1. ECN ENGINEERING CHANGE NOTICE. Originator's Name, Organization, MSIN, and Teleuhone No. 7. Bldg./Sys./Fac. Retained Gas Sampler System/NZO13

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1 1. ECN ENGINEERING CHANGE NOTICE I ECN Category (ark one) Suppleental Direct Revision Change ECN Teporary Standby Supersedure Cancellvoid [I 3 t1 Noran Scott Cannon, 8A200 L6-38, []Yes (fill12b) out Elk. [XI No (NA Elks. IZb, [I UsQ Required? 1 Yes [XI 9. Docuent Nubers Changed by this ECN IO. Related ECN No(s). 12c. Modification Work Coplete N/A 13a. Description of Change 13b. Design Baseline Docuent? [XI Environental Const. Error/Ornission ECN 5. Date 8. Approval Designator Related Po No. N/A N/A 12d. Restored to Original Condition (Tep. or Standby ECN only) N/A Design Authoritylcog. Engineer Signature & Date 12c. 12d) No. FGWL Tanks HNF-SD-WM-CN-092, Rev. 0 12b. Work Package NO. Pro,. 09/24/97 NO 7. Bldg./Sys./Fac. Retained Gas Sapler Syste/NZO13 (includes sheet no. and rev.) Ira. Modification Work I Project Title/No./Uork Order No. [I t1 Originator's Nae, Organization, MSIN, and Teleuhone No. P*W 1 o f N/A [I Design AuthoritylCog. Engineer Signature & Date Yes [XI No The docuent HNF-SD-WM-CN-092, Rev. 0 was updated to produce HNF-SD-WM-CN-092, ; these changes included additional field results. allowing further evaluation o f heliu backfilled RGS saplers. Also included was a coparison of in-tank holding ties with RGS oxygen levels to evaluate a possible oxygen/waste reaction, and a ore detailed calculation of the sapler interface volue. 14a. Justification (ark one) [] :riteria Change is-found [] 14b. Justification Details Design Iproveent Facilitate Const [] [I [] Facility Deactivation Design Errorloission [] [] ieliu backfilling of RGS saplers was added to iniize saple containation fro air and purge gas trapped in the sapler interface volue. This revision includes additional field data to deonstrate the success o f this design iproveent. A (05196) GEF095 A

2 ~ 16. Design Verification Required 11 Yes [XI No ENGINEERING CHANGE NOTICE Page 2 of 2 I. ECN (use no. fro pg. I) Cost Ipact 18. Schedule Ipact (days) ' ENGINEERING CONSTRUCTION Additional [N] $ Additional [N] $ Savings [Nl.$ Savings [NI $ Delay Iproveent [NI ' SsisiclStresP Analysis Tank Calibration Manual Functional Design Criteria Operating Specification Criticality Specification Conceptual Design Report Equipent Spec. const. spec. Pcureent spec. Vendor Inforation OM Manual 3ARISAR 3afety Equipent List iadiation Work Perit StressIDesign Repoft Interface Control Drawing Calibration Procedure Installation Procedure Maintenance Procedure Engineering Procedure Operating Instruction Operating Procedure Operational Safety Requireent iefd Drawing Cell Arrangeent Drawing Essential Material Specification Health Physics Procedure Spares Multiple Unit Listing Test Proc~dureslSpecification Coponent Index ASME Coded Ite Huan Factor Consideration Coputer Software Electric Circuit Schedule ICRS Procedure Process Control ManualIPlan Process Flow Chart Purchase Requisition Environental Ipact Stateent Fac. Proc. Sap. Schedule Tickler File [I Invinental Report Inspection Plan [I invironental Perit ' Inventory Adjustent Request LJ [I!O. Other Affected Docuents: (NOTE: Docuents Listed below will not be revised by this ECN.) Signatures below indicate that the signing organization has been notified of other affected docuents Listed below. Docuent Nuber/Revision Docuent NuberIRevision Docuent Nuber Revision inf-sd-cn-o92/revision 0!I. Approvals Signature lesign Authority NIA :og. Eng. N. S. Cannon 4 :og. Mgr. J. R. T h i e l g e y a IA K. Napora dl- :afety nviron. lther R. E. BaUer 87- Date Design Agent Safety Design Signature Date DEPARTMENT OF ENERGY Signature or a Control Nuber that tracks the Approval Signature ADDITIONAL A (05196) GEF096

3 ~~ HNF-SD-WM-CN-092, Retained Gas Sapler Interface Volue N. S. Cannon SGN Eurisys Services Corporation, Richland, WA U.S. Departent of Energy Contract DE-AC06-96RL13200 EDT/ECN: ECN UC: 510 Org Code: SI300 Charge Code: N2013 B&R Code: EW Total Pages: 34 Key Words: Retained Gas Sapler, RGS Containation Volue, Interface Volue, Heliu Backfill, RGS Air Containation, RGS Purge Gas Containation Abstract: The axiu Retained Gas Sapler (RGS) interface volue was deterined; this volue can trap containation gases during the sapling process. A new technique (heliu backfill) for eliinating containation gases fro the RGS sapler interface volue is described, and verification testing reported. Also deonstrated was that RGS data obtained prior to the introduction of the new heliu backfill technique can be copensated for air containation using the easured oxygen concentration and noral air coposition. TRADEMARK DISCLAIMER. Reference herein to any specific conercial product, process, or service by trade nae, tradeark, anufacturer, or otherwise, does not necessari ly constitute or iply its endorseent, reconendation, or favoring by the United States Governent or any agency thereof or its contractors or subcontractors. Printed in the United States of Aerica. To obtain copies of this docent, contact: Oocent Control Services, P.O. Box 950, Mailstop H6-08, Richland WA 99352, Phone (509) ; Fax (509) Release Approval Date Release Stap Approved for Public Release A (01/97) GEF321

4 RECORD OF REVISION (2) Title RETAINED GAS SAMPLER INTERFACE VOLUME (1) Docuent Nuber HNF-SD-WM-CN-092 Page 1 CHANGE CONTROL RECORD (3) Revision (4) Description of Change - Replace, Add, and Delete Pages - 0 (7) Issued on EDT , March Revision 1 is a rewrite with changes in text, figures, and appendices. is issued on ECN Authorized for Release (5) Cog. Engr. (6) Cog. Mgr. Date A (08/91) WEF168

5 HNF-SD-WM-CN-092 Page 1 RETAINED GAS SAMPLER INTERFACE VOLUME N. S. Cannon Septeber 1997

6 CONTENTS HNF-SD-WM-CN-092 Page 2 Page 1.0 INTRODUCTION Purpose Retained Gas Sapler Interface Volue Description O INTERFACE VOLUME DETERMINED EXPERIMENTALLY CALCULATED INTERFACE VOLUME INTERFACE VOLUME HELIUM BACKFILL Heliu Backfill Technique Heliu Backfill Laboratory Verification Testing Heliu Backfill RGS Results Oxygen Reaction with RGS Waste CONCLUSIONS REFERENCES ACKNOWLEDGEMENTS Aaoendixes A INTERFACE VOLUME RAW DATA/ANALYSIS A-1 B...._ INTERFACE VOLUME CALCULAT'ION B-I C INTERFACE VOLUME GAS TRANSFER DURING SAMPLING C-1 D IN-TANK HOLD TIME EFFECT ON RGS OXYGEN LEVEL - FIVE TANK DATA..,. D-1 Fiqures 1 Siplified Sketch of the RGS Geoetries Producing the Interface Volue. 5 2 Sketch of the RGS Sapler/Drill Bit Configuration Prior to Sapling Interface Volue Measureent Test Setup. Two configurations were used to deterine the interface volue, as shown The Portion of Sapler Piston Protruding Beyond the Sapler Interface is Illustrated. The volue V = n( ')/2 * (0.8 in3) = 9.48 c3. The rounded edges $t the piston end have negligible effect on the volue Coparison Plot of Containation Gas Volues (at STP) for RGS "Five Tank" Data, Heliu Backfill Lab Test Data and Heliu Backfilled RGS "Three Tank" Data RGS Oxygen Concentration Related to Lag Tie. The tie between sapler reoval fro the tank and the beginning of the extraction process is the lag tie B-1 Detailed Sketch of Geoetry Producing Interface Volue B-2 B-2 Siplified Sketch of RGS Valve Housing Showing Ball Valve Mounting Flats B-3 C-1 Coparison of Saple Air (Deterined zro Oxygen Concentration) with Leakage Air (Calculated fro Pretest Leak-Rate") for Individual Three Tank RGS Saples C-6 D-1 Five Tank Data Oxygen Levels (at STP) plotted versus In-Tank Hold Tie.... D-3

7 HNF-SD-WM-CN-092 Page 3 Tab1 es CONTENTS (Cont. ) A-1 He1 iu Backfill Verification Testing Raw Data: , Configuration A-1 A-2 Heliu Backfill Verification Testing Raw Data: , Configuration A-1 A-3 Heliu Backfill Verification Testing Raw Data: , Configuration A-2 A-4 Heliu Backfill Verification Testing Raw Data: , Configuration A-2 B-1 Coponent Calculation Suary B-4 C-1 Laboratory Siulation Tests - Heliu Backfilled Saplers C-1 C-2 RGS Trapped Air Volue Deterination C-3 C-3 Statistics for RGS "Containation" Volues at STP C-4 C-4 Effectiveness of Heliu Backfill Technique..., C-5 D-1 Five Tank In-Tank Hold Ties D-2

8 RETAINED GAS SAMPLER INTERFACE VOLUME N. S. Cannon ( ) 1.0 INTRODUCTION HNF-SD-WM-CN-092 Page 4 When a Retained Gas Sapler (RGS) is lowered down the drill string, there is an external "interface" volue in which air or purge gas can be trapped. During the actual segent sapling, soe or all of this external gas ay inadvertently be included as part of the RGS saple, adding to the saple gas coposition and volue errors. 1.1 Purpose The purpose of the work reported here was to deterine the axiu value of the interface volue using an experiental ethod, and additionally by direct calculation. Also presented in this report is a new technique to iniize saple containation fro external gases trapped in the RGS interface volue by using a sapler heliu backfill ethod. Validation testing results for this technique are included. In addition, it is shown that previous RGS tests (Shekarriz, 1996) perfored before the heliu backfill technique was developed can be copensated for air containation by using the easured saple oxygen concentration results and noral air coposition. 1.2 Retained Gas Sapler Interface Volue Description A sketch of the valve end of the RGS (a siplification of details provided in drawing H ) is given in Figure 1. The RGS piston starts in an extended position (0.8 inches, 2 c) beyond the sapler "interface" insert before the actual saple is taken. This extension lines up the end of the piston with the end of the drill bit, as illustrated in Figure 2. Having the piston flush with the end of the drill bit iniizes the aount of waste dragged along with the bit as the drill string is lowered into the tank. This positioning assures a ore representative saple at individual tank locations. As a sapler is lowered into the tank waste, the waste will trap air/purge gas in any volues that exist between the sapler interface and the piston O-rings (see Figure 1). The total volue available to trap gas in this way is defined as the interface volue (VI). 2.0 INTERFACE VOLUME DETERMINED EXPERIMENTALLY A test was devised to easure this interface volue using pressurization of the sapler interface with heliu or argon (starting with a known charge volue, pressure and teperature) and the ideal gas law. Two test configurations were used and are sketched in Figure 3.

9 HNF-SD-WM-CN-092 Page 5 RETAINED GAS SAMPLER INTERFACE VOLUME d EB WELD VALVE HOUSING VALVE STOP BALL VALVE VITON SEAL b THREAD SEAL Figure 1..Siplified Sketch of the RGS Geoetries Producing the Interface Vol ue.

10 HN F - SD - WM-CN ~ 092, Page 6 RGS SAMPLER/DRILL BIT CONFIGURATION I n DRILL BIT //,, J / SAMPLER VALVE H HOUSING / Figure 2. Sketch of the RGS Sapler/Drill Bit Configuration Prior to Sapling.

11 22 ga e l c $2 rl( E T / 1 1 J VI J L 3 VI E 0 o 5-J u- S 0 u.r.- n 3 o Lo +-' VI I- L 3.C U

12 HNF-SO-WM-CN-092 Page 8 In test Configuration 1, a polished surface "blank-off" disk was pressed against the attachent chaber's sealing O-ring, creating a basic syste volue of V,. The volue defined as V, includes the attachent chaber volue, line volues and the ain vacuu chaber volue that are shown in Figure 3. The ain chaber volue also includes two pressure transducers, PXDl and PXD2, which are not shown in Figure 3. The value of V, was deterined by charging the syste, including the reference canister (of known volue V,) with gas through Valve A (Valve B closed and Valve C open) to a starting pressure (PI) at abient teperature (TJ. Then, with Valves A and C closed, the reaining volue was evacuated through Valve B, leaving only V, charged at PI. After evacuation, Valve B was closed and Valve C was opened allowing V, gas to produce a new pressure (P,) in V,, eventually at the sae teperature T,. The volue V, was then calculated fro the ideal gas law as The reference canister volue had previously been easured by weighing it dry, and then filling it with water (essentially bubble free) and reweighing it. Using the water density, the canister volue was deterined as V, = L. In test Configuration 2, Sapler PR2 was ounted to the attachent chaber as also shown in Figure 3. The sapler piston was extended beyond the sapler O-ring insert assebly (sealing surface) 0.8 inches (2 c), as is required when the sapler is placed in the drill string for tank sapling. The volue of the portion of the piston extending beyond the sapler sealing surface (defined as Vp) is easily calculated fro the siple geoetry sketched in Figure 4 as 9.48 L. The new syste volue (V,) was then deterined by charging the reference volue with gas and discharging it into the syste volue as previously described, where The sapler interface volue (V,) can then be deterined fro VI = lvn + VpI - v, (3) Data was obtained on July 3, 1996 using heliu gas, and another set of data was taken July 15, 1996 using argon gas; raw data and analysis of this data are given in Appendix A. The heliu gas tests resulted in a value of 6.08 L for the interface volue while the argon test data produced a value of 6.10 L.

13 HNF-SD-WM-CN-092 Page 9 c W b-0 W Z 0 t v, - o_ v, c3 K

14 HNF-SO-WM-CN-092 Page 10 These are rearkably consistent values for VI considering that two different transducers (with different pressure ranges) were used for the volue deterination. Also the test syste volue was changed by about 0.9 L between the two testing days while the syste was used for other purposes. 3.0 CALCULATED INTERFACE VOLUME Early in the RGS progra, the interface volue had been estiated as about 1.1 L, based on deterining the "gap volue" between the sapler piston and the sapler tube. volue of 6.1 L, As a result of the experientally deterined interface a re-evaluation of the valve assebly construction was perfored. Details of the resulting calculation of the interface volue are given in Appendix B. A brief suary of these results follows directly. Re-exaining the scheatic of the sapler valve assebly shown in Figure 1, it can be noted that there is a substantial annulus volue within the Valve Housing coponent that is occupied by a total of three sapler parts: Valve Stop - Stationary coponent behind the valve. Viton Seal - Stationary coponent in front of the valve. Rotary Ball Valve - Rotates 90 degrees during valve closure. Using engineering drawing noinal diensions, the epty volue of this annulus was calculated (see Appendix B) to be 30.2 L. Note that this volue ay vary soewhat fro sapler-to-sapler due to the exact final position of the threaded Insert. However, inspection of several copleted saplers indicated that this variation would affect the volue by less than f 0.5 L. The next step was to deterine the volue of the three individual coponents that occupy this annulus. This was done using weight and density data for each coponent. The results were as follows: Valve Stop = 9.9 L Viton Seal = 5.6 L Rotary Ball Valve = 9.2 L Total = 24.7 L Therefore, the void volue for this section of the RGS valve assebly, which ay be expected to be filled with air or other external gases when the sapler is inserted into the waste, is calculated to be: 30.2 L L = 5.5 L This volue, coupled with a re-evaluated gap volue of 0.7 L, results in a total void volue of approxiately 6.2 L, in close agreeent with the volue deterined using the ideal gas law.

15 HNF-SD-WM-CN-092 Page 11 Another test series should be entioned which was perfored by M. White to easure the interface volue using a water fill ethod (White, 1997). A syringe was used to force water into void spaces and displace air, with weight easureents resulting in an interface volue deterination of 5.72 L. This value is slightly saller than those previously deterined, which is not surprising considering that water's surface tension would reduce its ability to penetrate through sall openings. However, it is clear that these three different ethods for deterining the interface volue are in relatively good agreeent with a value of 6 L. 4.0 INTERFACE VOLUME HELIUM BACKFILL In ost cases, oxygen was found in the RGS gas saples fro the first five tanks tested (Shekarriz, 1996). This oxygen has been attributed to air trapped in the interface volue of the sapler as it was lowered into the tank. If a inial oxygen interaction with the waste is assued, then the original quantity of air introduced into the saple can be calculated based on noral air coposition. This calculation is perfored for the five,tank RGS data in Appendix C (see Table C-2); the resulting trapped air volues generally fall within 1.3 to 4 L (at STP). Even when the saple argon (assued to be purge gas) is added to the air, all but one of the "containation" gas volues (STP) are less than 4 L. It appears that not all of the sapler interface gas was released into the sapler during the sapling process or that soe oxygen reacted with the waste. This subject will be discussed later in greater detail in Section 4.4 and Appendix C. 4.1 Heliu Backfill Technique In order to iniize the proble of RGS containation fro extraneous gases trapped in the interface volue, a heliu backfill technique has been developed. After an RGS sapler has been fabricated, it is placed in a glove box that is evacuated and then backfilled with heliu. The RGS piston is then oved forward to its final position through vacuu grease that seals the heliu into the interface volue. As an extra precaution, the sapler is enclosed in a heretic stainless steel cylinder for shipping, also backfilled with heliu. This provides a double heliu barrier that ensures that the interface volue heliu will not leak out (tested to over 1000 hours of storage tie). Heliu was chosen for the backfill gas because it is inert, inexpensive, and not found in the Hanford waste tanks. When heliu is detected in the RGS sapler gases, it is discarded fro the coposition analysis as a known and quantified containant.

16 4.2 Heliu Backfill Laboratory Verification Testing HNF-SD-WM-CN-092 Page 12 The heliu backfill concept was initially tested by "aging" backfilled saplers and then recovering the interface volue gas to analyze for coposition and quantity. This was done by installing the aged sapler in the Configuration 2 position (see Figure 3). An extra O-ring seal (not shown in Figure 3) was installed over the piston to seal against the interface ring which prevented the interface volue gases fro being lost when the attachent chaber, ain vacuu chaber and reference canister were evacuated. Valve B was then closed to isolate the vacuu chaber(s) fro the pup, and the RGS piston was pulled back so that the RGS ball valve could be closed (siulating taking a saple). After a few inutes, the ball valve was again opened, allowing the interface gases released (by taking the "saple") to flow into the rest of the syste. The piston was again pushed forward to its original position (re-establishing the known syste volue). The pressure and teperature were easured to deterine the quantity of released interface gas; then Valve C was closed and the reference canister reoved so that gas coposition could be deterined with a ass spectroeter. The raw data fro these tests is given in Appendix C, Table C-1. The average quantity of interface gas transferred into the sapler during ball valve operation was 2.64 L, significantly less than the available 6.1 L interface volue. These results also deonstrate that the interface volue heliu can be retained for over 1000 hours when the sapler is stored in a heliu backfilled canister. 4.3 Heliu Backfilled RGS Field Results Developent of the heliu backfill technique for the RGS was not copleted until after testing in the first five tanks was finished. However, heliu backfilled saplers were introduced when RGS sapling was restarted in the next set of Hanford waste tanks (241-U-103, S-106 and BY-109). The coplete results obtained fro the new RGS "three tank" set will be reported elsewhere, but an evaluation of the effectiveness of the heliu backfill saplers is ade here. The raw data for the quantities of heliu and oxygen identified in those saples are given in Appendix C, Table C-4. The heliu backfill (HBF) technique was very effective in replacing interface trapped air and argon with heliu in the three tank RGS saples. The oxygen content of these HBF saplers was greatly reduced, as was the resulting calculated air volue (fro an average of 2.04 L to 0.33 L at STP). These air volues were consistent with the RGSS easured pretest "leak-rate'' extrapolated over the duration of the gas extraction process (see Appendix C, Figure C-1); this iplies that the source of the air in the HBF saplers was probably due to extraction syste leakage or outgassing rather than the sapler interface volue. The cobined air and argon containation gases were reduced fro an average of 2.59 L to 0.37 L (at STP) by the heliu backf i 11 ing technique.

17 HNF-SD-WM-CN-092 Page Oxygen Reaction with RGS Waste The successful effort to validate the heliu backfill technique for RGS saplers also provides the opportunity to copare the "containation" gas volues observed fro several different types of RGS tests. This coparison is useful in aking a qualitative evaluation of the potential oxygen reaction with waste within the RGS sapler. If it can be shown that the oxygenlwaste reaction is inial, then the data fro the first five RGS tanks can be ore easily adjusted to eliinate containation effects fro the sapler interface volue. (Interface volue containation is not expected to be a proble for subsequent RGS saples because of the heliu backfill technique.) In Figure 5, a coparison is ade of the containation volues deterined fro the first "Five Tank" RGS results, the heliu backfill laboratory validation data, and the new heliu backfilled sapler data fro the 241-U-103, S-106 and BY-109 tanks. As used here, the "containation" gas volue refers the quantity of gas believed to be released fro the RGS interface volue into the sapler when its ball valve is operated, and is the su of the quantities of air, argon and heliu found in the saple. There are several points that can be ade fro Figure 5. It is clear that not all of the available interface gas enters the sapler when the valve is closed. Also, it appears that roughly the sae range and scatter is observed for all three types of data, although the "Three Tank" results average about 0.8 L higher than the other two data sets. Since there is no oxygenlwaste interaction possible during the heliu backfill laboratory testing, and this data for the ost part atches the five tank data, it is concluded that oxygenlwaste reaction within the RGS sapler over the lag tie between taking the saple and testing it is inial. This conclusion is further supported by exaining a plot ade by L. A. Mahoney (Shekarriz, 1996) coparing oxygen content with the lag tie. This plot has'been updated and reproduced here for the reader's convenience as Figure 6. The data presented does not support any significant decrease in RGS oxygen concentration versus lag tie. Although elevated tank teperature would enhance oxygenlwaste reaction rates in the RGS sapler, there is no evidence of a significant RGS oxygen level dependence on the "in-tank" hold tie (between when the RGS ball valve is closed to obtain the saple and when the sapler is reoved fro the tank). Data to support this conclusion is provided in Appendix D. 5.0 CONCLUSIONS The RGS sapler interface "trapping volue" deterined experientally for Sapler PR2 was about 6.1 L; this value i s in good agreeent with the calculated value of 6.2 L based on drawing diensions. Sapler-to-sapler interface volue variation is expected to be less than k 0.5 L. Although there is a noinal 6.1 L sapler interface volue which can trap air (and purge gas) as the sapler is lowered through the drill string into the tank waste (or be pre-filled with heliu), not all of this containation gas

18 c, n. 5s 2 o +- all! > s. U * I-I I I I I I I I I I I I I I I I I I I a IiI \D 0 I I I I I I I I I ' 8 d ~ 'I I I I I I I I I I I I I I I I (\I 11 'I, (7") 3WnlOA SVE) NOIlVNIWVlN03 LD al L S.U

19 HNF-SD-WM-CN-092 Page 15 A A-lO1C 0 AN-105C AN-104c Lag Tie (days) Figure 6. RGS Oxygen Concentration Related to Lag Tie. The tie between sapler reoval fro the tank and the beginning of the extraction process is the "lag tie".

20 HNF-SD-WM-CN-092 Page 16 is drawn in with the waste saple; it is concluded that this "draw-in" is alost always less than 4 L. It was shown that the heliu backfill technique iniizes the effects of RGS interface volue containation gases on saple gas coposition analysis. This conclusion is based on laboratory testing of this technique, and on the RGS field results fro Hanford waste tanks 241-U-103, S-106 and BY-109, where he1 iu backfilled saplers were used. The "Five Tank" RGS data given in the preliinary report (Shekarriz, 1996) can be corrected for interface air containation using the easured oxygen concentrations and noral air coposition. This conclusion can be ade because there was no evidence of a significant reaction of entrained oxygen with the saple waste, either during the hold tie before the sapler was reoved fro the tank, or during the lag tie after reoval and before saple extrusion to begin gas extraction. Also, it is concluded that argon found in RGS saples is purge gas containation and should also be excluded. 6.0 REFERENCES A. Skekarriz, et. al., "Preliinary Retained Gas Sapler Measureent Results for Hanford Waste Tanks 241-AW-101, 241-A-101, 241-AN-105, 241-AN-104 and 241-AN-103," PNNL-11450, Deceber M. White, Letter Report, "Retained Gas Sapler Lab Tests," PNNL TWSMI February 6, :090596, 7.0 ACKNOWLEDGEMENTS The author wishes to express his appreciation to L. A. Mahoney for providing Figure 6 which copares RGS oxygen levels with lag tie. Also, a special thanks is offered to E. R. Sicilano for his initiative and effort in copiling field data gleaned fro a variety of sources, including sapling truck logs; this inforation allowed the correlation of in-tank hold ties with RGS oxygen 1 eve1 s.

21 HNF-SD-WM-CN-092 Page A-I APPENDIX A Interface Volue Raw DatalAnalysis The raw data for the tests with heliu described in Section 2.0 are given in Tables A-1 and A-2. TABLE A-1 Date: Test Configuration #I Blank F1,ange V, = L Gas = He1 i u Charge Pressure P1 (KPa) Transducer: 100 T # Cobined Pressure P2 (KPa) Test Teperature 25 OC Calculated Vol. v, (L) Date: V, = L Gas = He1 i u Test Configuration #2 Sapler PR2 (Attached). Transducer: 100 T Test Teperature # OC Charge Pressure Cobined Pressure Calculated Vol. P1 (KPa) P2 (KPa) v, (L) '

22 ~ TABLE HNF-SD-WM-CN-092 Page A-2 Fro Table A-1 the average value of V, = L, with a standard deviation of 0.13 L; for Table A-2 the average value of V, = L with a standard deviation of 0.14 L. Calculation of VI = 6.08 L results fro using Equation '(3) and the above averages (note that V, = 9.48 L). The raw data obtained fro the argon tests described in Section 2.0 are given in Tables A-3 and A-4. I T - Date: Test Configuration #1 Blank Flange A-3 II V, = L Trans.: 1000 T Test Teperature Gas = Argon # 'C Charge Pressure Cobined Pressure Calculated Vol. PI (KPa) P2 (KPa) vb (L) Date: V, = L Trans.: 1000 T Gas = Argon # Test Charge Pressure Cobined Pressure Configuration P1 (KPa) P2 (KPa) # Sapler PR (Attached) Test Teperature 25 'C Calculated Vol. v, (l

23 HNF-SO-WM-CN-092 Page B-1 APPENDIX B INTERFACE VOLUME CALCULATION The interface volue is defined as that volue between the RGS sapler insert "interface" surface and the piston double O-rings; this volue can trap containation gases (see Figures 1 and B-1). The total interface volue was calculated in several steps by deterining individual contributions of several different coponents within the valve housing and suing the. Diensions used in the calculations are based on drawings H (Rev. l), H (Rev. 2) and H (Rev. 0). The annulus volue (V,) is shown in Figure B-1. The actual length of this volue is deterined by how far the insert is screwed into the valve housing; easureents of ten finished saplers showed that about 0.45 inches of the insert reained outside the housing, so that the annulus length is noinally 1.48 inches. The volue can then be calculated as v, = n [R,2 - R,21 L where R, = in., R, = in. and L = 1.48 in. When the calculation is ade, a result of V, = in3 (31.95 L) is obtained. However, the annulus volue is reduced by two "flats" that are achined into the valve housing as shown in Figure 8-2. The area one flat occupies can be calculated by deterining the angle 8 such that cos(8) = x/r = /0.853; thus, 8 = degrees. The volue of one flat is v, = ([-I 28 [nr21 - xy) L, 360 where R = R, = in., x = in., y = in. and L, = in. This leads to VF = in'. The odified annulus volue (V,,) is then v,, = v, - 2 v, so that V,, = in' = L. The annulus volue is filled with three ajor coponents that reduce its volue; these are the Valve Stop, the Rotary Ball Valve and the Viton Seal. The volue of these individual coponents was deterined by weighing five of each coponent, averaging the coponent weight and then coputing the volue fro the known densities of the coponent's aterial. Coponent ass

24 AN N U LU S VO L U M E D E S C R I P TI 0 N k k HNF-SD-UM-CN-092 Page SAMPLER HOUSING VALVE HOUSING I N TE R FAC E < 1 tf q Figure B-1. Detailed Sketch o f Geoetry Producing the Interface Volue.

25 RGS VALVE HOUSING HNF-SD-WM-CN-092 Page 8-3 \ T 1.I 55 k Figure B-2 Siplified Sketch of RGS Valve Housing Showing Ball Valve Mounting F1 ats.

26 HNF-SD-WM-CN-OPE Page 0-4 easureents were ade using a calibrated Sartortus Type 1507 scale, Standards Lab# A suary of these results is given in Table B-1. TABLE 6-1 Coponent Calculation Suary Average Mass (g) Materi a1 Density (g/l) Coponent Volue (L) Viton Seal SST 9.89 p = 7.7 g/l 304 SS 9.22 p = 8.0 g/l Viton 5.59 p = 1.85 g/l The total correction volue due to these coponents listed in Table B-1 adds up to V, = L. The reduced annulus volue (VAJ is thus v,, = v,, - v, giving V,,, = in = 5.89 L. Three inor adjustents for the annulus volue are ade for the volues of the cable piston (V,,), the cable (Vca,,) and the sapler housing sleeve isatch N,,) * When the ball valve is in the open position, about 0.3 inches of each of the two cable piston protrudes into the annulus volue, as well as about 2.5 inches of cable; these two diensions were deterined by direct easureent of one assebly. The diaeter of the cable piston is noinally inches, so that the protruding volue is easily calculated as V, = x in = L. The cable is approxiately inches in diaeter, so that treating the cable as a long cylinder, the resulting volue is Vcab = x in3, or L. The sleeve isatch is the result of the sapler housing insertion into the valve housing falling about inches short as shown in Figure B-1. Fro the diensions given in Figure B-1, V,, = x lo- in = L. The final annulus volue (VAF) is then calculated as

27 HNF-SD-WM-CN-092 Page 6-5 v, = v,, - 2vcp - 2V& + v,, resulting in VAF = 5.52 L. Finally, the gap volue (V,) is calculated for the space between the piston and the insert using the diensions shown in Figure B-1 (and Figure 4). This calculation is perfored in three steps; i) the volue for the inches to the start of the piston taper is x in3 = L, ii) over the inches of piston taper the volue is in3 = L, and over the last inches the volue is x in' = L. Suing these three coponents of the gap volue gives V, = 0.71 L. Since the interface volue is given by then VI = 6.23 L. This value is very consistent with the value of 6.1 l deterined experientally using the ideal gas law. The interface volue is ost sensitive to the distance that the insert is threaded into the valve housing. A inch difference in this distance results in a 0.22 L change in the interface volue, for exaple. One volue that has not been considered as part of the interface volue is the "Bit Volue" (VBrT) which exists between the piston and the drill string bit (see Figure 2) over the 0.8 inch piston extension beyond the sapler interface. If the insert O-ring seals properly in the drill bit, then this volue would potentially trap air and possibly contribute to saple gas containation. This description is coplicated by the fact that soe of the drill bits have press-in pins that ight release soe of this trapped containation gas prior to sapling. Characterizing this potential release echanis would be difficult, and will not be attepted here. However, the bit volue is calculated using an average piston diaeter of inches and the average bit inner diaeter of inches over the 0.8 inch extension. This results in VBIT = in' = 1.45 L. Since this quantity represents significantly ore air than is deterined for the heliu backfilled saples taken fro U-103 and S-106, it is assued that the bit does not hold or trap containation gas. The fact that very little argon was reported for the U-103 and S-106 saples also supports this assuption, since purge gas argon would be expected occasionally as a trapped gas in the bit vol ue.

28 HNF-SD-WM-CN-092 Page C-I APPENDIX C INTERFACE VOLUME GAS TRANSFER DURING SAMPLING The RGS sapler interface volue has been easured at 6.1 L. However, as will be shown, not all of the interface trapped gas is transferred inside the sapler during sapling. C.l Lab Tests A series of laboratory tests were perfored to verify the effectiveness of the heliu backfill technique in eliinating air containation of the RGS saple. These results are given in Table C-1. As can be seen fro the Table, the volues of transferred gas were scattered fro about 2 L to less than 4 L. TABLE C-1 LABORATORY SIMULATION TESTS - HELIUM BACKFILLED SAMPLERS Test # Total STP Volue He1 i urn Aging Tie (L) (XI (hrs) ' AVERAGE STD Saplers were enclosed in He backfilled (and sealed) PVC containers. The PVC glue outgassed organics - these organics are included as part of the heliu when calculating percentage, since they are not due to air in-leakage. The final sapler enclosure canisters will be ade out of stainless steel, so that the outgassing proble will be el iinated. It should be noted that the priary reason for perforing the laboratory tests was to deterine heliu retention versus tie in backfilled saplers. The first ten tests were perfored on heliu backfilled saplers not enclosed in a heliu backfilled canister during aging; the heliu concentration reained above 90 percent only for about three days. For the last three tests, the

29 HNF-SD-WM-CN-092 Page C-2 backfilled saplers were enclosed in heliu backfilled containers during the aging period, and the heliu (plus organics) concentration reained above 90 percent after 42 days. C.2 RGS Trapped Air - First 5 Tanks In Table C-2, the apparent volue of air containation introduced fro the interface volue during RGS sapling in the first five tanks is calculated fro oxygen concentration based on noral air coposition. These calculations assue that a inial aount of oxygen was lost to reaction with the waste; additional evidence supporting this assuption will be discussed later. With the exception of five "flyers" (four low, one high - out of the thirty segents evaluated in Table C-2), the calculated volues of air containation ranged fro 1.3 L to 4 L. The high flyer (AN-l04/10A/17) had ore air (9.47 L) than is possible fro interface volue, and it is assued that soe air in-leakage occurred, either during the sapler hold tie or during the extraction process. Also shown in Table C-2 are the argon volues found in these saples, and in the last colun of the Table, the air and argon volues are added together. Three of the four low "flyers" are "fixed" (brought to within the 2 to 4 L range) when argon is included, suggesting that in soe cases, argon purge gas ay have becoe a significant part of the trapped interface containation gas. Averages and standard deviations were calculated for the volue data in Tables C-1 and C-2, and are suarized in Table C-3. Note that the averages and standard deviations are siilar between the lab test heliu volues and the tank RGS air volues; when tank RGS argon volues are added to the air volues, the agreeent with the lab test data iproves significantly. Again, this result supports the conclusion that soe argon purge gas was often trapped with the RGS interface gases, and included with the saple gases. C.3 RGS Heliu Backfilled Sapler Field Results Valid RGS saples have been obtained fro a second set of three Hanford waste tanks (241-U-103, S-106, and BY-109). Heliu backfilled RGS saplers (described in Section 4.1) were used in all three of these tanks to iniize air entrapent in the interface volue (and subsequently the RGS saple), and will continue to be used in subsequent RGS tanks. A preliinary evaluation of the effectiveness of the heliu backfill saplers is ade here based on the quantities of heliu and oxygen identified in these saples, as given in Table C-4. As can be seen fro Table C-4, the heliu backfill technique was very effective in replacing interface trapped air with heliu. The oxygen content of these saplers was greatly reduced, as was the resulting calculated air volue (fro an average of 2.04 L to 0.33 L at STP). The cobined air and

30 * (Shekarriz, 1996) ' "Flyers" HNF-SD-WM-CN-092 Page C-3

31 HNF-SD-WM-CN-092 Page C-4 Statistic AVERAGE STANDARD DEVIATION Lab Test - Heliu Five Tank Five Tank Cal. Air Ai r+argon (L) (L) (L) argon containation gases were reduced fro an average of 2.59 L to 0.37 L (at STP) by the heliu backfilling technique. The air found in the RGS saples obtained with heliu backfilled saplers ay be due in part to test syste "leakage" during the extraction process. For exaple, at the RGSS axiu allowable pretest easured leak-rate (currently set at polesls) as uch as 0.48 L of air could leak (or outgas) into the syste over a typical two hour test. In Table C-4, the "Calcul. Leakrate Air" colun data is deterined by using the pretest easured leakrate ultiplied by the actual extraction tie (ranging fro 1 to 2 hours) for the particular test. The average leakage volue fro this colun is 0.32 L which copares favorably with the average air volue calculated at 0.33 L (STP). Previously, it has been.assued that the pretest easured leak-rate has been due to ostly outgassing (priarily water vapor) effects, rather than actual in-leakage fro outside the RGS extraction syste, since the leak-rate is reduced with increased pup-down tie. Although the individual test coparisons between saple air and "leakage" air don't correlate in all cases (as can be seen in Figure C-I), the correlation is good enough to suggest that the pretest leakage/outgassing ay contain a significant coponent of air as well as water vapor. C.4 Containation Gas Volue Differences between Five and Three Tank Results The total volue of "containation" gases shown in Table C-4 for heliu backfilled (HBF) saplers range fro 2.5 to 4.5 L, with an average value of 3.42 L; this average is larger than the 2.59 L average result obtained fro the original five tanks using the non-backfilled (NBF) saplers. It has been suggested that the roughly 0.8 L difference' between these averages ight be due to an oxygen reaction with saple waste reducing the apparent air volue calculated for the NBF sapler data. However, exaination of the trapped air (oxygen) dependence on saple hold (and in-tank) ties provides strong evidence that an oxygen/waste reaction was not significant for RGS saples (see Section 4.4).

32 Segent ID U103-R7-S2 U103-R7-S5 U103-R7-S7 U103-R7-S8 S106-R7-S3 S106-R7-S5 S106-R8-S6 S106-R8-S10 BY109-R12C-S4 BY109-RlOB-S5 BY109-RlOB-S6 AVERAGE STD Heliu Argon Oxygen Calcul. Calcul. Air+Argon Total BSTP (PSTP BSTP Air Leakrate Air BSTP Containation (L) (L) (L) (PSTP (L) BSTP (L) (L) Gas BSTP (L)

33 HNF-SD-WM-CN-092 Page C-6 f a 01s-901s 5 2 cc c u 87 v3 o -0 9s-901s E.r > ss-901s ES-9OI.S J E L 9 e p SU? E as+.- + a 3$

34 HNF-SD-UM-CN-092 Page C-7 The increase in the average containation gas observed for the field HBF saplers is probably due to the vacuu grease seal that keeps the heliu in the interface volue. This seal prevents in-tank gases fro diffusing into the interface (and displacing heliu) while the sapler is being lowered into position for sapling; for the NBF saplers used in the original five RGS tanks, tank gas that diffused into the interface volue could not be distinguished fro genuine saple gas, and thus would not be counted as containation gas. Also, the seal ay have affected the aount of gas transferred fro the interface into the saple during.the ball valve operation; as previously noted, not all of the available 6.1 L of interface,gas is transferred during the ball valve operation because of effects that are difficult to quantify. However, neither of these explanations are fully consistent with the HBF sapler laboratory test results which atched the NBF sapler results.

35 HNF-SD-WM-CN-092 Page D-I APPENDIX D IN-TANK HOLD TIME EFFECT ON RGS OXYGEN LEVEL - FIVE TANK DATA As was discussed in Section 4.4, there was no evidence of an oxygenlwaste reaction within the RGS sapler during the lag tie between when the sapler was reoved fro the waste tank and when extrusion of the waste saple was initiated (see Figure 6). However, there reained the possibility that a reaction between oxygen and waste occurred during the in-tank "hold tie" after the saple was obtained by closing the sapler ball valve, but before the sapler was reoved fro the waste tank. During this hold tie, the saple would be at the relatively higher tank teperature; the elevated teperature would generally accelerate an oxygen/waste reaction as copared to the abient teperature conditions that existed during the sapler's storage while awaiting testing. If a significant reaction consued soe of the oxygen during the in-tank hold tie, then copensation of interface air cpntaination for the Five Tank data would be ore coplicated. To investigate the possibility of an in-tank RGS saple oxygen reaction, field data assebled by E. R. Siciliano was exained to extract the length of tie each saple reained in the tank after the saple was obtained. These in-tank hold tie results are copiled in Table D-1; ost of the saplers were left in the tank less than an hour, but a few were left overnight providing a good contrast in hold ties. In Figure 1, the oxygen levels are plotted versus the in-tank hold tie (logarithic scale). The contrast of in-tank holding ties allows a conclusion that the oxygen depletion rate (if any) was low, and not significant for the RGS analysis.

36 HNF-SD-WM-CN-092 Page D-2 Tank/Ri ser Segent In-Tank Seg. Teperature ("C) AW-l01/24A AW-l01/24B Measured 0, In-Tank Coents Tie (u* (hrs) *45 Avg. 0, L STD L A-101/ A-101/ Avg. 0, L STD L

37 HNF-SD-WM-CN-092 Page D-3 I I I I I I I I I I I I 4 51 * o *O * O I I I I I I I I I I I I I I I t I I I 19 I I I I I I

38 To Distribution Project Title/Work Order Retained Gas Sapler Interface Volue DISTRIBUTION SHEET Fro Equipent Developent Laboratory Text Nae With All Attach. J. M. Bates K7-15 R. E. Bauer S7-14 N. S. Cannon (5) L6-38 A. B. Cockrell S7-12 P. R. Deichelbohrer S7-12 D. B. Graves L6-38 B. E. Hey T6-07 J. R. Jewett T6-07 G. D. Johnson S7-14 C. G. Linschooten S7-12 L. A. Mahoney K7-15 A. P. Mouse1 S7-12 K. Napora B1-13 L. R. Pederson K2-44 J. C. Person T6-07 D. R. Rector K7-15 J. S. Schofield S7-12 A. Shekarriz K7-15 E. R. Siciliano HO-3 1 C. W. Stewart K7-15 J. R. Thielges L6-38 Central Files (3) + Orig. A3-88 I Text Only Page 1 of 1 Date Septeber 24, 1997 EDT No ECN No Attach./ EDT/E Appendi CN X OdY Only A (01/93) WEFO67

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