Vermiculite Analysis & Libby Amphiboles

Transcription

1 Setting the Standard in Best Practice MTA P.A.L.M.S. II Advanced Environmental Workshop New York City Transit (December 2, 2014)

2 Today s Presentation Topics of Interest The history of Libby Amphiboles (LA) A toxicological overview of asbestos and LA NYS DOH ELAP Guidance requirements Description of the LAB chemical process Lab PLM/SEM/EDS analysis techniques Regulated and non-regulated asbestos types Overview of ELAP Method Future applications of LAB

3 Asbestos Expertise Richard J. Lee, Ph.D. For more than 30 years, Dr. Lee has been involved with the development of asbestos and vermiculite analysis methods. Early on, he participated in pioneering analytical methods for asbestos analysis including the drafting of the Yamate method and the EPA AHERA analytical method, which was based on RJ Lee Group s internal asbestos analysis methods. He was a member of the HEI peer-review panel to assess the significance of asbestos in public buildings, and helped author the resulting landmark report. Matthew Sanchez, Ph.D. Dr. Sanchez has been involved in the characterization of Libby vermiculite and associated amphiboles for the last decade. Along with Dr. Lee, he was active in method development for identification and quantification of vermiculite and asbestos in soil, air, and water as well as in characterizing vermiculite for the W. R. Grace & Company. Drew R. Van Orden Mr. Van Orden is a Registered Professional Engineer with over 20 years of experience in developing asbestos analytical methods, analyzing asbestos-containing materials (ACM), and conducting studies to measure potential asbestos release from ACM. He has participated in many national evaluations of ambient asbestos concentrations, directed a study of earthquake effects on airborne asbestos concentrations, and participated in EPA investigations into airborne asbestos concentrations in public buildings. Donald Ewert With 3 decades of experience providing consulting, industrial hygiene, litigation support and engineering services to those individuals impacted by asbestos, Mr. Ewert is a recognized expert in asbestos management, control and analysis. Not only was he responsible for drafting the first Operations and Management document utilized by EPA during creation of the 1985 Purple Book, he also shepherded the first EPA and NBS/NIST mobile laboratory through accreditation so that PLM services could be provided on-site rather than from a distant laboratory. Don has also served as expert witness in a range of property, tort and injury cases involving exposure to asbestos. 3

4 EM Instrumentation Cutting Edge Technology RJLG utilizes innovative technology for unprecedented materials characterization abilities. Hitachi HD-2300 STEM Hitachi S-5500 SEM/STEM 1 st Mira delivered to EPA 4

5 - Materials Sciences Microscopy Optical Microscopes Scanning electron microscopes Transmission electron microscopes High resolution electron microscopes Computer-controlled microscopy Surface Analysis: ESCA/XPS X-ray Diffraction X-ray Fluorescence Fourier Transform Infrared Spectroscopy Raman Imaging & Spectroscopy Analytical Chemistry ICP-ES and ICP-MS AA and IC GC-MS, GC-FID, GC-ECD DSC / TGA Counts / s Mg1s Na1s Zn2p Fe2p O1s N1s Ca2p K2p C1s Cl2p B1s Si2p Al2p 7.00E E E E E E E E+00 Thermo K-Alpha XPS Binding Energy (ev) 0 5

6 Asbestos A Summary Refresher Asbestos Occurs naturally in rock and soil, including the regulated forms of chrysotile, amosite, crocidolite, tremolite, and anthophyllite asbestiform minerals. All asbestos minerals have demonstrated an ability to produce cancer in animals as well as humans. In fact, asbestos is one of only a few known carcinogens regulated by USOSHA. AIHA Webinar - Wednesday, May 7, 2014 By: Andrey Korchevskiy, Eric Rasmuson, and James Rasmuson. The Synergist Edition 2, 2014 Asbestos use in the United States is limited as a result of laws passed in the 70 s and 80 s while it remains actively produced and used in other portions of the world. 6

7 Asbestos & Vermiculite - Definitions Regulated Asbestos - The EPA and OSHA definitions of 'asbestos' both include the six commercial forms of asbestos minerals: chrysotile, amosite, crocidolite, tremolite, anthophyllite, and actinolite (40 CFR 763 and 29 CFR ). All states, including New York regulate asbestos by the same standard. According to the US EPA, materials containing greater than 1 percent (>1%) asbestos are regulated as asbestos containing materials (ACM) while OSHA regulates exposure at all levels of asbestos content including trace. 7

8 Asbestos & Vermiculite - Definitions Non-Regulated Amphibole Asbestos (e.g., winchite/ richterite) - LAB reports these amphiboles when the morphological characteristics of the minerals are consistent with asbestos. However, the values are not used in determining whether a material is ACM. While winchite and richterite amphiboles are nonregulated forms of asbestos, they exhibit some of the same characteristics as regulated asbestos. As a result, they are often misreported as tremolite or actinolite asbestos because of the fact that their characteristics are consistent with these asbestiform minerals. 8

9 Libby Amphiboles (LA) Winchite 84% Richterite 11% Tremolite 6% Fibrous asbestiform winchite/richterite collected near Libby, Montana seen in hand sample (left) and scanning electron micrograph (right). Relationships between magnesium, calcium, and sodium content of the three amphibole minerals found in LA: tremolite, winchite, and richterite. All three names have been assigned to various amphibole samples from former vermiculite mining and milling sites near Libby, Montana. 9

10 Amphibole Optical Properties n α n γ Birefringence Elongation Pleochroism* Anthophyllite Amphibole Mineralogy by PLM PLM optical properties for Anthophyllite, Tremolite-Actinolite and Richterite-Winchite overlap L(+) X=Pale yellow Z=Pale brown Tremolite- Actinolite L(+) X=Pale yellow-grn Z=Pale brown-grn Richterite- Winchite L(+) X=Pale yellow-brn Z=orange * Level II processing dramatically increases the intensity of PLM pleochroism and causes some amphibole particles to exhibit a deep rust brown color. 10

11 USOSHA Interpretation - ACM with < 1% Asbestos November 24, 2003 Question 1: Are the OSHA letters dated April 17, 1997; August 7, 1998; and August 13, 1999 correct? They all say that items that do not contain >1% asbestos are covered to at least some extent by the Construction Asbestos Standard. Reply: Yes, those letters are correct although some requirements of the Construction Asbestos Standard, 29 CFR were not addressed. 29 CFR would apply even if neither asbestos permissible exposure limit (PEL) is exceeded. The standard contains numerous work practice requirements and prohibitions which apply, regardless of the exposure levels. However, only two of the requirements and three of the prohibitions must be observed in the case of work activities involving installed construction materials that do not contain >1% asbestos. 11

12 Asbestos: Still Legal, Still Lethal Asbestos Disease Awareness Organization 1.5 min 12

13 Vermiculite, Respiratory Disease, and Asbestos Exposure in Libby (2007) Patricia A. Sullivan; Field Studies Branch, Division of Respiratory Disease Studies, NIOSH BACKGROUND: Vermiculite from the mine near Libby, Montana, is contaminated with tremolite asbestos and other amphibole fibers (winchite and richterite). Asbestos-contaminated Libby vermiculite was used in loose-fill attic insulation that remains in millions of homes in the United States, Canada, and other countries. OBJECTIVE: This report describes asbestos-related occupational respiratory disease mortality among workers who mined, milled, and processed the Libby vermiculite. METHODS: This historical cohort mortality study uses life table analysis methods to compare the ageadjusted mortality experience through 2001 of 1,672 Libby workers to that of white men in the U.S. population. RESULTS: Libby workers were significantly more likely to die from asbestosis [standardized mortality ratio (SMR) = 165.8; 95% confidence interval (CI), ], lung cancer (SMR = 1.7; 95% CI, ), cancer of the pleura (SMR = 23.3; 95% CI, ), and mesothelioma. Mortality from asbestosis and lung cancer increased with increasing duration and cumulative exposure to airborne tremolite asbestos and other amphibole fibers. CONCLUSIONS: The observed dose-related increases in asbestosis and lung cancer mortality highlight the need for better understanding and control of exposures that may occur when homeowners or construction workers (including plumbers, cable installers, electricians, telephone repair personnel, and insulators) disturb loose-fill attic insulation made with asbestos-contaminated vermiculite from Libby, Montana. 13

14 Environmental Exposure to Libby Asbestos and Mesotheliomas Alan C. Whitehouse, et. al; Am. J. Ind. Med Wiley-Liss, Inc. Introduction - McDonald et al. [2004] described 12 confirmed cases of mesothelioma occurring before 1998 in former employees of the W.R. Grace Company (WRG). The company operated the world s largest vermiculite mine near Libby, MT, from 1963 to The mine was operated by the original Zonolite Corporation from the 1920s until purchased by W.R. Grace in The vermiculite ore bed was contaminated with up to 26% amphibole asbestos, originally believed to be tremolite; but more recent analysis indicates the asbestos is a combination of 84% winchite, 11% richterite and 6% tremolite [Meeker et al., 2003]. Background - Thirty-one cases of mesothelioma resulting from exposure to Libby Asbestos have been identified from Libby, Montana. Eleven cases not previously reported are the subject of this report. Methods - These cases are in non-occupationally exposed people, appearing to have resulted from exposure to contamination of the community, the surrounding forested area, and areas in proximity to the Kootenai river and railroad tracks used to haul vermiculite. Results - These exposures are considered to be of a low degree of magnitude, but are similar to those in Western Australia s crocidolite mine at Wittenoom Gorge. An epidemic of mesothelioma can likely be expected from this type of asbestos contamination over the next years. 14

15 NIOSH CURRENT INTELLIGENCE BULLETIN (January 2010) Asbestos Fibers and Other Elongate Mineral Particles There is little scientific debate that the asbestiform varieties of the five commercially important amphibole asbestos minerals are carcinogenic and should be covered in regulations to protect workers. However, concerns have been raised about whether the current OSHA and MSHA asbestos definitions, which explicitly cover only the asbestiform varieties of the six commercially important asbestos minerals, provide sufficient worker protection from exposure to other fibrous minerals. This concern is exemplified by exposures to winchite and richterite fibers at a vermiculite mine near Libby, Montana, where exposures to the these fibers have resulted in high rates of lung fibrosis and cancer among exposed workers, similar to the occurrence of asbestos-related diseases among asbestosexposed workers in other industries [Amandus and Wheeler 1987; Amandus et al. 1987a,b; McDonald et al. 2004; Sullivan 2007; Rohs et al. 2008]. 15

16 NIOSH CURRENT INTELLIGENCE BULLETIN (January 2010) Asbestos Fibers and Other Elongate Mineral Particles Because winchite and richterite are not explicitly listed among the six commercial asbestos minerals, it is sometimes assumed that they are not included in the regulatory definition for asbestos. However, some of what is now referred to as asbestiform winchite and richterite using the 1997 IMA nomenclature would have been accurately referred to as tremolite asbestos using the 1978 IMA nomenclature [Meeker et al. 2003]. Furthermore, an even greater portion of this richterite and winchite would have been identified as tremolite asbestos using the optical methods of identification used prior to In fact, over the years, amphibole minerals from the Libby mine that are now referred to as winchite and richterite have been identified by mineralogists as soda tremolite [Larsen 1942], soda-rich tremolite [Boettcher 1966], and tremolite asbestos and richterite asbestos [Langer et al. 1991; Nolan et al. 1991]; they were identified as tremolite in reports of the Libby mine epidemiological studies conducted by NIOSH in the 1980s [Amandus and Wheeler 1987; Amandus et al. 1987a,b]. 16

17 Cancer Experience by Mineral Group 17

18 Model Comparison Excess Cancer Cases/Million (0.1 f/cc, 45 years starting at 18) 18

19 International View on Asbestos Regulation European Union standard = 0.1 f/cc Health Council of the Netherlands proposals for asbestos: Amphiboles = f/cc Mixed Species = f/cc Chrysotile = f/cc Germany; instead of occupational exposure limits for asbestos, requirements exist for protective measures depending upon airborne fiber concentration (e.g. PPE can be waived if concentration < f/cc) Russia has extremely cumbersome regulation Occupational exposure regulated as a dust in mg/m 3 based on an assumed fiber content. Different standards for chrysotile and amphiboles (200 fold) Ambient standard of 0.06 f/cc by PCM, 0.08 mg/m 3 total dust having an asbestos content of >20%. 19

20 Introduction to NYS DOH ELAP Guidance 20

21 Vermiculite & Asbestos - Definitions Spray-On Fireproofing containing Vermiculite (SOF-V) SOF-V is defined as a material containing vermiculite, intended to act as a fire-retardant coating when applied to building structures via spraying equipment as opposed to a manually applied (trowel) material. SOF-V can be in the form of Thermal Systems Insulation (TSI), surfacing material, or other presumed ACM (PACM). No matter the form, it is a miscellaneous suspect ACM as specified in 12 NYCRR Part 56 which include, but are not limited to, existing or new surfacing material, plaster, pipe lagging, and spray-on fireproofing. 21

22 Chronology of NYS DOH Guidance on Vermiculite New York State DOH guidance FAQ #10 states that wherever SOF-V is calculated to be >10% vermiculite containing, the material must be reported as ACM. New York State DOH guidance FAQ #10 recommends that with no approved analytical methodology to reliably confirm vermiculite as non-asbestos containing, it is always best to assume that vermiculite is contaminated with asbestos and proceed accordingly. New York State law modified to designate vermiculite insulation as Suspect Miscellaneous ACM that must be treated as ACM unless proven otherwise by approved laboratory testing. 3/21/07 4/8/11 6/22/12 22

23 Chronology of NYS DOH Guidance on Vermiculite New York State DOH guidance FAQ #10 states that wherever SOF-V is calculated to be >10% vermiculite containing, Item may be used to evaluate the asbestos content of the material; provided, however, that any test results using this method must be reported with the following conspicuous disclaimer: This method does not remove vermiculite and may underestimate the level of asbestos present in a sample containing greater than 10% vermiculite. New York State DOH interpretation of vermiculite-related guidance does not prohibit the use or application of vermiculite materials, but instead applies during renovation and/or demolishing of structures when the origin of the vermiculite material is unknown. 8/27/12 7/9/13 23

24 Chronology of NYS DOH Guidance on Vermiculite New York DOH introduces publicly available Item 198.8, a modified Chatfield Method for the analysis of asbestos in Spray-On Fireproofing containing Vermiculite (SOF- V) by Polarized-Light Microscopy (PLM). New York State DOH notifies that validation for LAB has met the conditions set forth in 10NYCRR and is fully certified for SOF-V testing. New York State DOH announces the imminent availability of two new NYS DOH ELAP-approved methods for the detection and quantitation of asbestos content in spray-on fireproofing that contains vermiculite (SOF-V). These methods become known as Method LAB and NY ELAP Method /22/14 7/24/14 8/20/14 24

25 Testing Requirements for Sprayed-on Fireproofing Containing Vermiculite (SOF-V) This communication is in follow up to the July 9, 2013 interim guidance letter regarding testing alternatives for materials containing vermiculite, issued by the New York State Department of Health (NYS DOH), in collaboration with the New York State Department of Labor (NYS DOL). The enclosed communication announces the imminent availability of two new NYS DOH ELAP-approved methods for the detection and quantitation of asbestos content in spray-on fireproofing that contains vermiculite (SOF-V). The testing strategies for SOF-V outlined in the July 9, 2013 interim guidance letter may be used until October 31, After October 31, 2014, one of the new methods must be used to test SOF-V, regardless of the percent of vermiculite. Since the new methods will be capable of removing vermiculite content, they are the only results for SOF-V that may generate a Non-ACM result without the need for the disclaimer required in the July 9, 2013 interim guidance letter. 25

26 The following is a brief description of how and when these new methods must be utilized for analytical testing; please also refer to the enclosed Decision Tree for more guidance. In the field, when an inspector, using his/her professional judgment, determines that a sprayed-on fireproofing (SOF) may contain vermiculite, the material may be presumed ACM according to 12 NYCRR Part 56 (NYS Industrial Code Rule 56), or they must forward that material to a NYS DOH ELAP certified laboratory for analysis. Since all NYS approved PLM methods begin with a stereoscopic examination of the material, this stereoscopic examination can confirm the presence or absence of vermiculite. If vermiculite is present (regardless of the amount), one of the two new approved methods must be used for the detection and quantitation of asbestos content. If vermiculite is not present, then Items or must be used, as appropriate, and based upon the presence of organically-bound or microscopically interfering materials. 26

27 The following is a brief description of how and when these new methods must be utilized for analytical testing; please also refer to the enclosed Decision Tree for more guidance. In the field, when an inspector, using his/her professional judgment, can not make the determination if the (SOF) contains vermiculite, the material may be presumed ACM or sent to a laboratory certified for Items 198.1, 198.6, or one of the two new approved methods. If vermiculite is determined to be present at any concentration during the stereoscopic examination required in all NYS PLM approved methods, then the material must be further analyzed by one of the two new approved methods. If vermiculite is not present, then Items or must be used, as appropriate, and based upon the presence of organicallybound or microscopically interfering materials. 27

28 28

29 Industry Implications: The approval of these new methods for the identification and quantitation of asbestos in SOF-V will have the following implications during the demolition, renovation, remodeling and/or repair of buildings that fall under the authority of NYS Industrial Code Rule 56. For future projects that have no associated survey MUST use one of the new methods and current NYS guidance. For projects that have an existing survey, but no project plan MUST resample and resurvey and use one of the new methods and current NYS guidance prior to starting any new project. For projects with an existing survey, and project yet to be done (Phase 1A) MUST resample and resurvey and use one of the new methods and current NYS guidance. 29

30 Industry Implications: The approval of these new methods for the identification and quantitation of asbestos in SOF-V will have the following implications during the demolition, renovation, remodeling and/or repair of buildings that fall under the authority of NYS Industrial Code Rule 56. For projects in progress using an old survey, and work actively underway (Phase 2A-2D) re-sampling and use one of the new methods is RECOMMENDED, but NOT REQUIRED UNLESS there is a change to the project design requiring a change order. If a change order is required, then re-sampling and analysis by one of the new methods and current NYS guidance is REQUIRED on the new area. For completed projects that were conducted under an old survey there is no requirement to go back and re-sample. However, if there is a need to disturb a material in the future - MUST use one of the new methods and current NYS guidance. 30

31 Vermiculite Insulation & Asbestos Indoor Air Quality Association 2.25 min 31

32 Introduction to Method LAB

33 LAB Overview Purpose: An analytical method to determine the total asbestos content of six regulated asbestos minerals in vermiculite-containing spray-on fireproofing (VC-SOF). Process: Spray on fireproofing is digested to remove cellulose, gypsum, vermiculite and carbonates (anything combustible or readily soluble) in order to detect asbestos. 33

34 LAB Best Practice Defined Take advantage of common materials used in vermiculite fireproofing vermiculite, cellulose, carbonates, gypsum, cement, and fiberglass Selectively eliminate these materials to reveal materials of concern RJLG Method Sample Prep Features Benefits to Material Screening Level I (PLM) Level II (PLM & SEM) Removes gypsum, carbonates, and cellulose to make the chrysotile content visible and quantifiable. Removes vermiculite, fiberglass, and other soluble material in order to clearly identify and quantify amphibole asbestos. Fast and unambiguous results to determine serpentine asbestos content (> or <1%). Fast and unambiguous results to determine amphibole asbestos content (> or <1%). Creates a digital record of SEM results for later reference. 34

35 Samples Before and After Matrix Reduction RJLG Level II (Left) Light microscopy image of bulk vermiculite material and (right) scanning electron microscopy (SEM) image of Level II matrix reduction to remove vermiculite and other interfering materials leaving behind any amphiboles (circled). 35

36 Prep Process Overview 36

37 Gross Examination If layers are present, each layer is treated as a unique sample The presence or absence of vermiculite determines the analytical path Vermiculite-free SOF samples are evaluated by EPA 600/M4/82/020 (NYS DOH Equivalent) 37

38 Method Description - LAB Method LAB is a two tier analytical process in which Level I is used to detect and quantify chrysotile and Level II is used to detect, speciate and quantify both regulated and non-regulated amphibole asbestos. During Level I preparation, the raw material is ashed and washed using water and hydrochloric acid (HCl) to remove combustible materials along with any easily dissolved materials including gypsum and carbonate that may interfere with PLM analysis. This improves sample visibility allows the PLM analyst to accurately identify and quantify the chrysotile concentration. 38

39 Level I Digestion Pre-weigh polycarbonate filter and place onto a filtering apparatus. Transfer the sample from dilution vial to the funnel. Filter using a fine-tipped squirt bottle to rinse down remaining particulate. Turn off vacuum pressure, slowly lift the filter and slide back into case. Dry the filter, cool, and reweigh. 39

40 Level I Ashing After filtration, the filter and residual sample are transferred to a crucible. Crucibles are placed into a muffle furnace and heated to remove interfering materials. After ashing, samples are taken from the furnace and transferred to a hood for cooling and weighing. Once weighed, sample materials are analyzed for Chrysotile asbestos content using Polarized Light Microscopy. 40

41 Method Description - LAB Level II analysis is used to accurately detect and quantify the amount of amphibole asbestos, both regulated and nonregulated. The process involves ashing to remove cellulose followed by aggressive acid/base digestion to dissolve vermiculite, fiberglass and other soluble components. Once the interfering materials are eliminated, Level II employs a combination of PLM and SEM to detect, speciate and quantify the amphibole asbestos content. 41

42 Level II Ashing The representative sample portion for L2, obtained previously during cone and quartering, is placed into the appropriate pre-weighed crucible and re-weighed. Once weighed, Crucibles containing L2 sub-samples are placed into the oven for ashing. 42

43 Level II Digestion SOF-V materials are digested on a hot plate to remove vermiculite and non-asbestos materials. After digestion, samples are transferred to a filtration funnel where water is passed across the sample. Following filtration, the funnel is rinsed to capture particulate onto the filter. After rinsing, the filter is carefully lifted off and slid back into its case. 43

44 Level II Sample Sectioning After drying, the filter is removed from its case and sectioned for PLM /SEM analysis. Sectioning for PLM analysis consists of the removal of ¼ of the filter membrane and transfer into a new case. Sectioning for SEM analysis consists of the removal of a small square of the filter membrane with transfer onto a new SEM pin mount for carbon coating. 44

45 LAB Microscopic Analysis 45

46 Vermiculite & SOF-V Mineralogy by PLM Exfoliation can expand vermiculite up to 30 times. 8x Binocular photos of vermiculite sheets before (left) and after (right) expansion. Vermiculite Sheets on Basal Cleavage Exfoliation Direction 46

47 Vermiculite & SOF-V Mineralogy by PLM Vermiculite is moderately pleochroic from tan to brown, exhibits moderate birefringence, 0.02, and positive elongation along cleavage traces. It has perfect basal {001} cleavage. Refractive indices ~ n α =1.561 n β =1.581 n γ = Plane Polarized Light RI oil Cross Polarized Light RI oil 47

48 Vermiculite & SOF-V Mineralogy by PLM Chrysotile is an asbestiform serpentine mineral and was mined and used extensively in North America. Chrysotile: Mg 3 [Si 2 O 5 ](OH) 4 Chrysotile occurs as a rolled sheet which forms hollow fibers. 35x Binocular photo 48

49 Vermiculite & SOF-V Mineralogy by PLM PLM photos of Level I treated sample showing chrysotile and thin vermiculite in RI oil. Plane Polarized Light Cross Polarized Light 49

50 Vermiculite & SOF-V Mineralogy by PLM Fiber bundles separated from expanded vermiculite 10x Binocular photo Plane polarized light in RI oil Cross polarized light

51 Vermiculite & SOF-V Mineralogy by PLM Asbestiform amphibole intergrown with vermiculiteri oil 35x Binocular photo Plane Polarized light In RI oil Cross Polarized light

52 Vermiculite & SOF-V Mineralogy by SEM To identify amphibole mineral species a portion of the Level II filter residue is analyzed by SEM / EDS. EDS identification is then used to discriminate amosite, crocidolite, anthophyllite, tremolite and actinolite asbestos species. Observed amphibole particles similar to tremoliteactinolite, but with the additional elements Na or Na-K suggest origin from the vermiculite mine near Libby, Montana. These non-regulated amphiboles are normally identified as winchite-richterite. 52

53 Amosite Crocidolite Actinolite Fe 2+ 7Si 8 O 22 (OH) 2 Na 2 (Fe 2+ 3Fe 3+ 2)Si 8 O 22 (OH) 2 Ca 2 Fe 2+ 5Si 8 O 22 (OH) 2 Anthophylite Tremolite Winchite/Richterite Mg 7 Si 8 O 22 (OH) 2 Ca 2 Mg 5 Si 8 O 22 (OH) 2 Winchite: (NaCa)Mg 4 (Al,Fe 3+ )Si 8 O 22 (OH) 2 Richterite: Na(NaCa)Mg 5 Si 8 O 22 (OH) 2 53

54 VC-SOF Sample LAB Process Level I Treatment Chrysotile Analysis (400 Point Count) Level II Treatment Amphibole Analysis (PLM / SEM) If >2.0% Chrysotile Report As ACM If 0.5% - 2.0% Chrysotile If <0.5% Chrysotile Proceed to Level II If <1.0% Regulated Amphibole If >1.0% Regulated Amphibole Triplicate Analysis With Averaging of Results Sum the Results of Level I and Level II (Regulated Asbestos) If X >1.0% If X 1.0% If X 1.0% If X >1.0% Report As ACM Proceed to Level II Report As Non-ACM Report As ACM X = arithmetic mean Reporting Differentiates Regulated and Non-Regulated Amphibole Content 54

55 Introduction to ELAP Method

56 Method Description - NY DOH Item incorporates a two-step approach for the identification and quantitation of chrysotile and amphibole asbestos, including Libby amphiboles, in SOF-V. The first step utilizes gravimetric reduction including ashing to remove the organic materials and dilute acid treatment to remove gypsum and cement from SOF-V. The residue is then examined by PLM for the presence of chrysotile, which is quantitated by point counting. If the concentration of chrysotile is found to exceed 1%, the material is considered asbestos containing material (ACM) and the analysis is terminated. If chrysotile is either not detected, or is found at a concentration less than 1%, then the analysis is continued to determine the concentration of amphibole asbestos. 56

57 Method Description - NY DOH In the second step of processing, heavy liquid centrifugation is used to separate particles with densities exceeding 2.75 g/cc from the majority of the less dense matrix components. This results in a centrifugate that contains amphiboles present in the original sample. The concentration of the remaining amphibole is determined by PLM and point counting. The total asbestos content is obtained by adding the concentration of asbestos quantitated in step one (chrysotile) with the asbestos quantitated in step two (amphibole). If the final concentration is determined to be greater than 1%, the material is designated as ACM. 57

58 VC-SOF Sample Ash for 10 hours 1 st Centrifugation Remove Vermiculite Process Acid Treatment Disperse Centrifugate Filter Suspension 2 nd Centrifugation Chrysotile Analysis Aspirate Centrifugate If >1.0% Chrysotile Report As ACM If <1% Chrysotile Proceed to Centrifugation Amphibole Analysis (PLM Only) If <1.0% Amphibole Sum the Results Total Asbestos If >1.0% Amphibole If X >1.0% Report As ACM If X 1.0% Report As Non-ACM 58

59 59

60 SOF-V Analysis Methods Comparative Assessment & Performance Analysis 60

61 Detail LAB Vermiculite-Amphibole Separation Method Chemical Physical Microscopy Method SEM / PLM PLM Only Differentiation of Naturally Occurring Amphiboles Yes Analysis Pricing 18 Hour Process - $ Hour Process - $? Number of Contact and Transfer Processes Round Robin (Zonolite vs Spiked Samples) SOF-V Method Comparison No <5 >10 TBD TBD 61

62 Chrysotile Analysis by PLM; vs

63 Amphibole Analysis; (PLM) vs Level II (SEM) 63

64 Precision and Accuracy of Level II (SEM) 64

65 LAB SEM Residue Winchite Amphibole 65

66 SOF-V Method Comparison Sample ID 47W-01-FP-01B W-01-FP-02B W-01-FP-03B W-02-FP-04B W-02-FP-05B W-02-FP-06B Lin-03-FP-07B Lin-03-FP-08B Lin-03-FP-09B Chrysotile N/D N/D N/D N/D N/D N/D N/D N/D N/D ELAP Amphibole Trace - Actinolite Trace - Actinolite Trace - Actinolite Trace - Actinolite Trace - Actinolite Trace - Actinolite N/D Trace - Actinolite Trace - Actinolite LAB Amphibole 0.02% (Wi/Ri) 0.03% (Wi/Ri) 0.02% (Wi/Ri) 0.02% (Wi/Ri) 0.06% (Wi/Ri) 0.02% (Wi/Ri) 0.02% (Wi/Ri) 0.02% (Wi/Ri) 0.02% (Wi/Ri) Only Method LAB Offers the true asbestos content (prevents over and underestimation) - Differentiates between regulated and nonregulated Amphibole species - Exempts OSHA Monitoring (Wi/Ri are non-regulated) - Provides liability protection for Building Owners (best practice) 66

67 Zonolite Attic Insulation Comparative Analysis Results Sample ID Amphibole (%) Method Unground 0.17 (Wi/Ri) Unground 0.36 (Wi/Ri) Unground 0.45 (Wi/Ri) Ground 0.23 (Wi/Ri) Ground 0.22 (Wi/Ri) LAB Unable to Speciate Due to Filter Overloading (Assumed to be Wi/Ri Based on Experience) Ground 0.46 (Wi/Ri) Mortar 0.08 Actinolite Mortar 0.03 Actinolite Mortar <0.03 Actinolite ELAP PLM Analysis Only Only Method LAB Offers the true asbestos content (prevents underestimation) - Differentiates between Amphibole species (regulated.vs. non-regulated) - Exempts OSHA Monitoring (Wi/Ri are non-regulated) - Provides liability protection for Building Owners (best practices) 67

68 LAB Best Practice Defined The Method LAB.055.1: Provides sound data on vermiculite materials because of the chemical removal of vermiculite interferences from the analysis. Level I PLM accurately quantifies Chrysotile content while Level II SEM/EDS precisely ID s regulated and non-regulated amphiboles. Reliably determines whether a product is truly ACM at the new and more stringent NY DOH limit of 1.0% as well as existing international standards down to 0%. Accurately quantifies all amphibole asbestos down to 0.01%. Represents one of the only analysis methods capable of exempting owners and contractors from OSHA regulation for materials containing unregulated asbestos types. 68

69 For more information on LAB please contact VermicuLine: or Thank You for Participating 69