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particulate matter from the filter holder and place in a sample bottle. Place the contents (measured to +1 ml) of the first three impingers into another sample bottle. Rinse the probe and all glassware between it and the back half of the third impinger with water and acetone, and add this to the latter sample bottle. Clean the probe with a brush or a long slender rod and cotton balls. Use acetone while cleaning. Add these to the sample bottle. Retain a sample of the water and acetone as & blank. The total amount of wash water and acetone used should be measured for accurate blank correction. Place the silica gel in the plastic jar. Seal and secure all sample containers for shipment. If an additional test is desired, the glassware can be carefully double rinsed with distilled water and reassembled. However, if the glassware is to be out of
more than 2 days, the initial acid wash procedure must be followed.
4.8.1 Apparatus preparation.-Clean all glassware according to the procedure of section 4.5.1. Adjust the instrument settings according to the instrument manual, using an absorption wavelength of 234.8 nm.
4.8.2 Sample preparation.—The digestion of beryllium samples is accomplished in part in concentrated perchloric acid. Caution: The analyst must insure that the sample is heated to light brown fumes after the initial nitric acid addition; otherwise, dangerous perchlorates may result from the subsequent perchloric acid digestion. Perchloric acid also should be used only under a perchloric acid hood.
18.104.22.168 Transfer the filter and any Toose particulate matter from the sample container to a 150 ml beaker. Add 35 ml concentrated nitric acid. Heat on a hotplate until light brown fumes are evident to destroy all organic matter. Cool to room temperature and add 5 ml concentrated sulfuric acid and 5 ml concentrated perchloric acid. Then proceed with step 22.214.171.124.
126.96.36.199 Place a portion of the water and acetone sample into a 150 ml beaker and put on a hotplate. Add portions of the remainder as evaporation proceeds and evaporate to dryness. Cool the residue and add 35 ml concentrated nitric acid. Heat on a hotplate until light brown fumes are evident to destroy any organic matter. Cool to room temperature and add 5 ml concentrated sulfuric acid, and 5 ml concentrated perchloric acid. Then proceed with step 188.8.131.52.
184.108.40.206 Weigh the spent silica gel and report to the nearest gram.
220.127.116.11 Samples from 18.104.22.168 and 22.214.171.124 may be combined here for ease of analysis. Replace on a hotplate and evaporate to dryness in a perchloric acid hood. Cool and dissolve the residue in 10.0 ml of 25 percent V/V hydrochloric acid. Samples are now ready for the atomic absorption unit. The
beryllium concentration of the sample must be within the callbration range of the unit. If necessary, further dilution of sample with 25 percent V/V hydrochloric acid must be performed to bring the sample within the calibration range.
4.8.3 Beryllium determination.—Analyze the samples prepared in 4.8.2 at 234.8 nm using a nitrous oxide/acetylene flame. Aluminum, silicon and other elements can interfere with this method if present in large quantities. Standard methods are available, however, to effectively eliminate these interferences (see Reference 5).
5. Calibration-5.1 Sampling train. 5.1.1 Use standard methods and equipment as detailed in APTD-0576 to calibrate the rate meter, pitot tube, dry gas meter and probe heater (if used). Recallbrate prior to each test series.
5.2 Analysis.-5.2.1 Standardization is made with the procedure as suggested by the manufacturer with standard beryllium solution. Standard solutions will be prepared from the stock solution by dilution with 25 percent V/V hydrochloric acid. The linearity of working range should be established with a series of standard solutions. If collected samples are out of the linear range, the samples should be diluted. Standards should be interspersed with the samples since the calibration can change slightly with time.
6. Calculations-6.1 Average dry gas meter temperature, stack temperature, stack pressure and average orifice pressure drop. See data sheet (figure 104–6).
6.2 Dry gas volume.-Correct the sample volume measured by the dry gas meter to stack conditions by using equation 104–2.
where: Vme=Volume of gas sample through the dry gas meter
(stack conditions), ft3. Vm=Volume of gas sample through the dry gas meter
(meter conditions), ft3. T.=Average temperature of stack gas, °R. Tm=Average dry gas meter temperature, °R. Pbar=Barometric pressure at the orifice meter, in Hg. AH=Average pressure drop across the orifice meter,
in H20. 13. 6=Specific gravity of mercury.
Pi=Stack pressure, Pbar + static pressure, in Hg. 6.3 Volume of water vapor.
eq. 104-3 where: Vo=Volume of water vapor in the gas sample (stack
conditions), ft3. K=0.00267
when these units are used.
ml°R =Total volume of liquid collected in impingers
and silica gel (see figure 104-7), ml. T,= Average stack gas temperature, °R. P,=Stack pressure, Pbar+static pressure, in Hg.
6.4 Total gas volume.
V total=Vm, + V.,
where: Votat=Total volume of gas sample (stack conditions),
ft3. Vme=Volume of gas through dry gas meter (stack
conditions), ft3. Vw=Volume of water vapor in gas sample (stack
conditions), ft3. 6.5 Stack gas velocity.
Use equation 104-5 to calculate the stack gas velocity.
Ci=Concentration of beryllium found in
sample, ug/ml. Vw=Total volume of water used in sam
filing (impinger contents plus all
wash amounts), ml. Cw=Blank concentration of beryllium in
water, mg/ml. Va=Total volume of acetone used in sam
pling (all wash amounts), ml. Ca=Blank concentration of beryllium in
acetone, ug/ml. 6.7 Total beryllium emissions.-Calculate the total amount of beryllium emitted from each stack per day by equation 104–7. 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. W(v.) ave. A. 86,400
86,400 seconds/day R=
(v.) ave.=K,C,(V p)ove. V P,M, K
R=Rate of emission, g/day.
Wi=Total weight of beryllium collected, ug. Vtotal=Total volume of gas sample (stack conditions),
ft. (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).
when these units are used. Co-Pitot tube coefficient, dimensionless. (T.).vg.= Average stack gas temperature, °R. (MAD). -Average square root of the velocity head
of stack gas (inH;0)1/2 (see figure 104-8). P,=Stack pressure, Pbartstatic pressure, in
the summation of the products of the
in the mixture, lb/b-mole. Figure 104–8 shows a sample recording sheet for velocity traverse data. Use the averages in the last two columns of figure 104-8 to determine the average stack gas velocity from equation 104-5.
6.6 Beryllium collected.-Calculate the total weight of beryllium collected by using equation 104-6.
W:=VC1-V w Cw-VaCa.-eq. 104-6 where: Vi=Total weight of beryllium collected,
from step 126.96.36.199, ml.
eq. 104-8 where:
I=Percent of isokinetic sampling.
O=Sampling time, sec. (n.) 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 repetitions 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 percent <I>110 percent, the results are acceptable; otherwise, reject the test and repeat.
7. References.-1. Addendum to Specifications for Incinerator Testing at Federal Facilities, PHS, NCAPC, December 6, 1967.
2. Amos, M. D., and willis, J. B., "Use of High-Temperature Pre-Mixed Flames in Atomic Absorption Spectroscopy," Spectrochim. Acta, 22: 1325, 1966.
3. Determining Dust Concentration in a Gas Stream, ASME Performance Test Code No. 27, New York, N.Y., 1957.
4. Devorkin, Howard et al., Air Pollution Source Testing Manual, Air Pollution Control District, Los Angeles, Calif. November 1963.
5. Fleet, B., Liberty, K. V., and West, T. S., "A Study of Some Matrix Effects in the Determination of Berylllum by Atomic Absorption Spectroscopy in the Nitrous Oxide-Acetylene Flame," Talanta, 17: 203, 1970.
6. Mark, L. S., Mechanical Engineers' Handbook, McGraw-HW Book Co., Inc., New York, N.Y., 1951.
7. Martin, Robert M., Construction Details of Isokinetic Source Sampling Equipment, Environmental Protection Agency, APTD0581.
8. Methods for Determination of Velocity, Volume, Dust and Mist Content of Gases, Western Precipitation Division of Joy Manufacturing Co., Los Angeles, Calif. Bulletin WP-50, 1968.
9. Perkin Elmer Standard Conditions (Rev. March 1971).
10. Perry, J. H., Chemical Engineers' Handbook, McGraw-Hill Book Co., Inc., New York, N.Y., 1960.
11. Rem, Jerome J., Maintenance, Calibration, and Operation of Isokinetic Source Sampling Equipment, Environmental Protection Agency, APTD-0576.
12. 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.
13. Smith, W. S. et al., Stack Gas Sampling Improved and Simplified with New Equipment, APCA Paper No. 67–119, 1967.
14. 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.
15. Specifications for Incinerator Testing at Federal Facilities, PHS, NCAPC, 1967.
16. Standard Method for Sampling Stacks for Particulate Matter, In: 1971 Book of ASTM standards, Part 23, Philadelphia. 1971, ASTM Designation D-2928–71.
17. Vennard, J. K. Elementary Fluid Me. chanics. John Wiley and Sons, Inc., New York, 1947.
AUTHORITY: The provisions of this past 76 issued under Executive Order 11507; Heorg. Plan 3 of 1970; 3 CFR, 1970 Comp.
SOURCE: The provisions of this Part 76 appear at 36 F.R. 22417, Nov. 25, 1971, unless otherwise noted. & 76.1 Definitions.
As used in this part:
(a) "Executive Order" means Executive Order No. 11507.
(b) “Nonurban areas" means all areas other than urban areas.
(c) "Ringelmann Scale" means the Ringelmann Scale as published in the latest U.S. Bureau of Mines Information Circular entitled “Ringelmann Smoke Chart".
(d) “Administrator” means the Administrator of the Environmental Protection Agency or his authorized representative.
(e) “Urban areas" means those areas classified as urban in the latest available Federal census, or as Standard Metropolitan Statistical Areas.
(f) “Unit” means all indirect beat exchangers connected to a single stack.
(g) "Particulate matter" means any material, except uncombined water, that exists as a solid or liquid at standard conditions.
(h) “Standard conditions" means a temperature of 70° Fahrenheit and a pressure of 14.7 pounds per square inch, absolute.
(i) “Waste" means any solid, liquid, or gaseous substance, the disposal of which may create an air pollution problem. 8 76.2 Intent.
It is the intent of these standards that emissions to the atmosphere from Federal facilities and buildings shall not be permitted if such emissions endanger health or welfare and that emissions which are likely to be injurious or hazardous to people, animals, vegetation, or property shall be minimized. $ 76.3 Applicability.
(a) Unless otherwise indicated, the standards in this part apply to both new and existing Federal facilities and buildings.
(b) Except for discharges of radioactive effluents which are regulated by the Atomic Energy Commission, Federal facilities and buildings shall conform to the air pollution standards prescribed
PART 76 PREVENTION, CONTROL,
MEASUREMENT Sec. 76.1 Definitions. 76.2 Intent. 76.3 Applicability. 76.4 Combustion of fuel. 76.5 Sulfur oxides. 76.6 Stacks. 76.7 Storage and handling of fuels and ash. 76.8 Disposal of waste. 76.9 Other pollution producing processes.
by the State or community in which they are located. If State or local standards are not prescribed for a particular location, or if the State or local standards are less stringent than the standards prescribed herein, the standards in this part shall be applicable to discharges from such Federal facilities and buildings except as otherwise indicated.
(c) Temporary operations that may result in potential air pollution problems, such as those associated with research, development, test, evaluation, space, and military activities, shall be conducted with such precautions and safeguards as are needed to achieve the intent of these standards.
(d) The Administrator may, upon application of the relevant department, agency or establishment, exempt any Federal facility or building from any or all of these standards whenever he determines that the activities of such building or facility will not significantly conflict with the intent of the Executive order and that such an exemption is in the public interest. $ 76.4 Combustion of fuel.
(a) The following standards apply to the combustion units of facilities and buildings having a heat input of less than 1,000 million B.t.u./hour, other than fireplaces, stoves, or grills burning wood or charcoal:
(1) Manually fired equipment shall not be installed as new or replacement equipment, except for the burning of anthracite, coke, or smokeless fuel.
(2) (i) For new units, except during startup, cleaning of fires, or soot blowing, the density of any emission to the atmosphere shall not exceed No. 1 on the Ringelmann Scale.
(ii) For existing units, except during startup, cleaning of fires, or soot blowing, the density of any emission to the
atmosphere shall not exceed No. 2 on the Ringelmann Scale.
(3) A photoelectric or other type smoke detector, recorder, or alarm shall be installed on units larger than ten million BTU per hour input, except where gas or light oil (No. 2 or lighter), is burned. (4) During routine
operation, the emission of particles larger than 60 microns shall not normally occur.
(5) Means shall be provided in all newly constructed units and wherever practicable in existing units to allow the periodic measurement of flyash and other particulate matter..
(6) All new or replacement spreader stoker installations shall be of a type that automatically discharges ashes to the ash pit, either continuously or in very frequent small increments, and flyash shall be reinjected only from boller passes.
(7) For units of less than 10 million BTU/hour heat input, the emission of flyash and other particulate matter shall not exceed 0.6 pounds of particulate matter per million BTU heat input, as measured by the American Society of Mechanical Engineers Power Test Code No. 27 for “Determining Dust Concentrations in a Gas Stream,” or equivalent test method.
(8) For units between 10 million and 1,000 million BTU/hour heat input, the emission of flyash and other particulate matter shall not exceed that specified in figure 1, as measured by the test method specified in subparagraph (7) of this paragraph.
(b) For units having a heat input of more than 1,000 million BTU/hour, the appropriate department, agency, or establishment shall seek special advice from the Administrator with regard to smoke, flyash, and other particulate emissions.