ML20023C950

Control & Monitoring of Fluoride Emissions for Exxon Nuclear Fuel Fabrication Facility. Draft Procedure P69261, Rev 1 to XN-NF-103, Determination of Fluoride as Hf in Environ Filters or Liquid Samples, Encl

ML20023C950
Person / Time
Site:	Framatome ANP Richland
Issue date:	01/31/1983
From:	SIEMENS POWER CORP. (FORMERLY SIEMENS NUCLEAR POWER
To:
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ML20023C948	List: ML20023C947 ML20023C950
References
NUDOCS 8305180648
Download: ML20023C950 (22)

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l CONTROL AND MONI'IORING OF FLUORIDE EMISSIONS FROM THE EXXON NUCLEAR l

FUEL FABRICATION FACILITY 1

EXXON NUCLEAR COMPANY, INC.

RICHLAND, WASHINGEN i

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JANUARY 1983 8305180648 830419 PDR ADOCK 07001257 C

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h fI' CONTROL AND MONI'ICRING OF FLUORIDE EMISSIONS FROM THE EXXON NUCLEAR FUEL FABRICATION FACILITY

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EXXON NUCLEAR COMPANY, INC.

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11 CONTROL AND MONITORING OF FLUORIDE EMISSIONS FROM THE EXXON NUCLEAR FUEL FABRICATION FACILITY DISTRIBUTION DE Clark TL Davis RE Felt LM Finch DJ Hill R Nilson Depart 2nent of Ecology File E.10 i

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INTRODUCTION Exxon Nuclear Company, Inc. has operated a nuclear fuels manu-facturing plant for approximately thirteen years at 2101 Horn' Rapids Road in Richland, Washington subject to regulatory conditions of License Number SNM-1227, issued by the U.S. Nuclear Regulatory Comunission. A recent requirement of that license is to obtain approval of our pro-cedure for monitoring fluoride in stack gases by the state of Washington.

Earlier discussions with members of the Washington State Department of Ecology indicated that such approval would be dependent upon modifica-tion of the sampling procedure to include sample line loss.

This has been accomplished as discussed in this report and approval of the Exxon Nuclear sampling procedure is requested.

As investigation into sampling options progressed, a review of the total environmental monitoring program jor fluoride was conducted including historical data review. This review indicated that fluoride emissions have been low consistently and present no hazards, as confirmed by ambient air and vegetation sampling.

It is our conclusion that a fluoride monitoring program significantly reduced from that currently in place should be adequate. Summary data from the current program is discussed l

and a revised program outliaad. Your concurrence with the revised program is also requested.

l BACKGROUND The nuclear fuels manufacturing process consists of the following basic steps where fluoride release is a potential.

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I.

Hydrolysis of uranium hexafluoride (UF

1. ""Y 6

(UO F ) with a byproduct of hydrofluoric acid (hydrolyzed HF).

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. II.

Precipitation of ammonium diuranate (ADU) and anunonium fluoride by reacting the CO F and HF with anunonium hydroxide.

y2 III. Drying process (where a part.of the ammonium fluoride is~ removed and routed through the process offgas scrubber to the liquid waste chemical storage lagoon system).

IV.

Reduction of ADU to UO via calcining where more of the remaining y

fluoride is removed as NH F.

4 V.

Pelletizing and sintering of UO which removes still more of the 2

remaining fluoride as HF.

Releases of fluoride in the gaseous effluent from the fuels mar.;-

facturing process is controlled with wet scrubber and HEPA filtration systems installed withis the-process facilities. A stack gas sampling program has been used by Exxon Nuclear Ccmpany to monitor fluoride concentrations in the gaseous effluent throughout the operating lifetime of the nuclear fuels manufacturing plant.

An environmental surveillance program is conducted in addition to i

l the stack gas sampling program. The Exxon Nuclear environmental sur-veillance program includes monitoring the fluoride concentrations in the ambient air and vegetation at selected locations north of Richland near i

the fuels manufacturing plant.

l l

Measurements resulting from both the stack gas monitoring and i

j environmental monitoring programs have been consistently well below those standards outlined in WAC 18-48-120 and WAC 18-48-130.

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l

, GASEOUS EFFLUENT MONITORING Releases of fluoride -in the gaseous effluent from the fuels manu-facturing process is controlled with wet scrubber and HEPA filt. ration systems installed within the process facilities. Exxon Nuclear has monitored fluoride concentrations in the gaseous effluent throughout the operating lifetime of the nuclear fuels manufacturing plant. This has been accomplished by continuous isokinetic sampling of gas from each stack with the potential for fluoride emission. Gas is drawn from the stack through a sampling filter at the approximate rate of one cubic foot per minute. Sampling filters are one micron porosity, glass fiber, coated with sodium carbonate and are exchanged on a weekly basis.

Analytical procedures for determining fluoride on the sampling filters are described in Attachment I.

Results of the routine monitoring pro-gram are su=marized in Table I.

The sampling procedure used differs from the approved EPA method because the EPA method does not lend itself to routine continuous sampling of low fluoride concentrations.

It is similar to the procedure approved by the State for monitoring fluoride levels in ambient air breathed by workers.

i l

Discussions were held previously with niembers of the Department of Ecology concerning approval of the Exxon Nuclear monitoring method. At that time it was determined that the method could be approved if the line holdup of fluoride between the sampling head in the stack and the sample collector could be determined. Sampling procedures were modified to allow flushing of the sample lines following the removal of each weekly sample followed by analysis of the sample and the flush solution.

l A series of samples were taken using the revised procedure, and results i

j show that line holdup is less than one percent (Table II).

Based upon these test results indicating essentially no appreciable line holdup, your approval of the Exxon Nuclear stack gas sampling method for fluoride is requested.

(A description of the sampling line flushing apparatus and flushing procedures is presented in Attachment 2.)

1

ENVIRONMENTAL MONITORING In addition to the stack gas sampling program, an environmental surveillance program for areas peripheral to the plant site is con-ducted. The ENC environmental surveillance program includes monitoring the fluoride concentrations in the ambient air and vegetation at selected locations north of Richland near the fuels manufacturing plant (Figure I).

Data from the program show that fluoride concentrations in the ambient air and vegetation have been consistently less than the standards listed in the Washington Air Pollution Regulations, i.e.,

0.5 micrograms fluoride per cubic meter of air in WAC 18-48-130 and 40 parts fluoride per million parts forage in WAC 18-48-120.

Data from the ENC fluoride monitoring program are presented in Table III.

Periodic testing to determine the average atmospheric fluoride source term for the 00 fuel pr duction facility has been performed. A 2

l standard dispersion equation (Pasquill's method with Gifford's con-version

) was used to calculate fluoride concentrations in the plume centerlines from the UO pr cess building exhaust stacks that service 2

the UF ~

e nversi n fa ilities. Results, presented in Table IV, 6

2 l

predict concentrations of fluoride in ambient air well below the regu-latory limits. These data are based on the results of a fluoride source term determination completed in May 1982.

Since fluoride concentrations in and around the nuclear fuels manu-facturing plant have consistently been and are expected to remain less than the Washington Air Pollution Regulations Standards, ENC proposes the followibg program for controlling 'and monitoring fluoride releases:

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Control releases of fluoride in stack gases when necessary, by the use of engineered systems such as wet scrubbers and/or particulate filtration.

2)

Fample gaseous effluents semi-annually from those systems which have significant potential for fluoride release to confirm effec-tive operation of the control systems.

3)

Sample forage monthly within a one mile radius of the plant site durine. the normal growing season (March through October).

Reference 1.

Washington State Industrial Hygiene Laboratory Pro-cedure for Gaseous Fluoride (1974).

2.

" Modern Pollution Centrol Technology, Volume I", Chapter 2 - Estimating Atmospheric Dispersion, Compiled by Research and Education Association, Reprint 1980.

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h TABLE I MONTHLY FLUORIDE RELEASES IN GASEOUS EFFLUENT (grams) i TOTAL ALL STACKS Year Jan Feb Mar

Apr, M

Jun Jul Aug Sep Oct Nov Dec r

1971 6.24 3.85 1.64 2.86 3.07 3.92 2.29 1.27 1972 1.56 1.61 1.87 12.09 9.00 7.65 4.43 6.34 8.70 11.50 10.68 12.64 j

1973 9.81 7.99 18.18 5.22 8.68 3.85 2.62 6.13 9.66 11.83 25.81 32.57 1974 66.48 30.57 28.27 29.40 35.10 23.84 69.36 102.04 84.36 36.28 38.63 46.08 1975 57.42 45.67 10.36 36.94 57.17 59.52 74.07 38.39 36.10 52.23 52.69 22.64 1976 23.06 39.70 21.36 36.23 53.34 57.88 32.72 36.18 43.15 35.38 30.77 34.70 1977 105.48 33.10 28.80 22.37 29.35 8.49 27.39 6.75 4.48 12.78 17.35 3.38 m

1978 19.30 73.54 48.47 241.63 116.93 91.96 84.70 50.89 202.89 237.13 306.43 210.89 8

1979 131.31 217.37 10'.64 206.06 116.41 238.83 254.71 144.55 278.43 98.83 53.79 228.82 1980 329.26 196.25 155.88 331.80 289.11 253.67 303.47 478.41 438.65 229.66 338.24 1981 307.51 244.93 271.33 481.26 884.89 638.84 501.07 589.06 666.50 412.90 1982 879.23 553.60 1318.84 2007.84 894.54 2558.41 2344.26 935.10 2279.75 Out of Service.

. TABLE II TEST RESULTS FOR FLUORIDE HOLDUP IN SAMPLING LINES V

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w Stack No.

K3 K9 K10 K31-K32

-3

-4

-4

-4

-3 Grams F (1) 1.5x10-9.9x10 7.9x10 3.2x10 1.4x10

-4

-3

-4

-3 in Sample (2) 4.3x10,44

-3

-3

.6x10,4 5.5x10,4 1.3x10

.x0 Line (3) 4.8x10 1.6x10 1.7x10 3.1x10 4.3x10

-4

-4

-3

-4

-3 Flush (4) 2.1x10 3.5x10 5.7x10 2.6x10 1.9x10

-4

-4

-1

-4

-2 (5) 2.1x10 1.9x10 2.7x10 2.6x10 1.2x10

-4

-3 (6) 2.4x10 1.4x10

-4

-3 (7) 4.5x10 1.2x10-4 (8) 3.0x10 Grams F (1) 22.5 25.4 0.35 3.4

.71 Dis-(2) 172.

30.4 0.32 39.

.59 charged (3) 172.

2.4 33.

206.

.17 During (4) 44.

71.

76.

100.

.23 Sampling (5) 10.7 734.

16.

78.

8.7 Period (6) 158.

10.5 (7) 81.

4.7 (8) 4.3 l

Fluoride (1)

<.1

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.23

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l Holdup as (2)

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.47

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a Percent (3)

<.1

<.1

<.1

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.25 of Total (4)

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<.1

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.83 Emission (5)

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. TABLE III AVERAGE ANNUAL CONCENTRATION OF FLUORIDE Ambient Air Vegetation (ppm) 3 Ye,ar (ug/m )

Forage Sagebrush 1971

.011 15 20 1972

.023 33 23 1973

.027 29 34 1974

.053 9

6 1975

.019 6

1976

.031 18 1977

.13 32 1978

.42 50*'

1979

.14 59*

1980

.20 31 1981

.15 14 19 1982

.23 25 32 From sagebrush samples located between 1 and 3 miles from the plant.

These results c0mpared with plume modeling data from Table IV, are indicative of a fluoride source other than the ENC plant.

(1) The ambient air sampler employed is a static limed paper tape.

(2) The nearest vegetation used for forage is an alfalfa field approximately one mile east of the ENC fuels manufacturing plant site. This table shows labora-tory analysis results for samples from the alfalfa field as forage and samples of rabbitbrush from the area peripheral to the plant site as sagebrush.

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TABLE IV CALCULATED FLUORIDE CONCENTRATIONS IN EXHAUST PLUME.CENTERLINES (micrograms / cubic meter)

Distance UO Building Exhaust Stacks I

2 (meters)

K3 K9 K10 K31 K32

-8 100 6.55x10~

9.53x10 6 4.81x10 1.26x10 7.05x10

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610 1.46x10 1.84x10~

3.05x10 3.70x10 8.84x10

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-4 1609 4.96x10 5.22x10 8.32x10~

1.16x10~

2.26x10-

~4 3219 1.83x10~

1.85x10 2.93x10 4.22x10 7.88x10~

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~4 4828 1.25x10~

1.26x10~

1.99x10~

2.88x10 5.33x10~

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y E@ NUCLEAR COMPANY,Inc.

ANALYTICAL PROCEDURES stoRMATION ONLY RTTENMWWT 1 TITLE: Determination of Fluoride as HF in DOCUMENT No: XN-NF-103 Environmental Filters or Liquid Samples 2.4.5 DRAFT COPY BY: DJH PROCEDURE NO. P69261 Rev: 1 ISSUE DATE: January 18, 1983 SUPERSEDED ISSUE:

09/04/80 PAGE 1 0F 5 Changes in this revision:

1.

Minor changes in lab methodology and wording.

2.

Modified buffer solutior, used for analysis.

3.

Recertification of technicians not required.

F, k; b bcu? /-9-83 Issued by: M W ' AE k

Manager, Analytical > Labs Date Approved by:

(( ed

'8O Manager, Quality Corgrol

/ Date Approved by:

[M-M

/ P PJ Manager, Richland Plant Date Operations 1-B-22

Ep NUCLEAR COMPANY,ltn ANALYTICAL PROCEDURES MFORMAT!0N ONLY PROCEDURE N0: XN-NF-P69261 REY 1 PAGE 2 0F 5 1.0 SCOPE This method is used to determine the total fluoride as HF collected on filter samples or aqueous solutions used for environmental.or stack moni-toring. Fluorocarbons such as freons are not measured by this procedure.

2.0

SUMMARY

A fluoride specific ion meter is used to determine the fluoride content in aqueous solutions derived from adsorbent filter samples or aqueous solutions. The results are corrected for the airflow and sample duration (if recorded), to determine the fluoride level in air for environmental and stack samples.

3.0 INTERFERENCES Excessive condensed moisture during sampling with treated filters could cause erroneous results due to leaching of soluble fluorides from filter samples. The filters should be examined carefully prior to analysis to assess the possibility of excessive condensation.

The presence of signi-ficant levels of fluoride compounds which are not water-soluble require a fusion step prior to analysis. Altsnintsn and silicon dioxide at levels of about 0.3 g/l in the leach solution will prevent complete recovery of fluoride.

4.0 APPARATUS AND EQUIPMENT 1.

pH/MV meter (specific ion meter).

2.

Combination fluoride electrode or fluoride specific ion electrode and single or double junction reference electrode.

3.

Magnetic stirrer and small stirring bars.

4.

50 ml plastic beakers or equivalent.

5.

Carbonate treated absorbent filters. (Cellulose or glass fiber filter pads or paper strips pretreated with 6% soditsn carbonate solution and dried.)

1-B-23 u. r.ptooni n, tr.n.=itts or e.e ur o' th above iaror= ixm is s 6,=ct so es restration on the first or tette page of to document.

E(ON NUCLEAR COMPANY,Inc.

ANALYTICAL PROCEDURES RFORMATION ONLY PROCEDURE NO:

XN-NF-P69261 REV. 1 PAGE 3 0F 5 5.0 REAGENTS 1.

TISAB solution:

(Total Ionic Strength Adjusting Buffer) 57 ml glacial acetic acid, 58 g Nacl,12 g. Sodiun citrate; dilute to one liter and adjust to pH 5-5.5 with Na0H solution.

2.

Methyl Orange indicator or equivalent.

3.

Sodium carbonate solution - 6% aqueous.

4.

10 N H 504 (Slowly add 278 ml concentrated H SO4 to approxi-2 2

mately 600 ml deionized H O cool, and dilute to one liter).

2 5.

Stock Fluoride solution; 1 g/l F standard.

(Use reagent grade sodium or ammonium fluoride).

6.

Working fluoride standard;.1 g/l F- (1 ml = 100 pg F-).

6.0 REFERENCES

41 FR 52299 (EPA Method 13b); November 29, 1976 EHS-No. F-5-1 Analytical Procedure " Gaseous HF in Air" (HEHF - EHS Laboratory 6-26-75 MK Hamilton) 7.0 PROCEDURE STEPS KEY POINTS & SAFETY CAUTIONS Calibration Curve Preparation:

1.

Pipet 0 - 100 pg of fluoride 1.

O, 1, 10, 50 and 100 99 into labelled plastic beakers are reasonable amounts containing 10 ml of buffer to add.

solution. Dilute to 20 ml with deionized water, add stir bar and mix.

2.

Add one drop of methyl orange 2.

Add acid slowly, stirring indicator and neutralize to a constantly, salmon pink color by dropwise addition of H 504 solution.

2 3.

Setup the electrode and meter as directed in their respective instruction manuals, fill the electrode with the appropriate filling solution.

1-B-24 Uus, suproductaen, trernmettel or dedoeure of the above enformstoon is outsett

I ERON Pd) CLEAR COMPANY,Inc, INFORMATiON ONLY l

ANALYTICAL PROCEDURES PROCEDURE NO: XN-NF-P69261 REV. 1 PAGE 4 0F 5 STEPS KEY POINTS & SAFETY CAUTIONS Calibration Curve Preparation:

4.

Starting with the blank and 4.

Stir constantly during the progressing through the standards measurement.

Carefully from low to high concentration, rinse and blot electrodes record the millivolts for each with lint-free tissue be-solution as read with the tween samples.

Do not electrode.

wipe the electrodes.

5.

Plot the standards as ag F-5.

Plot pg on the log scale.

vs millivolts on 3 or 4 cycle semilog paper.

TREATED FILTER SAMPLES (See Note 1) 6.

Carefully open the sample 6.

Examine the filter for container and remove the distortion, discoloration or filter with clean tweezers.

other signs of damage or excessive moisture.

7.

Place the filter pad in a 7.

Soak for 15 - 30 minutes, clean plastic beaker and add stirring occasionally.

20 ml deionized water.

8.

Pipet from.025 to 10 ml of solution from the filter leach into a clean, labelled plastic beaker bring to 10 ml with DIW, l

and add 10 ml of buffer.

9.

Aod 1 drop methyl orange 9.

The color should change from indicator and neutralize by yellow to pale red.

Stir dropwise addition of 10 N H 50.

constantly and allow the color 2 4 to stabilize before adding additional acid.

10.

If available, Prepare a blank (unused) filter pad in an identical manner.

11. As in Step 4, read and record 11.

Record the volume of sanple the millivolts for each sample.

used.

12 From the calibration curve, determine the 99 fluoride corresponding to each sample.

1-B-25 Oc3, cprWtson, transm ttal or dedewe of the above wiformation is mulNett

ERON NUCLEAR COMPANY,Inc.

ANALYTICAL PROCEDURES INF0RMATl0N ONLY PROCEDURE NO: XN-NF-P69261 REV. 1 FAGE 5 0F 5 STEPS KEY POINTS & SAFETY CAUTIONS LIQUID SAMPLES

13. Measure the volume of the sample submitted.

14. Withdraw a 10 ml aliquot and

14. The sample size may be altered transfer to a 50 ml plastic beaker, if necessary to obtain a reading within the calibration range.

15. Proceed as in Steps 9 through 12.

16. When the measurements are completed, clean up the equipment and leave the meter in standby and electrodes in deionized water.

8.0 CALCULATIONS Environmental Filter Samples:

( t. g F)(.833M

= ppm by volume F as HF in air.

(ml sample)(F3)

• See Note 2 l

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Air Station Sarples:

(u g F)(20 ml) g7 (ml sample used)

Liquid Samples:

l (u g F)

= p m F in solution sample volme in ml Note 1:

Filter samples may be stack monitoring filters or passive sample filter strips (" air station" samples).

The ' Air Station' samples are usually low in fluoride, requiring the maxima sample aliquot for best sensitivity.

(20 ml)[20t g HF'[22.4 t.1 HF}

Note 2:

(.8332) is a conversion factor

=

(19 u g F / \\20 u g HF /

28. 3 1/F i

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n. ir meme., 4.e

.' *. *.... '.--i n i =*, ci to e, re.tret.on on to f rst or trtle paye of to document.

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ATTACHMENT 2 Exxon Nuclear Company (ENC) Maintenance Engineering personnel designed a system, including apparatus and procedural method, for flushing the stack gas sampling lines. Apparatus and method are described below.

f Apparatus:

The apparatus consists of a clear plastic cylinder with caps at each end for filling with deionized water and/or for cleaning.

Tube fittings at each end of the cylinder connect tubing and control valves through which the deionized water flows to the sampling lines and back into sample bottles.

The system of cylinder, tubing and valves is mounted on a portable metal panel with the longitudinal axis of the cylinder oriented vertically with respect to the surface of the earth.

The cylinder is calibrated and marked volumetrically so that the volumes of the various sampling lines will not be exceeded during the flushing process and the volume of deionized water used will be known.

Water pressure for the flushing procedure is provided by connecting a portable pressurized air tank to a flow regulator valve (with pressure gauge) which is part of the tube and valving system.

Equipment and Material Required:

(1)

Flushing Apparatus (1) Portable Compressed Air Tank (100 psi)

(3) One Gallon Plastic Sample Bottles i

(3) Gallons of Deionized Water (1) 7/8" Open End Wrench

~

n

. Procedure:

1.

Verify that the cylinder is vertical and remove the top cap.

2.

' Fill the cylinder with deionized water equal to the volume of the sampling line being flushed.

3.

Reinstall the cap, tighten with fingers only.

4.

Verify that valves V1, V2 and V3 are in the closed position.

5.

Attach the portable compressed air tank to the coupling on the regulator (back side of panel).

6.

Turn V1 valve handle to the open position and adjust the air pressure to 20 psi with the regulator valve (clockwise to increase pressure, counterclockwise to decrease pressure).

If pressure exceeds 20 psi, turn regulator valve handle counter-clockwise, close and reopen V1 valve to release pressure and readjust pressure to 20 psi with the regulator valve.

7.

Use a 7/8" open end wrench to remove the "Y" section from the sampling line.

Connect the flexible hose co=ing from V2 valve to the stack sampling line.

8.

Turn V2 valve handle to the open position and observe the deionized water in the cylinder. Turn the V2 valve handle to the off position when the deionized water decreases to the zero level in the cylinder.

4 9.

Turn V1 valve handle to the closed position.

. 10.

Place the 1/4" flexible' tubing from V3 valve into a sample bottle.

11.

Turn V3 valve handle and V2 valve handle to the open position until all of the flush water is collected.

Turn V2 and V3 valve handles to the off position and remove the flexible tubing from the sample bottle.

12.

Cap the sample bottle and label it with date, stack identi-fication and sample number -- there are ucually three samples collected.

-13.

Repeat steps 1 through 4, 6, and E through 12 for each sample.

14.

Af ter flushing and sa=ple collection are complete, verify that all valves are closed and disconnect the air tank and stack sampling line from the flush apparatus.

15.

Reinstall the "Y" section in the sampling line and resume normal sampling.

16.

Rinse flush apparatus several times with deionized water, especially the tubing sections.

I

a 1

ENCLOSURE 3 f

j KXW $PEUA1AN 4

DOWD W Moos Governor De

~ 5T ATE of WAsti:NGTON -

DEPARTMENT OF ECOLOGY

.g;Q 3b01 Mest Wartungton Manu Washington 96903 (509) 575-2800 e

e April 7, 1983

- _ _ t goo 3

. v ' ct0D'i Charles Malody

-Licensing and Compliance Exxon Nuclear Company,'Inc.

P.O. Box 130 Richland, WA 99352 Re: Air Pollution Monitoring

Dear Mr. Malody:

We have reviewed the fluoride emission test meth3d and monitoring pro-gram data that you have submitted to us.

The fluoride sampling procedure has been found to be satisfactory due to finding negligible sample line losses when sampling was proceeded by a line loss. The sample collec-tion and analysis methods have also been found to be acceptable since these methods have been correlated to the EPA method.

Three fluoride emissions levels are about 1 to 1 of the levels.

500 100 The stack sampling program may be modified to include less frequent sample collection. All stacks with a fluoride emission must have'emis-sions sampled no less frequently than once a month for a 24-hour period.

Those stacks with higher levels of fluoride emissions should be sampled for 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> once per week.

Forage sampling only needs to be done monthly during the normal growing season (irrigation season).

Sincerely, I

WW Alan Newman

[

Environmental Quality Division AN:mjj l

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