Office of Rasearch and EPA/600/R-93/116 Development July 1993 Washington, DC 20460 SEPA Test Method Environmental Protection Agency Method for the Determination of Asbestos in Bulk Building Materials IS» HyEPA/600/R-93/116 July 1993 TEST METHOD METHOD FOR THE DETERMINATION OF ASBESTOS IN BULK BUILDING MATERIALS by R. L. Perkins and B. W. Harvey EPA Project Officer Michael E. Beard Atmospheric Research and Exposure Assessment Laboratory U.S. Environmental Protection Agency Research Triangle Park, NC 27709 EPA Contracts Nos. 68024550 and 68D10009 RTI Project No. 91U-5960-181 June 1993 ® Pimeton neces PagerDISCLAIMER ‘The information in this document has been funded wholly or in part by the United States Environmental Protection Agency under Contracts 68-02-4550 and 68D10009 to the Methods Research and Development Division, Atmospheric Research and Exposure Assessment Laboratory, Research Triangle Park, North Carolina, It has been subjected to the Agency’s peer and administrative review, and it has been approved for publication as an EPA document. Mention of trade names or commercial products does not constitute endorsement or recommendation for use.TABLE OF CONTENTS SECTION 1.0 INTRODUCTION Ll 2.0 METHODS 2d 22 24 References Stereomicroscopic Examination 2.1.1 Applicability 2.1.2 Range 2.1.3 Interferences . . 2.1.4 Precision and Accuracy 2.1.5 Procedures . . 2.1.5.1 Sample Preparation 2.1.5.2 Analysis, 2.1.6 Calibration Materials . 2.1.7 References Polarized Light Microscopy 2:21 Principle and Appliceility 2.2.2 Range ..... 2.2.3. Interferences 2.2.4 Precision and Accuracy 2.2.5 Procedures : 2.2.5.1 Sample Preparation 2.2.5.1.1 Qualitative Analysis Preparation 2.2.5.1.2 Quantitative Analysis Preparation 2.2.5.2 Analysis 2.2.5.2.1 Identification 2.2.5.2.2 Quantitation of Asbestos Content 2.2.5.2.3. Microscope Alignment 2.2.6 References Gravimetry 2.3.1. Principle and Applicability 2.3.2. Interferences 2.3.3 Quantitation 2.3.4 Preliminary Examination and Evaluation 2.3.5. Sample Preparation 2.3.5.1 Drying 2.3.5.2 Homogenization/Grain Size Reduction 2.3.6 Procedure for Ashing 2.3.7 Use of Solvents for Removal of Organics 2.3.8 Procedure for Acid Dissolution 2.3.9 Determination of Optimal Precision and Accuracy 2.3.10 References X-Ray Powder Diffraction 2.4.1 Principle and Applicability 2.4.2. Range and Sensitivity 2.4.3 LimitationsTABLE OF CONTENTS (cont'd) CTION PAGE 2.4.3.1 Interferences 35 2.4.3.2 Matrix Effects 38 2.4.3.3. Particle Size Dependence 39 2.4.3.4 Preferred Orientation Effects 39 2.4.3.5 Lack of Suitably Characterized Standard Materials 39 2.4.4 Precision and Accuracy - 40 2.4.5. Procedure 40 2.4.5.1 Sampling 40 2.4.5.2 Analysis . eee te eee eee es 40 2.4.5.2.1 Sample Preparation... : cece 4 2.4.5.2.2 Milling cece oe : 41 2.4.5.2.3 Ashing feet 5 re’) 2.4.5.2.4. Acid Washing : . 4 2.4.5.3 Qualitative Analysis... aes 42 2.4.5.3.1 Initial Screening of Bulk Material oo... 2 2.4.5.3.2. Detection of Minor or Trace Constitu : 43 2.4.5.4 Quantitative Analysis . wens aa 2.4.6 Calibration . : ce - 4 2.4.6.1 Preparation of Calibration Standards. 46 2.4.6.2 Analysis of Calibration Standards... . ce : 47 2.4.7 Calculations... .. . : : . a 49 2.4.8 References .. : - St 2.8. Analytical Electron Microscopy : cee 31 2.5.1 Applicability . . . : fee ene 51 2.5.2 Range oe : : wee 52 2.5.3 Interferences... 20.20... : cece eee 52 2.5.4 Precision and Accuracy : : feveeeeee 82 2.5.5 Procedures. : wes 52 2.5.5.1 AEM Specimen Preparation for Semi-Quantitative Evaluation 3 2.5.5.2 AEM Specimen Preparation for Quantitative Evaluation ieee 2,5.5.2.1 Identification eee : = 54 2.5.6 References .. vee etter SM 2.6 Other Methodologies cee ee fet eece eens 5B 3.0 QUALITY CONTROL/QUALITY ASSURANCE OPERATIONS: PLM. . sees 5S 3.1 General Considerations eee wee 56 3.1.1 Training... . eEeCELeCE ee ereen tener se 56 3.1.2 Instrument Calibration and Maintenance 56 3.2. Quality Control of Asbestos Analysis : Lost 3.2.1 Qualitative Analysis 37 3.2.2. Quantitative Analysis ween o : 58 3.3 Interlaboratory Quality Control : arr) 3.4 Performance Audits. . B ee 3.5: Systems Audits ce ee 60 3.6 References wl 6TABLE OF CONTENTS (cont'd) APPENDIX A: GLOSSARY OF TERMS APPENDIX B: APPARATUS FOR SAMPLE PREPARATION AND ANALYSIS, APPENDIX C: PREPARATION AND USE OF CALIBRATION STANDARDS FOR BULK ASBESTOS APPENDIX D: SPECIAL-CASE BUILDING MATERIALS.TABLES TABLE 1-1 Simplified Flowchart for Analysis of Bulk Materials 2-1 Suggested Acceptable Errors For PLM Analysis 22 Optical Properties of Asbestos Fibers 2.3. Typical Central Stop Dispersion Staining Colors 2-4 Optical Properties of Man-Made Textile Fibers 2-5 Optical Properties of Selected Fibers 2-6 The Asbestos Minerals and Their Nonasbestiform Analogs 2-7. Principal Lattice Spacings of Asbestiform Minerals 2-8 Common Constituents in Building Materials 2-9 Interferences in XRD Analysis of Asbestiform Minerals -2 34 34 - 36 01.0 INTRODUCTION Laboratories are now called upon to identify asbestos in a variety of bulk building materials, including loose-fill insulations, acoustic and thermal sprays, pipe and boiler wraps, plasters, paints, flooring products, roofing materials and cementitious products The diversity of bulk materials necessitates the use of several different methods of sample preparation and analysis. An analysis with a simple stereomicroscope is always followed by a polarized light microscopic (PLM) analysis. ‘The results of these analyses are generally sufficient for identification and quantitation of major concentrations of asbestos. However, during these stereomicroscopic and PLM analyses, it may be found that additional techniques are needed to: 1) attain a positive identification of asbestos; 2) attain a reasonable accuracy for the quantity of asbestos in the sample; or 3) perform quality assurance activities to characterize a laboratory’s performance. The additional techniques include x-ray diffraction (XRD), analytical electron microscopy (AEM), and gravimetry, for which there are sections included in the method. Other techniques will be considered by the Environmental Protection Agency (EPA) and may be added at some future time, Table 1-1 presents a simplified flowchart for analysis of bulk materials. This Method for the Determination of Asbestos in Bulk Building Materials outlines the applicability of the various preparation and analysis methods to the broad spectrum of bulk building materials now being analyzed, This method has been evaluated by the EPA Atmospheric Research and Exposure Assessment Laboratory (EPA/AREAL) to determine if it offers improvements to current analytical techniques for building materials. ‘This method demonstrated a capability for improving the precision and accuracy of analytical results. It contains significant revisions to procedures outlined in the Interim Method, along with the addition of several new procedures. Each technique may reduce or introduce bias, or have some effect on the precision of the measurement, therefore results need to be interpreted judiciously. Data on each technique, especially those new to asbestos analysis, will be collected over time and carefully evaluated, with resulting recommendations for changes to the Method to be passed on to the appropriate program office within EPATABLE 1-1. SIMPLIFIED FLOWCHART FOR ANALYSIS OF BULK MATERIALS STEREOMICROSCOPIC EXAMINATION Qualitative (classification, fiber ID) and Mandatory Quantitative (calibrated volume estimate) Section 2.1 POLARIZED LIGHT MICROSCOPY Mandatory Qualitative (classification, fiber ID) and Quantitative (calibrated area estimate and/or point count) Section 2.2 Continue when problems are encountered with PLM and/or for Quality Assurance purposes Qualitative Problems Quantitative Problems (Fiber ID problems) (PACM?) Matrix removal|| XRD AEM Gravimetry XRD Section 2.3 ||Sec. 2.4||Sec. 2.5 Sec. 2.3 | |Sec. 2.4 PLM| | XRD] | AEM PLM] | xRD| | AEM (fiber identification) (amount of asbestos in residue)This is an analytical method. It is not intended to cover bulk material sampling, an area addressed previously***5 by the EPA. However, subsampling or sample splitting as it pertains to laboratory analysis procedures in this method, is discussed throughout 1.1. References 1. Interim Method for the Determination of Asbestos in Bulk Insulation Samples, U.S. E.P.A, 600/M4-82-020, 1982. 2. Asbestos-Containing Materials in School Buildings: A Guidance Document, Part 1 and 2, U.S. E.P.A./O.T.S NO. €00090, 1979. 3. Asbestos in Buildings: Simplified Sampling Scheme for Friable Surfacing Materials, U.S. E.P.A. 560/5-85-030a, 1985 Guidance for Controlling Asbestos-Containing Materials in Buildings, U.S. E.P.A. 560/5-85-024, 1985. 5. Asbestos-Containing Materials in Schools: Final Rule and Notice, 40 CFR Part 763, October, 1987. 2.0 METHODS 2.1 Stereomicroscopic Examination A preliminary visual examination using a simple stereomicroscope is mandatory for all samples. A sample should be of sufficient size to provide for an adequate examination. For many samples, observations on homogeneity, preliminary fiber identification and semi- quantitation of constituents can be made at this point. Another method of identification and semi-quantitation of asbestos must be used in conjunction with the stereomicroscopic examination. A description of the suggested apparatus needed for stereomicroscopic examination is given in Appendix B. The laboratory should note any samples of insufficient volume. A sufficient sample volume is sample-type dependent, For samples such as floor tiles, roofing felts, paper insulation, etc., three to four square inches of the layered material would be a preferred sample size. For materials such as ceiling tiles, loose-fill insulation, pipe insulation, etc., a sample size of approximately one cubic inch (~ IScc) would be preferred, For samples of thin-coating materials such as paints, mastics, spray plasters, tapes, etc., a smaller samplesize may be suitable for analysis. Generally, samples of insufficient volume should be rejected, and further analysis curtailed until the client is contacted. The quantity of sample affects the sensitivity of the analysis and reliability of the quantitation steps. If there is a question whether the sample is representative due to inhomogeneity, the sample should be rejected, at least until contacting the client to see if: 1) the client can provide more material or 2) the client wishes the laboratory to go ahead with the analysis, but with the laboratory including a statement on the limited sensitivity and reliability of quantitation. If the latter is the case, the report of analysis should state that the client was contacted, that the client decided that the lab should use less material than recommended by the method, and that the client acknowledges that this may have limited the sensitivity and quantitation of the method. At the time the client is contacted about the material, he or she should be informed that a statement reflecting these'facts will be placed in the report. 2.1.1 Applicability Stereomicroscopic analysis is applicable to all samples, although its use with vinyl Noor tile, asphaltic products, etc., may be limited because of small asbestos fiber size and/or the presence of interfering components. It does not provide positive identification of asbestos. 2.1.2 Range Asbestos may be detected at concentrations less than one percent by volume, but this detection is highly material dependent 2.1.3. Interferences Detection of possible asbestos fibers may be made more difficult by the presence of other nonasbestos fibrous components such as cellulose, fiber glass, etc., by binder/matrix materials which may mask or obscure fibrous components, and/or by exposure to conditions (acid environment, high temperature, ete.) capable of altering or transforming asbestos. 2.1.4 Precision and Accuracy The precision and accuracy of ttiese’ estimations are material dependent and must be determined by the individual laboratory for the percent range involved. These values may bedetermined for an individual analyst by the in-house preparation and analysis of standards and the use of error bars, control charts, etc. The labs should also compare to National Voluntary Laboratory Accreditation Program (NVLAP) proficiency testing samples, if the lab participates in the Bulk Asbestos NVLAP, or to external quality assurance system consensus results such as from proficiency testing programs using characterized materials. However, at this time, consensus values for the quantity of asbestos have been shown to be unreliable. Only proficiency testing materials characterized by multiple techniques should be used to determine accuracy and precision. 2.1.5 Procedures NOTE: Exposure to airborne asbestos fibers is a health hazard, Bulk samples submitted for analysis are oftentimes friable and may release fibers during handling or matrix reduction steps. All sample handling and examination must be carried out in a HEPA-filtered hood, a class 1 biohazard hood or a glove box with continuous airflow (negative pressure). Handling of samples without these precautions may result in exposure of the analyst to and contamination of samples by airborne fibers. 2.1.5.1 Sample Preparation No sample preparation should be undertaken before initial stereomicroscopic examination. Distinct changes in texture or color on a stereomicroscopic scale that might denote an uneven distribution of components should be noted. When a sample consists of two or more distinct layers or building materials, each should be treated as a separate sample, when possible. Thin coatings of paint, rust, mastic, etc., that cannot be separated from the sample without compromising the layer are an exception to this case and may be included with the layer to which they are attached. Drying (by heat lamp, warm plate, ete.) of wet or damp samples is recommended before further stereomicroscopic examination and is mandatory before PLM examination. Drying must be done in a safety hood. For nonlayered materials that are heterogeneous, homogenization by some means (mill, blender, mortar and pestle) may provide a more even distribution of sample components. Itmay also facilitate disaggregation of clumps and removal of binder from fibers (rarely however, it may mask fibers that were originally discernable), For materials such as cementitious products and floor tiles, breaking, pulverizing, or grinding may improve the likelihood of exposing fibrous components. It may be appropriate to treat some materials by dissolution with hydrochloric acid to remove binder/matrix materials. Components such as calcite, gypsum, magnesite, etc., may be removed by this method. For materials found to possess a high organic content (cellulose, organic binders), ashing by means of a muffle furnace or plasma asher (for small, cellulosic samples), or dissolution by solvents may be used to remove interfering material. In either case, it is recommended that matrix removal be tracked gravimetrically. Additional information concerning homogenization, ashing and acid dissolution may be found in Sections 2.2.5.1 and 2.3. 2.1.5.2 Analysis Samples should be examined with a’simple stereomicroscope by viewing multiple fields of view over the entire sample. The whole sample should be observed after placement in a suitable container (watchglass, weigh boat, etc.) substrate. Samples that are very large should be subsampled. The sample should be probed, by turning pieces over and breaking open large clumps. The purpose of the stereomicroscopic analysis is to determine homogeneity, texture, friability, color, and the extent of fibrous components of the sample. This information should then be used as a guide to the selection of further, more definitive qualitative and quantitative asbestos analysis methods. Homogeneity refers to whether each subsample made for other analytical techniques (e.g. the "pinch" mount used for the PLM analysis), is likely to be similar or dissimilar. Color can be used to help determine homogeneity, whether the sample has become wet (rust color), and to help identify or clarify sample labelling confusion between the building material sampler and the laboratory. Texture refers to size, shape and arrangement of sample components. Friability may be indicated by the ease with which the sample is disaggregated (see definitions in Appendix A) as received by the analyst. This does not necessarily represent the friability of the material as determined by the assessor at the collection site. The relative proportion of fibrous