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4.1 Accuracy
Since it is not possible to know the "true" fibre concentration of a
given dust cloud, the absolute accuracy of the described method can-
not be assessed. However, something is known about the bias associ-
ated with sample evaluation.
Microscopists generally undercount dense and overcount sparse
dust samples. When fibres are sampled in atmospheres relatively free
from interfering particles, the sample density range for optimal accu-
racy is between 100 and 1000 fibre~.mm-~; for densities above this,
results can be underestimates while for lower densities, results can be
overestimates. N o corrections should be made, however. Results out-
side the optimal range should simply be reported as having reduced
accuracy.
In environments where there is more than one type of fibre, the
presence of different fibre or particle types may interfere with the
accuracy of results. Chance superimposition of non-fibrous
may cause fibres not to be counted fully, by a proportion that depends
on the mean size and concentration of the interfering particles. In
practice, the effects of chance superimposition on counting results are
small compared with effects due to differences in individual microsco-
pists and will not be important for the counting rules described in this
method.
The counting procedure that is used can result in differences in the
counts produced by different microscopists within and, more particu-
larly, between laboratories. Such differences should be minimized by
proper training in the recommended procedure, internal quality con-
trol and proficiency testing (see section 5).
4. ACCURACY, PRECISION AND LOWER LIMIT OF MEASUREMENT
4.2 Precision
Factors contributing to poor precision are the relatively small portion
of the filter surface that is examined and the variable distribution of
fibres o n the surface (statistical variation), the existence of different
method specifications (systematic variation), and the possibility for
differences in counts made by different microscopists (subjective
variation). Systematic and subjective variation can be reduced by har-
monizing the methods used, training personnel, ensuring that labora-
tories participate in proficiency testing, and performing internal
quality control testing (see section 5). Even when such factors are
addressed, statistical variation is an unavoidable source of error. In this
method, statistical variation depends on the total number of fibres
counted and on the uniformity of fibre distribution on the filter.
Fibre distribution may reasonably be supposed to be approximated
by the Poisson distribution. Theoretically, the process of counting
randomly distributed (Poisson) fibres yields a coefficient of variation
(CV) equal to (.\IN)-' x 100, where N is the number of fibres counted.
The CV is thus 10% for 100 fibres and 32% for 10 fibres. Table 1 gives
theoretical CVs for different numbers of fibres counted, taking into
account only statistical variation.
In practice, however, the actual CV will be greater because of the
additional component of variation associated with subjective differ-
ences within and between microscopists. Table 2 (p. 38) gives typical
CVs within a laboratory where a satisfactory quality control scheme
operates and N fibres are counted.
It can be seen from Table 2 that counting more than 100 fibres gives
only a small improvement in precision. Also, methods lose precision as
90% confidence
limits for the mean of
repeated determinations
N Typical CV (%) Lower Upper
5 49 2.0 11.0
7 43 3.2 14.0
10 37 5.1 18.5
20 30 11.7 33.2
50 25 33 76
80 23 53 118
100 22 68 149
200 21 139 291
The results obtained by the membrane filter method are reliable only
if a comprehensive quality assurance programme is employed. The
provisions of the publication General requirements for the technical
competence of testing Iaboratories (ISO, 1990) should be followed.
National accreditation schemes based on the requirements of this
publication have been established in many countries, and, in some,
additional requirements are specified for fibre measurements (e.g.
NAMAS, 1989).
It is essential that those engaged in sampling or evaluating airborne
fibres not only use a single validated method but also be properly
trained in that method and regularly evaluated. Such training and
evaluation may require attendance at prescribed in-house or national
courses. Authorized personnel may be required to hold, or work
under the supervision of a person who holds, a relevant formal quali-
fication; such personnel should also have appropriate experience.
An essential part of quality assurance is the performance of counting
checks, because of the large differences in results obtained within and
between laboratories using visual counting. Laboratories using the
recommended method should participate in a national or international
proficiency testing scheme in order to minimize interlaboratory varia-
tion. An international proficiency testing scheme is currently envis-
aged as a supplement to this method specification. Microscopists
should also take part in intralaboratory counting checks. Inter-
laboratory exchange and verification of samples can further comple-
ment internal quality control efforts.
Two types of counting check should be performed within a labora-
tory: counting permanent, well characterized reference samples and
making duplicate counts on routine samples. A laboratory should
accordingly maintain a set of reference samples that includes a range of
fibre and background-material loadings from a variety of routine
sample sources. These reference samples should be evaluated periodi-
5. QUALITY ASSURANCE
cally (e.g. four samples per month) by all microscopists, and the counts
compared with reference counts made on the same samples. A refer-
ence count is usually derived from previous counts and may, for
example, be the mean of at least 15 previous visual counts. The results
of each microscopist should be judged against defined criteria for
satisfactory performance (these criteria should be more stringent than
those for proficiency testing schemes). In addition, a defined fraction
of a laboratory's routine samples (e.g. 1 in 10) should be re-counted,
wherever possible by a different analyst, and the difference between
the counts compared with criteria for satisfactory perforniance. If the
results fall outside the acceptable deviation, possible reasons should be
investigated and corrective action taken. Systematic records of quality
control testing should be kept.
References
AIHA (1991) A strategy for occupational exposure assessment. Fairfax, VA, American
Industrial Hygiene Association.
BOHS (1993) Sampling strategies for airborne contaminants in the workplace. Lecds,
H & H Scientific Consultants (British Occupational Hygiene Society Technical
Guide, No. 11).
Burdett GJ (1988) Calibration of low temperature ashers for etching mixed esters of
cellulosefibres for T E M analysis of asbestos. London, Health and Safety Executive
(unpublished document IR/L/DI/88/08, available on request from Health and
Safety Laboratory, Health and Safety Executive, Broad Lane, Sheffield, S. Yorks,
England).
I L O (1990) Safety in the use of mineral and synthetic fibres. Geneva, International
Labour Office (Working document and report of the Meeting of Experts on Safety
in the Use of Mineral and Synthetic Fibres, Geneva, 17-25 April 1989).
REFERENCES
Le Guen JMM, Rooker SJ, Vaughan N P (1980) A new technique for the scanning
electron microscopy of particles collected on membrane filters. Environmental
science and technology, 14:1008-1 01 1.
Mark D (1974) Problems associated with the use of membrane filters for dust sampling
when compositional analysis is required. Annals of occupational hygiene, 17:35-40.