Professional Documents
Culture Documents
1. Scope
1.1 This practice covers a method for the sampling of
atmospheres to determine the presence of certain organic
vapors by means of adsorption on activated charcoal using a
charcoal tube and a small portable sampling pump worn by a
worker. A list of some of the organic chemical vapors that can
be sampled by this practice is provided in Annex A1. This list
is presented as an information guide and should not be
considered as absolute or complete.
1.2 This practice does not cover any method of sampling
that requires special impregnation of activated charcoal or
other adsorption media.
1.3 The values stated in SI units are to be regarded as the
standard.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. A specific safety
precaution is given in 9.4.
2. Referenced Documents
2.1 ASTM Standards:2
D 1356 Terminology Relating to Sampling and Analysis of
Atmospheres
D 3687 Practice for Analysis of Organic Compound Vapors
Collected by the Activated Charcoal Tube Adsorption
Method
D 5337 Practice for Flow Rate Calibration of Personal
Sampling Pumps
2.2 NIOSH Standards:
CDC-99-74-45 Documentation of NIOSH Validation Tests3
4. Summary of Practice
4.1 Air samples are collected for organic vapor analysis by
aspirating air at a known rate and for an appropriate time
through sampling tubes containing activated charcoal.
4.2 Instructions are given to enable assembly of charcoal
tubes suitable for sampling purposes.
4.3 Information on the correct use of the charcoal tube
sampling device is presented.
4.4 Practice D 3687 describes a practice for the analysis of
these samples.
3. Terminology
3.1 For definitions of terms used in this method, refer to
Terminology D 1356.
3.2 Activated charcoal refers to properly conditioned charcoal.
This practice is under the jurisdiction of ASTM Committee D22 on Air Quality
and is the direct responsibility of Subcommittee D22.04 on Workplace Air Quality.
Current edition approved Dec. 15, 2008. Published January 2009. Originally
approved in 1978. Last previous edition approved in 2001 as D 3686 - 95(2001)1 .
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standards Document Summary page on
the ASTM website.
3
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D 3686 08
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D 3686 08
7.2.2 Pumps having stable low flow rates (10 to 200
mL/min) are preferable for long period sampling (up to 8 h) or
when the concentration of organic vapors is expected to be
high. Reduced sample volumes will avoid exceeding the
adsorptive capacity of the charcoal tubes. (Suggested flow rates
and sampling times are given in Annex A1 for anticipated
concentration ranges.) (Sample volumes are discussed in 9.5.)
7.2.3 Pumps are available that will provide stable flow rates
between 65 % of the desired flow rate. Pumps should be
calibrated before and after sampling.
7.2.4 All sampling pumps must be carefully calibrated with
the charcoal tube device in the proper sampling position.
7.2.5 A sampling tube holder with flexible tubing is used to
connect the sampling tube to the sampling pump. The sampling
tube holder is used to protect the worker from the sharp end of
the samping tube.
8. Reagents
8.1 Activated CharcoalPrior to being used to make sampling devices the charcoal should be heated in an inert gas at an
appropriate temperature for a sufficient time. Commercially
available coconut-shell charcoal (20/40 mesh) has been found
to have adequate adsorption capacity for many volatile chemicals. Other charcoals, such as JXC charcoal, petroleum-based
charcoal, and proprietary charcoals, can be used for appropriate
applications.
9. Sampling with Activated Charcoal Samplers
9.1 Calibration of the Sampling SystemCalibrate the sampling system, including pump, flow regulator, tubing to be
used, and a representative charcoal tube (or an equivalent
induced resistance) with a primary flow-rate standard or with a
calibrated secondary standard to within 65 % of the desired
flow rate as described in Practice D 5337. Calibrate the
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D 3686 08
Minimum sample volume, m3 5
(1)
(2)
(3)
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D 3686 08
ANNEX
(Mandatory Information)
A1. INFORMATION OF SOME ORGANIC COMPOUND VAPORS THAT CAN BE COLLECTED ON COCONUT-SHELL
CHARCOAL
(100/50 mg tubes)
TABLE A1.1 INFORMATION OF SOME ORGANIC COMPOUND VAPORS THAT CAN BE COLLECTED ON COCONUT-SHELL CHARCOAL
(100/50 mg tubes)
Substance PEL
ppm-mg/m3A
Recommended Sampling
Rate, mL/min to Detect Approximately 15 to 200 % of
PEL in Time GivenB
Recommended
Maximum Tube
Loading, mgC
2h
4h
8h
Acetonitrile, 4070
Allyl alcohol, 25
n-Amyl acetate, 100525
sec-Amyl acetate, 125650
Isoamyl alcohol, 100360
Benzene, 1031.3
Benzyl chloride, 15
2-Butoxy ethanol, 50240
50
200
50
50
50
100
100
25
100
25
25
25
100
200
50
25
50
10
10
10
50
200
25
50
50
50
100
50
50
100
100
200
200
200
50
25
100
50
25
100
25
100
50
50
25
100
25
25
25
25
50
25
25
50
50
100
100
100
25
10
50
25
10
50
10
50
25
25
10
50
10
10
10
10
25
10
10
25
25
50
50
50
10
50
25
10
25
10
G
25
2.7
<0.4
15
15.5
10
89 6 5
86 6 5
91 6 10
<0.4
96
90 6 5
99 6 5
15
15
12.5
10.5
6
5
11.5
2.5
13.4
7.5
15.5
9.3
11
11
6.3
10
25
10
10
G
25
12
15
7.5
5.1
13
25
10
200
100
50
10
50
100
100
100
10
10
50
50
50
50
25
25
100
50
25
50
25
10
25
50
50
50
10
25
25
25
25
25
25
25
10
10
10
10
10
10
G
G
Approximate
Desorption Efficiency %D
95
91 6 5
94 6 5
88 6 5
93 6 5
90 6 5
86 6 10
100+
98 6 5
95
97 6 5
90 6 5
94 6 5
96 6 5
100+
100+
99 6 5
100+
77 6 10
85 6 5
100+
100+
91 6 5
99 6 5
19
99 6 5
12.5
2.6
16
7.1
<5.5
7.5
4.8
<10.7
12
22.5
12.5
11
16.5
10
14
10.5
13
5.6
89 6 5
77 6 10
100+
83 6 5
93 6 5
98 6 5
80 6 10
86 6 5
95 6 5
90 6 5
96 6 5
94 6 5
90 6 5
99 6 5
92 6 5
84 6 10
85 6 5
94 6 5
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Eluent
GC ColumnE
CVTF
CS2 + 5 % 2-propanol
CS2
CS2
CS2 + 5 % 2-propanol
CS2
CS2
methylene chloride +
5 % methanol
CS2
CS2
CS2
CS2 + 1 % 2-propanol
CS2 + 1 % 2-propanol
CS2 + 1 % 2-butanol
CS2
CS2
CS2 + 1 % methanol
toluene
CS2
CS2
CS2
CS2
CS2
CS2
CS2 + 5 % 2-propanol
CS2
CS2 + 5 % 2-propanol
CS2
CS2
CS2
CS2
methylene chloride +5 %
methanol
methylene chloride +5 %
methanol
CS2
CS2 + 1 % 2-butanol
CS2
isopropanol
CS2 + 1 % methanol
ethyl acetate
CS2
xylene
CS2
tetrahydrofuran
CS2
CS2
CS2
CS2 + 5 % 2-propanol
CS2
CS2 + 1 % 2-propanol
CS2
CS2 + 1 % 2-butanol
2
4
4
2
1
2
2
0.072
0.11
0.051
0.071
0.077
0.060
0.096
0.060
4
4
4
2
2
2
2
2
8
1
2
2
1
2
3
2
3
2
6
2
2
1
2
0.069
0.054
0.091
0.065
0.066
0.075
0.074
0.067
0.074
0.059
0.092
0.056
0.061
0.057
0.059
0.066
0.080
0.073
0.101
0.067
0.057
0.052
0.054
0.064
0.062
4
2
2
2
2
3
1
2
6
2
6
1
4
2
4
2
4
2
0.058
0.065
0.041
0.054
0.086
0.053
0.074
0.077
0.079
0.080
0.056
0.062
0.056
0.065
0.065
0.073
0.067
0.064
D 3686 08
TABLE A1.1
Substance PEL
ppm-mg/m3A
Recommended Sampling
Rate, mL/min to Detect Approximately 15 to 200 % of
PEL in Time GivenB
Recommended
Maximum Tube
Loading, mgC
2h
4h
100
100
25
10
50
50
100
50
50
10
G
25
25
50
100
25
10
200
100
10
100
10
10
25
50
10
100
50
50
25
200
10
100
10
10
25
100
100
10
50
100
Continued
Approximate
Desorption Efficiency %D
Eluent
GC ColumnE
CVTF
CS2
CS2 + 1 % methanol
CS2
hexane
CS2 + 1 % methanol
CS2
methylene chloride + 5 %
methanol
methylene chloride + 5 %
methanol
CS2
CS2
CS2 + 5 % 2-propanol
CS2
CS2
CS2
CS2
CS2
CS2
CS2
OS2
CS2
CS2
CS2
CS2 + 1 % 2-propanol
CS2
methylene chloride
CS2
CS2
CS2
2
2
1
3
2
2
2
0.067
0.071
0.055
0.06
0.061
0.053
0.068
0.068
6
1
2
2
1
7
1
1
2
6
6
2
2
4
2
3
7
2
2
0.054
0.052
0.080
0.054
0.073
0.051
0.060
0.055
0.063
0.052
0.052
0.070
0.057
0.056
0.075
0.085
0.059
0.052
0.057
0.069
96 6 5
CS2
0.054
92 6 5
96 6 5
96 6 5
100+
CS2
CS2
CS2
CS2
3
6
6
5
0.055
0.057
0.082
0.07
CS2
CS2
7
2
0.055
0.058
8h
10
10
25
10.5
4.8
7
11.5
7.5
2.0
10
80 6 10
79 6 5
88 6 5
78 6 10
80 6 10
79 6 10
97 6 5
50
25
100 6 5
10
18
98+
95 6 5
99 6 5
91 6 5
95 6 5
88 6 5
93 6 5
96 6 5
88 6 5
95 6 5
96 6 5
90 6 5
97 6 5
93 6 5
87 6 5
90 6 5
70 6 10
96 6 5
87 6 5
100+
100
50
G
25
25
G
50
25
G
5.7
21
9.3
14.8
15
9
50
25
10
25
200
50
25
25
10
100
200
25
10
10
50
25
26
10
50
50
7.5
5
21
20
25
50
10
25
10
50
25
25
29
12.3
0.6
12.5
14.5
9
2
<7.3
13
18
19.5
13
17
96 6 5
85 6 10
Acknowledgements: The information in this table comes from NIOSH Standards Completion Program (6). We gratefully acknowledge NIOSHs contribution to this
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D 3686 08
only and each laboratory must develop its own precision and accuracy data.
CVT 5 =~CVA 1 DE!2 1 ~CVS!2 1 ~CVP!2
where:
= coefficient of variation of a single future assay including error in the desorption efficiency factor
CVA+DE
= coefficient of variation due to sampling errors (not including variation of the pump) along with variability in true desorption efficiency from tube-to-tube, and
CVS
= 0.05 assumed).
= coefficient of variation due to pump (CV
CVP
P
G
Sampling rates of less than 10 mL/min are not recommended. Shorter sampling periods are required.
REFERENCES
(1) Second NIOSH Solid Sorbents Roundtable, Ed. E. V. Ballou, 1976,
NIOSH Publication No. 76193.
(2) White, L. D., Taylor, D. G., Mauer, P. A., and Kupel, R. E., A
Convenient Optimized Method for the Analysis of Selected Solvent
Vapors in the Industrial Atmosphere, American Industrial Hygiene
Association Journal, Vol 31, 1970, pp. 225232.
(3) Otterson, E. J., and Guy, C. U., A Method of Atmospheric Solvent
Vapor Sampling on Activated Charcoal in Connection with Gas
Chromatography, Transactions of the 26th Annual Meeting of the
American Conference of Governmental Industrial Hygienists, Philadelphia, 1964, pp. 3746.
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