Document 3Q5aVwq7pNq0M4LoaxOrmg26O

SEFA Aqencv Research and Development ntSMrcn r a i EPA-600/M4-82-020 Oac. 1982 Test Method Interim Method for the Determination of Asbestos in Bulk Insulation Samples* 1. Polarized Light Microscopy 1.1 Principle and AppScabWty Bulk samples of building materials taken for asbestos identification are first examined for homogeneity and preliminary fiber identification at low magnification. Positive identification of suspect fibers is made by analysis of subsamples with the polarized light microscope. The principles of optical mineralogy ere well established.''* A light microscope equipped with two polarizing filters is used to observe specific optical characteristics of a sample. The use of plane potarizodlight allows the determination of refractive indices along specific crystallographic axas Morphology and color are also observed. A retardation Plato is pieced in the polarized light path for determination of the sign of elongation using orthoacopic illumination. Orientation of the two filters such that their vibration pianea are perpendicular (crossed polers) allows observation of the birefringence and extinction characteristics of anisotropic particles. Quantitative analysis involves the use of point counting, Point counting is e standard technique in petrography for determining the relative areas occupied by separate minoraIs in thin sections of rock. Background information on the use of point counting* and the interpretation of point count dsta*is available. ad iiwrto ami oftor arena a--m# kli lis inUmiiOiii. The mthoaOWSwiiOo iwnHtlan tnt amntmi la nOj--i te ruelw. This method is applicable to all bulk samples of friable insulation materials submitted for identification and quantitation of asbestos components. 1.2 llange The point counting method may be used lor analysis of samples containing from 0 to 100 percent asbestos. The upper detection limit is 100 percent The lower detection limit is loss chan 1 percent 1.3 Interferences Fibrous organic and inorganic constituents of bulk samples may interfere with the identification and quantitation of the asbestos mineral. content Spray-on binder materials may coat fibers and affect color or obacure optical characteristics to the extent of masking fibar identity. Fine particles of other materials may also adhere to fibers to an extant sufficient to cause confusion in identification. Procedures that may bo used lor the removal of interferences are presented in Section 1.7^2. 1.4 Precision and Aocurecy Adequate data for measuring the accuracy and precision of the method for samples with various matrices are not currently available. Data obtained for samples containing a single asbestoe type in a simple matrix ere available in the EPA report Bulk Sample Analyst* for AaOasto* Content' Evaluation of (he Tantatha Maihod.* 1.B Apparatus Ml SampleAnalyst* A low-power binocular microscope, preferably stereoscopic. is used to 0620318 examine the bulk insulation sample as received. Microscope: binocular, 10-45X (approximate) Light Source: incandascant or floorascant forceps. Dissecting Noodles, end Probes Glsssine Psper or Cleon Gloss Piste Compound microscope requirements: A polarized light microscope complete with polarizer, analyzer, port for wave retardation plate. 360 graduated rotating stage, substage condenser, lamp, and lamp iris. Polarised Light Microscope: described above e Objective Lenses: t OX 20X and 40X or nesr equivalent e Dispersion Stoining Objective Lens (optional) e Oculer Lens: 10X minimum e Cyepiece Reticle: cross hair or 25 point Chalk!ey Point Array e Componsotor Plots: 550 milli micron retardation 1.5.2 Semple Proporotion Sample preparation apparatus requirements will depend upon the type of insulation sample under consideration. Various physical and/or chemical means may be employed for an adequate sample assessment e Ventileted Hood or negative pressure glove box e Microscope Slides Coverslips e Morter end Pestle: agate or porcelain (optional) e Wylie Mill (optional) o Seekers S assorted glossworo (optional) Centrifuge (optional) e filtration apparatus (optional) Low temperature asher (optional)' 1.6 Reagents 1.8.1 Sample Proporotion e Distilled Water (optional) e Dilute CHyCOOH: ACS reagent grade (optional) e Dilute HCt ACS reagent grade (optional) e Sodium motaphospheta (NsPOjW (optional) -- 1.8.2 AnalyticalReagents e Refractive Index Liguids: 1.490- 1.570.1.590-1.720 in increment* of 0.002 or 0.004 e Refractive Index Liquids for Dispersion Staining: high- dispersion series. 1.550.1.605. 1.630 (optional) e UICC Asbestos Reference Sample Sat Available from: UICC MRC Pneumoconiosis unit, uanoougn Hospital. Penarth. Glamorgan CF6 1XW. UX and commercial distributors 0 TromoUto-asbostos (source to be determined) # AetinoUta-asbastos Isource to be determined) 1.7 Procedures Note- exposure to airborne asbestos fibers is a health hesard. Sulk samples submitted for analysis are usually friable end may release fibers during handling or matrix reduction stops All sample end slide preparations should bo carried out in e ventilated hood or glove box with continuous airflow (negative pressure!. Handling of samples without those precautions may result in exposure o1 the analyst and contamination of samples by airborne fibers 1.7.1 Sampling Samples for analysis of asbestos content shall be taken in the manner proscribed in Reference 5 and information on design of sampling and analysis programs may be found in Reference 6. If there are any questions about the representative nature of the sample, another sample should be requested before proceeding with the analysis. 1.7.2 Analysis 1.7.2.1 Gross examination Bulk samples of building materials taken tor the identification and quantitation of asbestos are first examined tor homogeneity at low magnification with the aid of a stereomicroscope. The core sample may be examined in its container or carefully removed from the container onto a glaaaine transfer paper or dean glass plate. If possible, note is made of the orientation of top and bottom surfaces. When discrete strata are identified, each is treated as a separate material so that fibers are first identified and quantified in that layer only, and then the results for each layer are combined to yield an estimate of asbestos content for the whole sample. 1.7.2.2 Semple Preparation Bulk materials submitted for asbestos analysis involve a wide variety of matrix material*. Representative subsamples may not be readily obtainable by simple means in heterogeneous materials, and various steps may be required to alleviate the difficulties encountered. In most cases, however, the best preparation is made by using forceps to sample at several places from the bulk material. Forcep samples are immersed in a refractive index liquid on a microscope slide. glass, and observed with the polanr mJ light microscope. Alternatively, attempts may be mad* to homogenize the sample or eliminate interferences before further characterization. The selection of appropriate procedures is dependent upon the samples encountered and personal preference. The following are presented as possible sample preparation steps. A mortar and pestle can sometimes be used in the size reduction of soft or loosely bound materials,though this may cause matting of some samples. Such samples may be reduced in a Wiley mill. Apparatus should be clean and extreme car* exercised to avoid cross-contamination of samples. Periodic checks of the particle sizes should be mad* during the grinding operation so as to preserve any fiber bundles present in an identifiable form. Those procedures are not recommended for samples that contain amphibol* minerals or vermiculits. Grinding of amphiboles may result in the separation of fiber bundles or the production of cleavage fragments that have aspect ratios greater than 3:1 end will be classified as asbestos fibers. Grinding of vermiculit* may also produce fragments with aspect ratios greater than 3:1. Acid treatment may occasionally be required to eliminet* interferences. Calcium carbonate, gypsum, and bassanite (plaster) are frequently present in sprayed or trowelled insulation*. These motorists may be removed by treatment with warm dilute acetic acid. Warm dilute hydrochloric acid may also be used to remove the above materials. If acid treatment is required, wssh the sample at least twice with distilled water, being careful not to lose the particulates during decanting staps. Centrifugation or filtration of the suspension will prevent significant fiber loss. The pore size of the filter should be 0.45 micron or less. Caution: prolonged acid contact with the sample may alter the optical characteristics ot chrysolite libers and should bo avoided. Coatings and binding materials adhering to fiber surfaces may also be removed by treatment with sodium metaphosphate.7 Add 10 mL of 10 g/L sodium metaphosphate solution to a small (0.1 to 0.5 mL) sample of bulk materiel in a 15-mL glass centrifuge tub*. For approximately 15 seconds each, stir the mixture on a vortex mixer, place in an ultrasonic bath and than shake by hand. Repeat the series. 2 *203l9 Collect the dispersedsolids by centrifugation at 1000 rpm for 5 minutes. Wash the samplathree times by suspending in 10 mL distilled water and recentrifuging. After washing, resuspend the pellet in S mL distilled water, place a drop of the suspension on a microscope slide, and dry the slide at 110*C. In samples with a large portion of collulosic or other organic fibers, it may be useful to ash part of the sample and examine the residua. Ashing should be performed in a low temperature asher. Ashing may also be performed in a muffle furnace at temperatures of 500*C or lower. Temperatures cf S50*C or higher will cause dehydroxylation of the asbestos minerals, resulting in changes of the refractive index and other key parameters. If a muffle furnace is to be used, the furnace thermostat should be checked and calibrated to ensure that samples will not be heated at temperatures greater than 500C. Ashing and acid treatment of samples should not be used as standard procedures. In order to monitor possible changes in fiber characteristics, the material should bo viewed microscopically before and after any sample preparation procedure. Use of these procedures on samples to be used for quantitation requires a correction for percent weight loss. 1.7.2.3 Fiber Identification Positive identification of asbestos requires the determination of the following optical propertiea. # Morphology e Color and plaochroism Refractive indices e Birefringence e Extinction characteristics a Sign of elongation Table 1*1 lists the above properties for commercial asbestos fibers. Figure 1*1 presents a flow diagram of the examination procedure. Natural variations in the conditions under which deposits of sebeetHorm minerals are formed wifi produce exceptions to the published values and differences from the UICC standards. The sign of elongation is determined by use of the compensator piste and crossed polars. Refractive indices may be determined by the Becks line test Alternatively, dispersion staining may be used. Inexperienced operators may find that the dispersion staining technique is more easily learned, and should consult Reference 9 for guidance. Central stop dispersion staining colors are presented in Table 1 -2. Available high-dispersion (HO) liquids should be used. 1.7.2.4 Quantitation ofAsbestos Contort Asbestos quantitation is performed by a point-counting procedure. An ocular retide (cross-hair or point array) is used to visually superimpose a point or points on the microscope field of view. Record the number of points positioned directly above each kind of particle or fiber of interest Score only points directly over asbestos fibers or nonasbestos matrix material. Do not score empty points for the closest panicle. If an asbestos fiber and a matrix panicle overlap so that a point is superimposed on their visual intersection, a point is scored for both categories. Point counting provides a determination of the area percent asbestos. Reliable conversion of area percent to percent of dry weight is not currently feasible unless the specific gravities and relative volumes of the motorists are known. For the purpose of this method, "asbestos fibers" are defined as having an aspect rstio greater than 3:1 and being positively identified as one of the minerals in Table 1 -1. A total of 400 points superimposed on either asbestos fibers or nonasbestos matrix material must be' counted over at least eight different preparations of representative subsamples. Take eight forcop samples and mount each separately with the appropriate refractive index liquid. The preparation should not be heavily loaded. The sample should be uniformly dispersed to avoid overlapping particles and allow 29-80 percent empty area within the fields of view. Count SO nonempty points on each preparation, using either e A cross-hair reticle and mechanical stage; or e A reticle with 29 points (Chalkloy Point Array) and counting at least 2 randomly selected fields. For samples with mixtures of isotropic and anisotropic materials present viewing the sample with slightly uncrossed polars or the addition of the compensator plate to the plane polarised light path will allow simultaneous discriminstion of both panicle types. Quantitation should be performed at 100X or at the lowest magnification of the polarised light microscope that can effectively distinguish the sample components. Confirmation of the quantitation result by a second analyst on some percentage of analysed samgiqg should be used as standard quality control procedure. The percent asbestos is calculated as follows: % asbestos * (a/n) 100% where a * number of asbestos counts, n * number of nonempty points counted (400). If * 0. report "No asbestos detected." If 0 < a 3. report "<1 % asbestos." The value reported should be rounded to the nearest percent 1.8 References 1. Paul F. Ken. Optical Mineralogy. 4th ed.. New York, McGraw-Hill. 1977. 2. E. M. Chamot and C. W. Mason. Handbook of Chotntcal Microscopy. Voiumo One. 3rd ad.. Naw York: John Wiley 9 Sons. 1958. 3. F. Chayes. Petrographic Modal Analysis: An Elementary StatisticalAppraisal New York: John Wiley B Sons. 1956. 4. E. P. Brandy. Jr.. K. W. Gold. L E. Myers, and 0. E. Lenuan. Bulk Sample Analysis tor Asbestos Content Evaluation of the Tentative Method. EPA-600/4-82021, U.S. Environmental Protection Agency, in preparation. 5. U.S. Environmental Protection Agency, Asbestos-Containing Materials in SchoolBuildings: A Guidance Document Pans 1 and 2. EPA/OTS No. C00090. March 1979. 6. 0. Lucas. T. Hartwell, and A. V. Rao. Asbestos-Containing Materials in School Buildings: Guidance lor Asbestos Anotytice! Programs. EPA-560/13-80-017A. U.S. Environmental Protection Agency. December 1980. 7. 0. H. Taylor and J. S. Bloom. Hexamotaphosphata pretreatment of insulation samples for identifi cation of fibrous constituents. Microscope. 2B. 1980. 8. W. J. Campbell. R. L Blake. L L Brown. E. E. Cather. and J. J. Sjoberg. Selected SMceta Minerals and Their Aabastdorm Varieties: Mineralogies! Definitions and Idantification-Charactaritstion. U.S. Bureau of Mines Information Circular 8791.1977. 9. Walter C. McCrone, Asbestos Particla Adas. Ann Arbor Ann Arbor Science Publishers. June 1980. 3 042*32* Table /-/. Optic*/properties of ssbastos fibers Mineral Morphology. color' Refractive indices* a "T Sirefringenee Extinction Chrysolite (esbestiform serpentine1 Wevy fibers. Fiber bundles 1.493-1.$60 hove spleyed ends end "kinks". Aspect retie typicelfy >10:1 Colorless*, nonpioochroic. 1.517-1.562* (normally 1.5561 .002- ||to fiber .014 length Amosite (esbestiform gruneritel Sfreight rigid fibers. Aspect retio typicelfy >10:1. Colorless to brown, nonpioo chroic or weekly so. Opaque inclusions mey be present 1.636-1.696 1.655-1.729* .020-.033 ||(o fiber (normally length 1.696-1.7101 Croddotite (esbestiform riebeckite) Streight rigid fibers. 1.654-1.701 1.668-1.717* .014-.016nto fiber Thick fibers end bundles (normally length common, blue to purple-blue in close to 1.7001 color. Pleochroic. Birefringence is genetetiy masked by blue color. Anthophyftito esbestos Streight single fibers, some terger composite 1.596-1.652 1.615-1676* .019- 024 fiber length fibers. Anthrophytiite cleevege fragments mey be present with aspect ratios 10:1.4 Colorless to tight brown. Sign of elongation + (length slow) + (length slow) (length fast) + (length siow) TremotiteectinoUte- esbestos TremoUta-asbestos mey be 1.599-1.66B 1.622-1.688* .023- 020 Oblique extinction. + present es single or composite 10-20* for (length slow) fibers. Tremotite cleavage fragments. fragments mey be present as Composite fibers single crystals with aspect ratios show Wextinction. < 10:1.4 Colorless to pale green. ' From reference 5: colors cited ere seen by observation * Fibers defined es having espect redo >3:1. with plane polarised tight `i to fiber length. * From references 5 end 8. *II to fiber length. * Fibers subjected to hooting mey be brownish. Table 1-2. Mineral Control stop dispersion staining colors * Rl Liquid X II Chrysolite 1.55CT Slue Blue-magenta i i "Amosite" Croddotite* Anthophytiite- asbestos 1.680 1.55CT 1.700 i.ssar0 1.605m to pale blue Yetiowto white Red magenta Yellow to white Blue Golden-yellow Yellow to white Blue-megente Yellow to white Gold to gold-magente Tremotiteasbestos Actinotiteesbestos 1.505** Pete blue Yellow 1.605" Gold-magenta Gold to blue 1.63&** Magenta Golden - yellow 'From reference 9. colors mey very slightly. *Btue ebsorption color. *Oblique extinction view. 4 Folarirad light microscopy quahtatna analysis: For each typo ofmaterialidentifiedby examination ofsample at low magnificanon. Mount specially difparsedsample in 1.550 Rl liquid (If usingdispersion staining, mount in l.550H0.IViawat lOOXwith both plana polarized light and crossed polors. Mora than one fiber type may be present. Fibers present Fibers absent < Fibers ere isotropic Idisappear at all angles of stage rotation with crossed polarsl Possible fibers include: Fiberglass: 1-20 pm uniform diameter. Rl typically < 1.53 Mineral wool: 8-200 pm diameter. bulbous ends and shot Rl typically >1.53 Examine two additional prepared slides at 100X Xk Fibers present 1 Fibers ere anisotropic (exhibit extinction at 90 intervals of stage rotation.) Fibers absent 4 Examination complete. Report no asbestos present \ 1. Determine extinction characteristics. 2. Determine sign of elongation. Positive -------- ) n = 1.550 AH n s >1.850----------- Determine n Check morphology for chrysotila. If fibers are twisted and exhibit internal details, cellulose is indicated. 4----------------n = 1.680 Determine n. Check morphology for "amosite". "1 Negative Mount in 1.700 Rl liquid O Mount in 1.580 Rl liquid Determine n. Check morphology for Alins < 1.680 crocidolite. 4 Mount in 1.605 Rl liquid. Determine n. Check morphology end characteristics tor anthophyllite-esbestos. tramolito-actmolito-osbostoz Figure 1-1. Flow chan tor qualitative analysis of bub samples by polarized light microscopy. 2. X*Ray Powder Diffraction 2.1 Principle and AppHeaMHty The principle of X-ray powder diffraction (XRD) analyst* is wall established.1'* Any solid, crystalline material will diffract an impingent beam of parallel, monochromatic Xrays whenever Bragg's Law. A * 2d sin I. is satisfied for a particular sot of pianos in the crystal lattice, where A * the X-rey wevelength. A; d the interplaner spacing* of the set of reflecting lattice planes, A; and i the angle of incidence between the X-ray beam and the reflecting lattice planes. By appropriate orientation of a sample relative to the incident X-ray beam, a diffraction pattern can be generated that in most cases, will be uniquely characteristic of both the chemical composition and structure of the crystalline phases present Unlike optical methods of analysis, however, XRD cannot determine crystal morphology. Therefore, in asbestos analysis. XRO does not distinguish botweon fibrous and nonfibrous forms of the serpentine and amphibole minerals (Table 2-1L However, whan used in conjunction with optical methods such as polarised light microscopy (PLM), XRD techniques can provide a reliable analytical method for the identification and characterisation of ssbestiform minerals in bulk materials. Per quaikativa analysis by XRO methods, samples are initially scanned over limited diagnostic peak regions for the serpentine (--7.4 A) end amphibole (8.2-3.S A) minerals (Table 2-2). Standard slow scanning methods for bulk sample anelysiqjnay be used for materials shown by RLM to contain significant amounts of asbestos OB10 percent). Detection of minor or trace amounts of asbestos.may require special sample preparation and step scanning analysis. All samples that exhibit diffraction peaks in the diagnostic regions for aabostiform minerals are submitted to a full (6a60* 2#. 1 * 21/min) qualitative XRD seen, and their diffraction patterns are compared with standard reference powder diffraction patterns* to verify initial peak assignments and to identify poasible matrix interferences when subsequent quantitative analysis will be performed. Accurate quantitativa analysis of asbestos in bulk samples by XRD is critically dependent on particle size distribution, crystallite size, preferred orientation and matrix absorption effects, and comparability of standard refarsnea and sample materials. The most intense diffraction peak that has been shown to bo free from interference by prior qualitative XRD analysis is selectad for quantitation of each ssbestiform mineral. A "thinlayer" method of analysis** is recommended in which, subsequent to comminution of the bulk material to --10pm by suitable cryogenic milling techniques, an accurately known amount of the sample is depositsd on a silver membrane filter. The mass of ssbestiform material is determined by measuring the integrated area of the selected diffraction peak using a step scanning mode, correcting for matrix absorption affects, and comparing with suitable calibration standards. Alternative "thick-layer" or bufc methods,7* may be used for samtquantkativa analysis. This XRD method is applicable as a confirmatory method for identification and quantitation of asbestos in bulk material samples that have undergone prior analysis by PLM or other optical methods. 2.2 Range and Sensitivity The range of the method has not been determined. The sensitivity of the method has not been determined. It will be variable and dependent upon many factors, including matrix effects (absorption and interferences), diagnostic reflections selected, end their relative intensities. 2.3 Limitations 2.3.1 intarfarancas Since the fibrous and nonfibrous forms of the serpentine and amphibole minerals (Table 2-1) are indistinguish able by XRD techniques unless special sample preparation techniques and instrumentation ara used,* the presence of nonasbastiform serpentines and amphibole* in a sample will pose severe interference problems in the identification and quantitative analysis of their asbestiform anakr 0620323 The use of XRD for identification and quantitation of ssbestiform minerals in bulk samples may also be limited by the presence of other interfering materials in the sample. For naturally occurring matsrials the commonly associated asbestos-related mineral interferences can usually be anticipated. However, for fabricated materials the nature of the interfer ences may vary greatly (Table 2-3) and present more serious problems in Identification and quantitation.<* Potential interferences are summarized In Table 2-4 and include the following: CNerka has major peaks at 7.19 A and 3.88 A that interfere with both 'the' primary (7.36 A) and secondary (3.66 A) peeks for chrysotile. Resolution of the primary peak to give good quantitative results may be possible when a step-scanning mode of operation is employed. Hakayska has a peak at 3.63 A that interferes with the secondary (3.66 A) peak for chrysotile. e Kaoiinka has a major peak at 7.16 A that may interfere with the primary peak of chrysotile at 7.36 A when present at concentrationr of >10 percent However, the secondary chrysotile peak at 3.66 A may be used for quantitation, e Gypsum haa a major peak at 7.8 A that overlaps the 7.36 A peak of chrysotile when present as a major sample constituent This may be removed by careful washing with distilled water, or by heating to 300*C to convert gypsum to piaster of peris. e Cailuioaa has a broad peak that partially overlaps the secondary (3.66 A) chrysotile peak.* e Overlap of major diagnostic peeks of the amphibole asbestos minerals, amosite. anthophyllite. crocidolite. and tremolite, at approximately 8.3 A and 3.1 A causes mutual interference when these minerals occur in the presence of one another. In some instances adequate resolution may be attained by using step-scanning methods and/or by decreasing the collimator slit width at the X-ray port e Carbonatas may also interfere with quantitative analysis of the amphi- bote asbestos minerals, amosite. anthophyllite. crocidolite, and tremolite. Calcium cartoonata (CaCOa) has a paak at 3.035 A that overlaps major amphibole peaks at approximately 3.1 A when praaant in concentrations of >6 percent Removal of carbonates with a dlluta acid wash is possible; howovar. if prasant chrysotile may ba partially dissolvad by this treatment" A major rale peak at 3.12 A inter- faras with tha primary trsmolita paak at this sama position and with sacondary paaks of crocidolita (3.10 A), amoaita (3.06 A), and anthophyilita (3.06 Aj. In the prasancs of talc tha major diagnostic paak at approximately 8.3 A should ba usad for quantitation of thass asbsstiform minerals. Tha problam of intraspacias and matrix intarfsrancas is furthar aggravatsd by tha variability of tha silicata minsral powder diffraction pattarna themsaivss. which oftan makes definitive identification of tha asbestos minsrals by comparison with standard reference diffraction patterns difficult. This variability results from alterations in tha crystal lattice associated with differences in isomorphous substitution and degree of crystafflmty. This is especially true for tha amphibotes. These minerals exhibit a wide variety of very similar chemical compositions, with tha result being that their diffraction patterns are characterized by having major (110J roflactione of tha monodinic amphibotes and (2101 reflections of the orthorhombic anthophyilita separated by leas than 0 A.11 2.3.2 Matrix 5fleets H a copper X-ray source is used, tha presence of iron at high concentrations in a sample will result in significant X-ray fluorescence, leading to loss of peak intensity with increased background intensity and an overall decrease in sensitivity. This situation may to corrected by use of an X-ray source other than copper, howovar. this ie oftan accompaniod both by loas of imonaity and by decreased resolution of closely spaced reflections. Alternatively, use of a tfiffractod beam monochromator will reduce background fluorescent radiation, enabling weaker diffraction paaks to to datsetsd. X-ray absorption by tha sample matrix will result in overall attenuation of tha diffracted beam and may seriously interfere with quantitative analysis. Absorption affects may to minimized by using sufficiently "thin" samples for analysis.*1*1" However, unless absorption effects are known to be tha sama for both samples and standards, appropriate corrections should ba made by referencing diagnostic peak areas to an intomal standard74 or Altar substrata (Ag) peak.*4 2.3.3 ParriMe Slat Dependence Because tha intensity of diffracted X-radiation is particle-size dependent it is essential for accurate quantitative analysis that both sample and standard reference materials have similar particle size distributions. Tha optimum partids size (La., fiber length) range for quantitative analysis of asbestos by XRO has bean reported to ba 1 to 10 pm.** Comparability of sample and standard rsfarance material panicle sizs distributions should to verified by optical microscopy (or another suitable method) prior to analysis. 2.3.4 Preferred Orientation Effects Preferred orientation of asbsstiform minerals during sample preparation oftan poses a serious problem in quantitative analysis by XRO. A number of techniques have bean developed for reducing preferred orientation effects in "thick layer" samples.7*'* For thin" samples on membrane filters, tha preferred orientation affects seam to ba both reproducible and favorable to enhancement of tha principal diagnostic reflections of asbestos minerals, actually incraaaing tha overall sensitivity of tha method.'*.'4 Howovar, furthar investigation into preferred orientation affects in both thin layer and bufe samples is required. 2.3.5 Lack atSuRaMy Characterised Standard Material* The problam of obtaining and characterizing suitable reference materials for eebsetos analysis is dearly recognized. NiOSH haa recently diroetad a major roeaarch offort toward tha preparation and characterization of analytical reference materials, induding asbestos standards;1*17 however, these are not available in large quantities for routine analysis. In addition, the problem of ensuring the comparability of standard referdtee and sample materials, particularly regardtog crystallite size, particle sizs distribution, and degree of crystallinity, has yot to to adequately addressed. For oxampio. Longer at at'* have observed that in insulating matrices, chryaotila lands to break open into bundles more frequently than amphiboies. This results in a linebroadening affect with a resultant decrease in sensitivity. Unless this effect is the same for both standard and sample materials, tha amount of chrysolite in the sample will to under estimated by XRO analysis. To minimize this problam. it is recommended that standardized matrix reduction procedures to usad for both sample and standard materials. 2^A irtdiiM and Aecuncv Precision of tha method has not boon determined. Accuracy of the method haa not been determined. 2.6 Apparatus 2.5.1 Sample Preparation Sample preparation apparatus requirements will depend upon tha sample type under consideration and tha kind of XRD analysis to to performed. Mortar and Pestle: Agate or porcelain Razor Blades a Sample Milt SPEX. Inc., freezer mill or equivalent Butt Semple Holden a Silver Membrane Pikers: 25-mm diameter, 0.45-pm pore size. Salas Corp. of America. Fknronics Dtv., 1957 Pioneer Road, Huntington Valley, PA 19006 Microscope Slider a Vacuum Filtration Apparatus: Caiman No. 1107 or equivalent. and side-arm vacuum flask a Mierobelonee a Ultrasonic Bath or Probe: Mode) W140, Ultrasonics. Inc., operated at a power density of approximately 0.1 W/mC or equivalent a Volumetric Flasks: 1-t volume a Assorted Pipes a Pipet Bulb a Nonsarrated Forceps a Polyethylene Wash Bottle a Pyres Beckon: 50-mi. volume a Filter Storage Cassettes a Magnetic Stirring Plate and Ban a Porcelain Crucibles a Muffle Furnace or Low Tomprature Asher 2.5.2 Semple Analysis Sample analysis requirements include an X-ray diffraction unit, equipped with: a Constant Potential Generator Voltage end mA Stabilison a Automated Oiffraetometar with Step-Scanning Mode a Copper Target X-Ray Tube: High intensity; fine focus, preferably a X-Ray Pulse Height Selector a X-Ray Detector (with high voltage power supply): Scintillation or proportional counter 7 0*20324  focusing Graphite Crystal . Monochromator: or Nickd fitter (if copper source is used, and iron fluorescanco is not a serious problem) Dot* Output Accessories: Strip Chart Recorder Decode Sceier/Timer Otgrtsl Printer e Semple Spinner (optional) Instrument Celibretion Reference Specimen: a-quara rofaranca crystal (Arkansas quartz standard. *180-147-00. Philips Electronics Instruments. Inc.. 88 McKee Drive. Mahwah. NJ 07430) or equivalent 2.8 Reagents 2.8.1 Stenderd Reference Materials The reference materials listed below ere intended to serve as a guide. Every attempt should be made to acquire pure reference materials that are comparable to sample materials being analyzed. Chrysotile: UICC Canadian, or NIEHS PIsstibesL (UICC reference materials available from: UICC. MRC Pneumoconiosis Unit. Uandough Hospital. Penarth, Glamorgan. CF61XW, UK) CroddoHta: UICC "Amosite": UICC m AnthophyHite-Asbestos: UICC TremoUte Asbestos.' Wards Natural Science Establishment Rochester, NY; Cyprus Research Standard, Cyprus Research. 2435 Military Ave.. Los Angeles. CA 90064 (washed with dilute HC1 to remove small amount of calcite impurity); Indian tramolite. Rajasthan State, India. 9 Actinolite Asbestos: (Source to be determined). 2.8.2 Adhosnro Tape, petroleum jelly, etc. (for ettaching silver membrane filters to sample holders). 2.8.2 Surfactant 1 Percent aerosol OT aqueous solution or equivalent. 2.8.4 Isapropanof ACS Reagent Grads. 2.7 Procedure 2.7.1 Sampling Samples for analysis of asbestos content shall be collected as specified in EPA Guidance Document SC0090, Asbestos-Containing Materials in School Buddings." 2.7.2 Aneffsis AH samples must be analyzed initially for asbestos content by PLM. XRD should be used es an auxiliary method when s second, independent analysis ^requested. Note: Asbestos is a toxic substance. AH handling of dry materials should be performed in an operating fume heed. 2.7.2.1 Sample Preparation The method of sample preparation ` required for XRO analysis will depend on: (1) the condition of the sample received (sample size, homogeneity, panicle size distribution, and overall composition as determined by PLM); and (2) the type of XRD analysis to be performed (qualitative or quantitative; thin layer or bulk). Bulk materials are usually received as inhomogeneous mixtures of complex composition with very wide panicle size distributions. Preparation of a homogeneous, representative sample from asbestos-containing materials is particularly difficult because the fibrous nature of the asbestos minerals inhibits mechanical mixing and stirring, and because milling procedures may cause adverse lattice alterations. A discussion of specific matrix reduction procedures is given below. Complete methods of sample prepara tion are derailed in Sections 27.22 and 2.7.2.X Note: AH samples should bo examinedmicroscopicallybefore and after each morris reduction step to monitor changes in sample particle site distribution, composition, end crystal linity. and to ensure sample representa tiveness and homogeneity for analysis. For accurate, reproducible quantita tive analysis. theDarticle size of both sample and standard materials should be reduced to --10pm (see Section 2.3.3). Ory ball milling at liquid nitrogen temperatures (e.g.. Spex Freezer Mill, or equivalent) for a maximum time of 10 min is recommended to obtain satisfactory particle size distributions while protecting the integrity of the crystal lattice.* Bulk samples of very large particle size may require grinding in two stages for full matrix reduction to <10pm.*'* Final particle size distributions should always be verified by optical microscopy or another suitable method. 272.1.2 Low temperature ashing-- For materials shown by PLM to contain large amounts of gypsum, cellulose, or other organic materials, it may be desirable to ash the ssmples prior to analysis to reduce background radiation or matrix interference. Since chrysotile undergoes dehydroxytation at temperatures between 550*C and 05OC. with subsequent transformation to forstorite.**** ashing temperatures should be kept below 500*C. Use of a low temperature asher la recommended. In all casas. calibration of the oven is essential to ensure that a maximum ashing temperature of 600*C is not exceydod. 2.72.1.1 Milling Mechanical milling of asbestos materials has been shown to decrease fiber crystallinity, with a resultant decrease in diffraction intensity of the specimen; the degree of lattice alteration is related to the duration and type of milling process.t*~l* Therefore, all mMing times should be kept to a minimum. For qualitative analyaia. panicle size is not usually of critical Importance and initial characterization of the material with a minimum of matrix reduction is oftan desirable to document the composition of tha sample as received. Buk samples of very large panicle size 02-3 mm) should be comminuted to --100pm. A mortar and pestle esn sometimes be used in size reduction of soft or loosely bound materials though this may cause matting of some samples. Such samples may be reduced by cutting with a razor Made in a mortar, or by grinding in a suitable mill (e.g.. a microhammer mill or equivalent). When using a mortar for grinding or cutting, the sample should be moistened with ethanol, or some other suitable wetting agent to minimize exposures. 2.7.2.1.3 Add lesching--Because of the interference caused by gypsum and some csrbonatas in the detection of asbestiform minerals by XRD (see Section 2.3.1 L it may be necessary to remove these interferants by a simple add leaching procedure prior to analysis (see Section 1.72.2). 2.7.2.2 Qualitative Analysis 27.221 Initial screening of bulk material--Qualitative analysis should bo performed on a representative, homogeneous portion of the sample with a minimum of sample treatment using the following procedure; 1. Grind and mix me sample with a mortar and pestle (or equivalent method, see Section 2.72.1.1) to a final particle size sufficiently small (--100 pm) to allow adequate packing into the sample holder. 2 Pack sample into a standard buk sample holder. Care should be taken to ensure that a representa tive portion of the milled sample is selected for analysis. Particular csre should be taken to avoid possible size segregation of the sample. (Note: Use of a back packing method1* for buk sample 0620325 preparation may reduce preferred orientation offacta) 3. Mount the sample on the diffrac tometer and scan ovor tho diagnostic peak regions for tho sorpontino (--7.4 A) and amphibole (8.2-8.S A) minerals (saa Tabla 2-21 The X-ray diffraction equip ment should be optimised for intensity. A slow scanning speed of 1 * 24/min is recommended for adequate resolution. Use of a sample spinner is recommended. 4. Submit all samples that exhibit diffraction peaks in the diagnostic regions for asbestiform minerals to a full qualitative XRO scan (S*-60* 2ft 1 24/min) to verify initial peak assignments and to identify potential matrix interferences when subsequent quantitative analysis is to be performed. 5. Compare the sample XRO pattern with standard reference powder diffraction patterns (i.a., JCPOS powder diffraction data' or those of other well-characterized reference materials). Principal lattice spacings of asbestiform minerals are given in Table 2-2; common constituents of bulk insulation and wall materials are listed in Table 2-3. 2.7.2.2.2 Detection of minor or trace constituents--Routine screening of bulk materials by XRO may fail to detect small concentrations 5 percent) of asbestos. The limits of detection will, in general, be improved H matrix absorption effects are mini mised, and if the sample particle sis* is reduced to the optimal 1 to 10pm range, provided that the crystal lattice is not degraded in the milling process. Therefore, in those instances where confirmation of the presence of an asbestiform mineral at very low levels is required, or where a negative result from initial screening of the bufit materiel by XRO (see Section 2.7.2.2.1) is in conflict with previous PIM results, it may be desirable to prepare the sample as described for quantitative analysis (sea Section 2.7.2-3) and step-scan ever appropriate 20 ranges of selected diegnostic peaks (Table 2-2). Accurate transfer of the sample to the silver membrane fitter is not necessary unless subsequent quantitative analysis is to be performed. 2.7.2.3 Quantitative Anafytie The proposed method for quentitation of asbestos in bulk samples is a modification of the NIOSHrocommended thin-layer method for chrysotiie in air.1 A thick-layer or bufc method involving pelletizing the sample may be used far semiquantitafive analyste'* however, this method requires the addition of an internal standard, use of a specially fabricated sample press, and relatively large amounts of standard reference materials. Additional research is required to evaluate the comparability of thin- and thick-layer methods for quantitative asbestos analysis. For quantitative analysis by thin- layer methods, the following procedure is recommended; 1. Mill and size all or a substantial representative portion of the sample as outlined in Section 2.7.2.I.I. 2. Dry at 100*C for 2 hr cool in a desiccator. 3. Weigh accurately to the nearest 0.01 mg. 4. Samples shown by RLM to contain large amounts of celluloeic or other organic materials, gypsum, or carbonates, should be submined to appropriate matrix reduction procedures described in Sections 2.7.2.1.2 and 2.7.2.1.3. After ashing and/or acid treatment, repeat the drying and weighing procedures described above, and determine the percent weight loss. L 5. Quantitatively transfer an accurately weighed amount (50- 100 mg) of the sample to a 1-L volumetric flask with approxi mately 200 ml Isopropanol to which 3 to 4 drops of surfactant have been added. 6. Ultraaonicate for 10 min at a power density of approximately 0.1 W/mC to dtoporse the sample material. 7. Dilute to volume with toopropenol. 8. Place flask on a magnetic stirring Plata. Stir. 9. Place a silver membrane filter on the filtration apparatus, apply a vacuum, and attach the rsaervoir. Release the vacuum and add several mMllitars of isopropanol to the reservoir. Vigorously hand shake the asbestos suspension and immediately withdraw an aliquot from the center of the suspension so that total sample weight WT. on the filter will be approximately 1 mg. Oo not adjust the volume in the pipe! by expelling part of the suspension; if more than the desired aliquot is withdrawn, discard the aliquot and resume the procedure with a eioan pipet. Transfer tho aliquot to the reservoir. Filter rapidly under vacuum. Oo not wash the reservoir walls, leave the filter apparatus under vacuum until dry. Remove the reservoir, release the vacuum, and remove the fitter with forceps. (Note: Water-soluble matrix interfer ences such as gypsum may bo removed at this time by careful washing of the filtrate with distilled water. Extreme care should be taken not to disturb the sample.) 10. Attach the filter to a flat holder with a suitable adhesive and place on the diffractometer. Use of a sample spinner is recommended. 11. For each asbestos mineral to be quantitatodselect a reflection (or reflections) that has been shown to be free from interferences by prior PIM or qualitative XRO analysis and that can be used unambiguously as an index of the amount of material present in the sample (see Table 2-2). 12. Analyse the selected diagnostic reflections by step scanning in incrementa of 0.02* 2* for an appropriate fixed time and integrating the cquntsAA fixed count scan may be used alternatively: however, the method choeen should be used consistently for all samples and standards.) An appropriate scanning interval should be selected for each peak, and background corrections made. For a fixed time scan, measure the background on-each side of the peak for one-half the peak scanning time. The net intensity. I*, is the difference between the peek integrated count and the total background count 13. Determine the net count b*. of the filter 2.36 A silver peak following the procedure in step 12. Remove the filter from the holder, reverse it and reattach it to the holder. Determine the net count for the unattonuatod silver peak, 1^ Scan times may be feat for measurement of silver peaks than for sample peaks; however, they should be constant throughout the analysis. 14. Normalise all raw. net intensities (to correct for instrument instabil ities) by referencing them to an external standard (e.g.. the 3.34 A peek of an a-quartz reference crystal). After each unknown is scanned, determine the net 9 0620326 count. IP. of the reference specimen following the procedure in stop 12. Determine the normalized intensities by dividing the peak intensities by IP: 2.8 Calibration 2..1 Preparation of Calibration Standard* 1. Mill and size standard asbestos materials according to the procedure outlined in Section 2.7.2.I.I. Equivalent standardised matrix reduction and siring techniques should be used ter both standard and sample materials. 2. Dry st 100C for 2 hr cool in a desiccator. 3. Prepare two suspensions of each standard in isopropanol by weighing approximately 10 and SO mg of the dry material to the nearest 0.01 mg. Quantitatively transfer each to a 1-1 volumetric flask with approximately 200 ml. isopropanol to which a few drape of surfactant have been added. 4. Ultrasonicate for 10 min at a power density of approximately 0.1 W/mL. to dtoperse the asbestos material. 6. Dilute to volume with isopropanol. 6. Place the flask on a magnetic stirring plate. Sdr. 7. Prepare, in triplicate, a series of at least five standard filters to cover the desired analytical range, using appropriate aliquots of the 10 and SO mg/l suspen sions. For each standard, mount a silver membrane fitter on the filtration apparatus. Piece a few ml of aoprepanol In the rsoenrair. Vigorously hand shako the asbestos suspeneion and immedi ately withdraw an aliquot from the center of the suspension. Do not adjust the volume in the pipet by expelling part of the suspeneion; if more than the desired afiquot is withdrawn, dtocard the aliquot and resume the procedure with a dean pipet Transfer the aliquotto the reservoir. Keep the tip of the pipet near the surface of the ieoprcpanol. FHtor rapdy under vacuum. Do net wash the sides of the reservoir. Leave the vecuum on for a time sufficient to dry the fitter. Release the vacuum and remove the filter with fnrrsps 2.2.2 Analysis at Calibration Standards 1. Mourn each filter on a flat holder. Perform step scans on selected diagnostic reflections of the standards and reference specimen using the procedure outlined in Section 2.7.2.3, stop 12. and the same conditions as those used for the samples. 2. Determine the normalized intensity for each peak measured. IW as outlined in Section 2.7.2.3. step 14. 2.9 Calculations For each asbestos refersnee material, calculate the exact weight deposited on each standard fitter from the concentrations of the standard suspensions and aliquot volumes. Record the weight w, of each standard. Prepare a calibration curve by regressing Cm on w. Poor reproducibility (15 percent RSO) at any given level indicates problems in the sample preparation technique, and a need for new standards. The data should fit a straight Una equation. Determine the slope, m. of the calibration curve in counts/microgram. The intercept b. of the line with the ISa axis should be approximately zero. A large negative intercept indicates an error in determining the background. This may arise from incorrectly measuring the baseline or from interference by another phase st the angle of back ground measurement A large positive intercept indicates an error in determining the baseline or that an impurity is included in the measured peak. Using the normalized intensity, U* for the attenuated silver peak of a sample, and the corresponding normalized intensity from the unattenuatod silver peak. of the sample fitter, calculate the transmittance. T. for each sample as follows:1**7 Determine the correction factor. ffH. for each sample according to the formula: f(T)-:R|ljT). 1-T* where Sin tm fi angular position of the measured silver peak (from Bragg's Law), and A angular position of the diagnostic fftitTtDI Calculate the weight W.. in micrograms, of the asbestos material analyzed for in each sample, using the appropriate calibration data and absorption corrections: W.a|.gt).b m Calculate the percent composition. Ffc of eoch asbestos mineral analyzed for in the parent material, from the tout sample weight Wr. on the filter: p^w.ii-oiu, 100 Pa percent asbestos mineral in parent materiel; Wa mass of asbestos mineral bn filter, in pg; Wr * total sample weight on filter, in : L percent weight loss of parent material on ashing and/or acid treatment (see Section 2.7.2.31. 2.10 References 1. H. P. Klug and L E. Alexander, Ar ray Diffraction Procedures for PoiycrystaHina andAmorphous Materials. 2nd ed.. New York: John Wiley and Sons; 1979. 2. L V. Azaroff and M. J. Buerger. The Powder Method ofX-ray Crystallography. New York: McGraw-Hill 1958. 3. JCPOS-intornational Cantor for Diffraction Data Powder Diffraction Pile, on Powder Diffraction Stucfies. 1801 Park Lane, Sworthmore. PA. 4. W. J. CempbeN. C. W. Huggins, and A. G. Wylie. Chemical and Physical Characterisation of Amoaka. Chrysolite. Croridolka. and Nonfibrous TramolMo for National Institute of Environmental Health Sciences Ora! ingestion Studies. U.S. Bureau of Minos Report of Investigation RI8462.1980. 5. 8. A. Lange and J. C. Hearts, Determination of microgram quantities of asbestos by X-ray diffraction: Chrysotile in thin dust layers of matrix material. Anal Cham.. ff/(4k520-625,1979. 6. NIOSH Manual ofAnalytical Methods. Volume 5. U.S. Dept HEW. August 1979. pp. 309-1 to 309-9. H.W. Dunn and J.H. Stewart Jr.. Determination of chrysotile In buiding materials by X-ray Diffractometry, Anal Chant. 54 (7k 1122-1125. 1982. to 0620327 8. M. Taylor. Methods lor the samples: Use of X-ray diffraction 19. A. M. Unger. M. S. Wolff. A N. quantiiativo dotormination of to supplement electron Rohl, and L J. Seiikoff, Variation asbestos and quartz in butt microscope analysis. Ire eiootron of properties of chrysolite samples using X-ray diffraction. Microscopy andX-ray asbestos subjected to milling, J. The Analyst *33(1231*1009- Applications to Environmental Toticoi andEnviron. Health. 102a 1978. 9. L Birks. M. Fatemi, J. V. Gilfrich, and Occupation Health Analysis. 4:173-188.1978. P. A. Russell and A. E. Hutchings 20. A M. Unger, A 0. Madder, and and E. T. Johnson. Quantitative (ads.), Ann Arbor Ann Arbor F. 0. Poofey. Electron Analysis ofAirborne Asbestos by Science Publications. 1977. microscopical investigation of X-ray Diffraction. Naval Research 16. A. N. Rohl and A. M. Longer, asbestos fibers. Environ. Health Laboratory Report 7879, Naval Research Laboratory, Identification and quantitation of PerspecL. 9:63-80. 1974. asbestos in talc. Environ. Haalth 21. E. Occells and G. Meddaion, X- Washington, DC 1975. Perspectives. 9:95-109.1974. ray diffraction characteristics of 10. U.S. Environmental Protection 16. J. L Graf. P. K. Asa, end R. G. some types of asbestos in Agency, Asbestos-Containing Drafts. Preparation and relation to different techniques of Materials in Softool Buildings: A Characterisation ofAnalytical comminution. Mad. Lavora. Guidance Documont. Parts 1 and Z EPA/OTS No. C00090, March .Reference Minerals, OHEW 54(10*628-636,1963. (NIOSH) Publication No. 79-139. 22 K. R. Spumy. W. Stdbor. H. 1979. Juno 1979. Opiela. and G. Weiss. On the 11. J. 8. Krause and W. H. Ashton, 17. J. C. Haartz. B. A Lange. R. G. problem of milling and ultrasonic Misidentification of asbestos in Oraftz. and R. F. Scholl. Selection treatment of asbestos and glass talc, pp. 399-353. In: and characterization of fibrous fibers in biological and analytical Proceedings of Workshop on and nonfibrous amphiboles for applications. Am. Ind Hyg Asbostos: Definitions ond analytical methods development Assoc. J.. 41:198-203.1980. Moosuromont Mothods (N8S pp. 295-312. In: Proceedings of 23. L G. Sorry and 8. Mason, Special Publication 506L C. C. Workshop on Asbestos: Mineralogy. San Francisco: W. H. Graven. P. 0. LaFleur. and K. P. Definitions and Measurement Graeman 8 Co., 1959. Heinrich (ads.* Washington. DC: Mothods (NBS Special 24. J. P. Scheiz, The detection of National Measurement Publication 6O6L C. C. Gravatt P. chrysotile asbestos at low levels Laboratory, National Bureau of 0. LaFleur, and K. F. Heinrich in talc by differential thermal Standards. 1977 (issued 1978). (ads.), Washington, DC: National analysis. Thormochimica Acta. 12. H. O. Stanley, The detaction and Measurement Laboratory, 9:197-204,1974. identification of asbestos and National Bureau of Standards, 25. Reference 1. pp. 372-374. asbeettform minerals in talc, pp. 1977 (issued 1978). 26. J. Leroux. Steub-Roinholt Luft, 325-337. In: Proceedings of 18. Personal communication, A. M. 29:26 (English). 1969. Workshop on Asbestos- Unger.Environmental Sciences 27. J. A Leroux. B. C. Davey, and A Definitions ondMoosuromont Laboratory, Mount Sinai School Paillard. Am. Ind. Hyg. Assoc. J.. Mothods (NBS Special of Medicine of the City University 34:409.1973. Publication 506), C. C. Graven. P. of Now York. New York. NY. 0. LaFleur. and K. F. Heinrich (ads.). Washington, DC: National Measurement Laboratory. National Bureau of Standards. Table 2-2. Principal lattica specings of asbestiform minerals.* 1977 (issued 1978). 13. A L. Rickards, Estimation of trace amounts of chrysolite asbestos by X-ray diffraction. Minerals JCPDS Principal d-specings fA/ Powder diffraction file1 and relative intensities number AnoL Cham. 44(11*1872-3. 1972. 14. P. M. Cook. P. L. Smith, and 0. G. Wilson, Amphiboie fiber concentration and determination for a series of community air Chrysotile 7.37.as 736iao 7. 10,m "Amostie' 833,0, 8.22,a. Anthophyllito 3.05,as 3 65m 3.66a, 2.33,, 3.06,0 3.060h 324m 4.57a, 2.45m 3.55m 2756m 3.25m 6.26m 21-543' 25-645 22-1162 1theoreticali 17745 (nonfibrous) 27-1170IUICC) 9-455 T0M0 3-1. Tho esbestos minorols ond thoir nonasbastdorm analogs. ActinoUte 3.06,ae 833m 3.23a, 16-401 (synthetic) 2.72,,, 2.54,,, 3.40m 25-157 Asbostitorm NonesbestHorm Crocidolito 8.3$ 100 3.10u 2.720m 27-1415 (UICC) Serpentine Chrysotile Amphiboie Arttigorito. Usardita TremoUte 8.38 too 2.706,ae 3. 100 3.12m 3.14a, 2.706m 2.705m 13-437* 8.43m 20-1310* (synthetic) 8.44m 23-666 (synthetic mtstura with richtarttal Anthophyllito asbostos Cummingtonito-grunorita asbestos fAntosha") Crocidolito TromoUta asbostos Actinohto asbestos Anthophyllita Cumnungtonka- grunerite Riabackita Tramoiita Actinolita Tlut mtarmauan is imanOad as a fwds. ant, Cotnetan aomOar Attraction data mcluAng mineral tyaa ana mores shauta as retarred to. to ensure eampermiley at samata and reference materials createpassible. Adddienalprecision s.no data on emasns croodotna. tromohtm. and dvrsanta art atadaUa from the US Buraev at Mines, tetanaaus .1. : *fram deferent, 3. *natosav avasuanabta. It 0820328 Table 2-3. Common constituents in insulation and wall materials (from Hat. 10f Tab!a 2-4. Interferences in XRO analysis of asbastdorm minerals A Insulation materials B. Spray finishes or paints Primary diagnostic Asbastdorm peaks {appronmeto ChrysotHa "Amosita" Crocrdolita 'Rock wool 'Slag wool 'Fibor glass Gypsum [CaSOt 2HyO) Varmieulita {micas) Bassanita Carbonate minerals [bakhe. dolomite, vatanta) mmorai Serpentina ChrysotHe Talc Tramolita Anthophyllita Serpentina {including chrysotHa) "Amosite* d-tpocings in Ai Interference 7.4 Nonasbestiform ser pentines {antigorita. Utardita) Chlorite Kaolinita Gypsum Partita Clays {kaolin) Wood pulp Paper fibors {talc. clay, carbonate fillers) Calcium silicates {synthetic) Opaouas (chromite, magnetite Croddolita Mineral wool Rock wool Slag wool Fiber glass Clays {kaolin) Micas 3.7 Nonasbestiform serp entines. iantigorita. liiardita/ Chlorite Halloysita Cellulose inclusion* in serpentine) Hematite (inclusions in 'amosite') Magnesite Oiatomacaous earth Chlorite Gypsum {CaSO*-2HtO) Quarts Organic binders and thickeners Hydromagnesite Wollastonita Amphiboie "Amosite" AnthophyUita Croddolita Tramolita 3.1 Nonasbestiform ampfuboles (cummmgtonita grunerite. anthophydita. riebeckita. tramolita) Mutual interferences Opaques {chromite, magnetite Carbonates inclusions in serpentina) Tale Hematite {inclusions in "amosite") 'Amorphous materials--contribute only to overallscattered' radiation and increased beckground radiation. 8.3 Nonasbestiform amphiboles (camming- tonite. grunerite. anthophydita. reibeckite, tramolitel Mutual interferences United States Environmental Prelection Agency Official Business Penalty ter Privets Use *300 Center ter Environmental fleesarch Information Gnonneti ON 452SS 042032?