ML20083F377
| ML20083F377 | |
| Person / Time | |
|---|---|
| Site: | West Valley Demonstration Project |
| Issue date: | 07/09/1991 |
| From: | Mahoney J WEST VALLEY NUCLEAR SERVICES CO., INC. |
| To: | |
| Shared Package | |
| ML20079E011 | List: |
| References | |
| REF-PROJ-M-32 WVNS-TRQ-034, WVNS-TRQ-34, NUDOCS 9110040229 | |
| Download: ML20083F377 (15) | |
Text
,
Doc. Number WVNS-TRQ-034 West Valley
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Revision Date 07/09/91 Demonstrat. ion Proj. ect En o nee u n, R a ea,e n n,
TEST REQUEST PPODUCTION OF CEMENT PRODUCT FROM ACTUAL LABORATORY SLUDCE WASH LIQUID
'/'/91 J. L. Ma'noney PREPARED BY cogni:
Enginee %
APPROVED BY Je D. C. Meess Cognizant System Design Manager d%l wg~, &g "".
O. L. Shugars APPR9VED BY
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p#As/tFatifelanag Qual APPRO :D BY
.f J. Harwarc Radiation & SaMty Manager /
APPROVED BY
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7[I/91 P. J. Valenti/
Pro 0jseCentro$ Engineer 1'ng' J. C. Cwynar West Valley Nuclear Services Co., Inc.
P.O. Box 191 MIB0897:3RM West Valley, NY 14171-0191 YN-1816, Rev.1 9110040229 911001 D f_
PROJ PDR
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WNS TRQ 034-Rev. O i
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 paragraph that contains a change, Example:
Th arrow in the margin indicates a change, Revision On Rev. No.
Description of Changes Page(s)
Dated 0
Original Issue All 07/09/91
.L W-1807, Rev. 1 1
MIB0897:3RM
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WNS.TRQ 034 -
Rev, 0
= RECORD 0F REVISION (CONTINUATION SliEF.T)
Revision,on Rev. No.
Description of Changes Page(sj Dated t-1 I
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W 1807, Rev.1 11
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WVNS TRQ-034 Rev. O PRODUCTION OF CEENT PRODUCT FROM ACTUAL IABORATORY SLUDGE WASH LIQUID
1.0 INTRODUCTION
1.1 This work is required to demonst ate the acceptability of an actual cement product made from radioactive sludge wash liquids, The work will provide a data point comparison to contrast radioactive cement against cement made with reagents simulating LVTS 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 Branch Technical Position of Waste Form, Psvision 1, dated January 1991.
1.2 The scope of this work is consistent with section 4.6 of VVNS-TPL-70-ll, " Test Plan for the Waste Form Qualification Program for Cement Solidification of Sludge Wash Liquid."
1.3 Production of the cement cube will require the use of sludge wash salution for wash cycle #1 created in WVNS TP-032, and decontaminated in WVNS TP 033.
1.4 Test Procedure WVNS TP 034, providing instructions for meeting the requesta specified in this Test Request shall be issued by the Analytical & Process Chemistry Cognizant Scientist per EP ll.003.
1.5 A Test Summary Report (TSR) documenting the results of this testing shall be issued by the Cognitant Test Engineer per EP-ll-003, 2.0 OBJECTIVES 2.1 After receipt of analytical results from test procedures WVNS-TP-032 and WVNS-TP-033, the decontaminated wash solution from wash cycle 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 evanorated 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 (oer available quantity of solids) following the analyces listed in Section 2.3.
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WVNS TRQ-034 Rev. 0-2.3 The. resultant concentrates shall be analyzed for:
10 '
E PO *3 Ti 2
4 NO '
Na S0 -2 Ca 3
C1 F'
Al J
_pH Total Dissolved Solids (TDS)
. density Total Suspended Solids (TSS) alpha Pu Cs-137 Sr 90 Tc 99 gross alpha gross beta 2.4 Approximately 96 nl of the concentrates shall be used to make a standard 2" cube per ACM 4801 using the nominal Sludge Wash Solution Cement Recipe developed in WVNS-TP-025, and WVNS-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..Followin5 a 28 day. curing period, the cube shall be destructively tested for compressive strength per ACM-4701, 3.0 SAFETY 3.1
' Industrial hy5 ene practices shall be as described in the UVNS i
Hygiene and Safety Manual, WVDP Oll.
3.2 RadioloS cal work shall be performed in accordance with the WVDP i
Radiological Controls Manual, WVDP 010, 3.3 Work in the Analytical & Process Chemistry Lab shall be performed in accordance with existing A&PC methods, supplemented by the test procedure VVNS TP-034.
4.0' EQUIPMENT CONFIGURATION 4.1 All lab equipment shall be set up as directed in test procedure VVNS TP-034 and the co5nizant A6PC scientist.
5.0 SAMPLING FREOUENCY 5.1 Sampling frequency and volume shall be specified in test procedure WVNS-TP 034 6.0 PERSONNEL QUALIFICATION 6.1 Tesr.ing shall be performed by qualified A&PC Technicians using ACMs per: test procedure WVN5-TP-034 MIB0897:3RM 2
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WVNS-TRQ-034 Rev. 0 I
6.2 Surveillance activity shall be performed by qualified Quality Assurance personnel.
7.0 REFERENCES
7.1
" Technical Position on Waste Form," Revision 1, dated January 1991.
1 7.2
" Preliminary 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 Prepared by UOP " WVNS TP 033 MIB0897:3RM 3
VEST VALI2Y NUCLEAR SERVICES CO.,
INC.
ACM-CUBE-4801, Rev. S ANALYTICAL CIIEMISTRY MET 110D Effective Date:
07/03/90 ANALYTICAL AND PROCESS CllEMISTRY CEMENT TEST CUBE PREPARATION MET 110D Approved by:
)
Lw umm kn.c.w 3
C. V. McVay, Manager j Analytical and Procesa, Chemistry i
Part I 1.0 SCOPE To establish a method for making a cube sample two by two by two inches using decontaminated SD 2 supernatant.
2.0 APPLICATION 2.1 The cement recipe presented in this method was developed to solidify liquid waste with a density of -1.3 g/mL, total solids of
-37 to 41 percent, and organic carbon content of -150 ppm.
2.2 The resultant two-inch cubic sample is used in determining or verifying a minimum compressive strength and density of the cement produced.
3.0 DISCUSSION To assure the quality of the CSS product, a test batch of cement must be made from the actual waste being solidified.
Parameters to be monitored include processibility (mixability, pourability). density, penetration resistance, compressive strength, and the presence and amount of resulting bleedwater.
Compressive strength test is covered under ACM-Cement-4701.
Total Organic Carbon (TOC) is not readily measurable in radioactive waste streams.
Instead of observing TOC levels several more readily measurable parameters will be monitored.
These parameters, pH and gross alpha, density, and total solids should indicate process upsets and possible changes in the level of TOC.
The expected limits for pH and MSS 0530:7RM Page 1 of 6
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i ACM. CUBE-4801, Rev. 5 e
Effective Date:
07/03/90 l
gross alpha, density, and solids are:
pH 9.0 to 11.0, gross alpha lE 1 to lE 3, density 1.300 to 1.335, and total solids 37 percent to 41 percent.
If a sample value from either a 5D15A1 or a 5D15A2 tank falls outside of this range, notify the Manager of Analytical and Process Chemistry.
4.0 REFERENCES
4,1 CSS Process Contral Plan Part II 5.0 EQUIPMENT NOTE:
All equipment to be calibrated and controlled by ACP 7.1 where appropriate.
5.1 Lightnin' Lab Mixer with high shear impellor 5.2 Cube Maker Mold with Liners 5.3 One 500 mL plastic bottle 5.4 250 mL plastic bottle 5.5 One 60.mL plastic bottle 5.6 Utility Knife 5.7 Magnetic Stir Plate and Stir Bar 5.8 Jackstand 5.9 Timer 5.10 Top Loading Analytical Balance 5,11 Convection Oven 5.12 Concrete penetrometer - Model CT-421 6.0 REACENTS 6.1 Portland type 1 cement / calcium nitrate blend, supplied by
. operations every time a cube is to be made 6.2 Silicon based antifoam CE AF9020 (shelf life of one year) 6.3 Sodium silicate, provided by operations every time a new tank truck is delivered to k'VDP 7.0 SAFETY 7.1 Do not touch the impellor shaft while the mixer is Ln operation.
7.2 Hold the mixing vessel steady while mixing to avoid spilling and throwing of contaminated cement from the impellor.
7.3 Standard laboratory procedures and radioactive materials handling procedures are to be followed per ACP 7.2 and ACP 7.4 MSS 0530:7RM Page 2 of 6 i
ACM-CUBE-4801. Rev. 5 i
Effective Date:
07/03/90 8.0 RECORDS All measurement data and sample identification shall be recorded on the Solidification Data Sheet (attachment A).
The final result shall be recorded on the analytical request sheet (PRD 5.1).
9.0 CALIBRATION AND CONTROL l
9.1 All balances and measuring equipment will be calibrated and verified per ACP 7.1.
10.0 PROCEDURE 10.1 Make a 5 percent antifoam solution.
Weigh 5.0 1 5 g of well 0
mixed AF9020 in a 100 mL volumetric flask and dilute to the mark.
Mix well, transfer to a suitable container with a-magnetic stir.bar and stir continuously on a stir plate.
10.2 Use a 500 mL bottle to make a mixing vessel by evenly cutting of f, the top producing an open ended cylinder.
10.3 Similarly cut the top off one 250 mL bottle.
This container will be used to add the dry cement / calcium nitrate mixture to the liquid waste.
10.4 Tate the cutoff 250 mL bottle and add 140.5 il g of the cement / calcium nitrate mixture.
Record the weight on the work sheet.
10.5 Deleted 10.6 Pour 100 mL (or 137 g) decontaminated supernatant into the mixing vessel prepared ir ;ep 10.2.
10.7 Calculate the water to cement ratio using the formula in 11.0 and report the results on the Sample Solidification Data Sheet (attachment A).
10.8 To the decontaminated supernatant, pipet 0.3 mL (or 0.3 g) of antifoaming solution from step 10,1.
10.9 Tare a 20 mL disposable plastic beaker and weigh ~11 grams'of sodium silicate solution.
Re-tare the balance to the weight of the beaker plus the sodium silicate.
(NOTE:
You want to add
(
about 10 grams of sodium silicate to the cement but the sodium o
silicate will stick to'the beaker.) The exact amount transferred will be found by weighing the used beaker after addition and noting the negative weight displayed on the balance.
MSS 0530:7RM Page 3 of 6 l
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r ACM-CUBE-4801, Rev. 5 Effectivo Date:
07/03/90 10.10 Support the mixing vessel containit.g the waste under the mixer with a jackstand so that the tip of the impeller is 1/8 to 1/4 inches from the bottom of the vessel.
Begin mixing at 1000 rpm.
10.11 See a timer for 3 minutes and slowly add the dry cement / calcium nitrate to the vaste.
(Transfer should take from 45 to 60 seconds.)
Begin timing immediately upon completion of cement transfer.
10.12 Immediately after the start of the timer, add the sodium silicate solution to the tement keeping the beaker clean (uncontaminated) for reveighing.
10.13 Upon completion of the 3 minute mix time, immediately fill the cube mold as full as possible.
Pour any remaining cement into a 20 mL scintillation vial and seal.
'10.14 Clean the impellor with water in a vaste container immediately after pouring.
10.15 When the cement has jelled (see step 10.16), scrape the excess off the top of the cube so that the level is even with the height of the mold.
Place the cube in a plastic zip lock bag and seal.
10,16 Transfer the cube from the hood to another clean plastic bag, making it doubly contained.
Printonouterbagthenameof sample,- time and date, and place in oven at 70 C +5 C for 24 to 48 hours5.555556e-4 days <br />0.0133 hours <br />7.936508e-5 weeks <br />1.8264e-5 months <br />. Record on the Data Sheet the time the cube was placed in the oven.
10.17 Af ter 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> but before 48 hours5.555556e-4 days <br />0.0133 hours <br />7.936508e-5 weeks <br />1.8264e-5 months <br /> the cube may now be taken out of the oven and a penetration resistance analysis performed on it. ' Record on the Data Sheet the time the cube was removed from the-oven.
10.18 Remove the cube from the double contaminant plastic bags inside a vented hood.
Do not remove the cube out of the plastic mold.,
10.19 Using a concrete penetrometer (model CT-421) perform the penetration resistance test by centering-the penetrometer plunger in the center of the exposed side of the cube.
Make sure the red indicator ring is located back to zero on the penetrometer.
With steady, vertical force, push the penetrometer against the cube until either the red indicator ring is all the way down the scale or the thin rad line around the penetrometer shaft is reached first.
MS30530:7RM Page 4 of 6
p-ACM-CUBE 4801 Rev. 5 Effectiva Date:
07/03/90 10.20' On'the-handle of_the penetrometer, read the value of the red indicator ring and record that value on the sample Solidification Data Sheit.
If the red indicator ring is all the way to.the end of the scale, a value of >700 psi should be recorded.
10.21 Place the cube, sitting inside it's own cube mold, into two cleau clear plastic ziplock bag and put into a 5 gallon storage can labeled "For-Cement Cubes only".
10.22 The sample cube is cured for a total time of 7 days and is analyzed for compressive strength test according to ACM Cement 4701.
10.23 Visually check for gelation of the cement in the 20 mL scintillation vial every 2 minutes for the first 35 minutes and every 10 minutes af ter the first 35 minutes.
Record gelation time on the work sheet. Celation has occurred when, upon tipping the bottle to one side, the cement does not flow and change its shape.
10.24 One hour after pouring the cement, estimate the amount of bleedwater-(if any) in the 20 mL scintillation vial by tipping the bottle to one side and observing.
Repeat this observation 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> after the pour time.
Record observations on work sheet.
11.0 CALCULATIONS 11.1 Water-to cement ratio:
(A) (B) (1 C)
(D) (0.95)
A - Volume in mLs of saepla
'B - Density value in ges/mL of sample C - Total solids value in decimal form D - Weight of cement used in grs.
11.2 Report compressive strength to three significant figures on Attachment A.
12.0 ATTACRMENTS Attachment A - Solidification Data Sheet L i-MSS 0530:7RM Page S of 6 l
t
i ACM CUBE 4801, Rev. 5 Iffectiva late:
07/03 90 f
Attachment A So11dificatina J}ata Sheet Page _ -f _
ACM CEMENT 4701
' rple Log No.
.sk and Sample Number:
noss alpha
,Ai/mL TS att Crosa beta pCi/mL Density g/mL Cs 137
_ 41/mL pil SU j
Calibrated Instruments used:
1 Total solids (TS) between 37% and 414
_ Yes No p!? between 9 and 11 Yes No
.x ity between 1.300 g/mL and 1.335 g/mL Yes No
> Gross alpha between IE 01 pCi/mL to 1E 03 pC1/mL Yes No Decontarninated Supernatan. Volume mL Veight of Ceiuent/ Calcium Nitrate mixture grama Antifoam Volume of A $ gr/100 mL. Sol.
cal Sodium Silicate g
Vater to Cement Rar,io (calculations: 11.0)
Time and Data Sample Produced Cure Oven Temperature C
Date/ Time in Oven Date/ Time out of Oven Free Liquid Volume mL Observations: (Includin5 pourability, gel time, visual inspection, etc. )
>Celation Time _
rninutes
>* NOTIFY A&PC MANAGER IF CEIATION TIME IS LESS TilAN 5 MINUTES OR CREATER TilAN 30 MINITTES.
Sample Prepared by:
Date:
Solidification Results:
Made note with test dates on " grease board" initials Penetration Resistance following 24-48 hr cure psi Analyst Date Compressive Strength (
x 1.25) -
?si Analyst Meter Reading Date Results Approved:
, Manager Analytical Laboratory Date:
MSS 0530:7RM Page 6 of 6
WASTE FORM QUALIFICATION PROGRAM 9722/91 FOR SLUDGE WASH LIQUID I TEST PL Ar4 )
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