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EXHIBIT
WCD-371
v, To: J. J. Travers
From: W, C. Forbes
Subject: Evaluation of proposed FDA teat for "Determination of Asbestos
in Talc by Optical Microscopy". In compliance with your letter of September 14th, I have evaluated the
test for "Determination of Asbestos in Talc by Optical Microscopy" which has been proposed by the FDA. In my opinion the'test is completely unsuitable for
the evaluation of asbestos abundance in talc.
j
The FDA procedure states that mineral abundances can be determined by
counting the number of grains of that mineral which occur within a grain mount. This approach is both naive and totally incorrect. The basic flow of the FDA procedure is that it completely ignores the size of the grains being counted. A chrysotile grain 1000 x 100 microns in size is treated exactly the way as a grain measuring 10 x 1 microns. In this case the actual
volume abundance varies by 4 orders of magnitude,
'
The only valid method for estimating mineral abundances using the
polarizing microscope is the point count method.' To briefly describe the
method, a thin section or grain mount is examined at regular intervals, the
interval spacing being selected to achieve a uniform coverage of the entire
sample'. At each sampling site, the mineral variety under the cross-hair is identified and individually tabulated. After covering the entire slide, the number of "hits" for each individual mineral species are summed and recal culated to percentage values. The number of times a given mineral is encount ered is, of course, proportional to the area occupied by that mineral in the entire sample. The areal percentage obtained is meaningful only when compared to the areas of all other mineral components. Thus, the PDA procedure has absolutely no value if isolated grains are counted with no regard to the size
of these grains or the abundance of other mineral species. Objections to the FDA test on technical grounds are summarized below: 1, The FDA test is predicated on the assumptions of: (a) the
"optical uniqueness" of asbestos-, (b) uniformity of the sample material and^
(c) uniform distribution of the sample over the slide. These assumptions
were found to be invalid.
-
a. Chrysotile is quoted as having indices of refraction substan
tially less than 1.574 and therefore should be easily detectable in an oil of that index. It should be noted that chrysotile invariably consists as an
aggregate of fibers variously disoriented so that a great deal of optical
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corapensation exists. The true maximum and minimum indices are probably never
measured. Also talo flakes and fibers oriented with their c_ crystallographic
axes parallel to the. stage will exhibit an index of refraction between 1.536
and 1.590 and on cursory examination may be identified as ohrysotile. Tho
probability for operator error is very large and will likely produce over
estimates of ohrysotile abundances.
',
An additional complication is that iron and aluminum isubstition
in chrysot|le will raise the indices of ohrysotile to levels d o s to those
of talc. However, the chanoe of this happening is slight.
b. The mineral contents of the sample must b e .completely uniform
if bias is to be avoided. Asbestiform minerals usually occur as fibrous
aggregates even after grinding.Xf the fibers of one such clot were oounted, -
and this "count" extrapolated over the entire slide area, a highly exaggerat
ed asbestiform content would result. Optical examination of several talc
samples supplied by Avon showed substantial inhomogenity in mineral abundances.
c. A very important assumption is that the sample can be distribut
' ed evenly over the slide area (l8ram square). This could not be achieved in
several attempts. Fine grained materials such as ground talo tend to aggregate
into large multi-grain particles which resist mechanical attempts to achieve
a uniform particle distribution. Thorough mixing of the talo sample with the
immersion oil also failed to achieve a uniform grain distribution. A talc ---
water slurry was evaporated onto the slide,- however, this did not produce
a marked improvement in sample distribution.
The homogenity of the sample distribution was tested in the
following way. One milligram samples of 815-157 and "Western Treated" talc
were prepared following the FDA procedure. For 815-157 the number of diopside grains observed in a 0.64mm2 field of view were tabulated; the slide
was then shifted 0.5mm and the procedure repeated. Fifteen such counts were
made per soan. Four other such scans were made at 4 intervals. The
. average number of diopside grains observed at each "sample site" and the
standard deviations are listed in Table 1. The large spread in the averages
(0.13-5.8grains/site) is immediately evident, indicating an almost complete
lack of homogeneity. This is reflected in the standard deviations which are
almost as large as the averages themselves. The-results for the "Western
Treated" talo are listed in Table 2 and show a similar lack of homogenity.
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Por this elide, carbonate, quartz and. dropside grains were oounted. There is
a six-fold difference between the maximum and minimum averages with corres
pondingly high standard deviations. The lack of homogeneity precludes any
accurate estimate of mineral abundances based on a ''grain count". It should bo
noted that the scanning and counting procedure is much more rigorous than that
called for by the PDA. Only clearly recognizable grains were counted and the
scan was made at regular intervals. This avoids the bias introduced by
judgement decisions |(chrysotile vs. fibrous talc?) and irregular scanning
methods.
.
2. A grain mount is not a two-dimensional surfaoe. The immersion
oil + grains may have a thickness of up to 50**75 microns. This can result
in mineral segregations based on density differences. As microscopes have a '
5-7 micron depth of focus at 400 magnification, apparent mineral abundances
will ba a function of the deptly of the focal plane within the grain mount.
3. The PDA test calls for a 1 milligram sample. As fine grained
materials may he hydroscopic, a large error in sample weight oan he introduced
at an'early stage of the test.
4 . The test calls for counting of asbestos fibers using an un specified scanning procedure, When I50 fibers are counted, total asbestos is
"determined" by the ratio of area scanned to total slide area. As the area
scanned is an estimate and the scan steps may be irregular, large errors
will be introduced,
5. Amphibole grains in the 5 1 2 micron size bracket will not be clearly apparent in 1.590 immersion oil as the test procedure implies.
the small grain size reduces relief and many small amphibole grains will be
overlooked. 6. The test does not specify the grain size of the sample to be
examined. The obvious extreme is to have a 1 mg. sample which consists
of a single talc flake and thus has 0$ impurities.
7 . This procedure is extremely tedious and there is a Btrong
'
possibility of operator error after 2-3 hours work.
8 . At one sample site (768-206), 26 grains were found in a
*
,65mm area which initially met the PDA criteria as chrysotile, i.e.
index of refraction less than 1 .574, and a length/width ratio greater than 3 .
Subsequent investigation showed all 26 grains to be talc, either as fibrous
talc or the curled edges of talc flakes. There is a very strong possibility
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Ot misidentifiction,. resulting In overestimates of chrysotile abundances. Respectfully submitted,
September 5/ 1973
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Table 1 Average number of dropside grains per sample site (0,64 ffl2) Sample #815-157. Percentage of slide covered equals 15$.
Soan # 1 *
2 3' 4
i
1:
Mean number 3-2 ;
5*8
1*4
0.13
dfopside grains
Standard
3.7 4.9
12 -- --
Deviation
-
,%
,
* Interval between scans is 4mm.
.
Area of individual scan site equals 0.64mm2
Distance between scan sites equals 0.5mm.'
5! 5.5
3.3
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Table 2
Average number of carbonate, quartz, and dropside grains per sample site.
Sample #"Y/estern Treated Talc".
'
Percentage of slide covered equals 30$. .
Scan # '
V)
12
5 6 7 8 9 10
r 4
Mean number couPfcIinS
7-3" 11.8 io.o 8.0 5.4 7.0 5.8 4.0 3.8 2.0
Standard Deviation
2.7 4.7
3.5 3.1 3.0 5.0 2.6 2.3 2.0 1.5
* n + v vai befwJ ***' &ca.n& 1 l m<n .
'
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