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asbestos analysis environmental protection quality control environmental science

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This document provides procedures for asbestos analysis, including quality control measures for sampling and analysis. It's a detailed guide for environmental testing and assessment. Key areas include laboratory procedures, sample preparation, and data analysis.

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Pt. 763, Subpt. E, App. A operations are within acceptable limits. In this way, the quality of the data is defined and the results are of known value. These checks and tests also provide timely and specific warning of any problems which might develop within the sampling and analysis operations. A...

Pt. 763, Subpt. E, App. A operations are within acceptable limits. In this way, the quality of the data is defined and the results are of known value. These checks and tests also provide timely and specific warning of any problems which might develop within the sampling and analysis operations. A description of these quality control/quality assurance procedures is summarized in the following Table III: 1. When the samples arrive at the laboratory, check the samples and documentation for completeness and requirements before initiating the analysis. 2. Check all laboratory reagents and supplies for acceptable asbestos background levels. 3. Conduct all sample preparation in a clean room environment monitored by laboratory blanks. Testing with blanks must also be done after cleaning or servicing the room. 4. Prepare multiple grids of each sample. 791 VerDate Aug<31>2005 14:36 Aug 06, 2007 Jkt 211171 PO 00000 Frm 00801 Fmt 8010 Sfmt 8002 Y:\SGML\211171.XXX 211171 EC01AP92.006</MATH> rfrederick on PROD1PC67 with CFR Environmental Protection Agency Pt. 763, Subpt. E, App. A 40 CFR Ch. I (7–1–07 Edition) 5. Provide laboratory blanks with each sample batch. Maintain a cumulative average of these results. If there are more than 53 fibers/mm2 per 10 200-mesh grid openings, the system must be checked for possible sources of contamination. 6. Perform a system check on the transmission electron microscope daily. 7. Make periodic performance checks of magnification, electron diffraction and energy dispersive X-ray systems as set forth in Table III under Unit II.I. 8. Ensure qualified operator performance by evaluation of replicate analysis and standard sample comparisons as set forth in Table III under Unit II.I. 9. Validate all data entries. 10. Recalculate a percentage of all computations and automatic data reduction steps as specified in Table III under Unit II.I. 11. Record an electron diffraction pattern of one asbestos structure from every five samples that contain asbestos. Verify the identification of the pattern by measurement or comparison of the pattern with patterns collected from standards under the same conditions. The records must also demonstrate that the identification of the pattern has been verified by a qualified individual and that the operator who made the identification is maintaining at least an 80 percent correct visual identification based on his measured patterns. 12. Appropriate logs or records must be maintained by the analytical laboratory verifying that it is in compliance with the mandatory quality assurance procedures. rfrederick on PROD1PC67 with CFR J. References For additional background information on this method, the following references should be consulted. 1. ‘‘Guidance for Controlling Asbestos-Containing Materials in Buildings,’’ EPA 560/5– 85–024, June 1985. 2. ‘‘Measuring Airborne Asbestos Following an Abatement Action,’’ USEPA, Office of Pollution Prevention and Toxics, EPA 600/4– 85–049, 1985. 3. Small, John and E. Steel. Asbestos Standards: Materials and Analytical Methods. N.B.S. Special Publication 619, 1982. 4. Campbell, W.J., R.L. Blake, L.L. Brown, E.E. Cather, and J.J. Sjoberg. Selected Silicate Minerals and Their Asbestiform Varieties. Information Circular 8751, U.S. Bureau of Mines, 1977. 5. Quality Assurance Handbook for Air Pollution Measurement System. Ambient Air Methods, EPA 600/4–77–027a, USEPA, Office of Research and Development, 1977. 6. Method 2A: Direct Measurement of Gas Volume through Pipes and Small Ducts. 40 CFR Part 60 Appendix A. 7. Burdette, G.J., Health & Safety Exec. Research & Lab. Services Div., London, ‘‘Proposed Analytical Method for Determination of Asbestos in Air.’’ 8. Chatfield, E.J., Chatfield Tech. Cons., Ltd., Clark, T., PEI Assoc., ‘‘Standard Operating Procedure for Determination of Airborne Asbestos Fibers by Transmission Electron Microscopy Using Polycarbonate Membrane Filters,’’ WERL SOP 87–1, March 5, 1987. 9. NIOSH Method 7402 for Asbestos Fibers, 12–11–86 Draft. 10. Yamate, G., Agarwall, S.C., Gibbons, R.D., IIT Research Institute, ‘‘Methodology for the Measurement of Airborne Asbestos by Electron Microscopy,’’ Draft report, USEPA Contract 68–02–3266, July 1984. 11. ‘‘Guidance to the Preparation of Quality Assurance Project Plans,’’ USEPA, Office of Pollution Prevention and Toxics, 1984. III. Nonmandatory Transmission Electron Microscopy Method A. Definitions of Terms 1. Analytical sensitivity—Airborne asbestos concentration represented by each fiber counted under the electron microscope. It is determined by the air volume collected and the proportion of the filter examined. This method requires that the analytical sensitivity be no greater than 0.005 s/cm3. 2. Asbestiform—A specific type of mineral fibrosity in which the fibers and fibrils possess high tensile strength and flexibility. 3. Aspect ratio—A ratio of the length to the width of a particle. Minimum aspect ratio as defined by this method is equal to or greater than 5:1. 4. Bundle—A structure composed of three or more fibers in a parallel arrangement with each fiber closer than one fiber diameter. 5. Clean area—A controlled environment which is maintained and monitored to assure a low probability of asbestos contamination to materials in that space. Clean areas used in this method have HEPA filtered air under positive pressure and are capable of sustained operation with an open laboratory blank which on subsequent analysis has an average of less than 18 structures/mm2 in an area of 0.057 mm2 (nominally 10 200 mesh grid openings) and a maximum of 53 structures/ mm2 for no more than one single preparation for that same area. 6. Cluster—A structure with fibers in a random arrangement such that all fibers are intermixed and no single fiber is isolated from the group. Groupings must have more than two intersections. 7. ED—Electron diffraction. 8. EDXA—Energy dispersive X-ray analysis. 9. Fiber—A structure greater than or equal to 0.5 µm in length with an aspect ratio (length to width) of 5:1 or greater and having substantially parallel sides. 792 VerDate Aug<31>2005 14:36 Aug 06, 2007 Jkt 211171 PO 00000 Frm 00802 Fmt 8010 Sfmt 8002 Y:\SGML\211171.XXX 211171 Environmental Protection Agency Pt. 763, Subpt. E, App. A 10. Grid—An open structure for mounting on the sample to aid in its examination in the TEM. The term is used here to denote a 200-mesh copper lattice approximately 3 mm in diameter. 11. Intersection—Nonparallel touching or crossing of fibers, with the projection having an aspect ratio of 5:1 or greater. 12. Laboratory sample coordinator—That person responsible for the conduct of sample handling and the certification of the testing procedures. 13. Filter background level—The concentration of structures per square millimeter of filter that is considered indistinguishable from the concentration measured on blanks (filters through which no air has been drawn). For this method the filter background level is defined as 70 structures/mm2. 14. Matrix—Fiber or fibers with one end free and the other end embedded in or hidden by a particulate. The exposed fiber must meet the fiber definition. 15. NSD—No structure detected. 16. Operator—A person responsible for the TEM instrumental analysis of the sample. 17. PCM—Phase contrast microscopy. 18. SAED—Selected area electron diffraction. 19. SEM—Scanning electron microscope. 20. STEM—Scanning transmission electron microscope. 21. Structure—a microscopic bundle, cluster, fiber, or matrix which may contain asbestos. 22. S/cm3—Structures per cubic centimeter. 23. S/mm2—Structures per square millimeter. 24. TEM—Transmission electron microscope. B. Sampling rfrederick on PROD1PC67 with CFR 1. Sampling operations must be performed by qualified individuals completely independent of the abatement contractor to avoid possible conflict of interest (See References 1, 2, and 5 of Unit III.L.) Special precautions should be taken to avoid contamination of the sample. For example, materials that have not been prescreened for their asbestos background content should not be used; also, sample handling procedures which do not take cross contamination possibilities into account should not be used. 2. Material and supply checks for asbestos contamination should be made on all critical supplies, reagents, and procedures before their use in a monitoring study. 3. Quality control and quality assurance steps are needed to identify problem areas and isolate the cause of the contamination (see Reference 5 of Unit III.L.). Control checks shall be permanently recorded to document the quality of the information produced. The sampling firm must have written quality control procedures and documents which verify compliance. Independent audits by a qualified consultant or firm should be performed once a year. All documentation of compliance should be retained indefinitely to provide a guarantee of quality. A summary of Sample Data Quality Objectives is shown in Table II of Unit II.B. 4. Sampling materials. a. Sample for airborne asbestos following an abatement action using commercially available cassettes. b. Use either a cowling or a filter-retaining middle piece. Conductive material may reduce the potential for particulates to adhere to the walls of the cowl. c. Cassettes must be verified as ‘‘clean’’ prior to use in the field. If packaged filters are used for loading or preloaded cassettes are purchased from the manufacturer or a distributor, the manufacturer’s name and lot number should be entered on all field data sheets provided to the laboratory, and are required to be listed on all reports from the laboratory. d. Assemble the cassettes in a clean facility (See definition of clean area under Unit III.A.). e. Reloading of used cassettes is not permitted. f. Use sample collection filters which are either polycarbonate having a pore size of less than or equal to 0.4 µm or mixed cellulose ester having a pore size of less than or equal to 0.45 µm. g. Place these filters in series with a backup filter with a pore size of 5.0 µm (to serve as a diffuser) and a support pad. See the following Figure 1: 793 VerDate Aug<31>2005 14:36 Aug 06, 2007 Jkt 211171 PO 00000 Frm 00803 Fmt 8010 Sfmt 8002 Y:\SGML\211171.XXX 211171 40 CFR Ch. I (7–1–07 Edition) h. When polycarbonate filters are used, position the highly reflective face such that the incoming particulate is received on this surface. i. Seal the cassettes to prevent leakage around the filter edges or between cassette part joints. A mechanical press may be useful to achieve a reproducible leak-free seal. 794 VerDate Aug<31>2005 14:36 Aug 06, 2007 Jkt 211171 PO 00000 Frm 00804 Fmt 8010 Sfmt 8002 Y:\SGML\211171.XXX 211171 EC01AP92.007</GPH> rfrederick on PROD1PC67 with CFR Pt. 763, Subpt. E, App. A Environmental Protection Agency Pt. 763, Subpt. E, App. A rfrederick on PROD1PC67 with CFR Shrink fit gel-bands may be used for this purpose and are available from filter manufacturers and their authorized distributors. j. Use wrinkle-free loaded cassettes in the sampling operation. 5. Pump setup. a. Calibrate the sampling pump over the range of flow rates and loads anticipated for the monitoring period with this flow measuring device in series. Perform this calibration using guidance from EPA Method 2A each time the unit is sent to the field (See Reference 6 of Unit III.L.). b. Configure the sampling system to preclude pump vibrations from being transmitted to the cassette by using a sampling stand separate from the pump station and making connections with flexible tubing. c. Maintain continuous smooth flow conditions by damping out any pump action fluctuations if necessary. d. Check the sampling system for leaks with the end cap still in place and the pump operating before initiating sample collection. Trace and stop the source of any flow indicated by the flowmeter under these conditions. e. Select an appropriate flow rate equal to or greater than 1 L/min or less than 10 L/min for 25 mm cassettes. Larger filters may be operated at proportionally higher flow rates. f. Orient the cassette downward at approximately 45 degrees from the horizontal. g. Maintain a log of all pertinent sampling information, such as pump identification number, calibration data, sample location, date, sample identification number, flow rates at the beginning, middle, and end, start and stop times, and other useful information or comments. Use of a sampling log form is recommended. See the following Figure 2: 795 VerDate Aug<31>2005 14:36 Aug 06, 2007 Jkt 211171 PO 00000 Frm 00805 Fmt 8010 Sfmt 8002 Y:\SGML\211171.XXX 211171 40 CFR Ch. I (7–1–07 Edition) h. Initiate a chain of custody procedure at the start of each sampling, if this is requested by the client. i. Maintain a close check of all aspects of the sampling operation on a regular basis. j. Continue sampling until at least the minimum volume is collected, as specified in the following Table I: 796 VerDate Aug<31>2005 14:36 Aug 06, 2007 Jkt 211171 PO 00000 Frm 00806 Fmt 8010 Sfmt 8002 Y:\SGML\211171.XXX 211171 EC01AP92.008</GPH> rfrederick on PROD1PC67 with CFR Pt. 763, Subpt. E, App. A Pt. 763, Subpt. E, App. A k. At the conclusion of sampling, turn the cassette upward before stopping the flow to minimize possible particle loss. If the sampling is resumed, restart the flow before reorienting the cassette downward. Note the condition of the filter at the conclusion of sampling. l. Double check to see that all information has been recorded on the data collection forms and that the cassette is securely closed and appropriately identified using a waterproof label. Protect cassettes in individual clean resealed polyethylene bags. Bags are to be used for storing cassette caps when they are removed for sampling purposes. Caps and plugs should only be removed or replaced using clean hands or clean disposable plastic gloves. m. Do not change containers if portions of these filters are taken for other purposes. 797 VerDate Aug<31>2005 14:36 Aug 06, 2007 Jkt 211171 PO 00000 Frm 00807 Fmt 8010 Sfmt 8002 Y:\SGML\211171.XXX 211171 EC01AP92.009</MATH> rfrederick on PROD1PC67 with CFR Environmental Protection Agency rfrederick on PROD1PC67 with CFR Pt. 763, Subpt. E, App. A 40 CFR Ch. I (7–1–07 Edition) 6. Minimum sample number per site. A minimum of 13 samples are to be collected for each testing consisting of the following: a. A minimum of five samples per abatement area. b. A minimum of five samples per ambient area positioned at locations representative of the air entering the abatement site. c. Two field blanks are to be taken by removing the cap for not more than 30 sec and replacing it at the time of sampling before sampling is initiated at the following places: i. Near the entrance to each ambient area. ii. At one of the ambient sites. (NOTE: Do not leave the blank open during the sampling period.) d. A sealed blank is to be carried with each sample set. This representative cassette is not to be opened in the field. 7. Abatement area sampling. a. Conduct final clearance sampling only after the primary containment barriers have been removed; the abatement area has been thoroughly dried; and, it has passed visual inspection tests by qualified personnel. (See Reference 1 of Unit III.L.) b. Containment barriers over windows, doors, and air passageways must remain in place until the TEM clearance sampling and analysis is completed and results meet clearance test criteria. The final plastic barrier remains in place for the sampling period. c. Select sampling sites in the abatement area on a random basis to provide unbiased and representative samples. d. After the area has passed a thorough visual inspection, use aggressive sampling conditions to dislodge any remaining dust. i. Equipment used in aggressive sampling such as a leaf blower and/or fan should be properly cleaned and decontaminated before use. ii. Air filtration units shall remain on during the air monitoring period. iii. Prior to air monitoring, floors, ceiling and walls shall be swept with the exhaust of a minimum one (1) horsepower leaf blower. iv. Stationary fans are placed in locations which will not interfere with air monitoring equipment. Fan air is directed toward the ceiling. One fan shall be used for each 10,000 ft3 of worksite. v. Monitoring of an abatement work area with high-volume pumps and the use of circulating fans will require electrical power. Electrical outlets in the abatement area may be used if available. If no such outlets are available, the equipment must be supplied with electricity by the use of extension cords and strip plug units. All electrical power supply equipment of this type must be approved Underwriter Laboratory equipment that has not been modified. All wiring must be grounded. Ground fault interrupters should be used. Extreme care must be taken to clean up any residual water and ensure that electrical equipment does not become wet while operational. vi. Low volume pumps may be carefully wrapped in 6-mil polyethylene to insulate the pump from the air. High volume pumps cannot be sealed in this manner since the heat of the motor may melt the plastic. The pump exhausts should be kept free. vii. If recleaning is necessary, removal of this equipment from the work area must be handled with care. It is not possible to completely decontaminate the pump motor and parts since these areas cannot be wetted. To minimize any problems in this area, all equipment such as fans and pumps should be carefully wet wiped prior to removal from the abatement area. Wrapping and sealing low volume pumps in 6-mil polyethylene will provide easier decontamination of this equipment. Use of clean water and disposable wipes should be available for this purpose. e. Pump flow rate equal to or greater than 1 L/min or less than 10 L/min may be used for 25 mm cassettes. The larger cassette diameters may have comparably increased flow. f. Sample a volume of air sufficient to ensure the minimum quantitation limits. (See Table I of Unit III.B.5.j.) 8. Ambient sampling. a. Position ambient samplers at locations representative of the air entering the abatement site. If makeup air entering the abatement site is drawn from another area of the building which is outside of the abatement area, place the pumps in the building, pumps should be placed out of doors located near the building and away from any obstructions that may influence wind patterns. If construction is in progress immediately outside the enclosure, it may be necessary to select another ambient site. Samples should be representative of any air entering the work site. b. Locate the ambient samplers at least 3 ft apart and protect them from adverse weather conditions. c. Sample same volume of air as samples taken inside the abatement site. C. Sample Shipment 1. Ship bulk samples in a separate container from air samples. Bulk samples and air samples delivered to the analytical laboratory in the same container shall be rejected. 2. Select a rigid shipping container and pack the cassettes upright in a noncontaminating nonfibrous medium such as a bubble pack. The use of resealable polyethylene bags may help to prevent jostling of individual cassettes. 3. Avoid using expanded polystyrene because of its static charge potential. Also avoid using particle-based packaging materials because of possible contamination. 4. Include a shipping bill and a detailed listing of samples shipped, their descriptions 798 VerDate Aug<31>2005 14:36 Aug 06, 2007 Jkt 211171 PO 00000 Frm 00808 Fmt 8010 Sfmt 8002 Y:\SGML\211171.XXX 211171 Environmental Protection Agency Pt. 763, Subpt. E, App. A and all identifying numbers or marks, sampling data, shipper’s name, and contact information. For each sample set, designate which are the ambient samples, which are the abatement area samples, which are the field blanks, and which is the sealed blank if sequential analysis is to be performed. 5. Hand-carry samples to the laboratory in an upright position if possible; otherwise choose that mode of transportation least likely to jar the samples in transit. 6. Address the package to the laboratory sample coordinator by name when known and alert him or her of the package description, shipment mode, and anticipated arrival as part of the chain of custody and sample tracking procedures. This will also help the laboratory schedule timely analysis for the samples when they are received. rfrederick on PROD1PC67 with CFR D. Quality Control/Quality Assurance Procedures (Data Quality Indicators) Monitoring the environment for airborne asbestos requires the use of sensitive sampling and analysis procedures. Because the test is sensitive, it may be influenced by a variety of factors. These include the supplies used in the sampling operation, the performance of the sampling, the preparation of the grid from the filter and the actual examination of this grid in the microscope. Each of these unit operations must produce a product of defined quality if the analytical result is to be a reliable and meaningful test result. Accordingly, a series of control checks and reference standards is performed along with the sample analysis as indicators that the materials used are adequate and the operations are within acceptable limits. In this way, the quality of the data is defined, and the results are of known value. These checks and tests also provide timely and specific warning of any problems which might develop within the sampling and analysis operations. A description of these quality control/quality assurance procedures is summarized in the text below. 1. Prescreen the loaded cassette collection filters to assure that they do not contain concentrations of asbestos which may interfere with the analysis of the sample. A filter blank average of less than 18 s/mm2 in an area of 0.057 mm2 (nominally 10 200-mesh grid openings) and a maximum of 53 s/mm2 for that same area for any single preparation is acceptable for this method. 2. Calibrate sampling pumps and their flow indicators over the range of their intended use with a recognized standard. Assemble the sampling system with a representative filter—not the filter which will be used in sampling—before and after the sampling operation. 3. Record all calibration information with the data to be used on a standard sampling form. 4. Ensure that the samples are stored in a secure and representative location. 5. Ensure that mechanical calibrations from the pump will be minimized to prevent transferral of vibration to the cassette. 6. Ensure that a continuous smooth flow of negative pressure is delivered by the pump by installing a damping chamber if necessary. 7. Open a loaded cassette momentarily at one of the indoor sampling sites when sampling is initiated. This sample will serve as an indoor field blank. 8. Open a loaded cassette momentarily at one of the outdoor sampling sites when sampling is initiated. This sample will serve as an outdoor field blank. 9. Carry a sealed blank into the field with each sample series. Do not open this cassette in the field. 10. Perform a leak check of the sampling system at each indoor and outdoor sampling site by activating the pump with the closed sampling cassette in line. Any flow indicates a leak which must be eliminated before initiating the sampling operation. 11. Ensure that the sampler is turned upright before interrupting the pump flow. 12. Check that all samples are clearly labeled and that all pertinent information has been enclosed before transfer of the samples to the laboratory. E. Sample Receiving 1. Designate one individual as sample coordinator at the laboratory. While that individual will normally be available to receive samples, the coordinator may train and supervise others in receiving procedures for those times when he/she is not available. 2. Adhere to the following procedures to ensure both the continued chain-of-custody and the accountability of all samples passing through the laboratory: a. Note the condition of the shipping package and data written on it upon receipt. b. Retain all bills of lading or shipping slips to document the shipper and delivery time. c. Examine the chain-of-custody seal, if any, and the package for its integrity. d. If there has been a break in the seal or substantive damage to the package, the sample coordinator shall immediately notify the shipper and a responsible laboratory manager before any action is taken to unpack the shipment. e. Packages with significant damage shall be accepted only by the responsible laboratory manager after discussions with the client. 3. Unwrap the shipment in a clean, uncluttered facility. The sample coordinator or his or her designee will record the contents, including a description of each item and all identifying numbers or marks. A 799 VerDate Aug<31>2005 14:36 Aug 06, 2007 Jkt 211171 PO 00000 Frm 00809 Fmt 8010 Sfmt 8002 Y:\SGML\211171.XXX 211171 Pt. 763, Subpt. E, App. A 40 CFR Ch. I (7–1–07 Edition) 800 VerDate Aug<31>2005 14:36 Aug 06, 2007 Jkt 211171 PO 00000 Frm 00810 Fmt 8010 Sfmt 8006 Y:\SGML\211171.XXX 211171 EC01AP92.010</GPH> rfrederick on PROD1PC67 with CFR Sample Receiving Form to document this information is attached for use when necessary. (See the following Figure 3.)

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