Method for the Determination of Asbestos in Bulk Building Materials
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·--·-··--···- ..... ----~ ed States Office of Research a nd EP AJ6(J01l·H :IJ/'1 16 ironmental Protection Oevelcpment July 1993 f.•ncr Washington, oc_20460 . I 'I - &EPA Test Method iO~i111rooM"ii~Mo 2000748 ADMINISTRATIVE RECORD Method for the Determination of Asbestos in Bulk Building Materials .. EPA16001R-931116 JuJyl993 TEST :METHOD METHOD FOR THE DETEAAfiNA TION OF ASBESTOS IN BULK BUILDING MA TERIA.LS 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 68010009 RTI Project No . 91 U-5960-181 June l993 @ Pnrued on Recycled Paper DISCLAIMER The information in this document has been funded wholly or in part by che United States Environmental Protection Agency under Contracts 68-02-4550 and 680 10009 to the Methods Research and Development Division, Atmospheric Research and Exposure Assessment Laboratory, Research Triangle Parle, 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 I 1.1 References 3 2.0 1'-IETHODS . 3 2.1 Sten!Omicroscopic Examin:ltion . 3 2.1. 1 Applicability . 4 '2.1.2 Range . ... .. : . 4 2.1 .3 ln t erferenc~ . ~ 1.1.4 Precision anu Accuracy . ~ 2. I~ Proc~ures . ... .. ... .. .... ..... .. ..... .... ... ·. 5 2. 1.5. I Sample Preparation . 5 2.1.5.2 Analysis . .. ..... .. .. .. .... .. ... .. ... .. 6 2. 1.6 Calibration Materials . 3 2. l . 7 Rcfcrcncc:s ... .. ... .... ... .. .. ... .... ........ ... 8 2.2 Pol:1rized Light ~ficroscopy . 9 2.2.1 Principle and Applicability . 9 2.2.2 Range . 10 2.2.3 Interferences . 10 2 .2.4 Precision and Accuracy . 10 2.2.5 Proc¢dures . I I 2.2. 5. l Sample Preparation . II 2.2.5. 1. 1 Qualitative Analysis Pn:paracion . 1 I 2. 2.5. I. 2 Quantitative Analysis Preparation . 12 2.2.5 .2 Analysis . IJ 2.2.5 .2.1 Identification . IJ 2.2.5.2.2 Quantitation of Asb.:stos Content . 16 2. 2.5.2.3 Microscope Alignment . 22 2.2.6 References . .,., 2.3 Gravimetry . 23 2.3.1 Principle and Applicability . 23 2 . 3. 2 lnterferencc:s . 24 2.3.3 Quantitation . 25 2.3.4 Preliminary E~amination and Evaluation .. ........... ..... .. .. ..~ . 2.5 2.3.5 Sample Preparation . 26 2.3.5.1 Drying . 26 2. 3. 5.2 . Homo~cnization/G rain Siu Rc:duction . 26 2.3.6 Proc¢dure for Ashing . 27 2.3.7 USc: of Solvents for Removal of Organics . 28 2.3. 8 Procedure for Acid Dissolution . 29 2.3.9 Determination of Optimal Precision and Accuracy . 3 I 2.3. 10 References . 31 2.4 X-Ray Powder Diffraction . J2 2.4. 1 Principle and Applicability . J2 2.4.2 Range and Sensitivity . 35 2.4. 3 Lirrutations . 35 TABLE Of CONTENTS (.:ont'u) SECf!ON 2.... 3.1 lntc:rfc:rc::nccs ... ..... .. ... ... .. .. ... .. 35 2 .... J . 2 ~alnx Eff~ts . .. 38 2A.J.J Particle Siz..: Oe~nd.mce ..... .. ·...... ..... ....... .. .. 39 2 .... 3A Prd'c:rred Oric:ntation Effects .... .... .. ... .. ... .. ... 39 2 ... J .5 Lack of Suitably Charactc:riw.l Stand.lnJ Matc:rials .... ....... .. ... 39 2.4.4 Pro;tsion :111d Accuracy . ......... .. ...... ... : . .. .... ~ 2.4.5 Procc:.Uure . ..... .. ... ... .... .. ...... .. .... ..... ... 40 2.~ . 5 . 1 Sampling .. .. ...... ... .. ..... ...... ... .. .. ... 40 2 . ~.5.2 .~alysis ..... .. .. .. ... .. ..... .. ... .. ..... .. ~ 2A.5.2.1 Sample: Preparation .... .. ... ... .. ... .. 41 2 . ~.5 . 2 . 2 Milling . ... .... ...... .. ... .. ......... ~I 2.4.5.1.3 Ashing .... .... .. ... ... ... ...... .. .. .. ~2 2A.5.2.4 Acid Washin~ .. ..... .... .. .... .... ... ..2 2.4.5.3 Qualitative: Analysis ... ... ............ .. .... .. .. ... 42 2.4. 5. 3. 1 Initial Screc:ning of Bulle Material .... .. .. ... n 2A.5.3.2 Detection of Minor or Trace: Constituc:nts ...... .. .... 43 2.4.5.4 Quantitative Analysis · . .. ........ .. .... ... .... .. .. 44 2.4.6 Calibration · . .. .. .... .......... .. ... ... ......... 46 2.4.6. 1 Prc:paration of Calibration Standards . 46 2.4.6.2 .'\nalysis of Cllibration Stanclarcls . 47 2.4. 7 Calculations . 49 2.4.8 Rc:fc:renccs . 51 2.5 Analytical Electron Microscopy . 51 2.5. 1 Applicability . 51 2.5.2 Range . 52 2.5.3 Interferenc~ . 51 2.5.4 Precision and Accuracy . 51 2.5.5 Proc~ures . 51 2.5.5 .1 AE~ Specimen Preparation tor Sc:mi-Quantitativc: Evaluation . 53 1.5.5.1 AEM Specimc:n Preparation for Quantitative: Evaluation . 54 2.5.5.2.1 Idc:ntification . 54 2.5.6 Rc:fc:renc~ . 54 2.6 Other Methodologies . 53 3.0 QUALITY CONTROL/QUALITY ASSURANCE OPERATIONS· PLM ... .. ... ~ . SS 3.1 Genera! Considerations . 56 3.1.1 Training . 56 3. 1.2 Instrument Calibration and Maintenance . 56 3.2 Quality Control of Asbestos Arullysis . 57 3.2.1 Qualitative: Analysis . 57 3.2.2 Quantitative Analysis . 58 3.3 Interlaboratory Quality Control . 59 3.4 Perfonnance Audits . 60 3.5 Systems Audits . ..