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Figure 1016. Field data 5.2 Analysts-5.2.1 Prepare & callbra 6.3 Volume of water vapor. tion curve for the spectrophotometer using the standard mercury solutions. Plot the peak heights read on the recorder versus the concentrations of mercury in the standard where: solutions. Standards should be interspersed V»-Volume of water vapor in the gas sample (stack with the samples since the callbration can

conditions), itd. .
change slightly with time. A new callbration
curve should be prepared for each new set

Kp=0.00267
moenin.Hg.-fts

when these units are used.

ml.-R of samples run,

Vir=Total volume of liquid collected in impingers 6. Calculations.-6.1 Average "drygas

and silica gel (see figure 101-7), ml. meter temperature, stack temperature, stack

· T, - Average stack gas temperature, °R.. . .

Pe=Stack pressure, Psar £ static pressure, in. Hg. pressure and averago orifico pressure drop.

6.4 Total gas volume. See data sheet (ig. 101-6).

Votal=Vm, tv,

eq. 101-4 • 6.2 Dry gas volume.-Correct the sample

where: volume measured by the dry gas meter to

Vtotal=Total volume of gas sample (stack conditions), stack conditions by using equation 101-2. V., Volume of gas through gas meter (stack condi.

tions), ft.

Volume of water vapor in gas sample (stack (Poart 13.6)

conditions), itd. T

- VOLUME OF LIQUID

WATER COLLECTED eq. 101-2

IMPINGER where:

SILICA GEL

WEIGHT, V.,-Volume of gas sample through the dry gas meter

(stack conditions), fts. V. -Yalume of gas sample through the dry gas meter

FINAL (meter conditions), fts. T. -Average temperature of stack gas, °R.

. INITIAL T. Average dry gas meter temperature. R.

LIQUID COLLECTED Puor=Barometric pressure at the orifice

TOTAL VOLUME COLLECTED meter, inHg. : Ad=Average pressure drop across the ori

CONVERT WEIGHT OF WATER TO VOLUME BY dividing total weight

INCREASE BY DENSITY OF WATER. (1 g/ml): Alce meter, InH20. 18.0=Speciflc gravity of mercury. "

INCREASE. I = VOLUME WATER, ml

71 g/ml) Po=Stack pressure, Pbarstatic pressure, InHg.

Figure 101-7. Analytical data.

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6.5 Stack gas velocity. Use equation 101–5 where: to calculate the stack gas velocity.

I= Percent of isokinetic sampling.

Vlotal= Total volume of gas sample (stack conditions), (v.) ave.=K,C,(Va

Ag-Probe tip area, fta.

O=Sampling time, sec.

(1.) ave. -Average stack gas velocity, feet per second.

eq. 101–5 7. Evaluation of results-7.1 Determina. where:

tion of compliance.-7.1.1 Each performance (P.)avs.= Average stack gas velocity, feet per second. test shall consist of three repetitions of the K,=85.532 11. ( lb.-in.Hg Tin

when

applicable test method. For the purpose of sec. lb.mole-R-in.H.O

determining compliance with an applicable these units are used. Co-Pitot tube coefficient, dimensionless.“

national emission standard, the average of (T.).rs. = Average stack gas temperature, °R.

results of all repetitions shall apply. (VAP).vs.= Average square root of the velocity head 7.2 Acceptable isokinetic results.-7.2.1

of stack gas (in. H70)1/2 (see fig. 101-8). The following range sets the limit on accept!P,= Stack pressure, Pburtstatic pressure, in. Hg.

able isokinetic sampling results:
M.- Molecular weight of stack gas (wet basis),
the summation of the products of the

II 90% SI$110%, the results are acceptmolecular weight of each component able; otherwise, reject the test and repeat. multiplied by its volumetric proportion. 8. References.-1. Addendum to Specificain the mixture, lb.Ab. mole.

tions for Incinerator Testing at Federal Figure 101_8 shows a sample recording sheet Facilities, PHS, NCAPC, Dec. 6, 1967. for velocity traverse data. Use the averages 2. Determining Dust Concentration in & in the last two columns of figure 101-8 to Gas Stream, ASME Performance Test Code determine the average stack gas velocity from No. 27, New York, N.Y., 1967 equation 101-5.

3. Devorkin, Howard, et al., Air Pollution 6.6 Mercury collected. Calculate the total Source Testing Manual, Air Pollution Con. weight of mercury collected by using equa trol District, Los Angeles, Call., Nov. 1963. tion 101-6.

4. Hatch, W. R. and W. L. Ott, “DeterminaW.=ViCi-VoCo (+V/CI)--eq. 101-6 tion of Sub-Microgram Quantities of Mercury where:

by Atomic Absorption Spectrophotometry." Wi=total weight of mercury collected, ug. Anal. Chem., 40:2085–87, 1968. Vi=Total volume of condensed moisture 5. Mark, L. S., Mechanical Engineers' Hand. and ICI in sample bottle, ml.

book, McGraw-Hill Book Co., Inc., New York, Ci=Concentration of mercury measured in N.Y., 1951. sample bottle, ug/ml.

6. Martin, Robert M., Construction Details V»=Total volume of ICl used in sampling of Isokinetic Source Sampling Equipment,

(impinger contents and all wash Environmental Protection Agency, APTD amounts), ml.

0581. Co=Blank concentration of mercury in ICI 7. Methods for Determination of Velocity, solution, ug/ml.

Volume, Dust and Mist Content of Gases, Vi=Total volume of ICI used in alter bottle Western Precipitation Division of Joy Mfg. (if used), ml.

Co., Los Angeles, Calli. Bul. WP-50, 1968. Ci=Concentration of mercury in filter 8. Perry, J. H., Chemical Engineers' Handbottle (ut used), ug/ml.

book, McGraw-Hill Book Co., Inc., New York,

N.Y., 1960. 6.7 Total mercury emission. Calculate the total amount of mercury emitted from each

9. Rom, Jerome J., Maintenance, Callbrastack per day by equation 101-7. This equa

tion, and Operation of Isokinetic Source Samtion is applicable for continuous operations.

pling Equipment, Environmental Protection For cyclic operations, use only the time per

Agency, APTD-0576. day each stack is in operation. The total

10. Shigehara, R. T., W. F. Todd, and W. S. mercury emissions from & source will be the

Smith, Significance of Errors in Stack Samsummation of results from all stacks.

pling Measurements, Paper presented at the

Annual Meeting of the Air Pollution Control D_W.(v.) sve. A., 86,400 seconds/day Association, St. Louis, Mo., June 14–19, 1970.

100 ug/g.

11. Smith, W. S., et al., Stack Gas Sampling

Improved and simplified with New Equipeq. 101-7

ment, APCA paper No. 67–119, 1967. where:

· 12. Smith, W. S., R. T. Shigehara, and w. R= Rate of emission, g/day. W = Total weight of mercury collected, ug.

F. Todd, A Method of Interpreting Stack Vhotar=Total volume of gas sample (stack conditions), Sampling Data, Paper presented at the 630 ft.

Annual Meeting of the Air Pollution Control (0.) ovs. Average stack gas velocity, feet per second. Association, St. Louis, Mo., June 14-19, 1970. A.- Stack area, fta.

13. Specifications for Incinerator Testing at 6.8 Isokinetic varlation (comparison of

Federal Facilities PHS, NCAPC, 1967. velocity of gas in probe tip to stack yelocity).

14. Standard Method for Sampling Stacks for Particulate Matter, In: 1971 Book of

ASTM Standards, part 23, Philadelphia, 1971, A, (v.) avg. . eg. 101-8 ASTM Designation D-292871.

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15. Vennard, J. K., Elementary Fluid Mechanics, John Wiley and Sons, Inc., New York, 1947. METHOD 102. REFERENCE METHOD FOR DETER

MINATION OF PARTICULATE AND GASEOUS MERCURY EMISSIONS FROM STATIONARY SOURCES (HYDROGEN STREAMS)

1. Principle and applicability-1.1 Principle.- Particulate and gaseous mercury emissions are isokinetically sampled from the source and collected in acidic iodine monochloride solution. The mercury collected (in the mercuric form) is reduced to elemental mercury in basic solution by hydroxylamine sulfate. Mercury is serated from the solution and analyzed using spectrophotometry.

1.2 Applicability. This method is applicable for the determination of particulate and gaseous mercury emissions when the carrier gas stream is principally hydrogen. The method is for use 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 102-1. Commercial models of this train are available, although complete construction detalls 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.

2.1.3 Pitot tube. Type 8 (figure 102–2), or equivalent, with a coefficient within 5 percent over the working range, attached to probe to monitor stack gas velocity.

2.1.4 Impingers. Four Greenburg-Smith impingers connected in series with glass balljoint fittings. The first, third, and fourth impingers may be modified by replacing the tip with one-half inch ID glass tube extending to one-half inch from the bottom of the flask.

2.1.5 Acid trap. Mine safety appliances air line filter, catalogue No. 81857, with acid absorbing cartridge and suitable connections, or equivalent.

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

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2.1.8 Metering system. Vacuum gage, leak less pump, thermometers capable of measuring temperature to within 5°F, dry gas meter with 2 percent accuracy, and related equip ment, described in APTD-0581, to maintain an isokinetic sampling rate and to determine sample volume.

2.1.7 Barometer. To measure atmospheric pressure to + 0.1 in hg.

2.2 Measurement of stack conditions (stack pressure, temperature, moisture, and velocity) -2.2.1 Pitot tube. Type S, or equivalent, with a coeficient within 5 percent over the working range.

2.2.2 Differential pressure gage. Inclined manometer, or equivalent, to measure velocity head to within 10 percent of the minimum value. Micromanometers should be used if warranted.

2.2.3 Temperature gage. Any temperature-measuring device to measure stack temperature to within 1° F.

2.2.4 Pressure gage. Pitot tube and inclined manometer, or equivalent, to measure stack pressure to within 0.1 in hg. .

2.2.5 Moisture determination. Drying tubes, condensers, or equivalent, to deter mine stack gas moisture content in hydrogen to within 1 percent.

2.3. Sample recovery-2.3.1 Leakless glass sample bottles. 500 ml and 200 ml with Terlon-lined tops.

2.3.2 Graduated cylinder. 250 ml. 2.3.3 Plastic jar. Approximately 300 ml.

2.4 Analysis-2.4.1 Spectrophotometer. To measure absorbance at 253.7 nm. Perkin

absorbance at 253.7 nm. Perkın Elmer model 303, with a cylindrical gas cell (approximately 1.5 in o.d.x7 in) with quartz glass windows, and hollow cathode source, or equivalent.

2.4.2 Gas sampling bubbler. Tudor Scien tifo Co. Smog Bubbler, catalogue No. TP1150, or equivalent.

2.4.3 Recorder. To match output of spectrophotometer.

3. Reagents.-3.1 Stock reagents.-3.1.1 Potassium iodide. Reagent grade.

3.1.2 Distilled water.

3.1.3 Potassium iodide solution, 25 percent. Dissolve 250 g of potassium iodide (reagent 3.1.1) in distilled water and dilute to i to 1.

3.1.4 Hydrochloric acid. Concentrated.
3.1.5 Potassium iodate. Reagent grade.

3.1.6 Iodine monochloride (ICI) 1.0M. TO 800 ml of 25 percent potassium iodido solution (reagent 3.1.3), add 800 ml of concentrated hydrochloric acid. Cool to room temperature. With vigorous stirring, slowly add 135 g of potassium iodate and continue stirring until all free lodine has dissolved to give a clear orange-red solution. Cool to room temperature and dilute to 1,800 ml with distilled water. The solution should be kept in amber bottles to prevent degradation.

3.1.7 Sodium hydroxide pellets. Reagent grade.

3.1.8 Nitric acid. Concentrated.

3.1.9 Hydroxylamine sulfate. Reagent grade.

3.1.10 Sodium chloride. Reagent grade.
3.1.11 Mercuric chloride. Reagent grade.

3.2 Sampling. 3.2.1 Absorbing solution, 0.1M ICI. Dilute 100 ml of the 1.0M ICI stock solution (reagent 3.1.6) to 1 1 with distsilled water. The solution should be kept in glass bottles to prevent degradation. This reagent should be stable for at least 2 months; however, periodic checks should be performed to insure quality.

3.2.2 Wash acid. 1:1 V/V nitric acid-water. 3.2.3 Distilled, deionized water.

3.2.4 Silica gel. Indicating type, 6 to 16 mesh, dried at 350°F for 2 hours.

3.3. Analysis-3.3.1 Sodium hydroxide, 10N. Dissolve 400 g of sodium hydroxide pellets in distilled water and dilute to i 1.

3.3.2 Reducing agent, 12 percent hydrolylamine sulfate, 12 percent sodium chloride. TO 60 ml of distilled water, add 12 g of hydroxylamine sulfate and 12 g of sodium chloride. Dilute to 100 ml. This quantity is suficient for 20 analyses and must be prepared daily.

3.3.3 Aeration gas. Zero grade air..

3.3.4 Hydrochloric acid, 0.3N. Dilute 25.5 ml of concentrated bydrochloric acid to 1 1 with distilled water..

3.4 Standard mercury solutions-3.4.1 Stock solution. Add 0.1354 g of mercuric chloride to 80 ml of 0.3N hydrochloric acid. After the mercuric chloride has dissolved, add 0.3N hydrochloric acid and adjust the volume to 100 ml. One ml of this solution is equivalent to 1 mg of free mercury.

3.4.2 Standard solutions. Prepare callbration solutions by serially diluting the stock solution (3.4.1) with 0.3N hydrochloric acid. Prepare solutions at concentrations in the linear working range for the instrument to be used. Solutions of 0.2 ug/ml, 0.4 kg/ml and 0.6 ug/ml have been found acceptable for most instruments. Store all solutions in glass-stoppered, glass bottles. These solutions should be stable for at least 2 months; however, periodic checks should be performed to insure quality.

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