ASBESTOS IN AIR
Method No.: |
ID-160 |
Matrix: |
Air |
OSHA Permissible Exposure Limits Time
Weighted Average: Excursion Level (30 minutes): |
0.1 fiber/cc 1.0 fiber/cc |
Collection Procedure: |
A known volume of air is drawn through a
25-mm diameter cassette containing a
mixed-cellulose ester filter. The cassette must be
equipped with an electrically conductive 50-mm extension cowl. The
sampling time and rate are chosen to give a fiber density of between
100 to 1,300 fibers/mm(2) on the filter. |
Recommended Sampling Rate: |
0.5 to 5.0 liters/minute (L/min) |
Recommended Air
Volumes Minimum: Maximum: |
25 L 2,400 L |
Analytical Procedure: |
A portion of the sample filter is cleared
and prepared for asbestos fiber counting by Phase Contrast
Microscopy (PCM) at 400X. |
Detection Limit: |
5.5 fibers/mm(2) or 0.001
fibers/cc (2,400 L Air Volume) |
Precision CV: |
0.12 (at 100
fibers/mm(2)) |
Method Classification: |
Validated Method |
Date (Date Revised): |
July 1988 (July 1997) |
Physical Scientist: |
Daniel T. Crane |
Commercial manufacturers and products mentioned in this method are for
descriptive use only and do not constitute endorsements by
USDOL-OSHA.Similar products from other sources can be
substituted.
Branch of Physical Measurements and Analysis OSHA Technical
Center Salt Lake City, Utah
1. Introduction
This method describes the collection of airborne asbestos fibers using
calibrated sampling pumps with mixed-cellulose ester (MCE)
filters and analysis by phase contrast microscopy (PCM). Some terms used
are unique to this method and are defined below:
Asbestos: A term for naturally occurring fibrous minerals.
Asbestos includes chrysotile, crocidolite, amosite
(cummingtonite-grunerite asbestos), tremolite asbestos, actinolite
asbestos, anthophyllite asbestos, and any of these minerals that have been
chemically treated and/or altered. The precise chemical formulation of
each species will vary with the location from which it was mined. Nominal
compositions are listed:
Chrysotile |
Mg(3)Si(2)O(5)(OH)(4) |
Crocidolite |
Na(2)Fe(3)(2+)Fe(2)(3+)Si(8)O(22)(OH)(2) |
Amosite |
(Mg,Fe)(7)Si(8)O(22)(OH)(2) |
Tremolite-actinolite series |
Ca(2)(Mg,Fe)(5)Si(8)O(22)(OH)(2)
|
Anthophyllite |
(Mg,Fe)(7)Si(8)O(22)(OH)(2) |
Asbestos Fiber: A fiber of asbestos which meets the criteria
specified below for a fiber. Aspect Ratio: The ratio of the
length of a fiber to it's diameter (e.g. 3:1, 5:1 aspect ratios).
Cleavage Fragments: Mineral particles formed by comminution of
minerals, especially those characterized by parallel sides and a moderate
aspect ratio (usually less than 20:1). Detection Limit: The
number of fibers necessary to be 95% certain that the result is greater
than zero. Differential Counting: The term applied to the
practice of excluding certain kinds of fibers from the fiber count because
they do not appear to be asbestos. Fiber: A particle that is 5
µm or longer, with a length-to-width ratio of 3 to 1 or
longer. Field: The area within the graticule circle that is
superimposed on the microscope image. Set: The samples which
are taken, submitted to the laboratory, analyzed, and for which, interim
or final result reports are generated. Tremolite, Anthophyllite,
and Actinolite: The non-asbestos form of these minerals
which meet the definition of a fiber. It includes any of these minerals
that have been chemically treated and/or altered. Walton-Beckett
Graticule: An eyepiece graticule specifically designed for asbestos
fiber counting. It consists of a circle with a projected diameter of 100 ±
2 µm (area of about 0.00785 mm(2)) with a crosshair having
tic-marks at 3-µm intervals in one direction and
5-µm in the orthogonal direction. There are marks around the
periphery of the circle to demonstrate the proper sizes and shapes of
fibers. This design is reproduced in Figure 2. The disk is placed in one
of the microscope eyepieces so that the design is superimposed on the
field of view.
1.1. History
Early surveys to determine asbestos exposures were conducted using
impinger counts of total dust with the counts expressed as million
particles per cubic foot (8.1.). The British Asbestos Research Council
(8.2.) recommended filter membrane counting in 1969. In July 1969, the
Bureau of Occupational Safety and Health published a filter membrane
method for counting asbestos fibers in the United States (8.3.). This
method was refined by NIOSH and published as P & CAM 239 (8.4.).
On May 29, 1971, OSHA specified filter membrane sampling with phase
contrast counting for evaluation of asbestos exposures at work sites
in the United States (8.5.). The use of this technique was again
required by OSHA in 1986 (8.6.). Phase contrast microscopy has
continued to be the method of choice for the measurement of
occupational exposure to asbestos (8.7.).
1.2. Principle
Air is drawn through a MCE filter to capture airborne asbestos
fibers. A wedge shaped portion of the filter is removed, placed on a
glass microscope slide and made transparent. A measured area (field)
is viewed by PCM. All the fibers meeting defined criteria for asbestos
are counted and considered a measure of the airborne asbestos
concentration.
1.3. Advantages and Disadvantages
There are four main advantages of PCM over other methods:
1) The technique is specific for fibers. Phase contrast is a fiber
counting technique which excludes non-fibrous particles
from the analysis.
2) The technique is inexpensive and does not require specialized
knowledge to carry out the analysis for total fiber counts.
3) The analysis is quick and can be performed on-site
for rapid determination of air concentrations of asbestos fibers.
4) The technique has continuity with historical epidemiological
studies so that estimates of expected disease can be inferred from
long-term determinations of asbestos exposures.
The main disadvantage of PCM is that it does not positively
identify asbestos fibers. Other fibers which are not asbestos may be
included in the count unless differential counting is performed. This
requires a great deal of experience to adequately differentiate
asbestos from non-asbestos fibers. Positive identification of asbestos
must be performed by polarized light or electron microscopy
techniques. A further disadvantage of PCM is that the smallest visible
fibers are about 0.2 µm in diameter while the finest asbestos fibers
may be as small as 0.02 µm in diameter. For some exposures,
substantially more fibers may be present than are actually counted.
1.4. Workplace Exposure
Asbestos is used by the construction industry in such products as
shingles, floor tiles, asbestos cement, roofing felts, insulation and
acoustical products. Non-construction uses include
brakes, clutch facings, paper, paints, plastics, and fabrics. One of
the most significant exposures in the workplace is the removal and
encapsulation of asbestos in schools, public buildings, and homes.
Many workers have the potential to be exposed to asbestos during these
operations.
About 95% of the asbestos in commercial use in the United States is
chrysotile. Crocidolite and amosite make up most of the remainder.
Anthophyllite and tremolite or actinolite are likely to be encountered
as contaminants in various industrial products.
1.5. Physical Properties
Asbestos fiber possesses a high tensile strength along its axis, is
chemically inert, non-combustible, and heat resistant. It has a high
electrical resistance and good sound absorbing properties. It can be
weaved into cables, fabrics or other textiles, and also matted into
asbestos papers, felts, or mats.
1.6. Toxic Effects
Information contained in this section is a synopsis of current
knowledge of the physiological effects of asbestos and is not intended as
a basis for OSHA policy.
Some possible physiologic results of respiratory exposure to
asbestos are mesothelioma of the pleura or peritoneum, interstitial
fibrosis, asbestosis, pneumoconiosis, or respiratory cancer (8.8.).
The possible consequences of asbestos exposure are further detailed in
reference 8.8 or in the asbestos standard preamble (8.6.).
2. Range and Detection Limit
2.1. The ideal counting range on the filter is 100 to 1,300
fibers/mm(2). With a Walton-Beckett graticule this range is
equivalent to 0.8 to 10 fibers/field. Using NIOSH counting statistics
(8.9.), a count of 0.8 fibers/field would give an approximate
coefficient of variation (CV) of 0.13.
2.2. The detection limit for this method is 4.0 fibers per 100
fields or 5.5 fibers/mm(2). This was determined using an
equation to estimate the maximum CV possible at a specific
concentration (95% confidence) and a Lower Control Limit of zero. The
CV value was then used to determine a corresponding concentration from
historical CV vs fiber relationships. As an example:
Lower Control Limit (95% Confidence) = AC - 1.645(CV)(AC)
Where: AC = Estimate of the airborne fiber concentration
(fibers/cc) Setting the Lower Control Limit = 0 and solving for
CV: 0 = AC - 1.645(CV)(AC) CV = 0.61
This value was compared with CV vs. count curves. The count at
which CV = 0.61 for Leidel-Busch counting statistics (8.9.) or for an
OSHA Salt Lake Technical Center (OSHA-SLTC) CV curve (see Appendix A
for further information) was 4.4 fibers or 3.9 fibers per 100 fields,
respectively. Although a lower detection limit of 4 fibers per 100
fields is supported by the OSHA-SLTC data, both data sets
support the 4.5 fibers per 100 fields value.
3. Method Performance - Precision and Accuracy
Precision is dependent upon the total number of fibers counted and the
uniformity of the fiber distribution on the filter. A general rule is to
count at least 20 and not more than 100 fields. The count is discontinued
when 100 fibers are counted, provided that 20 fields have already been
counted. Counting more than 100 fibers results in only a small gain in
precision. As the total count drops below 10 fibers, an accelerated loss
of precision is noted (8.9.).
At this time, there is no known method to determine the absolute
accuracy of the asbestos analysis. Results of samples prepared through the
Proficiency Analytical Testing (PAT) Program and analyzed by the
OSHA-SLTC showed no significant bias when compared to PAT
reference values. The PAT samples were analyzed from 1987 to 1989 (N=36)
and the concentration range was from 120 to 1,300 fibers/mm(2).
4. Interferences
Fibrous substances, if present, may interfere with asbestos analysis.
Some common fibers are:
fiber glass |
perlite veins |
anhydrite |
plant fibers |
gypsum |
some synthetic
fibers |
membrane structures |
sponge spicules and
diatoms |
microorganisms |
wollastonite | The use of
electron microscopy or optical tests such as polarized light, and
dispersion staining may be used to differentiate these materials from
asbestos when necessary.
5. Sampling
5.1. Equipment
5.1.1. Sample assembly (The assembly is shown in Figure 3):
Conductive filter holder consisting of a 25-mm
diameter, 3-piece cassette having a 50-mm long
electrically conductive extension cowl. Backup pad,
25-mm, cellulose. Membrane filter,
mixed-cellulose ester (MCE), 25-mm, plain,
white, 0.4- to 1.2-µm pore size.
NOTES: |
a) DO NOT RE-USE
CASSETTES. b) Fully conductive cassettes are required to reduce
fiber loss to the sides of the cassette due to electrostatic
attraction. c) Purchase filters which have been selected by the
manufacturer for asbestos counting or analyze representative filters
for fiber background before use. Discard the filter lot if more than
4 fibers/100 fields are found. d) To decrease the possibility of
contamination, the sampling system (filter-backup pad-cassette) for
asbestos is usually preassembled by the manufacturer. e) Other
cassettes such as the Bell-mouth® may be used within
the limits of validation. |
5.1.2. Gel bands for sealing cassettes.
5.1.3 Sampling pump: Each pump must be a battery operated,
self-contained unit small enough to be placed on the
monitored employee and not interfere with the work being performed.
The pump must be capable of sampling at the collection rate for the
required sampling time.
5.1.4. Flexible tubing, 6-mm bore.
5.1.5. Pump calibration: Stopwatch and bubble tube/burette or
electronic meter.
5.2. Sampling Procedure
5.2.1. Seal the point where the base and cowl of each cassette
meet (see Figure 3) with a gel band or tape.
5.2.2. Charge the pumps completely before beginning.
5.2.3. Connect each pump to a calibration cassette with an
appropriate length of 6-mm bore plastic tubing. Do not
use luer connectors - the type of cassette specified above has
built-in adapters.
5.2.4. Select an appropriate flow rate for the situation being
monitored. The sampling flow rate must be between 0.5 and 5.0 L/min
for personal sampling and is commonly set between 1 and 2 L/min.
Always choose a flow rate that will not produce overloaded filters.
5.2.5. Calibrate each sampling pump before and after sampling
with a calibration cassette in-line (Note: This calibration cassette
should be from the same lot of cassettes used for sampling). Use a
primary standard (e.g. bubble burette) to calibrate each pump. If
possible, calibrate at the sampling site.
NOTE: |
If sampling site
calibration is not possible, environmental influences may affect the
flow rate. The extent is dependent on the type of pump used. Consult
with the pump manufacturer to determine dependence on environmental
influences. If the pump is affected by temperature and pressure
changes, use the formula in Appendix B to calculate the actual flow
rate. |
5.2.6. Connect each pump to the base of each sampling cassette
with flexible tubing. Remove the end cap of each cassette and take
each air sample open face (see Figure 3). Assure that each
sample cassette is held open side down in the employee's breathing
zone during sampling. The distance from the nose/mouth of the
employee to the cassette should be about 10 cm. Secure the cassette
on the collar or lapel of the employee using spring clips or other
similar devices.
5.2.7. A suggested minimum air volume when sampling to determine
TWA compliance is 25 L. For Excursion Limit (30 min sampling
time) evaluations, a minimum air volume of 48 L is recommended.
5.2.8. The most significant problem when sampling for asbestos is
overloading the filter with non-asbestos dust. Suggested maximum air
sample volumes for specific environments are:
Environment |
Air Vol. (L) |
Asbestos removal operations
(visible dust) |
100 |
Asbestos removal operations (little
dust) |
240 |
Office environments |
400 to 2,400 |
CAUTION:
Do not overload the filter with dust. High levels of
non-fibrous dust particles may obscure fibers on the filter
and lower the count or make counting impossible. If more than about 25 to
30% of the field area is obscured with dust, the result may be biased low.
Smaller air volumes may be necessary when there is excessive
non-asbestos dust in the air.
While sampling, observe the filter with a small flashlight. If
there is a visible layer of dust on the filter, stop sampling,
remove and seal the cassette, and replace with a new sampling
assembly. The total dust loading should not exceed 1 mg.
5.2.9. Blank samples are used to determine if any contamination
has occurred during sample handling. Prepare two blanks for the
first 1 to 20 samples. For sets containing greater than 20 samples,
prepare blanks as 10% of the samples. Handle blank samples in the
same manner as air samples with one exception: Do not draw any air
through the blank samples. Open the blank cassette in the place
where the sample cassettes are mounted on the employee. Hold it open
for about 30 seconds. Close and seal the cassette appropriately.
Store blanks for shipment with the sample cassettes.
5.2.10. Immediately after sampling, close and seal each cassette
with the base and plastic plugs. Do not touch or puncture the filter
membrane as this will invalidate the analysis.
5.2.11. Attach a seal (OSHA-21 or equivalent) around each
cassette in such a way as to secure the end cap plug and base plug.
Tape the ends of the seal together since the seal is not long enough
to be wrapped end-to-end. Also wrap tape around the
cassette at each joint to keep the seal secure.
5.3. Sample Shipment
5.3.1. Send the samples to the laboratory with paperwork
requesting asbestos analysis. List any known fibrous interferences
present during sampling on the paperwork. Also, note the workplace
operation(s) sampled.
5.3.2. Secure and handle the samples so that they will not rattle
during shipment nor be exposed to static electricity. Do not ship
samples in expanded polystyrene peanuts, vermiculite, paper shreds,
or excelsior. Tape sample cassettes to sheet bubbles and place in a
container that will cushion the samples without rattling.
5.3.3. To avoid the possibility of sample contamination, always
ship bulk samples in separate mailing containers.
6. Analysis
6.1. Safety Precautions
6.1.1. Acetone is extremely flammable and precautions must be
taken not to ignite it. Avoid using large containers or quantities
of acetone. Transfer the solvent in a ventilated laboratory hood. Do
not use acetone near any open flame. For generation of acetone
vapor, use a spark free heat source.
6.1.2. Any asbestos spills should be cleaned up immediately to
prevent dispersal of fibers. Prudence should be exercised to avoid
contamination of laboratory facilities or exposure of personnel to
asbestos. Asbestos spills should be cleaned up with wet methods
and/or a High Efficiency Particulate-Air (HEPA)
filtered vacuum. CAUTION: Do not use a vacuum without a HEPA filter
- It will disperse fine asbestos fibers in the air.
6.2. Equipment
6.2.1. Phase contrast microscope with binocular or trinocular
head.
6.2.2. Widefield or Huygenian 10X eyepieces (NOTE: The eyepiece
containing the graticule must be a focusing eyepiece. Use a 40X
phase objective with a numerical aperture of 0.65 to 0.75).
6.2.3. Kohler illumination (if possible) with green or blue
filter.
6.2.4. Walton-Beckett Graticule, type
G-22 with 100 ± 2 µm projected diameter. See Appendix C
for further information regarding ordering the graticule.
6.2.5. Mechanical stage. A rotating mechanical stage is
convenient for use with polarized light.
6.2.6. Phase telescope.
6.2.7. Stage micrometer with 0.01-mm subdivisions.
6.2.8. Phase-shift test slide, mark II (Available
from PTR optics Ltd., and also McCrone).
6.2.9. Precleaned glass slides, 25 mm X 75 mm. One end can be
frosted for convenience in writing sample numbers, etc., or
paste-on labels can be used.
6.2.10. Cover glass #1½.
6.2.11. Scalpel (#10, curved blade).
6.2.12. Fine tipped forceps.
6.2.13. Aluminum block for clearing filter (see Appendix D and
Figure 4).
6.2.14. Automatic adjustable pipette, 100- to
500-µL.
6.2.15. Micropipette, 5 µL.
6.3. Reagents
6.3.1. Acetone (HPLC grade).
6.3.2. Triacetin (glycerol triacetate).
6.3.3. Lacquer or nail polish.
6.4. Standard Preparation
A way to prepare standard asbestos samples of known concentration
has not been developed. It is possible to prepare replicate samples of
nearly equal concentration. This has been performed through the PAT
program. These asbestos samples are distributed by the AIHA to
participating laboratories.
Since only about one-fourth of a 25-mm
sample membrane is required for an asbestos count, any PAT sample can
serve as a "standard" for replicate counting.
6.5. Sample Mounting
Note: See Safety Precautions in Section 6.1. before
proceeding.
The objective is to produce samples with a smooth (non-grainy)
background in a medium with a refractive index of approximately 1.46.
The technique below collapses the filter for easier focusing and
produces permanent mounts which are useful for quality control and
interlaboratory comparison.
An aluminum block or similar device is required for sample
preparation. A drawing is shown in Figure 4.
6.5.1. Heat the aluminum block to about 70°C. The hot block
should not be used on any surface that can be damaged by either the
heat or from exposure to acetone.
6.5.2. Ensure that the glass slides and cover glasses are free of
dust and fibers.
6.5.3. Remove the top plug to prevent a vacuum when the cassette
is opened. Clean the outside of the cassette if necessary. Cut the
seal and/or tape on the cassette with a razor blade. Very carefully
separate the base from the extension cowl, leaving the filter and
backup pad in the base.
6.5.4. With a rocking motion cut a triangular wedge from the
filter using the scalpel. This wedge should be
one-sixth to one-fourth of the filter.
Grasp the filter wedge with the forceps on the perimeter of the
filter which was clamped between the cassette pieces. DO NOT TOUCH
the filter with your finger. Place the filter on the glass slide
sample side up. Static electricity will usually keep the filter on
the slide until it is cleared.
6.5.5. Place the tip of the micropipette containing about 200 µL
acetone into the aluminum block. Insert the glass slide into the
receiving slot in the aluminum block. Inject the acetone into the
block with slow, steady pressure on the plunger while holding the
pipette firmly in place. Wait 3 to 5 seconds for the filter to
clear, then remove the pipette and slide from the aluminum block.
6.5.6. Immediately (less than 30 seconds) place 2.5 to 3.5 µL of
triacetin on the filter (NOTE: Waiting longer than 30 seconds will
result in increased index of refraction and decreased contrast
between the fibers and the preparation. This may also lead to
separation of the cover slip from the slide).
6.5.7. Lower a cover slip gently onto the filter at a slight
angle to reduce the possibility of forming air bubbles. If more than
30 seconds have elapsed between acetone exposure and triacetin
application, glue the edges of the cover slip to the slide with
lacquer or nail polish.
6.5.8. If clearing is slow, warm the slide for 15 min on a hot
plate having a surface temperature of about 50°C to hasten clearing.
The top of the hot block can be used if the slide is not heated too
long.
6.5.9. Counting may proceed immediately after clearing and
mounting are completed.
6.6. Sample Analysis
Completely align the microscope according to the manufacturer's
instructions. Then, align the microscope using the following general
alignment routine at the beginning of every counting session and more
often if necessary.
6.6.1. Alignment
1) Clean all optical surfaces. Even a small amount of dirt can
significantly degrade the image.
2) Rough focus the objective on a sample.
3) Close down the field iris so that it is visible in the field
of view. Focus the image of the iris with the condenser focus.
Center the image of the iris in the field of view.
4) Install the phase telescope and focus on the phase rings.
Critically center the rings. Misalignment of the rings results in
astigmatism which will degrade the image.
5) Place the phase-shift test slide on the
microscope stage and focus on the lines. The analyst must see line
set 3 and should see at least parts of 4 and 5 but, not see line set
6 or 7. A microscope/microscopist combination which does not pass
this test may not be used.
6.6.2. Counting Fibers
1) Place the prepared sample slide on the mechanical stage of the
microscope. Position the center of the wedge under the objective
lens and focus upon the sample.
2) Start counting from one end of the wedge and progress along a
radial line to the other end (count in either direction from
perimeter to wedge tip). Select fields randomly, without looking
into the eyepieces, by slightly advancing the slide in one direction
with the mechanical stage control.
3) Continually scan over a range of focal planes (generally the
upper 10 to 15 µm of the filter surface) with the fine focus control
during each field count. Spend at least 5 to 15 seconds per field.
4) Most samples will contain asbestos fibers with fiber diameters
less than 1 µm. Look carefully for faint fiber images. The small
diameter fibers will be very hard to see. However, they are an
important contribution to the total count.
5) Count only fibers equal to or longer than 5 µm. Measure the
length of curved fibers along the curve.
6) Count fibers which have a length to width ratio of 3:1 or
greater.
7) Count all the fibers in at least 20 fields. Continue counting
until either 100 fibers are counted or 100 fields have been viewed;
whichever occurs first. Count all the fibers in the final field.
8) Fibers lying entirely within the boundary of the
Walton-Beckett graticule field shall receive a count of
1. Fibers crossing the boundary once, having one end within the
circle shall receive a count of ½. Do not count any fiber that
crosses the graticule boundary more than once. Reject and do not
count any other fibers even though they may be visible outside the
graticule area. If a fiber touches the circle, it is considered to
cross the line.
9) Count bundles of fibers as one fiber unless individual fibers
can be clearly identified and each individual fiber is clearly not
connected to another counted fiber. See Figure 2 for counting
conventions.
10) Record the number of fibers in each field in a consistent way
such that filter non-uniformity can be assessed.
11) Regularly check phase ring alignment.
12) When an agglomerate (mass of material) covers more than 25%
of the field of view, reject the field and select another. Do not
include it in the number of fields counted.
13) Perform a "blind recount" of 1 in every 10 filter wedges
(slides). Re-label the slides using a person other than
the original counter.
6.7. Fiber Identification
As previously mentioned in Section 1.3., PCM does not provide
positive confirmation of asbestos fibers. Alternate differential
counting techniques should be used if discrimination is desirable.
Differential counting may include primary discrimination based on
morphology, polarized light analysis of fibers, or modification of PCM
data by Scanning Electron or Transmission Electron Microscopy.
A great deal of experience is required to routinely and correctly
perform differential counting. It is discouraged unless it is legally
necessary. Then, only if a fiber is obviously not asbestos should it
be excluded from the count. Further discussion of this technique can
be found in reference 8.10.
If there is a question whether a fiber is asbestos or not, follow
the rule:
"WHEN IN DOUBT, COUNT."
6.8. Analytical Recommendations - Quality Control System
6.8.1. All individuals performing asbestos analysis must have
taken the NIOSH course for sampling and evaluating airborne asbestos
or an equivalent course.
6.8.2. Each laboratory engaged in asbestos counting shall set up
a slide trading arrangement with at least two other laboratories in
order to compare performance and eliminate inbreeding of error. The
slide exchange occurs at least semiannually. The round robin results
shall be posted where all analysts can view individual analyst's
results.
6.8.3. Each laboratory engaged in asbestos counting shall
participate in the Proficiency Analytical Testing Program, the
Asbestos Analyst Registry or equivalent.
6.8.4. Each analyst shall select and count prepared slides from a
"slide bank". These are quality assurance counts. The slide bank
shall be prepared using uniformly distributed samples taken from the
workload. Fiber densities should cover the entire range routinely
analyzed by the laboratory. These slides are counted blind by all
counters to establish an original standard deviation. This
historical distribution is compared with the quality assurance
counts. A counter must have 95% of all quality control samples
counted within three standard deviations of the historical mean.
This count is then integrated into a new historical mean and
standard deviation for the slide.
The analyses done by the counters to establish the slide bank may
be used for an interim quality control program if the data are treated
in a proper statistical fashion.
7. Calculations
7.1. Calculate the estimated airborne asbestos fiber concentration
on the filter sample using the following formula:
where:
AC = Airborne fiber concentration FB = Total number of
fibers greater than 5 µm counted FL = Total number of fields
counted on the filter BFB = Total number of fibers greater than
5 µm counted in the blank BFL = Total number of fields counted
on the blank ECA = Effective collecting area of filter (385
mm(2) nominal for a 25-mm filter.) FR =
Pump flow rate (L/min) MFA = Microscope count field area
(mm(2)). This is 0.00785 mm(2) for a
Walton-Beckett Graticule. T = Sample collection
time (min) 1,000 = Conversion of L to cc
NOTE: |
The collection area of a filter is
seldom equal to 385 mm(2). It is appropriate for
laboratories to routinely monitor the exact diameter using an inside
micrometer. The collection area is calculated according to the
formula: |
Area = p(d/2)(2)
7.2. Short-cut Calculation
Since a given analyst always has the same interpupillary distance,
the number of fields per filter for a particular analyst will remain
constant for a given size filter. The field size for that analyst is
constant (i.e. the analyst is using an assigned microscope and is not
changing the reticle).
For example, if the exposed area of the filter is always 385
mm(2) and the size of the field is always 0.00785
mm(2), the number of fields per filter will always be
49,000. In addition it is necessary to convert liters of air to cc.
These three constants can then be combined such that ECA/(1,000 X MFA)
= 49. The previous equation simplifies to:
7.3. Recount Calculations
As mentioned in step 13 of Section 6.6.2., a "blind recount" of 10%
of the slides is performed. In all cases, differences will be observed
between the first and second counts of the same filter wedge. Most of
these differences will be due to chance alone, that is, due to the
random variability (precision) of the count method. Statistical
recount criteria enables one to decide whether observed differences
can be explained due to chance alone or are probably due to systematic
differences between analysts, microscopes, or other biasing factors.
The following recount criterion is for a pair of counts that
estimate AC in fibers/cc. The criterion is given at the
type-I error level. That is, there is 5% maximum risk
that we will reject a pair of counts for the reason that one might be
biased, when the large observed difference is really due to chance.
(8.11.)
Reject a pair of counts if:
Where: AC(1) = lower estimated airborne
fiber concentration AC(2) = higher estimated
airborne fiber concentration CV(FB) = Pooled
average CV for the two concentration estimates:
CV(1) = Coefficient of variation associated with
the lower count CV(2) = Coefficient of variation
associated with the higher count
Coefficients of variation (CV) may be determined as in Appendix A of
this method (ID-160) or as discussed in NIOSH Method 7400.
If a pair of counts are rejected by this criterion then, recount
the rest of the filters in the submitted set. Apply the test and
reject any other pairs failing the test. Rejection shall include a
memo to the industrial hygienist stating that the sample failed a
statistical test for homogeneity and the true air concentration may be
significantly different than the reported value.
7.4. Reporting Results
Report results to the industrial hygienist as fibers/cc. Use two
significant figures. If multiple analyses are performed on a sample,
an average of the results is to be reported unless any of the results
can be rejected for cause.
8. References
8.1. Dreesen, W.C., et al, U.S. Public Health Service: A
Study of Asbestosis in the Asbestos Textile Industry, (Public
Health Bulletin No. 241), US Treasury Dept., Washington, DC, 1938.
8.2. Asbestos Research Council: The Measurement of Airborne
Asbestos Dust by the Membrane Filter Method (Technical Note),
Asbestos Research Council, Rockdale, Lancashire, Great Britain, 1969.
8.3. Bayer, S.G., Zumwalde, R.D., Brown, T.A., Equipment
and Procedure for Mounting Millipore Filters and Counting Asbestos
Fibers by Phase Contrast Microscopy, Bureau of Occupational
Health, U.S. Dept. of Health, Education and Welfare,
Cincinnati,OH,1969.
8.4. NIOSH Manual of Analytical Methods, 2nd ed., Vol. 1
(DHEW/NIOSH Pub. No. 77-157-A). National Institute for
Occupational Safety and Health, Cincinnati, OH, 1977.
pp.239-1-239-21.
8.5. Asbestos, Code of Federal Regulations 29 CFR 1910.1001.
1971.
8.6. Occupational Exposure to Asbestos, Tremolite,
Anthophyllite, and Actinolite. Final Rule, Federal Register 51:
119 (20 June 1986). pp.22612-22790.
8.7. Asbestos, Tremolite, Anthophyllite, and Actinolite,
Code of Federal Regulations 1910.1001. 1988. pp 711-752.
8.8. Criteria for a Recommended Standard -- Occupational
Exposure to Asbestos (DHEW/NIOSH Pub. No. HSM
72-10267), National Institute for Occupational Safety and
Health NIOSH, Cincinnati,OH, 1972. pp. III-1-III-24.
8.9. Leidel, N.A., Bayer,S.G., Zumwalde, R.D.,Busch,
K.A., USPHS/NIOSH Membrane Filter Method for Evaluating
Airborne Asbestos Fibers (DHEW/NIOSH Pub. No.
79-127). National Institute for Occupational Safety and
Health, Cincinnati, OH, 1979.
8.10. Dixon, W.C., Applications of Optical Microscopy in
Analysis of Asbestos and Quartz, Analytical Techniques in
Occupational Health Chemistry, edited by D.D. Dollberg and A.W.
Verstuyft. Wash. D.C.: American Chemical Society, (ACS Symposium
Series 120) 1980. pp. 13-41.
8.11. Abell, M. T., et al.,The Quality of Fiber Count
Data, Appl. Ind. Hyg. Vol 4 No.11, November 1989, pp.
273-285
Appendix A
The OSHA asbestos regulations require each laboratory to establish a
quality control program. The following is presented as an example of how
the OSHA-SLTC constructed its internal CV curve as part of
meeting this requirement.
Data for the CV curve shown below is from 395 samples collected during
OSHA compliance inspections and analyzed from October 1980 through April
1986.
Each sample was counted by 2 to 5 different counters independently of
one another. The standard deviation and the CV statistic was calculated
for each sample. This data was then plotted on a graph of CV vs.
fibers/mm(2). A least squares regression was performed using
the following equation:
CV = antilog(10)[A(log(10)(x))(2)
+ B(log(10)(x)) + C]
where: |
x = the number of
fibers/mm(2) |
Application of least squares gave:
A = 0.182205 B = -0.973343 C = 0.327499
Using these values, the equation becomes:
CV =
antilog(10)[0.182205(log(10)(x))(2) -
0.973343(log(10)(x)) + 0.327499]
Figure 1: CV curve generated from OSHA Salt Lake
Technical Center data.
Appendix B
Sampling Pump Flow Rate Corrections
This correction is used if a difference greater than 5% in ambient
temperature and/or pressure is noted between calibration and sampling
sites and the pump does not compensate for the differences.
Where:
Q(act) = actual flow rate Q(cal) =
calibrated flow rate (if a rotameter was used, the rotameter value)
P(cal) = uncorrected air pressure at calibration
P(act) = uncorrected air pressure at sampling site
T(act) = temperature at sampling site (K)
T(cal) = temperature at calibration (K)
Appendix C Walton-Beckett Graticule
When ordering the Graticule for asbestos counting, specify the exact
disc diameter needed to fit the ocular of the microscope and the diameter
(mm) of the circular counting area. Instructions for measuring the
dimensions necessary are listed:
- Insert any available graticule into the focusing eyepiece and focus
so that the graticule lines are sharp and clear.
- Align the microscope.
- Place a stage micrometer on the microscope object stage and focus
the microscope on the graduated lines.
- Measure the magnified grid length, PL (µm), using the stage
micrometer.
- Remove the graticule from the microscope and measure its actual grid
length, AL (mm). This can be accomplished by using a mechanical stage
fitted with verniers, or a jeweler's loupe with a direct reading scale.
- Let D = 100 µm. Calculate the circle diameter, d(c) (mm),
for the Walton-Beckett graticule and specify the diameter
when making a purchase:
Example: If PL = 108 µm, AL = 2.93 mm and D = 100 µm,
then,
dc = |
2.93 × 100
108 |
= 2.71
mm |
- Each eyepiece-objective-reticle combination on the
microscope must be calibrated. Should any of the three be changed (by
zoom adjustment, disassembly, replacement, etc.), the combination must
be recalibrated. Calibration may change if interpupillary distance is
changed.
Measure the field diameter, D (acceptable range: 100 ± 2 µm) with a
stage micrometer upon receipt of the graticule from the manufacturer.
Determine the field area (mm(2)).
Field Area = p(D/2)(2)
If D = 100 µm = 0.1 mm, then Field Area = p(0.1 mm/2)(2) = 0.00785
mm(2)
The Graticule is available from: Graticules Ltd., Morley Road,
Tonbridge TN9 IRN, Kent, England (Telephone
011-44-732-359061). Also available from PTR Optics Ltd., 145
Newton Street, Waltham, MA 02154 [telephone (617) 891-6000]
or McCrone Accessories and Components, 2506 S. Michigan Ave., Chicago, IL
60616 [phone (312)-842-7100]. The graticule is custom made
for each microscope.
Appendix D
Aluminum Block
Diagrams of the block are provided in Figure 4.
The cartridge thermostat and heater used for this block have the
following dimensions:
Diameter: |
1/2" |
Cartridge length: |
2 3/8" |
These heating units were obtained from:
Vulcan Electric Company Kezar Falls, Maine
04047 (207)-625-3231
Thermostat part
number: |
N1A1C2 |
Heater part number: |
C516 |
MENTION OF ANY PRODUCT NAME IN THIS DOCUMENT IS FOR
INFORMATION ONLY AND DOES NOT CONSTITUTE ENDORSEMENT BY
DOL-OSHA.
Figure 3: Walton-Beckett Graticule with some
explanatory fibers.
Counts for the fibers in the figure
Structure number |
Count |
Explanation |
|
1 to 6 |
1 |
single fibers all contained
within the circle |
7 |
½ |
fiber crosses circle
once |
8 |
0 |
fiber too short |
9 |
2 |
two crossing fibers |
10 |
0 |
fiber outside graticule |
11 |
0 |
fiber crosses graticule
twice |
12 |
½ |
although split, fiber only
crosses once |
Figure 3. Exploded view of an asbestos sampling
casette.
Figure 4: Engineering Drawings for the aluminum "Hot
Block" as used at the Salt Lake Technical Center.
|