40 CFR Part 763 (EPA AHERA) - Asbestos Calibration Procedures PDF

Summary

This document outlines the calibration procedures for asbestos measurements, including the preparation of calibration standards and analysis of samples. The procedures involve milling and sizing asbestos materials, creating isopropanol suspensions, and measuring normalized intensities using step scans and diagnostic reflections. Calculations and correction factors, such as transmittance and correction factor f(T), complete the analysis.

Full Transcript

Pt. 763, Subpt. E, App. E 40 CFR Ch. I (7–1–07 Edition) rfrederick on PROD1PC67 with CFR 2.8.1 Calibration Preparation of Calibration Standards 1. Mill and size standard asbestos materials according to the procedure outlined in Section 2.7.2.1.1. Equivalent, standardized matrix reduction and s...

Pt. 763, Subpt. E, App. E 40 CFR Ch. I (7–1–07 Edition) rfrederick on PROD1PC67 with CFR 2.8.1 Calibration Preparation of Calibration Standards 1. Mill and size standard asbestos materials according to the procedure outlined in Section 2.7.2.1.1. Equivalent, standardized matrix reduction and sizing techniques should be used for both standard and sample materials. 2. Dry at 100 °C for 2 hr; cool in a desiccator. 3. Prepare two suspensions of each standard in isopropanol by weighing approximately 10 and 50 mg of the dry material to the nearest 0.01 mg. Quantitatively transfer each to a 1–L volumetric flask with approximately 200 mL isopropanol to which a few drops of surfactant have been added. 4. Ultrasonicate for 10 min at a power density of approximately 0.1 W/mL, to disperse the asbestos material. 5. Dilute to volume with isopropanol. 6. Place the flask on a magnetic stirring plate. Stir. 7. Prepare, in triplicate, a series of at least five standard filters to cover the desired analytical range, using appropriate aliquots of the 10 and 50 mg/L suspensions and the following procedure. Mount a silver membrane filter on the filtration apparatus. Place a few milliliters of isopropanol in the reservoir. Vigorously hand shake the asbestos suspension and immediately withdraw an aliquot from the center of the suspension. Do not adjust the volume in the pipet by expelling part of the suspension; if more than the desired aliquot is withdrawn, discard the aliquot and resume the procedure with a clean pipet. Transfer 2.8.2 Analysis of Calibration Standards 1. Mount each filter on a flat holder. Perform step scans on selected diagnostic reflections of the standards and reference specimen using the procedure outlined in Section 2.7.2.3, step 12, and the same conditions as those used for the samples. 2. Determine the normalized intensity for each peak measured, Îs̊td, as outlined in Section 2.7.2.3, step 14. 2.9 Calculations For each asbestos reference material, calculate the exact weight deposited on each standard filter from the concentrations of the standard suspensions and aliquot volumes. Record the weight, w, of each standard. Prepare a calibration curve by regressing Î2s̊td on w. Poor reproducibility (±15 percent RSD) at any given level indicates problems in the sample preparation technique, and a need for new standards. The data should fit a straight line equation. Determine the slope, m, of the calibration curve in counts/microgram. The intercept, b, of the line with the Îs̊td axis should be approximately zero. A large negative intercept indicates an error in determining the background. This may arise from incorrectly measuring the baseline or from interference by another phase at the angle of background measurement. A large positive intercept indicates an error in determining the baseline or that an impurity is included in the measured peak. Using the normalized intensity, ÎAg, for the attenuated silver peak of a sample, and the corresponding normalized intensity from the unattenuated silver peak, ÎA˚g, of the sample filter, calculate the transmittance, T, for each sample as follows: 26,27 Determine the correction factor, f(T), for each sample according to the formula: -R (ln T) f (T) = llll l-TR where 846 VerDate Aug<31>2005 14:36 Aug 06, 2007 Jkt 211171 PO 00000 Frm 00856 Fmt 8010 Sfmt 8003 Y:\SGML\211171.XXX 211171 EC01AP92.019</MATH> 2.8 the aliquot to the reservoir. Keep the tip of the pipet near the surface of the isopropanol. Filter rapidly under vacuum. Do not wash the sides of the reservoir. Leave the vacuum on for a time sufficient to dry the filter. Release the vacuum and remove the filter with forceps. EC01AP92.018</GPH> background on each side of the peak for onehalf the peak-scanning time. The net intensity, Ia, is the difference between the peak integrated count and the total background count. 13. Determine the net count, IAg, of the filter 2.36 Å silver peak following the procedure in step 12. Remove the filter from the holder, reverse it, and reattach it to the holder. Determine the net count for the unattenuated silver peak, IA˚g. Scan times may be less for measurement of silver peaks than for sample peaks; however, they should be constant throughout the analysis. 14. Normalize all raw, net intensities (to correct for instrument instabilities) by referencing them to an external standard (e.g., the 3.34 Å peak of an a-quartz reference crystal). After each unknown is scanned, determine the net count, Ir̊, of the reference specimen following the procedure in step 12. Determine the normalized intensities by dividing the peak intensities by Ir̊: Environmental Protection Agency R= Pt. 763, Subpt. E, App. E sin QAg llll sin Qa qAg=angular position of the measured silver peak (from Bragg’s Law), and qa=angular position of the diagnostic asbestos peak. Calculate the weight, Wa, in micrograms, of the asbestos material analyzed for in each sample, using the appropriate calibration data and absorption corrections: Calculate the percent composition, Pa, of each asbestos mineral analyzed for in the parent material, from the total sample weight, WT, on the filter: Pa = Wa(1-.01L) llll— WT x 100 where Pa=percent asbestos mineral in parent material; Wa=mass of asbestos mineral on filter, in µg; WT=total sample weight on filter, in µg; L=percent weight loss of parent material on ashing and/or acid treatment (see Section 2.7.2.3). References 1. H. P. Klug and L. E. Alexander, X-ray Diffraction Procedures for Polycrystalline and Amorphous Materials, 2nd ed., New York: John Wiley and Sons, 1979. 2. L. V. Azaroff and M. J. Buerger, The Powder Method of X-ray Crystallography, New York: McGraw-Hill, 1958. 3. JCPDS-International Center for Diffraction Data Powder Diffraction File, U.S. Department of Commerce, National Bureau of Standards, and Joint Committee on Powder Diffraction Studies, Swarthmore, PA. 4. W. J. Campbell, C. W. Huggins, and A. G. Wylie, Chemical and Physical Characterization of Amosite, Chrysotile, Crocidolite, and Nonfibrous Tremolite for National Institute of Environmental Health Sciences Oral Ingestion Studies, U.S. Bureau of Mines Report of Investigation RI8452, 1980. 5. B. A. Lange and J. C. Haartz, Determination of microgram quantities of asbestos by X-ray diffraction: Chrysotile in thin dust layers of matrix material, Anal. Chem., 51(4):520–525, 1979. 6. NIOSH Manual of Analytical Methods, Volume 5, U.S. Dept. HEW, August 1979, pp. 309–1 to 309–9. 847 VerDate Aug<31>2005 14:36 Aug 06, 2007 Jkt 211171 PO 00000 Frm 00857 Fmt 8010 Sfmt 8002 Y:\SGML\211171.XXX 211171 EC01AP92.020</MATH> rfrederick on PROD1PC67 with CFR 2.10 7. H. Dunn and J. H. Stewart, Jr., Quantitative determination of chrysotile in building materials, The Microscope, 29(1), 1981. 8. M. Taylor, Methods for the quantitative determination of asbestos and quartz in bulk samples using X-ray diffraction, The Analyst, 103(1231):1009–1020, 1978. 9. L. Birks, M. Fatemi, J. V. Gilfrich, and E. T. Johnson, Quantitative Analysis of Airborne Asbestos by X-ray Diffraction, Naval Research Laboratory Report 7879, Naval Research Laboratory, Washington, DC, 1975. 10. U.S. Environmental Protection Agency, Asbestos-Containing Materials in School Buildings: A Guidance Document, Parts 1 and 2, EPA/OPPT No. C00090, March 1979. 11. J. B. Krause and W. H. Ashton, Misidentification of asbestos in talc, pp. 339– 353, in: Proceedings of Workshop on Asbestos: Definitions and Measurement Methods (NBS Special Publication 506), C. C. Gravatt, P. D. LaFleur, and K. F. Heinrich (eds.), Washington, DC: National Measurement Laboratory, National Bureau of Standards, 1977 (issued 1978). 12. H. D. Stanley, The detection and identification of asbestos and asbesti-form minerals in talc, pp. 325–337, in Proceedings of Workshop on Asbestos: Definitions and Measurement Methods (NBS Special Publication 506), C. C. Gravatt, P. D. LaFleur, and K. F. Heinrich (eds.), Washington, DC, National Measurement Laboratory, National Bureau of Standards, 1977 (issued 1978). 13. A. L. Rickards, Estimation of trace amounts of chrysotile asbestos by X-ray diffraction, Anal. Chem., 44(11):1872–3, 1972. 14. P. M. Cook, P. L. Smith, and D. G. Wilson, Amphibole fiber concentration and determination for a series of community air samples: use of X-ray diffraction to supplement electron microscope analysis, in: Electron Microscopy and X-ray Applications to Environmental and Occupation Health Analysis, P. A. Russell and A. E. Hutchings (eds.), Ann Arbor: Ann Arbor Science Publications, 1977. 15. A. N. Rohl and A. M. Langer, Identification and quantitation of asbestos in talc, Environ. Health Perspectives, 9:95–109, 1974. 16. J. L. Graf, P. K. Ase, and R. G. Draftz, Preparation and Characterization of Analytical Reference Minerals, DHEW (NIOSH) Publication No. 79–139, June 1979. 17. J. C. Haartz, B. A. Lange, R. G. Draftz, and R. F. Scholl, Selection and characterization of fibrous and nonfibrous amphiboles for analytical methods development, pp. 295–312, in: Proceedings of Workshop on Asbestos: Definitions and Measurement Methods (NBS Special Publication 506), C. C. Gravatt, P. D. LaFleur, and K. F. Heinrich (eds.), Washington, DC: National Measurement Laboratory, National Bureau of Standards, 1977 (issued 1978). 18. Personal communication, A. M. Langer, Environmental Sciences Laboratory, Mount § 763.120 40 CFR Ch. I (7–1–07 Edition) Sinai School of Medicine of the City University of New York, New York, New York. 19. A. M. Langer, M. S. Wolff, A. N. Rohl, and I. J. Selikoff, Variation of properties of chrysotile asbestos subjected to milling, J. Toxicol. and Environ. Health, 4:173–188, 1978. 20. A. M. Langer, A. D. Mackler, and F. D. Pooley, Electron microscopical investigation of asbestos fibers, Environ. Health Perspect., 9:63–80, 1974. 21. E. Occella and G. Maddalon, X-ray diffraction characteristics of some types of asbestos in relation to different techniques of comminution, Med. Lavoro, 54(10):628–636, 1963. 22. K. R. Spurny, W. Stöber, H. Opiela, and G. Weiss, On the problem of milling and ultrasonic treatment of asbestos and glass fibers in biological and analytical applications, Am. Ind. Hyg. Assoc. J., 41:198–203, 1980. 23. L. G. Berry and B. Mason, Mineralogy, San Francisco: W. H. Greeman & Co., 1959. 24. J. P. Schelz, The detection of chrysotile asbestos at low levels in talc by differential thermal analysis, Thermochimica Acta, 8:197– 204, 1974. 25. Reference 1, pp. 372–374. 26. J. Leroux, Staub-Reinhalt Luft, 29:26 (English), 1969. 27. J. A. Leroux, B. C. Davey, and A. Paillard, Am. Ind. Hyg. Assoc. J., 34:409, 1973. [47 FR 23369, May 27, 1982; 47 FR 38535, Sept. 1, 1982; Redesignated at 60 FR 31922, June 19, 1995] Subpart F [Reserved] Subpart G—Asbestos Worker Protection SOURCE: 65 FR 69216, Nov. 15, 2000, unless otherwise noted. rfrederick on PROD1PC67 with CFR § 763.120 What is the purpose of this subpart? This subpart protects certain State and local government employees who are not protected by the Asbestos Standards of the Occupational Safety and Health Administration (OSHA). This subpart applies the OSHA Asbestos Standards in 29 CFR 1910.1001 and 29 CFR 1926.1101 to these employees. § 763.121 Does this subpart apply to me? If you are a State or local government employer and you are not subject to a State asbestos standard that OSHA has approved under section 18 of the Occupational Safety and Health Act or a State asbestos plan that EPA has exempted from the requirements of this subpart under § 763.123, you must follow the requirements of this subpart to protect your employees from occupational exposure to asbestos. § 763.122 What does this subpart require me to do? If you are a State or local government employer whose employees perform: (a) Construction activities identified in 29 CFR 1926.1101(a), you must: (1) Comply with the OSHA standards in 29 CFR 1926.1101. (2) Submit notifications required for alternative control methods to the Director, National Program Chemicals Division (7404), Office of Pollution Prevention and Toxics, Environmental Protection Agency, 1200 Pennsylvania Ave., NW., Washington, DC 20460. (b) Custodial activities not associated with the construction activities identified in 29 CFR 1926.1101(a), you must comply with the OSHA standards in 29 CFR 1910.1001. (c) Repair, cleaning, or replacement of asbestos-containing clutch plates and brake pads, shoes, and linings, or removal of asbestos-containing residue from brake drums or clutch housings, you must comply with the OSHA standards in 29 CFR 1910.1001. § 763.123 May a State implement its own asbestos worker protection plan? This section describes the process under which a State may be exempted from the requirements of this subpart. (a) States seeking an exemption. If your State wishes to implement its own asbestos worker protection plan, rather than complying with the requirements of this subpart, your State must apply for and receive an exemption from EPA. (1) What must my State do to apply for an exemption? To apply for an exemption from the requirements of this subpart, your State must send to the Director of EPA’s Office of Pollution Prevention and Toxics (OPPT) a copy of its asbestos worker protection regulations and a detailed explanation of how your State’s asbestos worker protection plan meets the requirements of TSCA section 18 (15 U.S.C. 2617). 848 VerDate Aug<31>2005 14:36 Aug 06, 2007 Jkt 211171 PO 00000 Frm 00858 Fmt 8010 Sfmt 8010 Y:\SGML\211171.XXX 211171 rfrederick on PROD1PC67 with CFR Environmental Protection Agency § 763.163 (2) What action will EPA take on my State’s application for an exemption? EPA will review your State’s application and make a preliminary determination whether your State’s asbestos worker protection plan meets the requirements of TSCA section 18. (i) If EPA’s preliminary determination is that your State’s plan does meet the requirements of TSCA section 18, EPA will initiate a rulemaking, including an opportunity for public comment, to exempt your State from the requirements of this subpart. After considering any comments, EPA will issue a final rule granting or denying the exemption. (ii) If EPA’s preliminary determination is that the State plan does not meet the requirements of TSCA section 18, EPA will notify your State in writing and will give your State a reasonable opportunity to respond to that determination. (iii) If EPA does not grant your State an exemption, then the State and local government employers in your State are subject to the requirements of this subpart. (b) States that have been granted an exemption. If EPA has exempted your State from the requirements of this subpart, your State must update its asbestos worker protection regulations as necessary to implement changes to meet the requirements of this subpart, and must apply to EPA for an amendment to its exemption. (1) What must my State do to apply for an amendment to its exemption? To apply for an amendment to its exemption, your State must send to the Director of OPPT a copy of its updated asbestos worker protection regulations and a detailed explanation of how your State’s updated asbestos worker protection plan meets the requirements of TSCA section 18. Your State must submit its application for an amendment within 6 months of the effective date of any changes to the requirements of this subpart, or within a reasonable time agreed upon by your State and OPPT. (2) What action will EPA take on my State’s application for an amendment? EPA will review your State’s application for an amendment and make a preliminary determination whether your State’s updated asbestos worker protection plan meets the requirements of TSCA section 18. (i) If EPA determines that the updated State plan does meet the requirements of TSCA section 18, EPA will issue your State an amended exemption. (ii) If EPA determines that the updated State plan does not meet the requirements of TSCA section 18, EPA will notify your State in writing and will give your State a reasonable opportunity to respond to that determination. (iii) If EPA does not grant your State an amended exemption, or if your State does not submit a timely request for amended exemption, then the State and local government employers in your State are subject to the requirements of this subpart. Subpart H [Reserved] Subpart I—Prohibition of the Manufacture, Importation, Processing, and Distribution in Commerce of Certain Asbestos-Containing Products; Labeling Requirements SOURCE: 54 FR 29507, July 12, 1989, unless otherwise noted. § 763.160 Scope. This subpart prohibits the manufacture, importation, processing, and distribution in commerce of the asbestoscontaining products identified and at the dates indicated in §§ 763.165, 763.167, and 763.169. This subpart requires that products subject to this rule’s bans, but not yet subject to a ban on distribution in commerce, be labeled. This subpart also includes general exemptions and procedures for requesting exemptions from the provisions of this subpart. § 763.163 Definitions. For purposes of this subpart: Act means the Toxic Substances Control Act, 15 U.S.C. 2601 et seq. Agency means the United States Environmental Protection Agency. 849 VerDate Aug<31>2005 14:36 Aug 06, 2007 Jkt 211171 PO 00000 Frm 00859 Fmt 8010 Sfmt 8010 Y:\SGML\211171.XXX 211171 rfrederick on PROD1PC67 with CFR § 763.163 40 CFR Ch. I (7–1–07 Edition) Asbestos means the asbestiform varieties of: chrysotile (serpentine); crocidolite (riebeckite); amosite (cummingtonite-grunerite); tremolite; anthophyllite; and actinolite. Asbestos-containing product means any product to which asbestos is deliberately added in any concentration or which contains more than 1.0 percent asbestos by weight or area. Chemical substance, has the same meaning as in section 3 of the Act. Commerce has the same meaning as in section 3 of the Act. Commercial paper means an asbestoscontaining product which is made of paper intended for use as general insulation paper or muffler paper. Major applications of commercial papers are insulation against fire, heat transfer, and corrosion in circumstances that require a thin, but durable, barrier. Corrugated paper means an asbestoscontaining product made of corrugated paper, which is often cemented to a flat backing, may be laminated with foils or other materials, and has a corrugated surface. Major applications of asbestos corrugated paper include: thermal insulation for pipe coverings; block insulation; panel insulation in elevators; insulation in appliances; and insulation in low-pressure steam, hot water, and process lines. Customs territory of the United States means the 50 States, Puerto Rico, and the District of Columbia. Distribute in commerce has the same meaning as in section 3 of the Act, but the term does not include actions taken with respect to an asbestos-containing product (to sell, resale, deliver, or hold) in connection with the end use of the product by persons who are users (persons who use the product for its intended purpose after it is manufactured or processed). The term also does not include distribution by manufacturers, importers, and processors, and other persons solely for purposes of disposal of an asbestos-containing product. Flooring felt means an asbestos-containing product which is made of paper felt intended for use as an underlayer for floor coverings, or to be bonded to the underside of vinyl sheet flooring. Import means to bring into the customs territory of the United States, except for: (1) Shipment through the cus- toms territory of the United States for export without any use, processing, or disposal within the customs territory of the United States; or (2) entering the customs territory of the United States as a component of a product during normal personal or business activities involving use of the product. Importer means anyone who imports a chemical substance, including a chemical substance as part of a mixture or article, into the customs territory of the United States. Importer includes the person primarily liable for the payment of any duties on the merchandise or an authorized agent acting on his or her behalf. The term includes as appropriate: (1) The consignee. (2) The importer of record. (3) The actual owner if an actual owner’s declaration and superseding bond has been filed in accordance with 19 CFR 141.20. (4) The transferee, if the right to withdraw merchandise in a bonded warehouse has been transferred in accordance with subpart C of 19 CFR part 144. Manufacture means to produce or manufacture in the United States. Manufacturer means a person who produces or manufactures in the United States. New uses of asbestos means commercial uses of asbestos not identified in § 763.165 the manufacture, importation or processing of which would be initiated for the first time after August 25, 1989. Person means any natural person, firm, company, corporation, joint-venture, partnership, sole proprietorship, association, or any other business entity; any State or political subdivision thereof, or any municipality; any interstate body and any department, agency, or instrumentality of the Federal Government. Process has the same meaning as in section 3 of the Act. Processor has the same meaning as in section 3 of the Act. Rollboard means an asbestos-containing product made of paper that is produced in a continuous sheet, is flexible, and is rolled to achieve a desired thickness. Asbestos rollboard consists of two sheets of asbestos paper 850 VerDate Aug<31>2005 14:36 Aug 06, 2007 Jkt 211171 PO 00000 Frm 00860 Fmt 8010 Sfmt 8010 Y:\SGML\211171.XXX 211171

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