification of Sludge Wash Liquids", Letter a FH:91:0088,

'da ted ' J une ' 17,11991, to J. ' A. Mahoney from L. E. Michnik -

TE WVNS TRQ 026 01 " Revised Salt Concentration for the " Nominal Simulant Recipe based mr 128.5 inch Heel" +

r-cj WVNS TSR 029A " Test Summary Report for Confirms.cory Cube" WVNS TRQ 034 " Production of Cement Product for Actual Sludge Wash 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 General Information 5.1 This test will be used to evaluate the nominal cement formulation recipe (see Attachment C) using actual sludge wash and supernacant

-from tank 8D-2 based upon a-nominal 130 inch supernatant heel. It will' confirm the accuracy of data and' observations generated by laboratory simulantr 'and determine if any unforeseen constituent are having an undesirable-effect on the cement. product.

.6.0 ? Procedure' 6.1 Prerequisite

-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 Balances shall be calibrated according to ACP 7.1 Safety procedures should be reviewed in ACP 7.2 DLSO460: 3RM .- .__ _ _ . . _ . _ _ _ . _ _ _. _ _ _ _ _ _ , . _ _ _ .. ___ _._ ~ - - . - _ . . . . _ . -__

, WNS TP-034 Rev. 0 6.1.1 A sufficient amount of liquid from WVNS TP 032, Sludge Wash #1 shall be used to generate at least 100 milliliters of 33 percent solid sludge wash liquid. This liquid shall be placed in a 250 ml 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 ba reduced to approximately three-quarters of its initial volume. At this point the total solids will 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 2501, 6.1.2 If the liquid is reduced to the point were solids are falling out of solution due to over evaporation, the evaporation should stop and nanopure water should be added in small increments and the solutien 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, the 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, c:

DLSO460: 3RM -

I L'VNS TP 034 Rev. 0 -l

. 1 a

The resulenne concentrates shall be analyzed for:

NO2 ' K PO4 *3 Ti

, NO3 ' Na 304 ' Ca B03 '3 TOC TIC Cr C1' F' Al U pH Total Dissolved Solids (TDS) .

density Total Suspended Solids (TSS) 4 l alpha Pu Cs-137 Sr-90 Tc 99 gross alpha gross bete 6.1.3 After the appropriate solid content has been achieved

• approximately 96 als 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 6.3.4 thru 6.1.27 and the remaining will be used for

the analysis in section 6.1.2.

6.1.4 Make a 5 percent antifoam solution. Weigh 5.00 +/- 0.05 gs 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.

6.1.5 Prepare 200 gs 5.7 percent calcium nitrate tetra-hydrate / cement mixture by adding 11.4 gs calcium nitrate tetra-hydrate to 188.6 gs Portland Type I cement in a 500 ml 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.

DLSO460: 3RM __.

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

'WVNS TP 034 Rev.'O 6.1.7 Similarly cut:the top off'a 250 ml 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 bottle and add 140.5 +/~ ig cement / calcium nitratc< Record weight on the appropriate Form WV 2301.

-6.1.9 Place-the cut 500 m1 mixing vessel prepared in step 6.1.6 under impeller and set mixer speed to 1000 rpm.

6.1.10 Measure 96 +/- 2 al of 29 33.Ut concentrate from step 6.2.3 using a 100 ml graduated cylinder and record on Form WV-2301.

- 1 6.1.11 Pour 96 mis of concentrate into the 500 m1 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 pipet and transfer 0.3

-+/ .0.006 al of the 5% antifoam mixture from step 6.3.1.

Record on Form WV-2301.

2 .

= 6.1.13. Tare:a 10 ml disposable-plasticycup and add to it approximately 11'00 +/- 0.5 gs sodium silicate. The exact o

amount transferred will.be found by reweighing the cup after-L o the material is poured into'the sludge wash. Record the p weight on' Form WV-2301

~ 6,1,14 Support;the' mixer on a lab stand so that the impeller blade l: is one-quarter to one-eighth-inch from the bottom of the 500 al plastic bottle. Use a wide mouth clamp to support the-500 al plastic bottle without crushing the side. Set a timer for 8 minutes.

l-I' l ?LSO460:3RM . . _. _ _ . - . , - , _ _ _ . . - - . - _ . . . _ , . . . _

l , WVNS TP-034 i Rev. 0 6.1.15 Begin the mixing at 1000 rpm and start the timer. Add the dry cement / calcium nitrate mixture to the vaste 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 .ifter the transfer of the sodium silicate reveigh the cup and calculate the amount added by difference, record on Form WV-2301. While mixing, mark a cube mold with a permanent marker with the date, sample type, numerical identification sequence number and then weigh the cube mold, record tha weight on Form WV-2301.

6.1.17 After completion of the eight minute mix, stop the mixer and -

transfer the contents to a plastic 2" cube mold. Fill to the top and transfer the remaining to a 20 ml plastic scintillation vial and seal. After weighing the cube care the scale to zero and reweigh the cube with the cement in it. Record the weight on Form WV-2301. Determine the wet density of the material by the formula below.

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 completirg 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 mi scintillation vial. Check every five minutes and do not disturb between there time intervals. Record the time it take the cement to gel. Celation is a subjective determination, however gelled cement is indicated when the l

DLS0460:3RM -

9-

?

VVNS-TP-034 Rav. 0 f

20 ml scintillation vial can be tipped slowly to a 90 degree position, parallel to the horizou. 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.

6.1.20 Transfer the cube to a dryin5 oven with the temperaturn 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 cuba ano not deform the exposed cube face. 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.

6.1.21 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 WV-2301.

6.1.22 Calculate the water to cement ratic by weight using formula below.

(A)(B)(1-C)

(D)(0.943)

A-Volume in mis of sample B-Density value in gs/ml of sample C-Total Solids value in decimal form D-Veight of cement used in as 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 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 VV-2301, 6.1.24 Caution: Do not remove the cube from the mold for the penetration test and only when ready to crush.

DLSO460: 3RM - 10

,1 4 -

VVNS TP 034 Rev. 0 6.1.25 Using 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.

6.1.26 ' 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 and of the scale, a -

value of >700 psi shall be. recorded.

6.1.27 When the sample cube is cured for a total of 28 days +/- 8 hours9.259259e-5 days <br />0.00222 hours <br />1.322751e-5 weeks <br />3.044e-6 months <br />. . Determine the dry density by the formula below

[.

D"y Density -Total weight of dry cube (g) - care weight of cube mold-(g) l l

131 mis l

l ~131 mis - Volume of 2x2x2 inch cube mold 1,

Record on form WV-2301

-6.1.28 Crush the cube according to ACM 4701 by sanding the cube in i-

, accordance with ASTM C-109-section 10.6.2

~7.0 Data Acquisition l 7.1 Two-inch cube preparation and Compressive strength information will be recorded on Form WV-2301, Rev 1.

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

WHS TP 034 Rev. 0 7.3 Density will be recorded on Form W 2401' 8.0 Attachments 8.1 Attachment A - Results frem 32" Heel Sludge Wash Confirmatory Cube

1. FH:91:0073 8.2 Attachment B - Nominal Recipe for Sludge Wash Cement 8.3 Attachment C - Nominal Cement Recipe Compressive Strength Data

1. nl:91:0088 4

DLSO460:3RM , . - . - ._ _, _ - _ , . - - . _ _ , - .

, L'VNS TP 034

, Rev. 0 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 tTDS 29.7 B. Cube

.talysis Result Gel Time 35.5 mins Slurry Density 1.76 g/ml Blevdwater None Penetration > 700 psi Compressive Strength 694 psi s

4 DLS0460: 3RM A- 1

. _ . . . - . _ . . . _ _ . . . . . _ . _ . _ . _ . . . - - - . _...._._ . _ m _ ._ _

--+

7 WNS TF 0*:4' Rev. 0

. .. 1 1

Attachment B ,

To: - John Cwynar Laeters: nl:91:0018-From: Frank Hara and Larry E. Michnik Subj ect: Coment Recipe-for Sludge Vash Simulant with 33 inch Supernacant heel . _.

-Date:- January 24, 1990 The recipe for the laboratory scale specimen cube (2x2x2) contain the following am:>unts of ingredient.s:

1.) 140.0 grams of Portland Type I Cemer.t with '

5.7% Calcium Nitrate 4 Hydrate 2.)L11.0 grams Sodium Silicate 3.) 0.3 als of 5.0 grams to 100 nls antifoas (AF 9020) 4.).96 als of 33.0 weight percent Sludge wash' simulant .

This recipe will produce a product with-a water / cement ratio of 0.61 Villiam F. MacKellar Manager A&PCs 5

j -t L

i t-DLSO460:3RM B-1

1 9 l

' 'a*VNS TP 034 Rov. 0 Attachment C l

Two Inch Cubes Laboratory ID. D rum 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. D rum No . Compressive Strength (psi)

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

+

DLS0460: 3RM C-1