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VOLUME OF LIQUID

P_W.(v.)ave. A, 86,400 seconds/day WATER COLLECTED

100 ug/g IMPINGER

eq. 102-8 VOLUME.

where:

R=Rate of emission, g/day.

W = Total weight of mercury collected, ug.
Vtotal= Total volume of gas sample (stack conditions),

SILICA GEL

WEIGHT.

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FINAL

INITIAL

LIQUID COLLECTED

TOTAL VOLUME COLLECTED

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I

Figure 102-7. Analytical data. 6.5 Stack gas velocity-Use equation 102–6 to calculate the stack gas velocity.

(Tavg (v.)ave.=K,C(VĀ

eq 102-6 where: (v.) ave. =Average stack gas velocity, feet per second.

Ave It lb -inHg__) when

sec lb mole-R-in!120 these units are used.

Pitot tube coefficient, dimensionless. (T.)ove. = Average stack gss temperature, °R.

=Average square root of the velocity head of

stack gas (in110)/2 (see figure 102-8). P, =Stack pressure, Poartstatic pressure, in

Hg.
M, =Molecular weight of stack gas (wet basis),

the summation of the products of the
molecular weight of each component
multiplied by its volumetric proportio u

in the mixture, Ib/Ib-mole. Figure 102–8 shows a sample recording sheet for velocity traverse data. Use the averages in the last two columns of figure 102–8 to determine the average stack gas velocity from equation 102-6.

6.6 Mercury collected. Calculate the total weight of mercury collected by using eq. 102–7.

Wo=ViCi-VoCo.-.-.eq. 102-7 where: Wi=Total weight of mercury collected, ug. Vi= Total volume of condensed moisture

and Ici in sample bottle, ml. Ci=Concentration of mercury measured in

sample bottle, ug/ml. Vo=Total volume of Ici used in sampling

(impinger contents and all wash

amounts), ml. Co=Blank concentration of mercury in ICI

solution, ug/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.

(v.) avg. = Average stack gas velocity, feet per second.

A.=Stack area, ft?. 6.8 Isokinetic variation (comparison of velocity of gas in probe tip to stack velocity).

100 V total

eq. 102-9 where:

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

ft.
An=Probe tip area, ft?.

=Sampling time, sec. (1) avg.=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% <I110%, 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 & 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, APTD0581.

7. Methods for Determination of Velocity, Volume, Dust and Mist Content of Gases, Western Precipitation Division of Joy Manu. facturing Co., Los Angeles, Call. 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, Callbration, and Operation of Isokinetic Source Sampling Equipment, Environmental Protection Agency, APTD-0576.

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10. Shigehara, R. T., W. F. Todd, and W. S.

FILTER Smith, Significance of Errors in Stack Sam

NOZZLE pling Measurements, Paper presented at the

PAQBE
Annual Meeting of the Air Pollution Control
Association, St. Louis, Mo., June 14-19, 1970.

11. Smith, W. S., et al., Stack Gas Sam. pling 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 Sam

METER-PUMP pling Data, Paper presented at the 63d An

SYSTEM nual Meeting of the Air Pollution Control Association, St. Louis, Mo., June 14-19, 1970.

Figure 103-1. Beryllium screening method: sample train schematic. 13. Specifications for Incinerator Testing

2.2.2 Differential pressure gauge.-Inat Federal Facilities PHS, NCAPC, 1967.

clined manometer, or equivalent, to measure 14. Standard Method for Sampling Stacks

velocity head to within 10 percent of the for Particulate Matter, In: 1971 Book of

minimum value. ASTM Standards, part 23, Philadelphia, 1971,

2.2.3. Temperature gauge.-Any temperaASTM Designation D-2928–71.

ture measuring device to measure stack tem15. Vennard, J. K., Elementary Fluid Me

perature to within 5° F. chanics, John Wiley and Sons, Inc., New

2.2.4 Pressure gauge.-Any device to York, 1947.

measure stack pressure to within 0.1 in. Hg. METHOD 103. BERYLLIUM SCREENING METHOD

2.2.5 Barometer.To measure atmos

pheric pressure to within 0.1 in. Hg. 1. Principle and applicability.-1.1 Prin

2.2.6 Moisture determination.Wet and ciple.-Beryllium emissions are isokinetically

dry bulb thermometers, drying tubes, consampled from three points in a duct or stack.

densers, or equivalent, to determine stack gas The collected sample is analyzed for beryl

moisture content to within 1 percent. llum using an appropriate technique.

2.3 Sample recovery.-2.3.1 Probe clean1.2 Applicability. This procedure details

ing equipment.-Probe brush or cleaning rod guidelines and requirements for methods

at least as long as probe, or equivalent. Clean acceptable for use in determining beryllium

cotton balls, or equivalent, should be used emissions in ducts or stacks at stationary

with the rod. sources, as specified under the provisions of 2.3.2 Leakless glass sample bottles. $ 61.14 of the regulations.

2.4 Analysis.-2.4.1 Equipment neces2. Apparatus-2.1 Sampling train.--A

sary to perform an atomic absorption, schematic of the required sampling train

spectrographic, fluorometric, chromatoconfiguration is shown in figure 103-1. The

graphic, or equivalent analysis. essential components of the train are the 3. Reagents.-3.1 Sample recovery.-3.1.1 following:

Acetone.Reagent grade. 2.1.1 Nozzle.-Stainless steel, or equiva 3.1.2 Wash acid.—1:1 V/V hydrochloric lent, with sharp, tapered leading edge.

acid-water. 2.1.2 Probe.Sheathed Pyrex 1 glass.

3.2 Analysis.-3.2.1 Reagents as neces2.1.3 Filter.-Millipore AA, or equivalent, sary for the selected analytical procedure. with appropriate filter holder that provides 4. Procedure.-4.1 Guidelines for sourco & positive seal against leakage from outside testing are detalled in the following sections. or around the filter. It is suggested that a These guidelines are generally applicable; Whatman 41, or equivalent, be placed imme however, most sample sites differ to some dediately against the back side of the Millipore gree and temporary alterations such as stack filter as & guard against breakage of the extensions or expansions often are required Millipore. Include the Whatman 41 in the to insure the best possible sample site. Furanalysis. Equivalent filters must be at least ther, since berylllum 18 hazardous, care 99.95 percent efficient (DOP Test) and should be taken to minimize exposure. amenable to the analytical procedure. Finally, since the total quantity of beryllium

2.1.4 Meter-pump system.-Any system to be collected is quite small, the test must that will maintain isokinetic sampling rate, be carefully conducted to prevent contamidetermine sample volume, and is capable of nation or loss of sample. & sampling rate of greater than 0.5 cfm.

4.2 Selection of a sampling site and num2.2 Measurement of stack conditions ber of runs.-4.2.1 Select & suitable sam(stack pressure, temperature, moisture and pling site that is as close as practicable to the velocity).The following equipment shall be point of atmospheric emission. Il possible, used in tlie manner specified in section 4.3.1.

stacks smaller than 1 foot in diameter should 2.2.1 Pitot tube.-Type S, or equivalent,

not be sampled. with a coefficient within 6 percent over the

4.2.2 The sampling site should be at least

eight stack or duct diameters downstream working range.

and two diameters upstream from any now

disturbance such as & bend, expansion or 1 Mention of trade names or specific prod. contraction. For rectangular cross-section, ucts does not constitute endorsement by the determine an equivalent diameter using the Environmental Protection Agency.

following equation:

D.= 2LW

--- oq. 108-1

sampling time of 2 hours is recommended. L+W

4.5.4 AN pertinent data should be in

cluded in the test report. where:

4.6 Sample recovery.-4.6.1 It is recomDe=equivalent diameter

mended that all glassware be precleaned as L=length

in $ 4.4.1. Sample recovery should also be W=width

performed in an area free of possible beryl4.2.3 Some sampling situations may ren

lium contamination. When the sampling der the above sampling site criteria imprac

train is moved, exercise care to prevent tical. When this is the case, an alternate

breakage and contamination. Set aside a porsite may be selected but must be no less

tion of the acetone used in the sample rethan two diameters downstream and one

covery as a blank for analysis. The total hall diameter upstream from any point of

amount of acetone used should be measured disturbance. Additional sample runs are rec

for accurate blank correction. Blanks can be ommended at any sample site not meeting

eliminated if prior analysis shows negligible the criteria of section 4.2.2.

amounts. 4.2.4 Three runs shall constitute & test.

4.6.2 Remove the filter and any loose parThe runs shall be conducted at three dii.

ticulate matter from alter holder and place ferent points. The three points shall pro

in a container. portionately divide the diameter, 1.e. be lo

4.6.3 Clean the probe with acetone and a cated at 25, 50 and 75 percent of the diameter

brush or long rod and cotton balls. Wash into from the inside wall. For horizontal ducts,

the container. Wash out the filter holder the diameter shall be in the vertical direc

with acetone and add to the same container. tion. For rectangular ducts, sample on a line

4.7 Analysis.-4.7.1 Make the necessary through the centroid and parallel to a side.

preparation of samples and analyze for beryl. II additional runs are required per section

llum. Any currently acceptable method such 4.2.3, proportionately divide the duct to ac

as atomic absorption, spectrographic, Auorocommodate the total number of runs.

metric, chromatographic, or equivalent may 4.3 Measurement of stack conditions. be used. 4.3.1 Measure the stack gas pressure, mois

5. Calibration and standard9–5.1 Sam. ture, and temperature, using the equipment

pling train.-5.1.1 As a procedural check, described in $ 2.2. Determine the molecular

sampling rate regulation should be compared

sampling rate reg weight of the stack gas. Sound engineering with a dry gas meter, spirometer, rotameter estimates may be made in lieu of direct (callbrated for prevailing atmospheric conmeasurements. The basis for such estimates ditions), or equivalent, attached to nozzle shall be given in the test report.

inlet of the complete sampling train. 4.4 Preparation of sampling train. 5.1.2 Data from this test and calculations 4.4.1 Assemble the sampling train as shown should be shown in test report. in figure 103-1, It is recommended that all 5.2 Analysis.-5.2.1 Standardization 18 glassware be precleaned by soaking in wash made as suggested by the manufacturer of acid for 2 hours.

the instrument or the procedures for the 4.4.2 Leak check the sampling train at the analytical method. . sampling site. The leakage rate should not be 6. Calculations_6.1 Total beryllium emisin excess of 1 percent of the desired sample sion, Calculate the total amount of berylrate.

lium emitted from each stack' per day by 4.5 Beryllium train operation.-4.5.1 For equation 103-2. This equation is applicable each run, measure the velocity at the selected for continuous operations. For cyclic operasampling point. Determine the isokinetic tions, use only the time per day each stack sampling rate. Record the velocity head and is in operation. The total beryllium emisthe required sampling rate.

sions from a source will be the summation 4.5.2 Place the nozzle at the sampling of results from all stacks. point with the tip pointing directly into the gas stream. Immediately start the pump and

P_W.(v.).ve. A., 86,400 seconds/day adjust the flow to isokinetic conditions. At

100 mg/8 the conclusion of the test, record the sampling rate. Again measure the velocity head

where:

R-Rate of emission, g/day. at the sampling point. The required isokinetici W-Total weight of beryllium collected, wg. rate at the end of the period should not have Vtotal=Total volume of gas sampled, ft3. deviated more than 20 percent from that

(6.) avg. -Average stack gas velocity, feet per second. originally calculated.

=Stack area, ft?. 4.5.3 Sample at a minimum rate of 0.5 7. Test report. 7.1 A test report shall be 1t3/min. Samples shall be taken over such & prepared which shall include as a minimum: period or periods as are necessary to deter 7.1.1 A detalled description of the sammine the maximum emissions which would pling train used and results of the proceoccur in & 24-hour period. In the case of dural check with all data and calculations cyclic operations, sufficient tests shall be made. made so as to allow determination or calcu 7.1.2 All pertinent data taken during lation of the emissions which would occur test, the basis for any estimates made, calover the duration of the cycle. A minimum culations, and results.

V total

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 DETER

MINATION 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 avallable, although construction details are described in APTD 0581,1 and operating and maintenance procedures are described in APTD-0576. The components essential to this sampling train are the following:

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 12-inch 1.d. glass tube extending to one-half inch from the bottom of the fask.

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.

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

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

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