ML20137K515

Rev 0 to Trojan Proof of Principle Test Summary

ML20137K515
Person / Time
Site:	Trojan File:Portland General Electric icon.png
Issue date:	03/04/1997
From:	Row C SCIENTIFIC ECOLOGY GROUP, INC.
To:
Shared Package
ML20137K508	List: ML20137K504 ML20137K509 ML20137K515 ML20137K532
References
SEG-TRJ-PRO-030, SEG-TRJ-PRO-030-R00, SEG-TRJ-PRO-30, SEG-TRJ-PRO-30-R, NUDOCS 9704070045
Download: ML20137K515 (18)

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Attachment 2  :

Trojan Proof of Principle Test Summary SEG/rRJ/ PRO-030 March 4,1997 .

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Trojan Nuclear Plant Spent Fuel Pool Debris Project 1

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1234 Columbia Drive SE Richland, WA 99352 Project Quality Project Rev. DCN No. Originator Engineer Assurance hD=^;e- Date o - '

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SC-tWTC ICDLOG' TKAP est TABLE OF CONTENTS Section Page i

1.0 EXE C UTI VE S UMMA R Y . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 l.1 B a c k g ro u n d . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 1.2 Descrip tio n o f Tes tin g . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 Resid u e Hyd rogen Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 1.3 1.4 Con trol o f In tegra ted Tes t . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 2.0 PROOF-OF-PRINCIPLE TESTING AT BEAR CREEK . . . . . . . . . . . . . . . . . . . . . . . . 6 2.1 Test Objectives and Results . . . . ...................... ............... 6 l 2.2 Ru n # 1 G a s An alys is . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 2.3 R u n #2 G a s An a lys is . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 ,

R u n #3 G as An alysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8 2.4 Da ta Q uality Objectives . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8 2.5 3.0 RESIDUE TESTING AT A COMMERCIAL ANALYTICAL LABORATORY . . . . 12 1

A n alytical A pp a ra t us . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12 3.1 ,

Ca li b ra tio n H 12  ;

3.2 2 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

S a m ple B la n k . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12 i 3.3 T rip B la n k . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12 3.4  ;

3.5 Hydrogen Quantitation Via Spiked Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13  ;

3.6 Hydrogen Quantitation Via Matrix Spike . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13 3.7 R u n # 1 Res id u e S a m ple . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13 3.8 R u n #2 Res id u e S a m pic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14 3.9 Ru n #2 Resid ue Replicate Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14 j Ru n #3 Resid u e S a mple . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14 3.10 14 I 3.11 Residue Hydrogen Content Computation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

15

4.0 CONCLUSION

S AND RECOMMENDATIONS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

4.1 Operational and Design Recommendations . . . . . . . . . . . . . . . . . . . . 16 4.2 Residual Hydrogen and End of Run Determinations . . . . . . . . . . . . . 16 16 5 . 0 A C R O N YM S . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

17 6.0 RE F E RE N C ES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

FIGURES FIGURE 1: TEST RESULTS . . . . ...... .... ............. .......... 17

.' ABLES TABLE 3.1: RESIDUE HYDROGEN, Hi , CONTENT . . . . . . . . . . . . . . . . . . . . 14 REV.O TR.fPRD iM -

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SEG/TRJ/ PRO-030, Trojan Proof of Principle Test Summary @ @ @j m.~ c m .. ~ .<

l.0 EXECUTIVE SUM 31ARY This test report consists of four main sections; -

Section 1.0: An executive summary of the Proof-of-Principle Testing l

Section 2.0: Operational results from the testing conducted on the full-scale steam-  :

reformer using a prototype can feed evaporator (CFE)

Section 3.0: Results from residue testing completed at a commercial labo atory  ;

i Section 4.0: Conclusions and recommendations for conducting the Integrated Test j l

1.1 Background

The purpose of the Trojan project is to clean up contaminated canisters located in the fuel pool rack, and produce a concentrated residue with a low hydrogen (H )2 content so that formation of radiolytic hydrogen in long-term storage casks is below 5 volume percent (vol %) of the container void space. This is a very restrictive limitation and translates to about 250 milligrams H 2in a treated process can capsule.

The fuel pool canisters contain deteriorated cylindrical sock and cartridge filters loaded with clay sediment, metallic electro-dielectric machining material, and other organics contaminated with failed fuel element fines and fuel pellets. The operation involves remote handling procedures for the recovery of this waste and the loading of steam-reforming process cans that will be inserted into the CFE. The waste will be thermally processed in the CFE, organic off-gases are further processed into syn-gas in the steam-reformer (Galloway,1996).

There are three major phases in this project:

• The Proof-of-Principle (POP) Test was completed at SEG's Bear Creek Facility ,

in Oak Ridge, TN, in the commercial steam-reformer. The objective of this test  :

was to verify the ability of steam reforming to achieve the requisite low {

hydrogen content in the final residue. .

• The Integrated Test will be conducted at the Washington Public Power Supply l System (WPPSS) Nuclear Plant #1. During this test the can feeder / steam-  !

reformer system will be integrated and demonstrated with full remote handling l

equipment.

• The actual processing of the Trojan Nuclear Power Plant debris.

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1.2 Description of Testing j The POP Test runs were conducted in accordance-with the Trojan Proof of Principle  ;

Test Plan (SEG/TRJ/R-001), the Trojan Proof of Principle Test Procedure l (SEG/TRJ/ PRO 005), and the Residue Hydrogen Analysis Protocol (SEG/TRJ/ PRO- l 006).

In the POP Test three runs were conducted, surrogate waste was processed at increasing increments in residence time and temperature. The median residence time and temperature proved to be optimum treatment conditions, resulting in a hydrogen  ;

content analysis for the residue of 25 milligrams in the process can. Based on these i findings, the residue and five process cans could be placed into the final process can .

capsule and still be less than the specified hydrogen limit. l The residue handling procedures used during the POP Test were designed to minimize i any potential contamination by room moisture, a component in the formation of radiolytic hydrogen. For example, when operators removed the residue samples from  ;

i the can feed evaporator, they had to unload the process can within an inerted tent while wearing self<ontained breathing apparatus. To quantify the residual moisture picked up during residue removal operation, trip blank samples were used.

1.3 Residue Hydrogen Analysis  ;

The residue H2 analysis performed at a commercial analytical laboratory (hereafter t referred to as "the lab") provided a unique challenge of maintaining very low H2 and H 2O background levels in the glove box, analytical instrumentation, sample bags, etc. -

A graphical display of the test results is shown in Figure 1. The top curve labeled ,

" Blank Spike" involved the ad " ion of a known hydrogen content in the process can.

Thus, this top curve reflects the maximum acceptable hydrogen content.  ;

Figure I also shows the residue hydrogen content of the waste stream after steam-  !

reforming for Runs #1, #2, and #3. Run #1 had the shortest residence time and the  ;

lowest temperature, and Run #3 the highest residence time and the highest temperature.

The almost horizontal curve, the " Trip Blank Sample" with chemisorbed and adsorbed water, verifies handling procedures were successful in minimizing H2 contamination of the test samples. The amount of moisture in the Trip Bbnk was 20 parts per million r

(ppm) H 2averaged over a gas evolution time of 50 minutes, equivalent to 1.6 micro-g-moles of H 2. r i

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e.%. . u . -1 SEG/TRJ/ PRO-030, Trojan Proof of Principle Test Summary {g 1.4 Control ofIntegrated Test Gas measured during Run #3 showed H2 production from the surrogate waste dropped from 15,000 ppm to 1000 ppm. Based on this information our process procedures provide an excellent opportunity for determining the appropriate end of each run. It is  ;

I recommended that this sampling approach be used for the integrated test. In addition, the temperature conditions used in Run #2 are recommended for the Integrated Test.

2.0 PROOF-OF-PRINCIPLE TESTING AT BEAR CREEK The POP Test was conducted in accordance with the Trojan Proof of Principle Test Plan l l

(SEG/TRJ/R-001). This section discusses the overall test objectives and results, the residual hydrogen and gas sample results for each run, and provides comments on achieving the data quality )

objectives. I i

2.1 Test Objectives and Results There were four objectives for the POP Test. Each of the objectives and comments ]

achievement are listed below:

2.1.1 Prove that the steam reformer can reduce organic filters and dross to less than 0.050 gram-moles (g-moles) elemental hydrogen per process can.

Results: All three test runs successfully met established hydrogen limits therefore, -

the steam reformer can reduce organic filters and dross to less than 0.050 g-moles elemental hydrogen per process can.

2.1.2 Evaluate the effectiveness of the seal between the bottom of the process can and the inlet of the CFE.

Results: Throughout the testing, the flow rate of steam to the process can remained I relatively steady. This indicates that the bottom process can seal successfully channeled the steam flow without excessive bypassing.

2.1.3 Determine if the filters in the process can are subject to plugging, evaluate the ability l of flow sensors to detect process can filter plugging, and determine the ability to i recoverif filter plugging occurs. l Results: During each test, the flow rate of steam to the process can remained relatively constant, indicating that the process can filters were not subject ,

to plugging. In all three runs, process can steam flow rates declined less than 7% over the first 12 hrs of processing. During Run #3, process can steam flow was reduced 33%, as the dross in the residue fused into a solid mass. partially blocking the process can bottom filter. An attempt to back REV 0 TRJ PRD t435 -

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SEG/TRJ/ PRO-030, Trojan Proof of Principle Test Sununary h_,.gM.

P llush resulted in an additional .fjowlo.m t#~12%. Apparently, back flushing forces the waste against the pracestcan battom filter.

2.1.4 Determine the optimunrpacestunriiTms's fwsteam reformer operation to ensure each process batch meets the hydrogen specification:

a. Determine the time, process temperature, and flow rate required to successfully reform a process can full of organic filters and dross.

Results: Using the times and temperatures in Runs #1, #2, and #3 and considering steam flow control problems, this tests objective could not be adequately determined. However, based on the data collected, the operating parameters in Run #2 will be used as a starting point for the Integrated Test.

b. Determine the maximum steam flow rate through the process can that does not cause plugging of the upper filter.

Results: Process can steam flow rates reached a sustained maximum of 4.8 scfm with peaks as high as 5.4 scfm, no evidence of plugging of the upper filter occurred.

c. Determine how the presence of carbon monoxide (CO) in the steam reformer vent relates to hydrogen concentration.

Results: The on-line gas analyzers were non-functional during most of the testing. Tedlar bag samples indicated CO belr,w detectable levels. However, H 2and carbon dioxide (CO2 )

were directly correlated. Since oxygen (O 2) levels generally were above 6%, it is probable that the CO was converted to CO2 -

2.2 Run #1 Gas Analysis Run #1 had the lowest temperature and the shortest processing time. The gas evolution was monitored carefully by gas chromatograph (GC) to detect any H2 evolution as temperature increased. Thi resulting data suggest that the dips in 02 correspond with the production of CO 2and H ,2 Providing validation of the reaction mechanism. The increased temperature resulted in added H production from the reduction of carbon.

2.3 Run #2 Gas Analysis Run #2 was designed to be of moderate intensity in terms of temperature and processing time. The gas composition analyzed by the GC, revealed additional H evolution as the temperature increased. 02 measured by the GC steadily dropped during the course of the run. CO production 2

resulted from the reaction ofleaked oxygen with CO that was co-TpJPRD1-(M REV O Page 6 ef 17

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produced with the H2 during steam-reforming. The data suggest that the dips in 0:  ;

correspond with the production of CO2 and H 2, again validating the reaction mechamsm.

)

The higher temperature provided evidence that an increased temperature produced more H and CO, even after steam-reforming of most organic hydrogen had been completed. At the j higher temperature, the steam reacts with the remaining carbon char to form H: and CO. 1 The computed quant}ty of H2 produced, was 2.5 g-moles H2 . This is an order of magnitude greater that the volume of H2 generated from the waste, after the initial H2 Peak. Thus, the H2levels generated from the waste, capable ofindicating process completion, could not be detected.

2.4 - Run #3 Gas Analysis Run #3 was designed to be of maximum intensity in terms of temperature and processing time. Because of the high temperatures used in this run, the metal dross in the surrogate waste fused together, creating a solid mass. This blockage inhibited steam movement and  !

reaction with the organics. As a result, the reaction rates were much slower than Run #1 or #2 Also the H2 Peaked at a lower level as compared with the peak in Run #2, indicating a slower rate. -

The curves of O2 , H 2, and CO2sampled correlate well for the last 30 hours3.472222e-4 days <br />0.00833 hours <br />4.960317e-5 weeks <br />1.1415e-5 months <br /> of the run, l suggesting that the steam-carbon reaction was producing 2H from the steam supply. At the end of the run when the steam flow was stopped and the cooling was initiated, additional gas samples were taken to check for additional H2 evolution, none was detected. l 2.5 Data Quality Obje:tives )

l The data quality objectives, as listed in the Test Plan (SEG/fRJ/R-001), are provided below with comments on the success achieved during testing:

2.5.1 Measure the weight of the process can upper filter assembly before and after processing to determine how much, if any, of the residue has been captured in the filter.

Results: De mass ofresidue captured in the filter varied between <1 grams (g ) and 7 g.

2.5.2 Measure the weight of the surrogate waste filters, sufficient filter material should be selected and used to obtain a weight of 0.96 kilograms (kg) 57 g.

Results: For each run, seven filters were used as surrogate waste, filling the process can to capacity. The total mass of the filters in each run ranged between 1007.6 and 1010.6 g.

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• Color., che ac 2.5.3 Measure the weight of the surrogate waste dross load, sufficient dross will be used to obtain a weight of 3.71 kg 85 g.

Results: Actual surrogate dross load in eaci run rariged between 3.635 and 3.704 kg.

2.5.4 The weight of the residue remaining after each test run is anticipated to consist of the dross, plus a few ounces of processed filter residue.

Results: Actual residue weights ranged between 3.685 and 3.778 kg.

2.5.5 Steam temperature entering the lower inlet of the process can should meet previou tly determined specifications.

Results: Throughout Runs #1, #2, and the first 29 hours3.356481e-4 days <br />0.00806 hours <br />4.794974e-5 weeks <br />1.10345e-5 months <br /> of Run #3, stear.1 temperatures were not able to reach specified criteria. Lack of sufficient heat tracing, two orifices in series, and two piping transitions caused excessive heat loss. As steam flow into the process can slowed the temperature decreased. This was especially evident during the latter stages of Run #3.

2.5.6 Steam temperature in the CFE chamber should reach previously determined specifications.

Results: The highest steam chamber temperature achieved during Run #1, Run #2, Run #3 was not able to reach specified limits. Additional insulation was added to the can feed evaporator prior to Run #2, and hot syn-gas was introduced into the drum feed evaporator (DFE) during Run #3 to apply additional heat to the can feed evaporator. Each modification increase the steam chamber temperature.

2.5.7 Syn-gas temperature, exiting the process can, should reach previously determined specifications.

Results: Due to excessive heat loss and improper placement of the thermocouple, exit temperatures were not able to reach specified limits.

2.5.8 Steam pressure entering the bottom of the process can should meet previous specified criteria during operation.

Results: Steam pressure entering the process can exceeded planned values; pressure in the CFE was raised above atmosphere pressure in an effort to minimize oxygen leakage into DFE.

2.5.9 Steam pressure in the CFE chamber should be maintained within previously specified limits when steam is applied, and must remain negative at all times during processing.

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Results: Pressure in the steam chamber exceeded specified pressure, dependent on i flow rate and downstream pressures. A one inch restriction in the piping plus several tight radius elbows,- between the detector and the steam chamber, caused a significant pressure change. In addition, the CFE was l operated at a slight positive pressures to reduce oxygen leakage into the DFE.

2.5.10 Exit chamber pressure in the CFE should range between -7 and -12 inches water column (in. w.c.), and must remain negative during processing.

Results: Because of excessive oxygen leakage into the CFE, when attempting to operate the system at a negative pressure, the system ran at a i positive pressure most of the time. When leakage was minimized, it was possible to obtain a negative pressure.

i 2.5.11 Steam flow rate entering the bottom of the process can should range between previously specified limits. Steam flow less than the specified limits indicates a l l

plugged process can upper filter.

Results: During Run #1 process can steam flow slightly exceeded specified limits. Although 7 g of residue were imbedded in the process can upper filter after the run, flow was not restricted. During Run #2 process can steam flow wasjust above specified limits, with less than I g of residue imbedded in the process can upper filter after the run.

During Ruri #3 process can steam flow was above specified limits,  ;

with less then 1 g of residue imbedded in the process can upper filter after the run. These results indicate that the upper filter is not plugging even after extended operation. Reduced flow in Run #3 was presumed to be caused by blockage of the bottom filter.

2.5.12 Temperature of the superheater outlet should be within specifica limits.

Results: With preheated steam entering the superheater, temperatures exceeding specified limits were achieved at the outlet. The superheater was operated at an increased temperature to make up for excessive heat loss in the down stream piping.

2.5.13 Steam pressure at the superheater outlet should be within specified limits.

Results: During Runs #1 and #2, superheater outlet pressure, was maintained within specified limits. In order to achieve higher processing temperatures during Run #3, steam flow was increased by raising superheater outlet pressure above specified limits.

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2.5.14 CO.should range from.zmo at the 3stan-of processing to a peak value during processing, and back tazero.auheerid ofprxessing. The curve should correlate with the measured H,muwe -

Results: Durig the POP Test, the gas analyzers system was not functional, preventing CO readings. The gas chromatograph analysis measured

. CO below minimum detection levels (MDL) throughout testing.

Excessive oxygen present in the DFE converted CO to CO2 , which correlated with the H2 content.

2.5.15 O at the SSR vent should be within a specified range, and should always re mein 2

below the upper limit of the range.

Results: Tedlar bag samples from the CFE outlet were measured above the specified range. The DFE had excessive oxygen leaks.

2.5.16 Syn-gas, sampled at the CFE outlet, will be analyzed for H2 , CO, CO2 by GC.

Concentrations should range from zero at the start of processing to a peak value and back to zero at the end of processing in parallel curves. H2 should have the largest peak value with CO and CO2 peak values below that of H 2-Results: The Tedlar bag sampling results did not indicate peak and tailing off curves as expected. Most likely the peak occurred early in the processing and passed too rapidly to be sampled. The Integrated Tests will include additional sampling to determine the best way to sample and measure gas levels.

2.5.17 Syn-gas analysis for O 2 sampled at DFE outlet should be within specified limits.

Results: DFE outlet samples for 02were measured in excess of the specified limits. Filter inlet samples indicated 02 levels within specified limits due to the dilution caused by the carrier gas, 2.5.18 Residual elemental hydrogen in process can residue must be <0.05 g-mole or

<0.05 g total hydrogen content.

Results: Residual hydrogen content analysis results for all three runs met the criteria.

Run 1 0.0376 g-moles H Run 2 0.0260 g moles H Run 2 0.0267 g-moles H (duplicate analysis)

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3.0 RESIDUE TESTING AT A COh!31ERCIAL ANALYTICAL LABORATORY Residue testing at the lab involved three test runs plus several blank and duplicate tests for quality assurance. The following sections describe each of the runs and results. More detailed descriptions are provided in the labs Final Work Plan and Quality Assurance Project Plan.

3.1 Analytical Apparatus The analytical H 2apparatus was contained inside an inerted glove box. The sample handling and treatment was established in SEG/TRJ/R-002.

3.2 Calibration H:

A five point calibration of the apparatus was performed in accordance with the Final Work Plan and Quality Assurance Plan. Just prior to and following every run, a single point verification was performed.

l 3.3 Sample Blank Just prior to processing the sample blank a background curve was obtained for H2 . The l

data scatter was less than 1.5 ppm.

l The background curve for H 2provides the best estimate of the background that must ise subtracted from each sample. The experimental uncertainty in establishing this curve was estimated as *0.014 millimoles Hi with a 90% certainty.

The background curve should be subtracted from the H2 profile for each residue sample.

Thus, a more conservative approach was adopted resulting in the highest possible H2 content being used.

3.4 Trip Blank At the lab, the trip blank was loaded into the H 2apparatus. Just before the sample processing began, a background curve was obtained for H2 . A decay rate and data i scatter of 1.5 ppm was observed.

Once the background curve was determined the H: apparatus was opened and the sample inserted. As the trip blank processed, the H 20, H , and other gas evolutions increased.

The tail end of the curve leveled out 20% higher than the original background, indicating a background shift.

The gas sample bag, collecting gases produced from the analytical H2 apparatus, was thoroughly mixed, and the contents sampled every 15 minute to determine an average H:

concentration. Using these values the H: concentration was determined to be 0.0099 g-mole H, in the trip blank.

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3.5 Hydrogen Quantitation Via Spiked Sample This section verifies the H, apparatus can quantitatively simulate the total hydrogen production expected from the long-term radiolysis in the repository.

A spike, was selected to simulate the residue remaining after steam-reforming based on it's availability as a . certified analytical reagent, known hydrogen content, and the material similarity to partially steam-reformed substances. The quantity used was calculated so the H2 evolved would be at the critical level of 0.05 g-moles H i.

The concentration of H 2generated from the first run of the spike was measured at 510 ppm, with a background level of 150 ppm,72% of the hydrogen in the spike was recovered.

The concentration of H 2generated from the duplicate run of the spike was measured at 654 ppm,146% of the hydrogen in the spike was recovered (without moisture correction) and 107% after moisture correction, with no blank / trip correction.

For both runs the curve for H evolution was comparable to the actual residue sample; thus, it is concluded that the spike is a good sunogate for validating and quantifying H 2 recovery. [

3.6 Hydrogen Quantitation Via Matrix Spike ,

The matrix spike run was performed to ensure that the presence of waste matrix did not ,

adversely affect the H2 recovery. The method involved placing a spike under a sample of actual residue from Run #2, so the gases evolved from the spike had to diffuse

. through the residue. If there were any diffusion, hydrate formation, or readsorption this test would identify them.

The results for the spike in the matrix compares almost exactly to the spike alone. The matrix spike curve should have been the sum of the spike samples and the Run #2 sample. The actual recovery was only 74.6% of the expected results.

The 72% recovery of the blank spike and the 74.6% recovery of the matrix spike indicate that measured H, values should be corrected for a 28% loss rate.  ;

3.7 Run #1 Residue Sample  !

Approximately 16 grams of residue was taken from vial #1 from. After 300 min, the H level was at a relatively steady value of 228 ppm, the run was stopped. The gas sample bag measured 389 ppm, subtracting the background 91 ppm, the result is 298 ppm, or 0.0376 g-mole Hi . In addition, the correction factor of 0.0099 g-moles Hi for sample handling should be subtracted.

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3.8 Run #2 F ,idue Sample Approximately 16 grams of residue was taken from vial #2 from Run #2. After 193 min, the H: level was below the background and the run stopped. The gas sample bag measured 334 ppm, subtracting the background of 160 ppm, the result is 174 ppm, or 0.0121 g-mole Hi . As determined in Section 3.4, the correction value for sample handling is 0.0099 g-moles K.

3.9 Run #2 Residue Replicate Sample The residue was taken from vial #1 from Run #2, approximately 15g was analyzed.

After 216 min the H 2level was changing at a rate of <0.2 ppm per minute and the mn was stopped, ne gas sample bag measured 388 ppm. Subtracting the background at an average value of 67 ppm, the results were 321 ppm, or 0.0267 g-mole Hi . As determined in Section 3.4, the correction value for sample handling is 0.0099 g-moles i H i. He results of the Run #2 Sample and the Run #2 replicate showed reasonably good repeatability. The replicate run was biasly sampled to contain more organic char, and therefore, produced a higher H2 content.

3.10 Run #3 Residue Sample The residue was taken from vial #1 from Run #3, approximately 13g was analyzed.

After 521 min, the H level 2

was at 161.5 ppm, and changing about 0.2 ppm / min so the run was stopped. The gas sample bag measured 294.1 ppm. Subtracting the background at an average value of 131 ppm, the results were 163.1 ppm, or 0.0237 g-mole iH . As determined in Section 3.4, the correction value for sample handling is 0.0099 g-moles Hi 3.11 Residue Hydrogen Content Computation The H 2concentration remaining in the residue after the waste sample was steam-reformed was calculated from the mass of the residue taken out of the process can, the measured H2 level collected in the gas bag, the volume of gas mixture in the gas bag, the density of the gas in the sample bag, the mass of the residue sample placed into the H2 apparatus, and the molecular weight of atomic hydrogen, Hi . The equation used for calculation purposes is as follows:

T10 PRD-tm REV 0 Page 13 of 17

~ .. .

SEG/TRJiPRO-030, Trojan Proof of Principle Test Summary lIN,an@seaw se g-moles H, = 2-(c residueg,MH in bag. nom-L :g 13,,1-(Bag Vol. L 3 ,,1 fo. gH:1g,)

in residue lx10*-(2.01594 gH:/g-moleH,)-(g sample) where: L = liters of gas, and p = gas density calculated by: p = P Mw/R T(typically around 0.083 gH:/Lm) where: P = 1 atmosphere (with small correction for 1100 ft altitude)

Mw = molecular weight of H2= 2.01594 R = Universal Gas Constant = 0.08205 L atmos /g-mole "K T = Gas Bag Absolute Temperatiire K. (approximately 294.82"K)

NOTE: Normally g-moles of hydrogen are reported in g-moles H2; however, NRC requires that it be reported in g-moles Hi . Accordingly, there are two g-moles of Hi in one g-mole of H 2-g-moles Hi = 2 g-moles H 2-A summary of the calculated elemental hydrogen, H , results for each run is presented in Table 1.

TABLE 1 RESIDUE HYDROGEN, H,, CONTENT RUN# Sample Mass Residue stuckin CFE Residue in CFE Uncorrected Corrected (g) (% estimate) (g) ,

H, Content  : H, Content (g-moles) (g-moles) ~_

3680.85 0.10 3684.53 0.0376 0.0382 1

3703.14 1.00 3740.17 0.0121 0.0056 2

1.00 3740.17 0.0267 0.0243 2 rep. 3703.14 5.96 3777.68 0.0237 0.0204 3 3565.19 trip blank 6.821 -- --- 0.0099* ---

Spike correction +28% --

• This content was calculated from the measured content of 0.84 g-moles H2 then normalized to a typical total re<idue sample size of 3600 g.

4.0 CONCLUSION

S AND RECOMMENDATIONS This section analyzes the Bear Creek " Proof of-Principle" test runs as well as the residue hydrogen content detenninations and makes suggestions for improving the performance of the integrated test.

REV 0 TRJPRD1At Page 14 of 17

SEG/TRJ/ PRO-030, Trojan Proof of Principle Test Summary @@@@

m < ,m. m, <

4.1 Operational and Design Recommendations Throughout all test runs, the process can upper filter assembly showed no signs of plugging. One attempt at back flushing during Run #3 actually reduced flow by compacting the metal dross against the lower filter. Therefore, the design of the Trojan CFE was simplified by removing the back flush piping and valves.

The process can/CFE bottom seal performed adequately ensuring that steam flow directed to the process can interior did not bypass around the process can through the steam chamber. The design of the CFE and associated piping and access gates has been

. reviewed to minimize oxygen leaks. To provide a more direct reading of hydrogen content in the syn gt.s, a hydrogen gas analyzer has replaced the CO2 analyzer.

Difficulties in obtaining expected operating temperatures and pressures during the POP Test dictated that the Trojan CFE be designed with shorter pipe runs and fewer restrictions to minimize pressure loss and a maximum ofinsulation and heat tracing to minimize heat loss. Plans have been made to install the stear. superheater directly on the outside of the CFE shielding and to add heat tracing to the CFE shell. In addition, the CFE exit thermocouple will be moved to a higher location.

4.2 Residual Hydrogen and End of Run Determinations The test results are best summarized by concluding that Run #1 was barely long enough in residence time and high enough in temperature to reach the required H2 content with an adequate margin of safety. Rtm #2 was acceptable in temperature, but probably could have been shorter, since the H production from the steam-carbon reaction confused the end of-run criterion. Run #3 was too hot and too long, causing the stainless steel dross filings in the surrogate waste to fuse together, slowing the reaction and blocking flow.

Gas samples measured during the end portion of Run #3 showed no detectable H2 -

H 2production from the surrogate waste could have been monitored dtuing processing.

5.0 ACRONYMS CFE Can Feed Evaporator CO Carbon Monoxide i Carbon Dioxide DFE dntm feed evaporator g gam (s) g-mole gram mole REV U TRJ.PRD 145 Page 15 of 17

SEG/TRJ/ PRO-030, Trojan Proof of Principle Test Summary lEMM@  !

GC gas chromatograph ,

H, Hydrogen in its normal state ,

in. w.c. inches water column kg kilogram (s)

(

MDL minimum det'ection level ,

O2 Oxygen ppm parts per million POP Proof-of-Principle ,

vol % volume percent WPPSS Washington Public Power Supply System.

i

6.0 REFERENCES

l 6.1 T. R. Galloway, D. F. Gagel, & N. W. Dunaway, Recent Erperience With SEGSteam-Reforming Of Various Types ofRadwaste, invited paper for Winter AIChE Meeting e in San Francisco, CA Nov. 10-15,1996.

6.2 SEG Procedure Trojan Proofoffrinciple Test Plan, SEG/TRJ/R-001, Rev 1, Sep 19, l 1996.

6.3 SEG Procedure Trojan ProofofPrinciple Test Procedure, SEGTTR11 PRO-005, Rev 1, Sep X,1996.

6.4 SEG Procedure Residue Hydrogen Analysis Protocol, SEGTTR1/ PRO-006, Rev 0, ,

Sep 3,1996. l i

'l f

l TRJ.PRD 1.ng REV.O Page 16 of 17 i

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SEG/TRJ/ PRO-030, Trej:n Proof cf Principle Test Summ ;ry [

t Hydrogen Analysis Proflies m

ene 3eo-

$g O 3000 -+-Run 82 Sample 9/27!96

-u-Run 83 Sample 10/1/96 g

o u. -

-*-Run 81 Sample 10/2/96

-*- , Blank Spike 9/30/96 MRun #2 Dup Semple 10/3/96 8 88 -

j'

+ Trip Blank Sample 10/4/96 i.

imo .

. =

mver" --  := = =+e

=

Mph..sntIItaltsth e so im ino m-m a m Run Time (min.)

FIGURE 1: TEST RESULTS TR3 PkD-145 P ge 17 of 17

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