&EPA United States Environmental Protection Agency PB2009-102750 Sampling and Analysis of Asbestos Fibers on Filter Media to Support Exposure Assessments: Bench-Scale Testing ------- ------- EPA 600/R-08/046 November 2008 www.epa.gov Sampling and Analysis of Asbestos Fibers on Filter Media to Support Exposure Assessments: Bench-Scale Testing Daniel A. Vallero, Ph.D. U.S. Environmental Protection Agency National Exposure Research Laboratory Research Triangle Park, NC 27711 John R. Kominsky Environmental Quality Management, Inc. Cincinnati, OH 45240 Michael E. Beard and Owen Crankshaw RTI International Research Triangle Park, NC 27709 U.S. Environmental Protection Agency Office of Research and Development Washington, DC 20460 ------- April 6, 2008 (Revised November 5, 2008) ------- NTIS DISCLAIMER This document has been reproduced from the best copy furnished by the sponsoring agency. ------- ABSTRACT Sampling efficiency is essential in exposure assessments of contaminants in air, as well as other matrices. In the measurement of airborne contaminants, it is critical to collect a sample of air containing representative contaminants in the air of concern, that is, contaminant concentration and size distribution in the sampled air must be the same as that of the air of concern. Typically, mixed cellulose ester (MCE, 0.45 or 0.8 |im pore size) and to a much lesser extent, capillary-pore polycarbonate (PC, 0.4 |im pore size) membrane filters are used to collect airborne asbestos for count measurement and fiber size analysis. A literature review did not identify any study that compared the fiber retention efficiencies of 0.45 |im and 0.8 |im pore size MCE or 0.4 |im pore size PC membrane filters for asbestos aerosols. In this research study chrysotile asbestos (fibers both shorter and longer than 5 jam) were generated in an aerosol chamber and sampled by 25-mm diameter MCE filter media to compare the efficiency of a 0.45 |im pore size filters versus 0,8 p. pore size filter media. In addition, the effect of plasma etching times on fiber densities was evaluated. Polycarbonate filters were not tested in this study. This study demonstrated a significant difference in fiber retention efficiency between 0.45 |im and 0.8 |im pore size MCE filters for chrysotile asbestos aerosols (structures >0.5 |im length; s = 0.5 |im). That is, the fiber retention efficiency of a 0.45 |im pore size MCE filter is statistically significantly higher than that of the 0.8 |im pore size MCE filter. However, for chrysotile asbestos structures > 5|im in length, there is no statistically significant difference between the fiber retention efficiencies of the 0.45 jam and 0.8 |im pore size MCE filters. The mean density of chrysotile asbestos fibers (>0.5 |im in length) increased with etching time (2, 4, 8, and 16 minutes). Regression analysis of etching time and density showed that doubling the etching time adds an average of 13% to the total chrysotile asbestos density within the density range tested. Plasma etching time had no effect on the reported fiber densities of fibers longer than 5 |im. Many asbestos exposure risk models attribute most of the health effects to fibers longer than 5 |im in length. In these models, both the 0.45 |im and 0.8 |im pore size MCE filter can produce suitable estimates of the airborne asbestos densities. However, some models suggest a more significant role for asbestos fibers <5 |im in length. Exposure monitoring for these models should consider only the 0.45 |im pore size MCE filters as recommended by the U.S. EPA AHERA protocol and other methods. 11 ------- This report is based upon study findings and information submitted in fulfillment of Contract No. 68-C-00-186, Task Order No. 0020 by Environmental Quality Management, Inc. under the sponsorship of the United States Environmental Protection Agency, covering a period from April 28, 2006 to December 24, 2006, and work was completed as of December 31, 2006. The information in this document has been funded wholly by the United States Environmental Protection Agency under Contract No. 68-C-00-186, Task Order No. 0020 to Environmental Quality Management, Inc. It has been subjected to the Agency's peer and administrative review and has been approved for publication as an EPA document. Mention of trade names or commercial products does not constitute endorsement or recommendation by EPA for use. in ------- CONTENTS Section Page Abstract ii Contents iv Tables v Figures vii 1 Introduction 1 1.1 Proj ect Obj ectives 4 2 Study Design and Methodology 5 2.1 Preparation of Samples for Analysis 5 2.1.1 Dust Generation and Collection System 5 2.1.1.1 FluidizedBed Generator 6 2.1.1.2 Sonic Velocity Disperser and Settling Tower 6 2.1.1.3 Sample Collection Chamber 6 2.1.1.4 Dust Feeder 7 2.1.1.5 Sonic Velocity Disperser and Settling Tower 8 2.1.1.6 Sample Collection Chamber 8 2.2 Sample Analysis Strategy 9 2.2.1 Fiber Retention Efficiency of 0.45 |im and 0.8 |im Pore Size MCE Filters 9 2.2.2 Effect of Plasma Etching Time of Total Chrysotile Asbestos Density 9 2.3 Analyti cal Methodol ogy 9 2.3.1 TEM Specimen Preparation 9 2.3.2 TEM Measurement Strategy 10 2.3.3 Determination of Stopping Point 11 2.4 Quality Control/Quality Assurance 11 2.4.1 MCE Filters (0.45 and 0.8 |im Pore Size) 11 2.4.2 Lot Blanks 11 2.4.3 Laboratory Blanks 12 iv ------- 2.4.4 Interlaboratory QA/QC 12 2.4.4.1 Duplicate Analysis 12 2.4.4.2 Verified Counts 13 3 Results and Discussion 15 3.1 Fiber Retention Efficiency (Fibers >0.5 |im) 0.45 & 0.8 |im Pore Size MCE Filters 15 3.2 Effect of Plasma Etching on Total Chrysotile Asbestos Density (Fibers >0.5 |im) 18 3.3 Fiber Retention Efficiency (Fibers >5 |im) 0.45 and 0.8 |im Pore Size MCE Filters 22 3.4 Effect of Plasma Etching on Total Chrysotile Asbestos Density (Fibers >5 |im) 23 4 Conclusions and Recommendations 25 4.1 Fiber Retention Efficiency of 0.45 and 0.8 |im pore size MCE Filters 25 4.2 Effect of Etching Time for 0.45 |im pore size MCE Filters 26 4.3 Additional Recommendations 26 5 Acknowledgments 27 6 References 28 Appendix Chrysotile Asbestos Data Listing TABLES Number Page 1 Batch setup for 25-mm diameter MCE filter loading experiment 5 2 Plasma etching time for 0.45 |im pore size MCE filters 9 3 Interlab oratory duplicate analysis of MCE filters for chrysotile asbestos by TEM 13 4 Interlab oratory verified count analysis of MCE filters for chrysotile asbestos by TEM 14 v ------- 5 Mean chrysotile asbestos density (s/mm2) by batch and fiber length 16 6 Mean total chrysotile asbestos (fibers >0.5 |im) density (s/mm2) by batch and filter type 17 7 Mean total chrysotile asbestos (fibers >0.5 |im) density (s/mm2) for variable etching times .18 8 Mean chrysotile asbestos density for fibers >5 |im (s/mm2) by batch and filter type 22 9 Mean chrysotile asbestos density for fibers >5 |im (s/mm2) for variable etching times 23 vi ------- FIGURES Number Page 1 Transmission electron microscope photograph of 0.4 |im pore size capillary pore polycarbonate membrane filter (16,000X magnification) 2 2 Scanning electron microscope photograph of 0.8 |im pore size cellulose ester membrane filter (8,000X magnification) 2 3 A. Fiber densities (fibers > 0.5 |im in length) observed on 0.45 |im pore size MCE Filter by etch time in minutes: A. Mean fiber densities; B. Scatter plot showing range of density values of individually sampled filters (N=48) 20 4 Fiber densities (fibers >0.5 to 5 |im in length) observed on 0.45 |im pore size MCE filter 21 5 Fiber densities (fibers >5 to 10 |im in length) observed on 0.45 |im pore size MCE filter 21 6 Fiber densities (fibers >10 |im in length) observed on 0.45 |im pore size MCE filter 22 vii ------- ------- SECTION 1 INTRODUCTION Over the years, a number of optical and electron microscopy methods have been developed to detect and quantify asbestos in air, as well as in other matrices. Each method has its own strengths and weaknesses, and they must be carefully evaluated to determine how best to detect and quantify asbestos under a given circumstance.1"10 Typically, mixed cellulose ester (0.45 |im or 0.8 |im pore size) and to a lesser extent, capillary-pore polycarbonate (0.4 |im pore size) membrane filters are used to collect airborne asbestos for count measurement and fiber size analysis. It is important to recognize that pore size specification for a membrane filter is an absolute specification only for capillary-pore type filters such as the polycarbonate (PC). The pore size rating for tortuous path filters, such as the mixed-cellulose ester (MCE) filters, is an effective pore size and not a specification that particles exceeding that size are retained by the filter.11 The two types of filters differ in their chemical and physical composition. Polycarbonate filters have a smooth filtering surface; the pores are cylindrical, almost uniform in diameter, and essentially perpendicular to the surface (Figure 1). A mixed-cellulose ester filter is a thicker filter with a sponge-like appearance and relies on a tangled maze of cellulose ester strands to trap fibers (Figure 2). For microscopic analysis of asbestos deposited on the filter, it is critical that the fibers be in a single plane to assure they are in focus during the analysis. This requirement is simple to achieve for PC filters because of the smooth filtering surface. Whereas, the MCE filter requires two additional steps in the direct preparation procedure. The MCE filter must be collapsed with an organic solvent and then the top layer of the collapsed filter material must be etched away with a low temperature plasma asher. The U.S. EPA1 and the National Institute for Occupational Safety and Health (NIOSH)5 recommend using 0.45 |im pore size MCE filters when performing transmission electron microscopy (TEM) analysis on the samples because the particles deposit closer to the surface than in larger pore size (e.g., 0.8 |im pore size) MCE filters. However, the higher pressure drop through the 0.45 |im pore size MCE filters normally preclude their use with battery-powered personal sampling pumps.5 In order to obtain a uniform distribution of collected particulates across the surface of the collecting filter, EPA1 requires a 5.0 |im pore size MCE backing filter 1 ------- be placed behind the collecting filter followed by a cellulose support. This tandem filter assembly further increases the pressure drop, which at given velocity is directly proportional to the thickness of the filter. ISO Method 10312:1995 also recommends the tandem filter assembly for 0.45 jam pore size MCE as well as for the 0.4 jam pore size PC filters.' Figure 1. Transmission electron microscope photograph of a 0.4 jtun pore size capillary pore polycarbonate membrane filter (16,000X magnification) (Source RT1 International, S. Doom with permission.) Figure 2. Scanning electron microscope photograph of a 0.8 fini pore size mixed cellulose ester membrane filter (8,000X magnification). (Source MVA Scientific, J. Millette with permission.) 2 ------- Studies reporting the fiber retention efficiencies of MCE and PC membrane filters for asbestos aerosols are meager. One study investigated the collection efficiencies of 8 |im pore size MCE filters and 0.2, 0.4, and 0.8 |im pore size PC filters for aerosols of chrysotile asbestos.13 For MCE filters with 8-|im pores, the collection efficiency at a face velocity of 3.5 cm/s fell from 100% for fibers >5 |im in length to 75% for fibers of 2 |im in length, and to 25% for fibers approximately 0.5 |im in length. For PC filters with pore diameters of 0.2, 0.4, and 0.8 |im, collection efficiencies began to drop for fiber lengths <3 |im and fiber diameters <0.2 |im. For 0.2 |im pores, the efficiencies for fibers >0.5 |im did not drop below approximately 80%, whereas for 0.8 |im pores, the efficiencies dropped to near zero for fiber lengths below 0.5 |im and diameters below 0.05 |im. This study showed that fiber retention efficiencies decrease substantially with fiber length for both MCE and PC pore filters of larger pore size. The orientation of the airborne fibers as they approach the filter pore entrances may have an important effect on their ability to penetrate the filter. A literature review did not identify any study that compared the fiber retention efficiencies of 0.45 |im and 0.8 |im pore size MCE or 0.4 |im pore size PC membrane filters for asbestos aerosols.12 Information culled from an informal survey12 of asbestos analytical laboratories, members of the American Society for Testing and Materials (ASTM) and Environmental Information Association (EIA) revealed that MCE filters were primarily used for airborne asbestos sampling. Accordingly, it was concluded that testing of the PC filters would not be conducted in this study allowing the project to concentrate its efforts and funding on 0.45 |im and 0.8 |im pore size MCE filters that are widely used in asbestos exposure studies today. Therefore, U.S. EPA's National Exposure Research Laboratory (NERL) conducted a study in which chrysotile asbestos (fibers both shorter and longer than 5 |im) were generated in an aerosol chamber and sampled by 25-mm diameter MCE filter media to compare the efficiency of 0.45 |im pore size versus 0.8 |i pore size filter media. In addition, the effect of plasma etching times on fiber densities was evaluated. 3 ------- 1.1 Project Objectives The goal of this research study was to determine the effect of mixed cellulose ester membrane filter pore size on fiber retention efficiency of chrysotile asbestos fiber aerosols. The following are the specific objectives of this study: • Compare the fiber retention efficiency (structures >0.5 |im in length) of chrysotile asbestos aerosols of 0.45 |im and 0.8 |im pore size mixed cellulose ester filters. • Compare the fiber retention efficiency (structures >5 |im in length) of chrysotile asbestos aerosols of 0.45 |im and 0.8 |im pore size mixed cellulose ester filters. • To evaluate the effect of plasma etching time (2, 4, 6, 8, and 16 minutes) on 0.45 |im pore size mixed cellulose ester filters on total chrysotile asbestos density (structures >0.5 |im in length). • To evaluate the effect of plasma etching time (2, 4, 6, 8, and 16 minutes) on 0.45 |im pore size mixed cellulose ester filters on total chrysotile asbestos density (structures >5 |im in length). 4 ------- SECTION 2 STUDY DESIGN AND METHODOLOGY 2.1 Preparation of Samples for Analysis SRI International (SRI) loaded the 25-mm diameter (0.45 |im and 0.8 |im pore size) MCE filters with chrysotile asbestos in an aerosol chamber. The filters were prepared at two fiber loading levels: "low" nominal loading (2-5 fibers per grid opening) and "high" nominal loading (>5 fibers per grid opening). The filters were prepared in four batches of 18 filters each as shown in Table 1. Table 1. Batch setup for 25-mm MCE filter loading experiment Filter Pore Size/Loading and Number of Samples Batch 0.45 jim 0.8 jim Low High Low High 1 12 - 6 - 2 - 6 - 12 3 6 - 12 - 4 - 12 - 6 Total 18 18 18 18 2.1.1 SRI Dust Generation and Collection System Test atmospheres of dusts and fibers are dynamically generated in a dust generation and collection system engineered and built by SRI. The main components are: • A fluidized bed generator, which delivers a continuous stream of aerosol material; • A sonic velocity disperser, which disperses, de-agglomerates, and dilutes the aerosol; • A settling tower, where large particles are removed; and • Sample collection chambers, where 320 samples can be collected simultaneously. 5 ------- All of the air streams pass through ionizers to prevent static charge effects. The components are described in detail below. 2.1.1.1. Fluidized Bed Generator A variety of SRI custom-designed and constructed feeders can be used to introduce particulates and fibers into the collection system. Asbestos fiber atmospheres have been generated using a two-component fluidized bed consisting of bronze powder and sized chrysotile asbestos fibers. By proper adjustment of air flow through the bottom and across the top of the bed, a pressure differential is established sufficient to fluidize the bronze powder bed and the chrysotile asbestos fibers are stripped at a low rate and fed to the sonic velocity disperser. There is a concentration gradient using this system because the chrysotile asbestos is depleted from the fluidized bed. However, because a homogeneous atmosphere is produced, all 320 sampling ports will still collect an equivalent amount of chrysotile asbestos. By varying the sampling time, the chrysotile asbestos loading on the cassettes can be adjusted. 2.1.1.2. Sonic Velocity Disperser and Settling Tower The air stream from the dust feeder carries the aerosol to the sonic velocity disperser. Dilution air is also delivered to the sonic velocity disperser, where it de-agglomerates the aerosol under the action of an on-line static eliminator and high air velocity. The aerosol then enters the settling tower, the linear velocity is reduced, and the larger particles settle out to the base of the settling tower. The diluted aerosol is then divided uniformly among the four collection chambers. 2.1.1.3. Sample Collection Chamber The base section of the sample collection chamber consists of layers of gaskets and machined aluminum sheets. Eighty sampling ports are situated in an 8 x 10 matrix arrangement. Downstream from each port is a critical flow orifice. The mounting sheet in which the 80 critical flow orifices are embedded forms the upper section of a vacuum chamber, so that a vacuum to 6 ------- this chamber creates the necessary pressure differential to operate the orifices. Aerosol enters the collection chambers through 20 symmetrically located passages. The 320 orifices (80 for each of four sample collection chambers) all have the same diameter and were calibrated at the time the system was constructed to ensure that all the ports sample at the same flow rate. The orifices form a matched set, with a maximum flow rate of 2 L/min through each air monitor in the system. The collection chambers can be opened from the top by removing a cover. Air monitor cassettes are connected to the sampling port by a Luer fitting. A variety of cassette and filter types and sizes, including 25- and 37-mm-diameter cassettes, mixed cellulose ester filters, and polycarbonate filters, can be accommodated in the collection chambers. 2.1.1.4 Dust Feeder The chrysotile asbestos-containing powder was metered into the collection system by a grooved disk, which rotates at a known rate. The powder is pneumatically unloaded from a groove in the disk and then conveyed to a sonic velocity disperser. Powder is loaded into the top of the powder hopper through the powder feed port. The powder then drops down into the hopper connector, where it is pushed into the groove of the disk by rubber wipers attached to the bottom of the agitator shaft. A spring-loaded guard ring surrounds the hopper connector and scrapes the disk to prevent the disk from carrying away excess powder. The rotation of the disk continuously carries the powder in the groove to the unloading nozzle, where it is removed pneumatically by compressed air. The powder feed rate is determined entirely by the rotation speed of the disk and the size of the groove. The loading of powder on sample filters is further adjusted by varying the collection time. Chrysotile asbestos fiber atmospheres are generated using a two-component fluidized bed consisting of bronze powder and sized chrysotile asbestos fibers. By proper adjustment of air flow through the bottom and across the top of the bed, the bronze powder bed is fluidized and the chrysotile asbestos fibers are stripped at a low rate and fed to the sonic velocity disperser. There is a concentration gradient using this system because the chrysotile asbestos is depleted from the fluidized bed. However, because a homogeneous atmosphere is produced, each sampling port still collects an equivalent amount of chrysotile asbestos. By varying the sampling time, the 7 ------- chrysotile asbestos loading on the cassettes is adjusted. By using a combination of the fluidized bed and the powder feeder, a variety of fibers and particulates is loaded onto a filter. 2.1.1.5 Sonic Velocity Disperser and Settling Tower The air stream from the dust feeder carries the aerosol to the sonic velocity disperser. Dilution air is also delivered to the sonic velocity disperser, where it de-agglomerates the aerosol under the action of an on-line static eliminator and high air velocity. The aerosol then enters the settling tower, the linear velocity is reduced, and the larger particles settle out to the base of the settling tower. The diluted aerosol is then divided uniformly among the four collection chambers. 2.1.1.6 Sample Collection Chamber The base section of the sample collection chamber consists of layers of gaskets and machined-aluminum sheets. Eighty sampling ports are situated in an 8 x 10 matrix arrangement. Downstream from each port is a critical flow orifice. The mounting sheet in which the 80 critical flow orifices are embedded forms the upper section of a vacuum chamber, so that a vacuum to this chamber creates the necessary pressure differential to operate the orifices. Aerosol enters the collection chambers through 20 symmetrically located passages. The 320 orifices (80 for each of four sample collection chambers) all have the same diameter and were calibrated at the time the system was constructed to ensure that all the ports sample at the same flow rate. The orifices form a matched set, with a maximum flow rate of 2 L/min through each air monitor in the system. SRI collected 100 filters in each batch, and utilized 80 of the primary filter cassettes (e.g., in a 0.45 |_im pore size batch the 0.45 |_im pore size filters are the primary filter cassettes) and 20 of the secondary filter cassettes (e.g., in a 0.45 |_im pore size batch the 0.8 |_im pore size filters are the secondary filter cassettes), so that the variable loadings of different batches could be adequately measured and controlled. The 80 primary filter cassettes and 20 secondary filter cassettes were divided evenly between the four quadrants of the chamber. It should be noted that the fiber loading process is trial and error. That is, the chrysotile asbestos structures per area of filter will be different for two filters in the same loading category. 8 ------- The collection chambers are opened from the top by removing a cover. Air monitoring filter cassettes are connected to the sampling port using a luer fitting. Quality control activities include checking each orifice flow rate with a digital flow meter before and after sample generation and analyzing for background levels to prevent carryover contamination. 2.2 Sample Analysis Strategy 2.2.1 Fiber Retention Efficiency of 0.45 jim and 0.8 jim Pore Size MCE Filters Seventy-two filter samples were prepared and analyzed to test pore size differences and fiber loading differences between the two MCE filter types (see Table 1). Eighteen filters were analyzed for each of four batches. Twelve of the primary filters and six of the secondary filters were analyzed for each batch. 2.2.2 Effect of Plasma Etching Time on Chrysotile Asbestos Density Annex A "Determination of Operating Conditions for Plasma Asher" of ISO Method 10312:1995 requires etching of collapsed filters for 8 minutes using operating parameters determined for completely ashing uncollapsed filters in 15 minutes. Including the specified 8 minute etching time, three additional etching times were used to etch the 0.45 |_im MCE filters (Table 2). Hence, a total of 12 filters were etched for each of four different times (2, 4, 8, and 16-minutes). The filters were loaded at a "high" nominal loading. Table 2. Plasma etching time for 0.45 jum pore size MCE filters Filter Loading Plasma Etching Time (Minutes) and Number of Samples 2 4 8 16 High 12 12 12 12 2.3 Analytical Methodology 2.3.1 TEM Specimen Preparation 9 ------- TEM specimens were prepared from the air filters using the dimethylformamide (DMF) collapsing procedure of ISO 10312:1995, as specified for cellulose ester filters. DMF was used as the solvent for dissolution of the filter in the Jaffe washer. Prior to etching the filters, a March Plasmod asher was calibrated in accordance with ISO 10312:1995 procedures whereby an uncollapsed filter was oxidized under controlled settings in approximately 15 minutes. After asher calibration, the filters were prepared using ISO 10312:1995 procedures and etched for either 2, 4, 8, or 16-minutes. For each filter, an equal number of grid openings were examined on at least two prepared TEM specimen prepared from a one-quarter sector of the filter using 200 mesh-indexed copper grids. The remaining part of the filter was archived in the original cassette in clean and secure storage. 2.3.2 TEM Measurement Strategy 1. The minimum aspect ratio for the analyses was 3:1, as permitted by ISO 10312:1995. As required in the ISO Method, any identified compact clusters and compact matrices were counted as total chrysotile asbestos fibers, even if the 3:1 aspect ratio was not met. 2. All fibers larger than or equal to (>) 0.5 |_im in length were quantified with the following breakdown according to ranges by length: a) >0.5 to 5.0 |_im; b) >5.0 to 10.0 |_im; and c) >10.0 |_im. 3. The fiber counting data was distributed approximately equally among a minimum of two specimen grids prepared from different parts of the filter sector. 4. The TEM specimen examinations were performed at approximately 20,000 magnification. 5. Phase contrast microscopy-equivalent chrysotile asbestos structures (PCME) were also determined. PCME chrysotile asbestos structures, as defined by ISO 10312:1995, are >5 |_im in length and from 0.2 to 3.0 |_im in diameter with an aspect ration >3:1. 10 ------- 2.3.3 Determination of Stopping Point The analytical sensitivity was > 6 chrysotile asbestos structures per square millimeter (s/mm ). In principle, any analytical sensitivity can be achieved by increasing the number of grid openings or fields examined. Likewise, statistical uncertainty around the number of fibers observed can be reduced by counting more fibers. Stopping rules are needed to identify when microscopic examination should stop, both at the low end (zero or very few fibers observed) and at the high end (many fibers observed). The analysis was terminated upon completion of counting >25 chrysotile asbestos structures in a minimum of 10 grid openings or 100 chrysotile asbestos structures in 4 grid openings. In any case completion of the grid opening being analyzed when the stopping rules have been met was completed. 2.4 Quality Control/Quality Assurance 2.4.1 MCE Filters (0.45 jim and 0.8 jim pore size) The filter samples generated by SRI were monitored for absolute concentration and for intra-batch uniformity by an independent quality control (QC) laboratory, RTI International (RTI). RTI prepared and analyzed samples and provided feedback to SRI regarding filter density so that the batches meet the target densities. They also used the data to validate the uniformity of density of filters within each batch. For each batch of filters produced, a relative standard deviation (RSD) of fibers per grid opening was developed with 40 grid openings analyzed. Based upon historical RSD levels for SRI filters, each batch was expected to have an RSD at or below 0.50, which was the case for this study. 2.4.2 Lot Blanks Before filter samples were loaded with chrysotile asbestos two unused filters from each filter lot of 0.45 and 0.8 jam filters were analyzed by the QC laboratory to determine the mean chrysotile asbestos structure count. The lot blanks were analyzed for chrysotile asbestos structures by using ISO 10312:1995. In all cases the mean count for all types of chrysotile asbestos structures was <18 structures/mm2. 11 ------- 2.4.3 Laboratory Blank Laboratory blanks are unused filters that are prepared and analyzed in the same manner as the field samples to verify that reagents and equipment are free of the subject analyte, and that contamination has not occurred during the analysis process. The laboratory analyzed two 0.45 |im and two 0.8 |im pore size MCE filters. Blanks were prepared and analyzed along with the other samples. Chrysotile asbestos was not present on any of the samples at an analytical sensitivity of 8.9 s/mm2. 2.4.4 Interlaboratory QA/QC After analysis by the primary laboratory (Clayton Group Services, Inc.), selected filters and grid preparations were sent to the QC laboratory for analysis as an independent QA/QC check. The QA/QC sample analyses included duplicates and verified counts by TEM. 2.4.4.1 Duplicate Analyses The duplicate analyses was conducted by repreparing and analyzing the same filter using the same ISO 10312:1995 counting rules. Results of the QC duplicate analysis are presented in Table 3. In Table 3, the third column lists the number of structures analyzed, and the fourth column lists the density of chrysotile asbestos structures per unit area. Note: The primary laboratory used a grid opening size of 0.011 mm2, and the QC laboratory used a grid opening size of 0.0086 mm2. Column 5 presents the results of the duplicate sample variability. All four interlaboratory duplicate samples met the acceptance criteria. 12 ------- Table 3. Interlaboratory duplicates analysis of MCE filters for chrysotile asbestos by TEM Sample No. Laboratory Analyses Actual Variability11 Accepted Variability # Structures Structures/mm2 A0611022- 001A Primary 26 230 QC 23 270 1.8 2.24 A0611022- 002A Primary 28 250 QC 19 220 1.3 2.24 A0611022- 003A Primary 34 300 QC 27 310 0.39 2.24 A0611022- 004A Primary 31 280 QC 22 280 0.86 2.24 aAnalvtical Variability = (Analysis A) - (Analysis B) V(Analysis A + Analysis B) This variability is the absolute value of the difference of the two analyses, divided by the square root of the sum, which is an estimate of the standard deviation of the difference based on a Poisson counting model. The value 2.24 was selected as targeting false positive rates of 2.5% (1/40) for the Poisson model. 2.4.4.2 Verified Counts Verification counting involved re-examination of the same grid openings analyzed by the primary laboratory. The verification counting was performed on two of the analyses for each of the filter pore sizes. Verified counting was conducted using the procedure defined in NISTIR 5351, "Airborne Asbestos Method: Standard Test Methodfor Verified Analysis of Asbestos by Transmission Electron Microscopy - Version 2.0." Results of interlaboratory QC verified counting by TEM are presented in Table 4. In Table 4, the third column gives the total number of chrysotile asbestos structures counted in the specified grid openings which were determined to be true positives (TP). Column 4 gives the number of false positives (FP) and Column 5 gives the number of false negatives (FN). The results of all four analyses are combined at the bottom, and ratios of true positives, false positives, and false negatives are developed in the final two rows for both the primary and QC laboratory. Column 6 shows the "pass" (Yes) or "fail" (No) status of the comparison. The acceptable variability is >80% true positives, <20% false negatives, and <20% false positives. All interlaboratory verified count analysis met the acceptance criteria. 13 ------- Table 4. Interlaboratory verified count analysis of MCE filters for chrysotile asbestos by TEM Sample No. Laboratory Number of Structures Pass? True Positive False Positive False Negative A0611024- Primary 24 0 1 003A QC 25 1 0 A0611024- Primary 35 3 0 002A QC 32 0 3 A0611024- Primary 5 0 1 004A QC 6 1 0 A0611024- Primary 8 0 0 005A QC 7 0 1 Totals Primary 72 3 2 QC 70 2 4 Percentages Primary 97% 4% 3% Yes QC 95% 3% 5% Yes 14 ------- SECTION 3 RESULTS AND DISCUSSION 3.1 Fiber Retention Efficiency (Fibers >0.5 jim) of 0.45 and 0.8 jim Pore Size MCE Filters Chrysotile asbestos fibers are the most difficult to see and count after capture, so they present a worst case for retaining and counting fibers after they are retained on filters. Amphiboles are easier to see and count after capture. Therefore, this study was not so concerned about the capture of fibers, but in seeing them with electron microscopy after capture. Deeply embedded fibers present a particular challenge. Filtration theory13 states that the most penetrating particle size decreases with decreasing size of filter medium. Thinner fibers, therefore, penetrate a filter matrix more deeply than thicker fibers, making microscopy more difficult. Due to the fact that it is the most common fiber type in most asbestos exposure scenarios to date and owing to its finely fibrous nature it is also the ideal form of asbestos to study post-preparation fiber retention in filters.14 equation for predicting most penetrating particle diameter (dp.min) is: Where, K is the hydrodynamic factor, a = solidity of filter (1 - porosity), X is the mean free path of the gas molecules, &is the Boltzmann constant, T is the absolute temperature, rj is the air viscosity, df is the filter fiber diameter, and U is average air velocity inside the filter medium. Therefore, the most penetrating particle diameter decreases with decreasing pore size in the filter medium. This relationship holds for both fibrous and membrane filters16, and in porous-membrane filters 14 Of all asbestos fiber types, chrysotile is the most likely to penetrate the tortuous matrix of MCE filter material, thus optimizing the ability of the study to employ electron microscopy to characterize differences in asbestos post-preparation fiber retention, due to MCE pore size (larger pore sizes equate to greater potential penetration of fibers into the 15 ------- matrix) and due to differential plasma etching time. Amphibole asbestos fibers, with their larger average diameter and length,17 are less likely to penetrate the MCE matrix, and therefore more easily visible than most chrysotile fibers by microscopy. In addition, since chrysotile asbestos is by far the most commonly seen asbestos type on air filters (such as from remediation sites), it best reflects real-world situations. Thus, these results for chrysotile asbestos provide an indication of filter effectiveness for numerous fibers, including amphibole asbestos. A total of 72 filters (18 of 0.45 [j,m pore size and 18 of 0.8 [j,m pore size) were loaded with chrysotile asbestos at two filter loadings (low = 2-5 fibers/grid opening; and high = >5 fibers/grid opening). The experiment was conducted in 4 batches of 18 filters each (Table 1). All chrysotile asbestos structures >0.5 |im in length were quantified and categorized according to three ranges by length: >0.5 to 5 |im; >5 to 10 |im; and >10 |im. The chrysotile asbestos fiber distribution for the low and high filter loadings is presented in Table 5. Table 5. Mean chrysotile asbestos density (s/mm2) by batch and fiber length Mean fiber density (s/mm2) by length of fibers (standard deviation) Batch Filter Low Loading Filter High Loading >0.5-5 |im >5-10 |im >10 |im >0.5-5 |im >5-10 |im >10 |im 0.45 |im pore size 1 237 (113) 63 (22) 21 (112) 2 - - - 585 (92) 284(86) 89(30) 3 317(41) 71(21) 21(14) 4 - - - 1200(296) 235 (91) 66(48) 0.8 |im pore size 1 194(44) 60(21) 19(13) 2 - - - 429 (80) 225 (76) 88 (33) 3 288 (69) 78 (30) 22(10) 4 - - - 960 (299) 261 (70) 71 (27) The mean filter density (total chrysotile asbestos structures per mm2) for the two filter types in each batch is presented in Table 6. In each batch, the mean density on the 0.45 |im filters is higher than on the 0.8 |im filters. In Batch 2, the difference is statistically significant using both the two-sample t-test (p = 0.008) and the nonparametric Wilcoxon Rank-Sum test (p = 0.01). In the other 3 batches, the difference is not statistically significant. 16 ------- Table 6. Mean total chrysotile asbestos density (s/mm2) by batch and filter type Batch Mean fiber density (s/mm2) by filter pore size and nominal loading (standard deviation) 0.45 jim 0.8 jim Low Loading High Loading Low Loading High Loading 1 321 (114) - 274(57) 2 - 958 (170) - 743 (125) 3 413 (55) - 388 (89) 4 - 1512(369) - 1304 (336) It is apparent from Table 6 that the two "Low Loading" batches differ substantially, as do the two "High Loading" batches. For example, the 0.8 |im density in Batch 3 is higher than the 0.45 |im density in Batch 1, even though both batches were loaded at the same nominal level. Likewise, the 0.8 |im density in Batch 4 is higher than the 0.45 |im density in Batch 2. In fact, the between-batch differences (at the same nominal loading) are greater than the differences between the two filter types. Thus, it is not appropriate to combine the 4 batches into a single dataset for purposes of an overall comparison between the two filter types (Primary Objective 1). To make the overall comparison, the sum of the Wilcoxon statistics for the 4 separate batches was used. In each batch, the Wilcoxon statistic is the rank-sum for the 0.45 |im densities in the 18 samples comprising the batch. Under the null hypothesis that the two filter types have the same fiber retention efficiency, this statistic has (approximately) a normal distribution with mean 57 (Batches 2 and 3) or 114 (Batches 1 and 4), and variance 114 (all batches). Thus, under the null hypothesis, the sum of the 4 Wilcoxon statistics is approximately normal with mean 342 and variance 456. The observed value of the sum is 395.5, resulting in a test statistic z = (395.5- 342)/21.4 = 2.50, with a p-value of 0.01. Thus, the null hypothesis is rejected, and we conclude that the fiber retention efficiency of the 0.45 |im pore size filter for fibers >0.5 |im in length is significantly higher than that of the 0.8 |im pore size filter. However, for fibers >5 |im in length there is no difference in the two filter pore sizes (see Figures 5 and 6, Section 3.2). 3.2 Effect of Plasma Etching Time on Total Chrysotile Asbestos Density (Fibers >0.5 jim) Four different etching times were used to etch 0.45 |im filters. A total of 12 filters were etched for each of the 4 times (2, 4, 8 and 16 minutes). The filters were loaded in at the "High" nominal loading. Table 7 shows the mean total chrysotile asbestos density (s/mm2) for fibers >0.5 jam in length for each etching time. 17 ------- Table 7. Mean total chrysotile asbestos (fibers >0.5 jim) density (s/mm2) for variable etching times Filter Loading Plasma etching time for 0.45 jim MCE filters (minutes). Standard deviation in parentheses. 2 4 8 16 High 1123 (295) 1251 (442) 1512(369) 1635 (236) The mean fiber retention density increases with etching time. To examine the relationship between etching time and density, two regression models were fit to the data. The first model assumes a linear relationship between etching time (t) and density (TA): TA = a + b*t (1) The fitted equation was TA (s/mm2) =1113+ 35.7*t (R2 = 0.24) The relatively low value of R2 is due to the considerable variability in densities observed at each etching time. However, the coefficient of t is highly significant (SE = 9.27). This regression indicates that each additional minute of etching time adds an average of 35.7 s/mm2 to the total chrysotile asbestos density within the range tested. The second regression model assumes a logarithmic relationship between density and etching time, of the form TA = a + b*log(t) (2) Here, "log" denotes the natural logarithm (In). The fitted equation was TA (s/cm2) = 931 + 259*ln(t) (R2 = 0.27) R2 is slightly higher than for the linear model. Again, the regression is highly significant (SE of coefficient = 63). This model estimates that a doubling of the etching time adds an average of 13% to the total chrysotile asbestos density within the range tested. On physical grounds, it would appear that a point of diminishing returns for increased 18 ------- etching time would be reached, i.e., there is a level of etching time beyond which no increase in density is expected (Figures 3 and 4). The data from this experiment do not appear to shed light on what this level might be. For example, the increase in density from 8 to 16 minutes is comparable to that from 2 to 4 minutes. However, the increase in density with etching time does not appear to be the case for fibers >5 |im in length (Figures 5 and 6). These data suggest that the etching time of 8 minutes that is specified in ISO 10312:1995 is adequate for fibers >5 |im in length. If fibers <5 |im in length are of interest, additional research may be needed to determine the optimum etching time. Etch Time (min) A 19 ------- 2500 2000 1500 1000 ~ ~ ~ ~ 500 ~ ~ B 8 10 Etch Time (min) 12 14 16 18 Figure 3. A. Fiber densities (fibers > 0.5 jim in length) observed on 0.45 jim pore size MCE Filter by etch time in minutes: A. Mean fiber densities; B. Scatter plot showing range of density values of individually sampled filters (N=48). Etch time (min) Figure 4. Mean chrysotile asbestos fiber densities (fibers > 0.5 to 5 jim in length) observed on 0.45 jim pore size MCE filter at varying etching times. 20 ------- E E £ 0) 0) Si E 3 1100 900 700 500 300 100 10 Etch time (min) 15 20 Figure 5. Mean chrysotile asbestos fiber densities (fibers 5 to 10 jim in length) observed on 0.45 jim pore size MCE filter at varying etching times. 300 10 Etch time (min) 15 20 Figure 6. Mean chrysotile asbestos fiber densities (fibers >10 jim in length) observed on 0.45 jim pore size MCE filter at varying etching times. 3.3 Comparison of Fiber Retention Efficiency of 0.45 jim and 0.8 jim Pore Size Filters for Fibers > 5 jim in Length The mean filter loading (total chrysotile asbestos structures, > 5 [j,m, per mm2) for the two filter types in each batch is shown in Table 8. 21 ------- Table 8. Mean chrysotile asbestos density (s/mm2) for fibers >5 jim in length by batch and filter type Batch Mean fiber density (s/mm2) by filter pore size and nominal loading (standard deviation) 0.45 jim 0.8 jim Low Loading High Loading Low Loading High Loading 1 84 (30) - 80 (28) 2 - 373 (102) - 313 (104) 3 92 (33) - 100(32) 4 - 301 (118) - 333 (85) In Batches 1 (Low loading) and 2 (High loading), the mean density on the 0.45 jam filters is higher than on the 0.8 jam filters. In Batches 3 (Low loading) and 4 (High loading), the reverse is true; i.e., the 0.8 |im filters are higher. None of the differences are statistically significant using both the two-sample t-test. When Batches 1 and 3 (Low loading), and Batches 2 and 4 (High loading), are combined, the differences between the filter types are even smaller. We conclude that, for fibers > 5 |iin, there is no difference between the fiber retention efficiencies of the 0.45 |im and 0.8 |im filters. 3.4 Effect of Plasma Etching Time on Chrysotile Asbestos Fibers >5 jim Table 9 shows the mean total chrysotile asbestos density for fibers > 5 [j,m (s/mm2) for each etching time. The mean densities for the 2, 8 and 16 minute etching times are virtually identical. The mean density for the 4 minute etching time is a little lower. Table 9. Mean chrysotile asbestos density for fibers > 5 jim (s/mm2) for variable etching times (standard deviation) Filter Loading Plasma etching time for 0.45 jim MCE filters (minutes) 2 4 8 16 High 301 (75) 232(99) 301 (118) 303 (77) To examine the relationship between etching time and density, two regression models were fit to the data. The first model assumes a linear relationship between etching time (t) and density (TA): 22 ------- TA = a + b*t (3) The fitted equation was TA (s/mm2) = 267 + 2.2*t (R2 = 0.016) The regression is not statistically significant. The second regression model assumes a logarithmic relationship between density and etching time, of the form Again, the regression is not statistically significant. The fact that neither regression is statistically significant indicates that, for 0.45 |im filters, there is no statistically significant relationship between etching time and density of fibers > 5 |im. This is consistent with a study conducted by Chatifield.11 The study showed that fiber densities for fibers longer 5 |im are similar for 0.2 |im pore size PC filters and various etching schedules for 0.22 |im pore size MCE filters. In particular, plasma etching had no effect on the reported fiber densities of fibers longer than 5 |im. At the 1% significance level, there was no statistically significant differences between the mean fiber densities for any of the etching preparations evaluated. TA = a + b*log(t) (4) Here, "log" denotes the natural logarithm. The fitted equation was TA (s/mm2) = 266 + 10.5*log(t) (R2 = 0.007) 23 ------- SECTION 4 CONCLUSIONS AND RECOMMENDATIONS Fiber Retention Efficiency of 0.45 and 0.8 jim Pore Size MCE Filters The type of asbestos chosen for this study was chrysotile asbestos, due to its finely fibrous nature. Of all asbestos fiber types, chrysotile is the most likely to penetrate the tortuous matrix of MCE filter material, thus optimizing the ability of the study to see differences in asbestos fiber retention efficiency, due to MCE pore size (larger pore sizes equate to greater potential penetration of fibers into the matrix) and due to differential plasma etching time. Amphibole asbestos fibers, with their larger average diameter and length, are less likely to penetrate the MCE matrix. In addition, since chrysotile asbestos is by far the most commonly seen asbestos type on air filters (such as from remediation sites), it best reflects real-world situations. Thus, these results for chrysotile asbestos provide an indication of filter effectiveness for numerous fibers, including amphibole asbestos. Conclusion—The null hypothesis was that the two mixed-cellulose ester (MCE) filter types (0.45 |im and 0.8 |im pore size) have the same fiber retention efficiency for chrysotile asbestos aerosol (structures >0.5 |im length). The null hypothesis was rejected, and it is concluded the fiber retention efficiency of the 0.45 |im pore size MCE filter is statistically significantly higher than that of the 0.8 |im pore size MCE filter (p=0.01) for fibers >0.5 |im in length. However, for chrysotile asbestos structures >5 |im in length, there is no statistically significant difference between the fiber retention efficiencies of 0.45 |im and 0.8 |im pore size MCE filters (p>0.05). Recommendation—This research study demonstrates that the fiber retention efficiency of a 0.45 |im pore size MCE filter for aerosols of chrysotile asbestos fibers (structures >0.5 |im) is greater than that for a 0.8 |im pore size MCE filter. However, there is no difference in fiber retention efficiency between these pore sizes for structures longer than 5.0 |im. If the exposure study is focused on fibers less than 5.0 |im, the investigator ------- should use filters with 0.45 jam pore size. If the exposure study is only interested in structures longer than 5.0 |im, then either filter pore size may be used. 4.2 Effect of Etching Time for 0.45 jim MCE Filters Conclusion—There is a significant difference in the effect of etching times for fibers <5.0 |im and fibers >5.0 |im in length. The mean density of chrysotile asbestos fibers >0.5 |im in length increases with etching time (2, 4, 8, and 16-minutes) of 0.45 |im pore size MCE filters. Regression analysis of etching time and densities showed that doubling the etching time adds an average of 13% to the total chrysotile asbestos density within the range tested. This increase is a diminishing percentage of the total fiber count as the etching time increases; e.g., 20% at 2 minutes, and 12% at 8 minutes. There is likely an etching time beyond which no increase in density is expected and in fact would decrease; the data from this experiment did not identify this etching time. However, etching the filter for longer periods may remove too much filter so that a specimen for TEM analysis cannot be prepared. For fibers > 5.0 |im in length, there is no significant difference in numbers of structures counted at the etching times used in these tests. Recommendation—Since most asbestos exposure risk models include fibers >5.0 |im in length, the 8 minute etching time specified in ISO 10312:1995 is adequate. However, if an exposure study is focused on fibers < 5.0 |im in length, the etching time of 8-minutes should be reviewed. A study should be conducted to determine the etching time beyond which no significant increase in asbestos density of fibers <5.0 |im in length is expected. 4.3 Additional Recommendations • NIOSH Method 7402 notes that a 0.45 |im pore size filter may be difficult to use with some personal sampling pumps due to the pressure drop across this filter. The tandem MCE filter assembly (0.45 |im pore size filter and 5 |im pore size diffusing filter) recommended by AHERA (40 CFR §761), ISO Method 10312:1995, and 25 ------- ASTM Method D 6281-04 may preclude the use of some battery-powered personal sampling pumps due to the resultant high pressure drop. Analysis of filters by TEM require the use of the 5 |im pore size diffusing filter to assure uniform deposition on the primary collection filter. A study should be conducted to evaluate the difference between chrysotile asbestos aerosols collected on 0.45 |im and 0.8 |im pore size MCE filters with and without the 5 |im pore size MCE diffusing filter. Also, specifications for personal pumps should be investigated to determine optimum requirements for sampling using the 0.45 |im pore size collection filter and 5 |im pore size diffusing filter combination. • This study has focused on MCE filters since this filter type is the primary choice for air monitoring. Exposure to asbestos through inhalation is considered the most likely route for asbestos exposure. Polycarbonate (PC) filters are used in monitoring asbestos in water and possibly by some studies of inhalation. Since no data has been found comparing the relative effectiveness of MCE and PC filters, research should be considered to compare the retention of asbestos fibers on 0.45 |im pore size MCE filters to 0.4 |im pore size polycarbonate filters. SECTION 5 ACKNOWLEDGMENTS This report is the result of recommendations and insights from numerous scientists interested in advancing the state-of-the-science of airborne fiber measurements. In particular, the experts in the EPA Regional Offices, most notably Julie Wroble, Mark Maddaloni, Aubrey Miller, Phil King and Mary Goldade, provided reviews and recommendations from the onset. The comments and recommendations gained from the peer review of a companion article to be published in the Journal of Occupational and Environmental Hygiene also enhanced the presentation of the information gained from this research. 26 ------- SECTION 6 REFERENCES 1. US Code of Federal Regulations, 40 CFR Part 763, Appendix A to Subpart E. "Interim Transmission Electron Microscopy Analytical Methods - Mandatory and Nonmandatory - and the Mandatory Section to Determine Completion of Response Action." 2. American Society for Testing and Materials, "Standard Test Method for Airborne Asbestos Concentration in Ambient and Indoor Air as Determined by Transmission Electron Microscopy Direct Transfer (TEM)", ASTM D 6281. 3. International Organization for Standardization, "Ambient Air - Determination of asbestos fibres - Direct-transfer transmission electron microscopy method," ISO 10312, 1995. 4. International Organization for Standardization, "Ambient Air - Determination of asbestos fibres - indirect-transfer transmission electron microscopy method," ISO 13794, 1999. 5. National Institute for Occupational Safety and Health. "Asbestos by TEM," Method 7402, Issued August 15, 1994. NIOSH Manual of Methods, http://www.cdc.gov/niosh/nmam/. 6. United States Environmental Protection Agency. "Superfund Method for the Determination of Asbestos in Ambient Air, Part 1: Method." EPA 540/2-90-005a. May 1990. 7. United States Environmental Protection Agency. "Methodology for the Measurement of Airborne Asbestos by Electron Microscopy," Yamate, G. Agarwal, S. C. and Gibbons, R. D. Draft Report, EPA Contract 68-02-3266 for Environmental Monitoring Systems Laboratory, Office of Research and Development, Research Triangle Park, NC 27711. 27 ------- 8. National Institute for Occupational Safety and Health. "Asbestos and Other Fibers by PCM," Method 7400, Issue 2, August 15, 1994. NIOSH Manual of Methods, http://www.cdc.gov/niosh/nmam/. 9. Occupational Safety and Health Administration, U. S. Department of Labor. "Asbestos in Air, Method Number ID-160." July 1997, http://www.osha.gov/dts/sltc/methods/toc.html 10. International Organization for Standardization, "Air Quality - Determination of the number concentration of airborne inorganic fibers by phase contrast microscopy - Membrane filter method." ISO 8672, 1993. 11. Chatfield, E.J. Measurements of Chrysotile Fiber Retention Efficiencies for Polycarbonate and Mixed Cellulose Ester Filters, Eric J. Chatfield, Advances in Environmental Measurement Methods for Asbestos, American Society for Testing and Materials, Special Technical Publication 1342, 2000. 12. Beard, M.E. and J.R. Kominsky. Sampling and Analysis of Asbestos Fibers on Filter Media to Support Exposure Assessments: Scoping Effort. Report prepared by Environmental Quality Management, Inc., Cincinnati, OH and RTI International, Research Triangle Park, NC for U.S. EPA, National Exposure Research Laboratory, Task Order No. 0020, Contract No. 68-C-00-186 (December 2006). 13. Spurny, K. On the Filtration of Fibrous Aerosols. J. Aerosol. Sci. 16(3): 450-455 (1986). 14. Baron, P. A. and K. Willeke, (2005). Aerosol Measurement: Principles, Techniques, and Applications. 2nd Edition. Wiley-Interscience, Hoboken, NJ. 213-215. 15. Lee, K.W. and B.Y.H. Liu.(1980). On the minimum efficiency and the most penetrating particle size for fibrous filters. Journal of the Air Pollution Control Assocation. 30: 377- 381. 28 ------- Wylie AG, R.L. Virta, and E. Russek (1985). Characterizing and discriminating airborne amphibole cleavage fragments and amosite fibers: implications for the NIOSH method: American Industrial Hygiene Journal. 46:197-201. Rubow, K.L. (1981). Submicrometer Aerosol Filtration Characteristics of Membrane Filters. Ph.D. thesis, University of Minnesota, Minneapolis, MN. 29 ------- Appendix - Chrysotile Asbestos Data Listing Batch Loading Sample ID Grid Openings Counted Grid Opening Size (mm) Filter Type (MCE = mixed cellulose ester) Size (mm) Effective Filter Area (mm2) Total Chrysotile Asbestos Structures (s/mm2) 1 Low A0611022- 002A 10 0.01122 MCE Filter, 0.45 jjm 25 385 249.6 1 Low A0611022- 003A 10 0.01122 MCE Filter, 0.45|jm 25 385 303.0 1 Low A0611022- 006A 10 0.01122 MCE Filter, 0.45|jm 25 385 249.6 1 Low A0611022- 008A 10 0.01122 MCE Filter, 0.45|jm 25 385 606.1 1 Low A0611022- 01 OA 10 0.01122 MCE Filter, ,45|jm 25 385 267.4 1 Low A0611022- 012A 10 0.01122 MCE Filter, 0.45|jm 25 385 311.9 1 Low A0611022- 013A 10 0.01122 MCE Filter, 0.45|jm 25 385 294.1 1 Low A0611022- 014A 10 0.01122 MCE Filter, 0.45|jm 25 385 267.4 1 Low A0611022- 015A 12 0.01122 MCE Filter, 0.45|jm 25 385 185.7 1 Low A0611022- 016A 10 0.01122 MCE Filter, 0.45|jm 25 385 481.3 1 Low A0611022- 017A 10 0.01122 MCE Filter, 0.45|jm 25 385 338.7 1 Low A0611022- 018A 10 0.01122 MCE Filter, 0.45|jm 25 385 294.1 1 Low A0611022- 001A 10 0.01122 MCE Filter, 0.8|jm 25 385 231.7 1 Low A0611022- 004A 10 0.01122 MCE Filter, 0.8|jm 25 385 276.3 ------- Batch Loading Sample ID Grid Openings Counted Grid Opening Size (mm) Filter Type (MCE = mixed cellulose ester) Size (mm) Effective Filter Area (mm2) Total Chrysotile Asbestos Structures (s/mm2) 1 Low A0611022- 005A 10 0.01122 MCE Filter, 0.8|jm 25 385 267.4 1 Low A0611022- 007A 11 0.01122 MCE Filter, 0.8|jm 25 385 210.7 1 Low A0611022- 009A 10 0.01122 MCE Filter, 0.8|jm 25 385 285.2 1 Low A0611022- 011A 10 0.01122 MCE Filter, 0.8|jm 25 385 374.3 2 High A0611023- 001A 8 0.01122 MCE Filter, 0.45|jm 25 385 1114.1 2 High A0611023- 002A 8 0.01122 MCE Filter, 0.45|jm 25 385 1192.1 2 High A0611023- 004A 10 0.01122 MCE Filter, 0.45|jm 25 385 748.7 2 High A0611023- 005A 10 0.01122 MCE Filter, 0.45|jm 25 385 944.7 2 High A0611023- 009A 10 0.01122 MCE Filter, 0.45|jm 25 385 935.8 2 High A0611023- 01 OA 10 0.01122 MCE Filter, 0.45|jm 25 385 811.1 2 High A0611023- 003A 10 0.01122 MCE Filter, 0.8|jm 25 385 748.7 2 High A0611023- 006A 10 0.01122 MCE Filter, 0.8|jm 25 385 713.0 2 High A0611023- 007A 10 0.01122 MCE Filter, 0.8|jm 25 385 641.7 2 High A0611023- 008A 10 0.01122 MCE Filter, 0.8|jm 25 385 606.1 2 High A0611023- 011A 10 0.01122 MCE Filter, 0.8|jm 25 385 980.4 2 High A0611023- 012A 10 0.01122 MCE Filter, 0.8|jm 25 385 891.3 ------- Batch Loading Sample ID Grid Openings Counted Grid Opening Size (mm) Filter Type (MCE = mixed cellulose ester) Size (mm) Effective Filter Area (mm2) Total Chrysotile Asbestos Structures (s/mm2) 2 High A0611023- 013A 10 0.01122 MCE Filter, 0.8|jm 25 385 641.7 2 High A0611023- 014A 10 0.01122 MCE Filter, 0.8|jm 25 385 730.8 2 High A0611023- 015A 10 0.01122 MCE Filter, 0.8|jm 25 385 935.8 2 High A0611023- 016A 10 0.01122 MCE Filter, 0.8|jm 25 385 650.6 2 High A0611023- 017A 10 0.01122 MCE Filter, 0.8|jm 25 385 730.8 2 High A0611023- 018A 10 0.01122 MCE Filter, 0.8|jm 25 385 650.6 3 Low A0611025- 001A 10 0.01122 MCE Filter, 0.45|jm 25 385 463.5 3 Low A0611025- 002A 10 0.01122 MCE Filter, 0.45|jm 25 385 436.7 3 Low A0611025- 003A 10 0.01122 MCE Filter, 0.45|jm 25 385 392.2 3 Low A0611025- 004A 10 0.01122 MCE Filter, 0.45|jm 25 385 436.7 3 Low A0611025- 005A 10 0.01122 MCE Filter, 0.45|jm 25 385 311.9 3 Low A0611025- 007A 10 0.01122 MCE Filter, 0.45|jm 25 385 436.7 3 Low A0611025- 006A 10 0.01122 MCE Filter, 0.8|jm 25 385 267.4 3 Low A0611025- 008A 10 0.01122 MCE Filter, 0.8|jm 25 385 445.6 3 Low A0611025- 009A 10 0.01122 MCE Filter, 0.8|jm 25 385 472.4 3 Low A0611025- 01 OA 10 0.01122 MCE Filter, 0.8|jm 25 385 499.1 3 Low A0611025- 10 0.01122 MCE Filter, 25 385 383.2 ------- Batch Loading Sample ID Grid Openings Counted Grid Opening Size (mm) Filter Type (MCE = mixed cellulose ester) Size (mm) Effective Filter Area (mm2) Total Chrysotile Asbestos Structures (s/mm2) 011A 0.8|jm 3 Low A0611025- 012A 10 0.01122 MCE Filter, 0.8|jm 25 385 383.2 3 Low A0611025- 013A 10 0.01122 MCE Filter, 0.8|jm 25 385 267.4 3 Low A0611025- 014A 10 0.01122 MCE Filter, 0.8|jm 25 385 508.0 3 Low A0611025- 015A 10 0.01122 MCE Filter, 0.8|jm 25 385 463.5 3 Low A0611025- 016A 10 0.01122 MCE Filter, 0.8|jm 25 385 356.5 3 Low A0611025- 017A 10 0.01122 MCE Filter, 0.8|jm 25 385 303.0 3 Low A0611025- 018A 10 0.01122 MCE Filter, 0.8|jm 25 385 303.0 4 High A0611028- 001A 9 0.01122 MCE Filter, 0.45|jm 25 385 1029.9 4 High A0611028- 002A 5 0.01122 MCE Filter, 0.45|jm 25 385 1836.0 4 High A0611028- 003A 7 0.01122 MCE Filter, 0.45|jm 25 385 1311.4 4 High A0611028- 007A 9 0.01122 MCE Filter, 0.45|jm 25 385 1029.9 4 High A0611028- 008A 8 0.01122 MCE Filter, 0.45|jm 25 385 1225.5 4 High A0611028- 01 OA 9 0.01122 MCE Filter, 0.45|jm 25 385 1099.2 4 High A0611028- 011A 5 0.01122 MCE Filter, 0.45|jm 25 385 1978.6 4 High A0611028- 012A 5 0.01122 MCE Filter, 0.45|jm 25 385 2014.3 4 High A0611028- 014A 5 0.01122 MCE Filter, 0.45|jm 25 385 1853.8 ------- Batch Loading Sample ID Grid Openings Counted Grid Opening Size (mm) Filter Type (MCE = mixed cellulose ester) Size (mm) Effective Filter Area (mm2) Total Chrysotile Asbestos Structures (s/mm2) 4 High A0611028- 015A 6 0.01122 MCE Filter, 0.45|jm 25 385 1738.0 4 High A0611028- 016A 6 0.01122 MCE Filter, 0.45|jm 25 385 1515.2 4 High A0611028- 017A 7 0.01122 MCE Filter, 0.45|jm 25 385 1515.2 4 High A0611028- 004A 8 0.01122 MCE Filter, 0.8|jm 25 385 1214.3 4 High A0611028- 005A 7 0.01122 MCE Filter, 0.8|jm 25 385 1286.0 4 High A0611028- 006A 6 0.01122 MCE Filter, 0.8|jm 25 385 1515.2 4 High A0611028- 009A 10 0.01122 MCE Filter, 0.8|jm 25 385 873.4 4 High A0611028- 013A 9 0.01122 MCE Filter, 0.8|jm 25 385 1099.2 4 High A0611028- 018A 5 0.01122 MCE Filter, 0.8|jm 25 385 1836.0 ------- 16 16 16 16 16 16 16 16 16 16 16 16 4 4 4 4 Loading Sample ID Grid Openings Counted Grid Opening Size (mm) Filter Type (MCE = mixed cellulose ester) A0611024- 001A 0.0112 MCE Filter 0.45|jm 25 A0611024- 002A 0.0112 MCE Filter 0.45|jm 25 A0611024- 003A 0.0112 MCE Filter 0.45|jm 25 A0611024- 004A 0.0112 MCE Filter 0.45|jm 25 A0611024- 005A 0.0112 MCE Filter 0.45|jm 25 A0611024- 006A 0.0112 MCE Filter 0.45|jm 25 A0611024- 007A 0.0112 MCE Filter 0.45|jm 25 A0611024- 008A 0.0112 MCE Filter 0.45|jm 25 A0611024- 009A 0.0112 MCE Filter 0.45|jm 25 A0611024- 01 OA 0.0112 MCE Filter 0.45|jm 25 A0611024- 011A 0.0112 MCE Filter 0.45|jm 25 A0611024- 012A 0.0112 MCE Filter 0.45|jm 25 A0611026- 001A 0.0112 MCE Filter 0.45|jm 25 A0611026- 002A 10 0.0112 MCE Filter 0.45|jm 25 A0611026- 003A 10 0.0112 MCE Filter 0.45|jm 25 A0611026- 004A 0.0112 MCE Filter 0.45|jm 25 ------- 4 4 4 4 4 4 4 4 2 2 2 2 2 2 2 2 Loading Sample ID Grid Openings Counted Grid Opening Size (mm) Filter Type (MCE = mixed cellulose ester) A0611026- 005A 0.0112 MCE Filter 0.45|jm 25 A0611026- 006A 0.0112 MCE Filter 0.45|jm 25 A0611026- 007A 0.0112 MCE Filter 0.45|jm 25 A0611026- 008A 0.0112 MCE Filter 0.45|jm 25 A0611026- 009A 0.0112 MCE Filter 0.45|jm 25 A0611026- 01 OA 10 0.0112 MCE Filter 0.45|jm 25 A0611026- 011A 0.0112 MCE Filter 0.45|jm 25 A0611026- 012A 0.0112 MCE Filter 0.45|jm 25 A0611027- 001A 10 0.0112 MCE Filter 0.45|jm 25 A0611027- 002A 10 0.0112 MCE Filter 0.45|jm 25 A0611027- 003A 0.0112 MCE Filter 0.45|jm 25 A0611027- 004A 0.0112 MCE Filter 0.45|jm 25 A0611027- 005A 0.0112 MCE Filter 0.45|jm 25 A0611027- 006A 0.0112 MCE Filter 0.45|jm 25 A0611027- 007A 10 0.0112 MCE Filter 0.45|jm 25 A0611027- 008A 0.0112 MCE Filter 0.45|jm 25 ------- 2 2 2 2 8 8 8 8 8 8 8 8 8 8 8 8 Loading Sample ID Grid Openings Counted Grid Opening Size (mm) Filter Type (MCE = mixed cellulose ester) A0611027- 009A 0.0112 MCE Filter 0.45|jm 25 A0611027- 01 OA 0.0112 MCE Filter 0.45|jm 25 A0611027- 011A 0.0112 MCE Filter 0.45|jm 25 A0611027- 012A 0.0112 MCE Filter 0.45|jm 25 A0611028- 001A 0.0112 MCE Filter 0.45|jm 25 A0611028- 002A 0.0112 MCE Filter 0.45|jm 25 A0611028- 003A 0.0112 MCE Filter 0.45|jm 25 A0611028- 007A 0.0112 MCE Filter 0.45|jm 25 A0611028- 008A 0.0112 MCE Filter 0.45|jm 25 A0611028- 01 OA 0.0112 MCE Filter 0.45|jm 25 A0611028- 011A 0.0112 MCE Filter 0.45|jm 25 A0611028- 012A 0.0112 MCE Filter 0.45|jm 25 A0611028- 014A 0.0112 MCE Filter 0.45|jm 25 A0611028- 015A 0.0112 MCE Filter 0.45|jm 25 A0611028- 016A 0.0112 MCE Filter 0.45|jm 25 A0611028- 017A 0.0112 MCE Filter 0.45|jm 25 ------- &EPA United States Environmental Protection Agency (8101R) Washington, DC 20460 Official Business Penalty for Private Use $300 EPA 600/R-08/046 November 2008 www.epa.gov Recycled/Recyclable Printed with vegetable-based ink on paper that contains a minimum of 50% post-consumer fiber content processed chlorine free ------- |