4.3 Analysis. Record the data required on the example sheet shown in Figure 5-3. Handle each sample container as follows:

Container No. 1. Transfer the filter and any loose particulate matter from the sample container to a tared glass weighing dish, desiccate, and dry to a constant weight. Report results to the nearest 0.5 mg.

Container No. 2. Transfer the acetone washings to a tared beaker and evaporate to dryness at ambient temperature and pressure. Desiccate and dry to a constant weight. Report results to the nearest 0.5 mg.

Container No. 3. Weigh the spent silica gel and report to the nearest gram.

Poart

ΔΗ 13.6

where: Bw.

Tm

equation 5-1

Proportion by volume of water vapor in the gas stream, dimensionless.

Volume of water in the gas sample (standard conditions), cu. ft.

Vtd-Volume of gas sample through the dry gas meter (standard conditions), cu. ft.

6.5 Total particulate weight. Determine the total particulate catch from the sum of the weights on the analysis data sheet (Figure 5-3).

=

V1, Total volume of liquid collected in impingers and silica gel (See Fig. 5-3), ml.

PH,O=Density of water, 1 g./ml.

R-Ideal gas constant, 21.83 inches Hg-cu. ft./lb. mole-°R.

Mн,0=Molecular weight of water, 18 lb./lb.-mole. V=Volume of gas sample through the dry gas meter (meter conditions), cu. ft.

T-Absolute average dry gas meter temperature (see Figure 5-2), °R.

Pbar Barometric pressure at sampling site, inches
Hg.

AH Average pressure drop across the orifice (see
Fig. 5-2), inches H.Ö.

T. Absolute average stack gas temperature (see
Fig. 5-2). R.

6 Total sampling time, min.

V. Stack gas velocity calculated by Method 2,
Equation 2-2, ft./sec.

P, Absolute stack gas pressure, inches Hg.
A Cross-sectional area of nozzle, sq. ft.

6.8 Acceptable results. The following range sets the limit on acceptable isokinetic sampling results:

If 90% <I<110%, the results are acceptable; otherwise, reject the results and repeat the test.

7. Reference.

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

Martin, Robert M., Construction Details of Isokinetic Source Sampling Equipment, Environmental Protection Agency, APTD-0581.

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

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

Specifications for Incinerator Testing at Federal Facilities, PHS, NCAPC, 1967.

METHOD 6-DETERMINATION OF SULFUR DIOXIDE EMISSIONS FROM STATIONARY SOURCES

1. Principle and applicability.

1.1 Principle. A gas sample is extracted from the sampling point in the stack. The acid mist, including sulfur trioxide, is separated from the sulfur dioxide. The sulfur dioxide fraction is measured by the bariumthorin titration method.

1.2 Applicability. This method is applicable for the determination of sulfur dioxide emissions from stationary sources only when specified by the test procedures for determining compliance with New Source Performance Standards.

2. Apparatus.

2.1 Sampling. See Figure 6-1.

2.1.1 Probe-Pyrex1 glass, approximately 5 to 6 mm. ID, with a heating system to prevent condensation and a filtering medium to remove particulate matter including sulfuric acid mist.

2.1.2 Midget bubbler-One, with glass wool packed in top to prevent sulfuric acid mist carryover. 2.1.3 2.1.4

Glass wool.

Midget impingers-Three.

2.1.5 Drying tube--Packed with 6 to 16 mesh indicating-type silica gel, or equivalent, to dry the sample.

2.1.6 Valve-Needle valve, or equivalent, to adjust flow rate.

2.1.7 Pump-Leak-free, vacuum type. 2.1.8 Rate meter-Rotameter or equivalent, to measure a 0-10 s.c.f.h. flow range. 2.1.9 Dry gas meter-Sufficiently accurate to measure the sample volume within 1%. 2.1.10 Pitot tube-Type S, or equivalent, necessary only if a sample traverse is required, or if stack gas velocity varies with time.

2.2 Sample recovery. 2.2.1 Glass wash bottles-Two. 2.2.2 Polyethylene storage bottles-To store impinger samples. 2.3 Analysis.

1 Trade names.

3.3.3 Thorin indicator-1-(o-arsonophenylazo)-2-naphthol-3,6-disulfonic acid, disodium salt (or equivalent). Dissolve 0.20 g. in 100 ml. distilled water.

3.3.4 Barium perchlorate (0.01 N)-Dissolve 1.95 g. of barium perchlorate [Ba (ClO), 3H,O] in 200 ml. distilled water and dilute to 1 liter with isopropanol. Standardize with sulfuric acid. Barium chloride may be used.

3.3.5 Sulfuric acid standard (0.01 N)Purchase or standardize to +0.0002 N against 0.01N NaOH which has previously been standardized against potassium acid phthalate (primary standard grade).

4. Procedure.

4.1 Sampling.

4.1.1 Preparation of collection train. Pour 15 ml. of 80% isopropanol into the midget bubbler and 15 ml. of 3% hydrogen peroxide into each of the first two midget impingers. Leave the final midget impinger dry. Assemble the train as shown in Figure 6-1. Leak check the sampling train at the sampling site by plugging the probe inlet and pulling a 10 inches Hg vacuum. A leakage rate not in excess of 1% of the sampling rate is acceptable. Carefully release the probe inlet plug and turn off the pump. Place crushed ice around the impingers. Add more ice during the run to keep the temperature of the gases leaving the last impinger at 70° F. or less.

4.1.2 Sample collection. Adjust the sample flow rate proportional to the stack gas velocity. Take readings at least every five minutes and when significant changes in stack conditions necessitate additional adjustments in flow rate. To begin sampling, position the tip of the probe at the first sampling point and start the pump. Sample proportionally throughout the run. At the conclusion of each run, turn off the pump and record the final readings. Remove the probe from the stack and disconnect it from the train. Drain the ice bath and purge the remaining part of the train by drawing clean ambient air through the system for 15 minutes.

4.2 Sample recovery. Disconnect the impingers after purging. Discard the contents of the midget bubbler. Pour the contents of the midget impingers into a polyethylene shipment bottle. Rinse the three midget impingers and the connecting tubes with dis

Concentration of sulfur dioxide

at standard conditions, dry basis, lb./cu. ft.

7.05 X 10-5 Conversion factor, including the number of grams per gram equivalent of sulfur dioxide (32 g./g.-eq.), 453.6 g./lb., and 1,000 ml./1., lb.-1./g.-ml.

=

V1- Volume of barium perchlorate titrant used for the sample, ml.

V-Volume of barium perchlorate titrant used for the blank, ml. N=Normality of barium perchlorate titrant, g.-eq./1.

Voln Total solution volume of sulfur dioxide, 50 ml.

V=Volume of sample aliquot titrated, ml.

Vmta Volume of gas sample through the dry gas meter (standard conditions), cu. ft., see Equation 6-1.

7. References. Atmospheric Emissions from Sulfuric Acid Manufacturing Processes, U.S. DHEW, PHS, Division of Air Pollution, Public Health Service Publication No. 999-AP-13, Cincinnati, Ohio, 1965.

Corbett, P. F., The Determination of SO, and SO, in Flue Gases, Journal of the Institute of Fuel, 24:237-243, 1961.

Matty, R. E. and E. K. Diehl, Measuring Flue-Gas SO, and SO,, Power 101:94-97, November, 1957.

Patton, W. F. and J. A. Brink, Jr., New Equipment and Techniques for Sampling Chemical Process Gases, J. Air Pollution Control Association, 13, 162 (1963).

°R

std.

=

in. Hg (Vabar)

equation 6-1

Vm.td- Volume of gas sample through the dry gas meter (standard conditions), cu. ft.

m

V Volume of gas sample through the dry gas meter (meter conditions), cu. ft.

Tata Absolute temperature at standard conditions, 530° R. T-Average dry gas meter temperature, °R.

Pbar Barometric pressure at the orifice meter, inches Hg.

Patd-Absolute pressure at standard conditions, 29.92 inches Hg.

6.2 Sulfur dioxide concentration.

(V2-V) N (V.)

Vmatd

equation 6-2

METHOD 7—DETERMINATION OF NITROGEN OXIDE EMISSIONS FROM STATIONARY SOURCES

1. Principle and applicability.

1.1 Principle. A grab sample is collected in an evacuated flask containing a dilute sulfuric acid-hydrogen peroxide absorbing solution, and the nitrogen oxides, except nitrous oxide, are measure colorimetrically using the phenoldisulfonic acid (PDS) procedure.

1.2 Applicability. This method is applicable for the measurement of nitrogen oxides from stationary sources only when specified by the test procedures for determining compliance with New Source Performance Standards.

2. Apparatus.

2.1 Sampling. See Figure 7-1.

2.1.1 Probe-Pyrex1 glass, heated, with filter to remove particulate matter. Heating is unnecessary if the probe remains dry during the purging period.

2.1.2 Collection flask-Two-liter, Pyrex,1 round bottom with short neck and 24/40 standard taper opening, protected against implosion or breakage.

2.1.3 Flask valve-T-bore stopcock connected to a 24/40 standard taper joint.

2.1.4 Temperature gauge-Dial-type thermometer, or equivalent, capable of measuring 2° F. intervals from 25° to 125° F.

2.1.5 Vacuum line-Tubing capable of withstanding a vacuum of 3 inches Hg absolute pressure, with "T" connection and T-bore stopcock, or equivalent.

2.1.6 Pressure gauge-U-tube manometer, 36 inches, with 0.1-inch divisions, or equivalent.

1 Trade name.