DISCUSSION OF THE Asbestos bulk sample analysis quality assurance programs There is no way to be certain of the identity of all' of thesefibroucs materials unless the probl'emis approached scientifically andvtaith proper training in the characterization of f hers by all of the parameters that can be rneasured with tlie polarized light rnicroscmpe .. Ti-ts a:NAt.YriCAt; Ptzoat.Fms involved! in properly identifying asbestos and asbestos substitutes in, bulk insulation are documented in Reference 1 . Harvey evaluated 35,000 0 analytical results submitted' to Research Triangle Institute (Research Triangle Park,, North Carolina) under the : United States Environmental Pro tection . Agency's (U .S . EPA), Asbestos Bulk Sample Analiysis QualityAssurance Program and!the UIS . Navy Asbestos Identification Proficiency 'I'esting, Program . False positive : results, that is, reporting asbestos when none ! is present, are usually due to confusing shredded pol'yethylene,, nemalite (fibrous brucite), wollastonite, or talc : fibers with chrysotile . False negatives are more often associated with low percentages of asbestos . There are also identification errors, especially between anthophyllite and tremolite, chrysotile and shredded' polyethylene, and between wollastoniite and'actinolite, By WNalter C'. IW1cGrone Df:MeCtrorte is Director, McCrone Research Institute, Chicago, Illinois, U:S.A . The Irrstitute teaches a varietyaf one-week intensive courses in the application of microscopy to industrial research', con tamination control, criminalistics, etc ., nearly 150 times eachl year in different' cities in the United! States and' other countries : Dr. McCrone is Editor and,Publistier of The Microscope, an applied' quarterly jpurnal of microscopy. This article is adapted from one which appeared in The Microscope 37 47-56 (1989). 16 : 4/90 1 http://legacy.library.ucsf.edu/tid/fgt20e00/pdf Discussion The morphological and, especially,,the optical!properties of all l of these substances are distinctive and form the basis for certain identification for anyone proficient with the pol'arized light!microscope and d'ispersion staining (DS) . It is not strictiy neeessary to use DS because it is based on refractive index and this can be determined by the usual Becke line methods . The rapidlidentification of small! particles by DS is faster and easier . There is no way to be certain of'the identity of'all of these fibrous materials unless the problem is approached scientifically and with proper training in thee characterization, of fibers by all I of the parameters that' can be measured! with the polarized light microscope . These incltrde shape, size, color, refractive indices, DS colors (both parallel (11) land perpendicular (1)' to thee fiber, length), pleochroism, birefringence, extinctronn angles, and signs of elongatiom Unfortunately, many analysts working on bulk samples lack a scientific attittidb andVor a scientific background . A few years ago, there were far fewer analysts and most of'them, had'~ taken mineralogy courses including opticali crystallography . With that background~ one would! expect very little difficulty in identifying asbestos when it is present and not finding, it! when it is absent. M'ore recently, with the tremendous number of' samples that must be analyzed, many additional analysts have been ipressed into service . Few of them, are mineralogists, some have little or no chemical background ; and some have no science background . These people can be expected to have considerable difficulty unless they develop the proper scientific approach and have : access to proper training . It should be noted that the samples selected for these quality assurance programs are somewhat skewed toward more : unusual' problem compositions . Few ana+ lysts, even those with little microscopical training, have trouble identifying, chrysotile when it is present in a : reasonable percentage . Most samples in, the rreal' world contain ~chrysotile with amosite as a close second : Prob1em samples are very much in, the minority andl they are the ones that (very properly) have been emphasized by the U .S . EPA program . . Presumably, errors on the easier real-world samples should be less frequent! than ~ the results Harvey reported for the U .S . EPA and Navy programs . This may be some consolation but it is stilll not a proper situation to have analysts able to do all of the easy samples, but who fail lwhenever the occasional unusual sample comes along . In spite of this, I believe the pereentage of false negatives and especially false J REFRACTIVE INDEX LIQUIDS RENT QUALITY RENT QU!ANTUM U QUANTUM ANAIL1lTICS' For Particle and Fiber idontifi'ication to Obtain the Most Reliable ResulUs Crystallographyr • Optfcat Coupling * CalfbRation Custom liquids developed continuously to meet thee needs of research environments . Dispersion staining double variation refractometry, focal masking ; and: polariscopic immersion techniques are among those used all over the worki in conjunction, with ~ Cargille Refractive Index liquids in optical analysis and identification of solids, glasses ; crystals, stress and lstrain effects, and~ flow patterns . RESEARCH' OUA'tIT K IS OUR STAYNDal4D, STATE-O F -TH E-A RT ANALYTICAL INSTRUMENT RENTAL AND SALE GC LC UV FL IR' AA TOC TOk . HNU 1011and .FO)tRO'ROOVA 128 portahleGC's For irrfortrratiamon our latest, : produets, CaIII (800) 992-4199 Quantum Analytics 363-D Vintage Park Drive Foster City, CA 94404 Tel (415) 570-5656 • Fax (415) 57016087 R . P . CARGILLE LABORATORIES,INC . Cedar Grove, N .J . ®7009 U .S .A . •(2©1) 239-6633 Circle Read'erService Card~ No. 2 Circle Reader Service Card NoL 8 QUALITY ASSURANCE continuedd positives in the real world is even greater than the reported UIS . EPA and Navy result's : Those who work the U .S . EPA and' Navy samples are most likely on their best behavior and under pressure to be right . In the real world, where some analysts are trying toaanalyze : 50 to 100 bulk samples per day, ,the results are far worse . The major problemis obviousiy the difficult detection of shredded polyethylene fibers and theirresulting ;id'entiification as chrysotile. There is no excuse for thatierror based! on the optical'. properties (and as polyethylene melts with a match) but the number, of real world sampl'es one can expect to encounter containing polyethylene are few and far between . Most analysts will never see such ~a sample . Shredded'.polyethylene ; though common today ini ceiling sprays, has only been available during the last few years and! iis found in almost none of the buildings that have : fiber-containing insulation. The following, describes the specific procedures for reliable detection of each of the problem fibers : chrysotile, polyethylene, talc,,brucite, tremol'ite„anthophyllite, actinolite, wollastionite, amosite, and crocidolite : Chrysotile Any fibers, whether straight or meandering, with, widely varying,diameters from broad bundles down to . 18 ; e, 4l90' http://legacy.library.ucsf.edu/tid/fgt20e00/pdf the resolving,power limit of the light microscope„with matchimg, wavelength (Xa) colors in 1 .55 Cargillle highdispersion (HD) liquid of magenta (11) and blue (1) or with Ao close to those values, and a difference in ko values of about 100 nm, are almost undbubtedly chrysotile . The only conceivable look-alikes that come close to these properties are animal hairs, spider webs, leather, and shredded!polyethyl'ene . These would all be eliminated by a flame test; ehrysotiile wouldl not change optically in a quick exposure to any temperature below 5()D°'F, whereas polyethylene melts at 1L35°C or less . Polyethylene In shredded'' form, polyethylene shows a, variety of diameters and morphology nou distinctively different from chrysotile . Idowever,, it shows DS colors of yellbw (11) and blue (1) with a difference in ko of about .200'. nm . Its birefringence is nearly three times greater than chrysotile. The unknown thickness of particular fibers makes it difficult to use this parameter however . The difference iniao values shouldl alerrthe carefully trained analyst to the possibility that s/he has polyethylene . . Then, holding the 1 .55' HID preparation over an alcohol I ~ lamp, cigarette lighroer, or match„ or placing it on ai hotplate at about 160QC for about 30, sec will melt C polyethylene fibers . dV Talc Another chrysotile look-alike is talc . Talc fibers are thin ribbons, some of which may resemble chrysotile in shape ; however a study of knowns shows that they are usually straighter . When not straight, the fibers usually bend abruptly between straight segments . Talc fibers have two much higher refractive indices in the plane of the ribbon that are much higher than any indexx of chrysotile and therefore, show a pale yellow color lengthwise in 1 .55' HD liquid, very different from any of the chrysotile 7ia colors . The confirmation of' talce fibers would be that one of the two differentcrosswi'set orientations shows two different h, colors ; chrysotile shows the same color in allicrosswise orientations . Talcc shows a pale yellow in the crosswise direction, if thee ribbon is lying, flat, and blue if the ribbon is on edge . Slh'ght pressure on the coverslip with a gentle up-an&down motion of the needle exerting the pressure, shows, any talc fiber oriented crosswise of the vibration, direction of the polars changing in ko colors fromi yellow too blue : Btucite (nemalite) 1 Nemalite, the fibrous form, of the mineral brucite, has a definite asbestiform shape, although usually straight and stiff (imore like the amphiboles) . It is positively identified as nemalite by its refractive indices . All three indices are higher than chrysotile and the k ;p colors in 1 .550 HD are pale yellow to yellow . Most distinctive is that the palest yellows are crosswise of the length, hence, nemalite fibers have a1 negative sign of elongation . However, it should be noted that, if heated, nemalite then shows a positive sign of elongation although the indices change only slightly . Both Ao colors of yellow to pale yellow in the 1 .55 HD liqµid or only pale blues in the 1 .605 ~ Hm liquid should still identify this chrysotile look-alike no matter which sign of elongation is observed . HeatedInemalite also assumes a yellow absorption color and becomes more brittle with respect to crosswise fracture . Environmental Resource Associates, the largest and most experienced manufacturer of' certified environmental quality control stan+ dards; is changing to better serve the needs of our customers. Within the past twelve months we've more than doubled our product line and added to our services to meet al I your quality control needs . And i we've developed a new look and I a new catalog to bring these products toyou. Please call or write fora new catalog, we'd love to discuss how uve're changing to serve youu better. TremolFte Tremolite fibers are usually straigYst! andl stiff and closer to a blocky, shape than amosite, or especially chrysotile . Its refractive indices are very close to 1 .605 HD:One obtains threedifferentJte colors, yellow nearly parallel to the length and magenta or bliue perpendicular to the length, Again, a given fiber of tnemolite, free to move in the 1 .605 HD, liiquid, can show either bllue or magenta crosswise Xa colors with slight up and down movement of the coverslip with a needle . At this point, however, the fibers eould be tremolite or anthophyllite . A positive way of d'ifferentiating, tremolite from an+ thophyllite is the presence of oblique extinction for tremolite and i parallel eztinction, for anthophyllite . The extinction angles for tremolite vary from 0-20°'depending on the position of rotation about, its length . Ran- http://legacy.library.ucsf.edu/tid/fgt20e00/pdf EIfJ1i/I ROMIM Ef 11Ti4 L RESOURCE ASSOCIIATES Your , Symbol of'4uality Control m ~ N ~ 554& Marshall Street! Arvada, Colorado 80002 1 ~8o0-ERA-0122 2~7 O Circle Reader Service Card No. 18 AEL : 19 . ' QUALITY ASSURANCE continued domly oriented~ nonfibrous crystals will show any anglee between 0'-20°; however, most of them will show at't least a small oblique extinctiion angle and some may, exceed 10q . Fibrous tremolite shows lower extinctioni angles, usually from 0° to about 4° . Anthophyllite Anthophyllite is a tremolite look-alike with the added I problem that' its refractive indices are very similar . One, would expect to obtain very similar Xa, colors, again, with yellow parallel to the length and blue or magenta crosswise . However, anthophyllite is differentiatedd from t'remol'ite by its lack of oblique extinction . All orientations of randomly oriented' anthophyllite fibers willl show 0° extinction angles . I'n practice„ one ex amines a number of different fibers showing blue, magenta, and yellow DS colors in 11 .605 HDD for extinc tion angles, If alll show parallel extinction, the fibers are anthophyllite ; if most show oblique extinction they are tremolite . The determination, of extinction angles requires thatt the polar vibration, directions coincide with the crosslines . This does not happen automatically . It must be set and confirmed by the analyst. If they are not coincident, then an oblique extrnction i angle may be observed, and mistakenly reported . If, however, alll of the crystals observedlshow the same, say, 3°obl'iqueextinction on either side of the crossline, it means that the extinction is parallel and that the polars are misalignedl relative to the crosslines by 3° : Actinolite . Actinol'ite is a higher refractive index member of the tremolite series and, as such; shows yellow to pale yellow DS colors in the 1 . 605 HD liquid. The morphol, ogy of actinolite is similar to tremolite and both show similar extinction behavior (0-20P when nonfibrous and 0-49 when fibrous) . It is notnecessaryto remountactinolite in 1 .630 HD liquid ini which it shows DS colors close to those of tremolite in 1 .605 HD . Allthoughlit is not necessary to remount the sample, it is necessary, in the 11 .605 HD liquid, to see only yellow ko, colbrs in all orientations to differentiate it from tremolite and' to check the sign, of elongation on a dozen or more particles . If a positive sign of'elongation is determined on alll particles, the fibers are actinolite and not wollastonite which also has yellow DS colors in 1' .605 HD . . The actUali refractive indices for actinolite or any of the asbestos mineral'fibers can, be determined from dispersion staining data using the procedure published by the author.2 liquid . Its chief andi very important distinctive feature is the fact that its intermediate (3 refractive index lies (more or less) parallel to the length, whereas actinolite has its highest refractive index (more or less), parallel to the length Actinolite, therefore, always has a positive sign of elongation but wollastonite may be either posi~tive or negative . If a large number of fibers are presentt in 1 the sample, then examination with a red' I-plate and crossed polars will show a positive sign of elongationn for most wollastonite fibers but perhaps one ini five willl show a negative sign of elongation . This is a corroboration for wollastonite . Gentle pressure on the coverslip with a needle usually rotates most wollastonite fibers from a positive to a negative sign of'elongation, . Amosite Amosite has the highest refractive indices of any of the colodess asbestos-types . It is made up of long, straightl, stiff fibers with highly variable diameters and X. colors in 1 .6801HD liquidlof'bllue (1) and gold (11) . Its sign of'elongation is positive and its extinction i is parallell or oblique but because of lamellar twinning, the maxiimum, oblique extinctioniangle is only 4" or 5°, altlioughi some very fine fibers show higher angles. If'heated (as in boiler insul'atlon), amosite changess in refractive index and color . It develops a yellow to red color with pleochroism ;,the strongest absorption is parallel to the length . Rotation of the stage shows it then to be pleochroiic . Accompanying the color change is a corresponding change in refractive index ; the redder the fiber, the higher the refractive index . We have observedlindices in excess of'1 .90 flj) andI 1 .80 (1) . Crocidolite . Crocidolite (blue asbestos), is easily identified' by its shape, highly variable diameters, blue colbr, and pleochroism with deep blue (11)'and!gcay blue (1l) . Its refractive indices are higher than those of amosite and the ko colors for all orientations are yellow in 1 .680 HD liquid . The palest yellow is perpendill to the length indicating a negative sign of elongation ;,this is confumed' with the red 1-plate . Concluslon, Anyone confidentim their understanding of these tests and able to carry out and! interpret the results of such tests, should have no problem in id'entifying,anyof the above materials . Anyone unable to do so has either not had proper training or has not taken full advantage of that training . 1+W ~~ollastoroite References Wollastonite is another asbestos llaok-alike and by shape alone, cannot be differentiated from, any of the asbestos minerals (except~ chrysotile) . Wollastonite has refractive indices very similar to actinolite and, therefore, shows yellow to pale yellbw ini the 11 .605 HD' 20, : 1 . HARVEY ., B ., ~"ClassitiCationlandidentification eliortendenCiesinbulk insulation proficiency testing matCrialS,"M'icroscope373891 398 (1989) ;,A'm . Env . Lab ;,2(1) 8-14(I990) . 2. t.accRONE ; w ., "Detennining,refractive indices from dispersion staining data ; " Microscope 37 47-56 (1989) . 4190 http://legacy.library.ucsf.edu/tid/fgt20e00/pdf ~ 0 4:1 l ~
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