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ASBESTOS by TEM: METHOD 7402, Issue 2,dated 15 August 1994 -Page 5 of 7 b. Center a fiber, focus, and center the smallest field-limiting aperture on the fiber. Obtain a diffraction pattern. Photograph each distinctive pattern and keep the photo for comparison to unknowns. NOTE: Not all fibers will present diffraction patterns. The objective lens current may need adjustment to give optimum pattern visibility. There are many more amphiboles which give diffraction patterns similar to the analytes named on p. 7402-1. Some, but not all, of these can be eliminated by chemical separations. Also, some non-amphiboles (e.g., pyroxenes, some talc fibers) may interfere. 17. Acquire energy-dispersive X-ray (EDX) spectra on approximately 5 fibers having diameters between 0.25 and 0.5 prn of each asbestos variety obtained from standard reference materials [71- NOTE: The sample may require tilting to obtain adequate signal. Use same tilt angle for all spectra. a. Prepare TEM grids of all asbestos varieties. b. Use acquisition times(at least 100 sec)sufficient to show a silicon peak at least 75%of the monitor screen height at a vertical scale of >_500 counts per channel. c. Estimate the elemental peak heights visually as follows: (1) Normalize all peaks to silicon (assigned an arbitrary value of 10). (2) Visually interpret all other peaks present and assign values relative to the silicon peak. (3) Determine an elemental profile for the fiber using the elements Na, Mg, Si, Ca, and Fe. Example: 0-4-10-3-<1 [7]. NOTE: In fibers other than asbestos, determination of Al, K, Ti, S, P, and F may also be required for fiber characterization. (4) Determine a typical range of profiles for each asbestos variety and record the profiles for comparison to unknowns. MEASUREMENT: 18. Perform a diffraction pattern inspection on all sample fibers counted under the TEM, using the procedures given in step 17. Assign the diffraction pattern to one of the following structures: a. chrysotile; b. amphibole; c. ambiguous; d. none. NOTE: There are some crystalline substances which exhibit diffraction patterns similar to those of asbestos fibers. Many of these, (brucite, halloysite, etc.) can be eliminated from consideration by chemistry. There are, however, several minerals(e.g., pyroxenes, massive amphiboles, and talc fibers)which are chemically similar to asbestos and can be considered interferences. The presence of these substances may warrant the use of more powerful diffraction pattern analysis before positive identification can be made. If interferences are suspected, morphology can play an important role in making positive identification. 19. Obtain EDX spectra in either the TEM or STEM modes from fibers on field samples using the procedure of step 18. Using the diffraction pattern and EDX spectrum, classify the fiber: a_ For a chrysotile structure, obtain EDX spectra on the first five fibers and one out of ten thereafter. Label the range profiles from 0-5-10-0-0 to 0-10-10-0-0 as"chrysotile" b. For an amphibole structure, obtain EDX spectra on the first 10 fibers and one out of ten thereafter. Label profiles ca. 0-2-10-0-7 as"possible amosite"; profiles ca. 1-1-10-" as "possible crocidolite'; profiles ca. 04-10-3-<1 as "possible tremolite'; and profiles ca. 0-3-10-0-1 as"possible anthophyllite" NOTE: The range of profiles for the amphiboles will vary up to ± 1 unit for each of the elements present according to the relative detector efficiency of the spectrometer. c. For an ambiguous structure,obtain EDX spectra on all fibers. Label profiles similar to the chrysotile profile as"possible chrysotile." Label profiles similar to the various amphiboles as "possible amphiboles." Label all others as"unknown" or"non-asbestos." NIOSH Manual of Analytical Methods(NMAM). Fourth Edition, 8/15194