W: Total weight of mercury collected, μg. VI Total volume of condensed moisture and ICI in sample bottle, ml.

CI Concentration of mercury measured in sample bottle, μg/ml.

V Total volume of ICI used in sampling (impinger contents and all wash amounts), ml.

Co Blank concentration of mercury in ICI solution, μg/ml.

6.7 Total mercury emission.-Calculate the total amount of mercury emitted from each stack per day by equation 102-8. This equation is applicable for continuous operations. For cyclic operations, use only the time per day each stack is in operation. The total mercury emissions from a source will be the summation of results from all stacks.

100 V total

I=

An(s) avg.

eq. 102-9

where:

Vtotal

I=Percent of isokinetic sampling. Total volume of gas sample (stack conditions), ft3.

Probe tip area, ft2.

Sampling time, sec.

(r.) av.

Average stack gas velocity, feet per second.

7. Evaluation of results.-7.1 Determination of compliance.-7.1.1 Each performance test shall consist of three repititions of the applicable test method. For the purpose of determining compliance with an applicable national emission standard, the average of results of all repetitions shall apply.

7.2 Acceptable isokinetic results.-7.2.1 The following range sets the limit on acceptable isokinetic sampling results: If 90% 110%, the results are acceptable; otherwise, reject the test and repeat.

8. References.-1. Addendum to Specifications for Incinerator Testing at Federal Facilities, PHS, NCAPC, Dec. 6, 1967.

2. Determining Dust Concentration in a Gas Stream, ASME Performance Test Code No. 27, New York, N.Y., 1957.

3. Devorkin, Howard, et al., Air Pollution Source Testing Manual, Air Pollution Control District, Los Angeles, Calif., Nov. 1963.

4. Hatch, W. R. and W. L. Ott, "Determination of Sub-Microgram Quantities of Mercury by Atomic Absorption Spectrophotometry." Anal. Chem., 40: 2085-87, 1968.

5. Mark, L. S., Mechanical Engineers' Handbook, McGraw-Hill Book Co., Inc., New York, N.Y., 1951.

6. Martin, Robert M., Construction Details of Isokinetic Source Sampling Equipment, Environmental Protection Agency, APTD

0581.

7. Methods for Determination of Velocity, Volume, Dust and Mist Content of Gases, Western Precipitation Division of Joy Manufacturing Co., Los Angeles, Calif. Bull. WP-50, 1968.

8. Perry, J. H., Chemical Engineers' Handbook, McGraw-Hill Book Co., Inc., New York, N.Y., 1960.

9. Rom, Jerome J., Maintenance, Calibration, and Operation of Isokinetic Source Sampling Equipment, Environmental Protection Agency, APTD-0576.

10. Shigehara, R. T., W. F. Todd, and W. S. Smith, Significance of Errors in Stack Sampling Measurements, Paper presented at the Annual Meeting of the Air Pollution Control Association, St. Louis, Mo., June 14-19, 1970.

11. Smith, W. S., et al., Stack Gas Sampling Improved and Simplified with New Equipment, APCA paper No. 67-119, 1967.

12. Smith, W. S., R. T. Shigehara, and W. F. Todd, A Method of Interpreting Stack Sampling Data, Paper presented at the 63d Annual Meeting of the Air Pollution Control Association, St. Louis, Mo., June 14-19, 1970. 13. Specifications for Incinerator Testing at Federal Facilities PHS, NCAPC, 1967.

14. Standard Method for Sampling Stacks for Particulate Matter, In: 1971 Book of ASTM Standards, part 23, Philadelphia, 1971, ASTM Designation D-2928-71.

15. Vennard, J. K., Elementary Fluid Mechanics, John Wiley and Sons, Inc., New York, 1947.

METHOD 103. BERYLLIUM SCREENING METHOD

1. Principle and applicability.-1.1 Principle.-Beryllium emissions are isokinetically sampled from three points in a duct or stack. The collected sample is analyzed for beryllium using an appropriate technique.

1.2 Applicability.-This procedure details guidelines and requirements for methods acceptable for use in determining beryllium emissions in ducts or stacks at stationary sources, as specified under the provisions of § 61.14 of the regulations.

2. Apparatus-2.1 Sampling train.-A schematic of the required sampling train configuration is shown in figure 103-1. The essential components of the train are the following:

2.1.1 Nozzle.-Stainless steel, or equivalent, with sharp, tapered leading edge.

2.1.2 Probe.-Sheathed Pyrex 1 glass. 2.1.3 Filter.-Millipore AA, or equivalent, with appropriate filter holder that provides a positive seal against leakage from outside or around the filter. It is suggested that a Whatman 41, or equivalent, be placed immediately against the back side of the Millipore filter as a guard against breakage of the Millipore. Include the Whatman 41 in the analysis. Equivalent filters must be at least 99.95 percent efficient (DOP Test) and amenable to the analytical procedure.

2.1.4 Meter-pump system.-Any system that will maintain isokinetic sampling rate, determine sample volume, and is capable of a sampling rate of greater than 0.5 cfm.

2.2 Measurement of stack conditions (stack pressure, temperature, moisture and velocity).—The following equipment shall be used in the manner specified in section 4.3.1.

2.2.1 Pitot tube.-Type S, or equivalent, with a coefficient within 5 percent over the working range.

1 Mention of trade names or specific products does not constitute endorsement by the Environmental Protection Agency.

NOZZLE

PROBE

FILTER

METER-PUMP SYSTEM

Figure 103-1. Beryllium screening method: sample train schematic.

2.2.2 Differential pressure gauge.-Inclined manometer, or equivalent, to measure velocity head to within 10 percent of the minimum value.

2.2.3. Temperature gauge.-Any temperature measuring device to measure stack temperature to within 5° F.

2.2.4 Pressure gauge.-Any device to measure stack pressure to within 0.1 in. Hg. 2.2.5 Barometer.-To measure atmospheric pressure to within 0.1 in. Hg.

2.2.6 Moisture determination.-Wet and dry bulb thermometers, drying tubes, condensers, or equivalent, to determine stack gas moisture content to within 1 percent.

2.3 Sample recovery.-2.3.1 Probe cleaning equipment.-Probe brush or cleaning rod at least as long as probe, or equivalent. Clean cotton balls, or equivalent, should be used with the rod.

2.3.2 Leakless glass sample bottles.

2.4 Analysis.-2.4.1 Equipment necessary to perform an atomic absorption, spectrographic, fluorometric, chromatographic, or equivalent analysis.

3. Reagents.-3.1 Sample recovery.-3.1.1 Acetone.-Reagent grade.

3.1.2 Wash acid.-1:1 V/V hydrochloric acid-water.

3.2 Analysis.-3.2.1

Reagents as necessary for the selected analytical procedure. 4. Procedure.-4.1 Guidelines for source testing are detailed in the following sections. These guidelines are generally applicable; however, most sample sites differ to some degree and temporary alterations such as stack extensions or expansions often are required to insure the best possible sample site. Further, since beryllium is hazardous, care should be taken to minimize exposure. Finally, since the total quantity of beryllium to be collected is quite small, the test must be carefully conducted to prevent contamination or loss of sample.

4.2 Selection of a sampling site and number of runs.-4.2.1 Select a suitable sampling site that is as close as practicable to the point of atmospheric emission. If possible, stacks smaller than 1 foot in diameter should not be sampled.

4.2.2 The sampling site should be at least eight stack or duct diameters downstream and two diameters upstream from any flow disturbance such as a bend, expansion or contraction. For rectangular cross-section, determine an equivalent diameter using the following equation:

4.2.3 Some sampling situations may render the above sampling site criteria impractical. When this is the case, an alternate site may be selected but must be no less than two diameters downstream and onehalf diameter upstream from any point of disturbance. Additional sample runs are recommended at any sample site not meeting the criteria of section 4.2.2.

4.2.4 Three runs shall constitute a test. The runs shall be conducted at three different points. The three points shall proportionately divide the diameter, i.e. be located at 25, 50 and 75 percent of the diameter from the inside wall. For horizontal ducts, the diameter shall be in the vertical direction. For rectangular ducts, sample on a line through the centroid and parallel to a side. If additional runs are required per section 4.2.3, proportionately divide the duct to accommodate the total number of runs.

4.3 Measurement of stack conditions. 4.3.1 Measure the stack gas pressure, moisture, and temperature, using the equipment described in § 2.2. Determine the molecular weight of the stack gas. Sound engineering estimates may be made in lieu of direct measurements. The basis for such estimates shall be given in the test report.

4.4 Preparation of sampling train.4.4.1 Assemble the sampling train as shown in figure 103-1. It is recommended that all glassware be precleaned by soaking in wash acid for 2 hours.

4.4.2 Leak check the sampling train at the sampling site. The leakage rate should not be in excess of 1 percent of the desired sample rate.

4.5 Beryllium train operation.-4.5.1 For each run, measure the velocity at the selected sampling point. Determine the isokinetic sampling rate. Record the velocity head and the required sampling rate.

4.5.2 Place the nozzle at the sampling point with the tip pointing directly into the gas stream. Immediately start the pump and adjust the flow to isokinetic conditions. At the conclusion of the test, record the sampling rate. Again measure the velocity head at the sampling point. The required isokinetic rate at the end of the period should not have deviated more than 20 percent from that originally calculated.

4.5.3 Sample at a minimum rate of 0.5 ft3/min. Samples shall be taken over such a period or periods as are necessary to determine the maximum emissions which would occur in a 24-hour period. In the case of cyclic operations, sufficient tests shall be made so as to allow determination or calculation of the emissions which would occur over the duration of the cycle. A minimum

sampling time of 2 hours is recommended. 4.5.4 All pertinent data should be included in the test report.

4.6 Sample recovery.-4.6.1 It is recommended that all glassware be precleaned as in 4.4.1. Sample recovery should also be performed in an area free of possible beryllium contamination. When the sampling train is moved, exercise care to prevent breakage and contamination. Set aside a portion of the acetone used in the sample recovery as a blank for analysis. The total amount of acetone used should be measured for accurate blank correction. Blanks can be eliminated if prior analysis shows negligible amounts.

4.6.2 Remove the filter and any loose particulate matter from filter holder and place in a container.

4.6.3 Clean the probe with acetone and a brush or long rod and cotton balls. Wash into the container. Wash out the filter holder with acetone and add to the same container.

4.7 Analysis.-4.7.1 Make the necessary preparation of samples and analyze for beryllium. Any currently acceptable method such as atomic absorption, spectrographic, fluorometric, chromatographic, or equivalent may be used.

5. Calibration and standards-5.1 Sampling train.-5.1.1 As a procedural check, sampling rate regulation should be compared with a dry gas meter, spirometer, rotameter (calibrated for prevailing atmospheric conditions), or equivalent, attached to nozzle inlet of the complete sampling train.

5.1.2 Data from this test and calculations should be shown in test report.

Standardization is 5.2 Analysis.-5.2.1 made as suggested by the manufacturer of the instrument or the procedures for the analytical method.

6. Calculations-6.1 Total beryllium emission. Calculate the total amount of beryllium emitted from each stack per day by equation 103-2. This equation is applicable for continuous operations. For cyclic operations, use only the time per day each stack is in operation. The total beryllium emissions from a source will be the summation of results from all stacks.

R=Rate of emission, g/day.

W-Total weight of beryllium collected, ug. Vtotal Total volume of gas sampled, ft3. (0) Avg. Average stack gas velocity, feet per second. A. Stack area, ft2.

7. Test report. 7.1 A test report shall be prepared which shall include as a minimum:

7.1.1 A detailed description of the sampling train used and results of the procedural check with all data and calculations made.

7.1.2 All pertinent data taken during test, the basis for any estimates made, calculations, and results.

7.1.3 A description of the test site, including a block diagram with a brief description of the process, location of the sample points in the cross section, dimensions and distances from any point of disturbance. METHOD 104. REFERENCE METHOD FOR DETERMINATION OF BERYLLIUM EMISSIONS FROM STATIONARY SOURCES

1. Principle and applicability-1.1 Principle.-Beryllium emissions are isokinetically sampled from the source, and the collected sample is digested in an acid solution and analyzed by atomic absorption spectrophotometry.

1.2 Applicability.-This method is applicable for the determination of beryllium emissions in ducts or stacks at stationary sources. Unless otherwise specified, this method is not intended to apply to gas streams other than those emitted directly to the atmosphere without further processing.

2. Apparatus-2.1 Sampling train.-A schematic of the sampling train used by EPA is shown in figure 104-1. Commercial models of this train are available, although construction details are described in APTD0581,1 and operating and maintenance procedures are described in APTD-0576. The components essential to this sampling train are the following:

1 These documents are available for a nominal cost from the National Technical Information Service, U.S. Department of Commerce, 5285 Port Royal Road, Springfield, Va. 22151.

2.1.1 Nozzle.-Stainless steel or glass with sharp, tapered leading edge.

2.1.2 Probe.-Sheathed Pyrex glass. A heating system capable of maintaining a minimum gas temperature in the range of the stack temperature at the probe outlet during sampling may be used to prevent condensation from occurring.

2.1.3 Pitot tube.-Type S (figure 104-2), or equivalent, with a coefficient within 5 percent over the working range, attached to probe to monitor stack gas velocity.

2.1.4 Filter holder.-Pyrex glass. The filter holder must provide a positive seal against leakage from outside or around the filter. A heating system capable of maintaining the filter at a minimum temperature in the range of the stack temperature may be used to prevent condensation from occurring.

2.1.5 Impingers.-Four Greenburg-Smith impingers connected in series with glass ball joint fittings. The first, third, and fourth impingers may be modified by replacing the tip with a 2-inch 1.d. glass tube extending to one-half inch from the bottom of the flask.

2.1.6 Metering system.-Vacuum gauge, leakless pump, thermometers capable of measuring temperature to within 5° F, dry gås meter with 2 percent accuracy, and related equipment, described in APTD-0581, to maintain an isokinetic sampling rate and to determine sample volume.

Mention of trade names on specific products does not constitute endorsement by the Environmental Protection Agency.