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4.3 Analysis. Record the data required on 6.3 Volume of water vapor. the example sheet shown in Figure 6-3. Handle each sample container as follows:

-V. pH0 RT. lb. Container No. 1. Transfer the filter and

atd . MH,0 Potd 454 gm. 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.

equation 5-2 Container No. 2. Transfer the acetone washings to a tared beaker and evaporate to where: dryness at ambient temperature and pres Vw.ra=Volume of water vapor in the gas sure. Desiccate and dry to a constant weight.

sample (standard conditions), Report results to the nearest 0.5 mg.

cu. ft. Container No. 3. Weigh the spent silica gel Vir=Total volume of liquid collected in and report to the nearest gram.

impingers and silica gel (see Fig5. Calibration.

uro 5–3), ml. Use methods and equipment which have

21,0- Density of water, 1 g/ml. been approved by the Administrator to Mu,o=Molecular weight of water, 18 lb./ calibrate the orifice meter, pitot tube, dry

Ib.-mole. gas meter, and probe heater. Recalibrate

R=Ideal gas constant, 21.83 inches after each test series.

Hg-cu. ft./lb.-mole-°R. 6. Calculations.

T..a=Absolute temperature at standard 6.1 Average dry gas meter temperature

conditions, 530° R. and average orifice pressure drop. See data sheet (Figure 5-2).

Para- Absolute pressure at standard con

ditions, 29.92 inches Hg. 6.2 Dry gas volume. Correct the sample volume measured by the dry gas meter to 6.4 Moisture content. standard conditions (70° F., 29.92 inches Hg) by using Equation 5–1.

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equation 5-3

equation 5-1 where: Vm.: Volume of gas sample through the

dry gas meter (standard condi

tions), cu. ft. V.= Volume of gas sample through the

dry gas meter (meter condi

tions), cu. ft. T... Absolute temperature at standard

conditions, 530° R. T.= Average dry gas meter temperature,

where:
Bwo =Proportion by volume of water vapor in the gas

stream, dimensionless.
Vwotd-Volume of water in the gas sample (standard

conditions), cu. ft. Vmd=Volume of gas sample through the dry gas meter

(standard conditions), cu. ft.
6.5 Total particulate weight. Determino
the total particulate catch from the sum of
the weights on the analysis data sheet
(Figure 5-3).

6.6 Concentration.
6.6.1 Concentration in gr./8.c.1.

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Pbar - Barometric pressure at the orifice

meter, inches Hg. AH= Average pressure drop across the

orifice meter, inches H,O. 13.6=Specific gravity of mercury. P..- Absolute pressure at standard con

ditions, 29.92 inches Hg.

equation 5-4 where: d'=Concentration of particulato matter in stack

gas, gr./s.c.f., dry basis. Mg=Total amount of particulate matter collected,

mg. Vand Volume of gas sample through dry gas meter

(standard conditions), cu. ft.

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CONVERT WEIGHT OF WATER TO VOLUME BY DIVIDING TOTAL WEIGHT
INCREASE BY DENSITY OF WATER. (1 g. ml):

INCREASE. 9 - VOLUME WATER, ml

(1 g/ml)

Figure 5-3. Analytical data.

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6.6.2 Concentration in lb./cu. ft.

1 lb. m
153,600 mg.)
-=2.205X10-

equation 5–5 where:

Mg-Total amount of particulate matter collected Co=Concentration of particulate matter in stack

mg. gas, lb./s.c.f., dry basis.

V. -Volume of gas sample through dry gas meter 453,600 Mg/16.

(standard conditions), cu. ft. 6.7 Isokinetic variation.

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where:

I=Percent of isokinetic sampling.
V1.- Total volume of liquid collected in Impingers

and sllica gel (See Fig. 5-3), ml.
P8,0=Density of water, 18./mnl.
R-Ideal gas constant, 21.83 inches Hg-cu. ft./lb.

mole°R. MA,o=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.O.
T,=Absolute average stack gas temperature (see

Fig. 5-2). "R
0=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: I 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 63 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 apple cable for the determination of sulfur dioxido emissions from stationary sources only when specified by the test procedures for determining compliance with New Source Performanco Standards.

2. Apparatus.
2.1 Sampling. See Figure 6-1.

2.1.1 Probe Pyrexglass, approximately 5 to 6 mm. D, 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 glase wool packed in top to prevent sulfuric acid mist carryover.

2.1.3 Glass wool.
2.1.4 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 accurato to measure the sample volume within 1%.

2.1.10 Pltot tube-Type S, or equivalent necessary only 11 a sample traverse is required, or 1 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.

PROBE (END PACKED
WITH QUARTZ OR
PYREX WOOLL

STACK WALL

SILICA GEL DRYING TUBE
MIDGET BUBBLER MIDGET IMPINGERS
GLASS WOOL

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Figure 6-1. SO2 sampling train. 2.3.1 Pipettes-Transfer type, 5 ml, and 4.1.1 Preparation of collection train. Pour 10 ml. sizes (0.1 ml. divisions) and 25 ml. 15 ml. of 80% isopropanol into the midget size (0.2 ml. divisions).

bubbler and 15 ml. of 3% hydrogen peroxido 2.3.2 Volumetric flasks-50 ml., 100 ml., into each of the first two midget impingers. and 1,000 ml.

Leave the final midget impinger dry. Assem2.3.3 Burettes—5 ml. and 50 ml.

ble the train as shown in Figure 6-1. Leak 2.3.4 Erlenmeyer flask—125 ml.

check the sampling train at the sampling 3. Reagents.

site by plugging the probe inlet and pulling 3.1 Sampling.

a 10 inches Hg vacuum. A leakage rate not 3.1.1 Water-Deionized, distilled.

in excess of 1% of the sampling rate is ac3.1.2 Isopropanol, 80%-MIX 80 ml, of iso ceptable. Carefully release the probe inlet propanol with 20 ml. of distilled water.

plug and turn off the pump. Place crushed 3.1.3 Hydrogen peroxide, 3%-dilute 100 ice around the impingers. Add more ice durm!. of 30% hydrogen peroxide to 1 liter with ing the run to keep the temperature of the distilled water. Prepare fresh daily.

gases leaving the last impinger at 70° F. or 3.2 Sample recovery.

less. 3.2.1 Water-Delonized, distilled.

4.1.2 Sample collection. Adjust the sam3.2.2 Isopropanol, 80%.

ple flow rate proportional to the stack gas 3.3 Analysis.

velocity. Take readings at least every five 3.3.1 Water-Delonized, distilled.

minutes and when significant changes in 3.3.2 Isopropanol.

stack conditions necessitate additional ad3.3.3 Thorin Indicator-1-(0-arsonophen

justments in flow rate. To begin sampling, ylazo)-2-naphthol-3,6-disulfonic acid, diso

position the tip of the probe at the first dium salt (or equivalent). Dissolve 0.20 g. in sampling point and start the pump. Sam100 ml. distilled water.

ple proportionally throughout the run. At 3.3.4 Barlum perchlorate (0.01 N)-Dis

the conclusion of each run, turn off tho solve 1.95 g of barlum perchlorate

pump and record the final readings. Remove (Ba(CIO), 3H,O) in 200 ml. distilled water

the probe from the stack and disconnect it and dilute to 1 liter with isopropanol. Stand

from the train. Drain the ice bath and purge ardize with sulfuric acid. Barlum chloride

the remaining part of the train by drawing may be used.

clean ambient air through the system for 15 3.3.5 Sulfuric acid standard (0.01 N)

minutes. Purchase or standardize to +0.0002 N

4.2 Sample recovery. Disconnect the imagainst 0.01N NaOH which has previously

pingers after purging. Discard the contents been standardized against potassium acid

of the midget bubbler. Pour the contents of phthalate (primary standard grade).

the midget impingers into a polyethylene 4. Procedure.

shipment bottle. Rinse the three midget im. 4.1 Sampling.

pingers and the connecting tubes with dis

standard conditions (70° F. and 29.92 inches Hg) by using equation 6–1.

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tilled water and add these washings to the same storage container.

4.3 Sample analysis. Transfer the contents of the storage container to & 50 ml. volumetric flask. Dilute to the mark with deionized, distilled water. Pipette & 10 ml. aliquot of this solution into a 125 ml. Erlenmeyer flask. Add 40 ml. of isopropanol and two to four drops of thorin indicator. Titrate to & pink endpoint using 0.01 N barium perchlorate. Run a blank with each series of samples.

5. Calibration.

5.1 Use standard methods and equipment which have been approved by the Administrator to calibrate the rotameter, pitot tube, dry gas meter, and probe heater.

5.2 Standardize the barium perchlorate against 25 ml. of standard sulfuric acid containing 100 ml, of isopropanol.

0. Calculations.

8.1 Dry gas volume. Correct the sample volume measured by the dry gas meter to

where: Vmeta= Volume of gas sample through the

dry gas meter (standard condi

tions), cu. ft. V.- Volume of gas sample through the

dry gas meter (meter condi

tions), cu. ft. T...- Absolute temperature at standard

conditions, 530° R.
T.= Average dry gas meter temperature,

°R.
Pber=Barometric pressure at the orifice

meter, inches Hg.
Para- Absolute pressure at standard con-

ditions, 29.92 inches Hg. 6.2 Sulfur dioxide concentration.

ota)

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where: Cso,= Concentration of sulfur dioxide

at standard conditions, dry

basis, lb./cu. ft. 7.05 X 10-6= 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., Ib.-1./g.-ml. V, 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. Vsop=Total solution volume of sullur

dioxide, 50 ml. V.= Volume of sample aliquot ti

trated, ml. Vmate Volume of gas sample through

the dry gas meter (standard conditions), cu. ft., see Equa

tion 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 soz, 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).

mata

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--Pyrex 1 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 ther. mometer, 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.

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