ASTM D5075-96e1
(Test Method)Standard Test Method for Nicotine and 3-Ethenylpyridine in Indoor Air
Standard Test Method for Nicotine and 3-Ethenylpyridine in Indoor Air
SCOPE
1.1 This test method covers the sampling/analysis of nicotine and 3-ethenylpyridine (3-EP) in indoor air. This test method is based upon the collection of nicotine and 3-EP by adsorption on a sorbent resin, extraction of nicotine and 3-EP from the sorbent resin, and determination by gas chromatography (GC) with nitrogen selective detection. (1)
1.2 The active samplers consist of an XAD-4 sorbent tube attached to a sampling pump. This test method is applicable to personal or area sampling.
1.3 This test method is limited in sample duration by the capacity of the XAD-4 tube for nicotine (about 300 g). This test method has been evaluated up to 24-h sample duration; however, samples are typically acquired for at least 1 h (sometimes only 1 h). (2)
1.4 For this test method, limits of detection (LOD) and quantitation (LOQ) for nicotine at a sampling rate of 1.5 L/min are, respectively, 0.11 g/m3 and 0.37 g/m3 for 1-h sample duration and 0.01 g/m3 and 0.05 g/m3 for 8-h sample duration. The LOD and LOQ for 3-EP at a sampling rate of 1.5 L/min are, respectively, 0.06 g/m3 and 0.19 g/m3 for 1-h sample duration and 0.01 g/m3 and 0.02 g/m 3 for 8-h sample duration (2). Both LOD and LOQ can be reduced by increasing the sensitivity of the thermionic specific detector.
1.5 The values stated in SI units are to be regarded as standard.
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. Specific precautionary information is given in 13.6 .
General Information
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e1
Designation: D 5075 – 96 An American National Standard
Standard Test Method for
Nicotine and 3-Ethenylpyridine in Indoor Air
This standard is issued under the fixed designation D 5075; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
e NOTE—The Keywords section was added editorially in November 1996.
1. Scope D 1356 Terminology Relating to Sampling and Analysis of
Atmospheres
1.1 This test method covers the sampling/analysis of nico-
D 1357 Practice for Planning the Sampling of the Ambient
tine and 3-ethenylpyridine (3-EP) in indoor air. This test
Atmosphere
method is based upon the collection of nicotine and 3-EP by
D 3631 Test Methods for Measuring Surface Atmospheric
adsorption on a sorbent resin, extraction of nicotine and 3-EP
Pressure
from the sorbent resin, and determination by gas chromatog-
D 5337 Practice for Flow Rate for Calibration of Personal
raphy (GC) with nitrogen selective detection. (1)
Sampling Pumps
1.2 The active samplers consist of an XAD-4 sorbent tube
E 260 Practice for Packed Column Gas Chromatography
attached to a sampling pump. This test method is applicable to
E 355 Practice for Gas Chromatography Terms and Rela-
personal or area sampling.
tionships
1.3 This test method is limited in sample duration by the
capacity of the XAD-4 tube for nicotine (about 300 μg). This
3. Terminology
test method has been evaluated up to 24-h sample duration;
3.1 Definitions—For definitions of terms used in this test
however, samples are typically acquired for at least 1h
method, refer to Terminology D 1356 and Practice E 355.
(sometimes only 1 h). (2)
3.2 Definitions of Terms Specific to This Standard:
1.4 For this test method, limits of detection (LOD) and
3.2.1 environmental tobacco smoke (ETS)—an aged, dilute
quantitation (LOQ) for nicotine at a sampling rate of 1.5 L/min
3 3
composite of exhaled tobacco smoke and smoke from tobacco
are, respectively, 0.11 μg/m and 0.37 μg/m for 1-h sample
3 3
products.
duration and 0.01 μg/m and 0.05 μg/m for 8-h sample
3.2.2 nitrogen-phosphorus detector (NPD)—a highly sensi-
duration. The LOD and LOQ for 3-EP at a sampling rate of 1.5
3 3
tive device selective for detection of nitrogen- and phosphorus-
L/min are, respectively, 0.06 μg/m and 0.19 μg/m for 1-h
3 3
containing organic compounds.
sample duration and 0.01 μg/m and 0.02 μg/m for 8-h sample
3.2.3 XAD-4 resin—macroreticular polystyrene-
duration (2). Both LOD and LOQ can be reduced by increasing
divinylbenzene copolymer beads.
the sensitivity of the thermionicspecific detector.
1.5 The values stated in SI units are to be regarded as
4. Summary of Test Method
standard.
4.1 A known volume of air is drawn through a sorbent
1.6 This standard does not purport to address all of the
sampling tube containing XAD-4 resin to absorb the nicotine
safety concerns, if any, associated with its use. It is the
and 3-EP present.
responsibility of the user of this standard to establish appro-
4.2 The XAD-4 sorbent tube contents are transferred to a
priate safety and health practices and determine the applica-
2-mL autosampler vial, and the nicotine and 3-EP are desorbed
bility of regulatory limitations prior to use. Specific precau-
with ethyl acetate containing 0.01 % triethylamine and a
tionary information is given in 13.6.
known quantity of quinoline, the internal standard.
2. Referenced Documents 4.3 An aliquot of the desorbed sample is injected into a gas
chromatograph equipped with a thermionic-specific (nitrogen-
2.1 ASTM Standards:
phosphorus) detector.
4.4 The areas of the resulting nicotine and 3-EP peaks are
each divided by the area of the internal standard peak and
compared with area ratios obtained from the injection of
This test method is under the jurisdiction of ASTM Committee D-22 on
Sampling and Analysis of Atmospheres and is the direct responsibility of Subcom-
standards.
mittee D22.05 on Indoor Air.
Current edition approved May 10, 1996. Published July 1996. Originally
published as D 5075 – 90. Last previous edition D 5075 – 90a.
The boldface numbers in parentheses refer to a list of references at the end of
Annual Book of ASTM Standards, Vol 11.03.
the text.
Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 5075
values usually at the lower end of this range (9). Because such
low concentrations of nicotine are often encountered, sophis-
ticated analytical procedures and equipment are required for
quantifying nicotine in indoor air. Other methods for the
determination of nicotine in indoor air have also been reported
(6,10,11,12). 3-Ethenylpyridine concentrations typically are
about one third the concentrations of nicotine in real-world
environments (13).
6. Interferences
6.1 Use of packed GC columns may result in readings lower
than expected because nicotine can adsorb onto undeactivated
FIG. 1 1 XAD-4 Sorbent Tube
glass, metal, and solid support particles. Fused silica capillary
5. Significance and Use
columns and the modified extraction solvent prescribed here
5.1 In order to estimate ETS concentrations, there needs to can circumvent this problem.
be a marker or tracer for ETS that is unique or highly specific 6.2 Quinoline (internal standard) is present in ETS at a
to tobacco smoke, in sufficient concentrations in air to be concentration approximately 1 % of that for nicotine and is
measured easily at realistic smoking rates, and in constant collected by the XAD-4 resin. If >10 μg nicotine is collected on
proportion to the other components of ETS for a variety of the resin, there will be sufficient quinoline present to cause a
tobacco blends and environmental conditions. Nicotine and detectable bias in results (approximately 1 %). (For example,
3-Ethenylpyridine have been used as tracers of the vapor phase this quantity of nicotine would be collected if a nicotine
of ETS. Nicotine is the major alkaloid of tobacco and a major concentration of 167 μg/m was sampled at 1 L/min for 1 h.) In
constituent of ETS. The determination of nicotine concentra- these cases, one of the following alternative procedures should
tion has often been used to estimate the concentration of ETS; be followed:
however, due to its unpredictable decay kinetics, nicotine may 6.2.1 Quantitatively dilute the sample with the same modi-
not be an ideal tracer. Because nicotine readily adsorbs to fied solvent containing internal standard (described in 11.2)
building materials and room furnishings and is depleted from used to extract the original sample; that is, decrease the amount
ETS at a rate faster than most other components, some have of quinoline (and also nicotine) present in the sample while
suggested that nicotine concentrations underestimate ETS keeping the quinoline concentration in the solvent constant. To
prevent significant interference, the nicotine concentration in
concentrations. Although this is true in many environments
during the generation of smoke, the converse is true in the most concentrated sample should be less than or equal to
environments with a recent past history of smoking. The the quinoline concentration in the solvent.
adsorbed nicotine slowly desorbs over time, resulting in an 6.2.2 Use an alternate internal standard [N8-
overestimation of ETS concentrations. Thus, measured concen- ethylnornicotine is recommended (14)].
trations of nicotine precisely assess only airborne nicotine and
7. Apparatus
indicate only that smoking has taken place; they do not
7.1 Sample Collection:
necessarily indicate the presence, and certainly not the concen-
7.1.1 XAD-4 Sorbent Tube, see Fig. 1.
trations, of other ETS constituents. 3-Ethenylpyridine, on the
7.1.2 XAD-4 Sorbent Tube —Glass tube with both ends
other hand, has been shown to track exactly the vapor phase of
flame-sealed, approximately 7 cm long with 6-mm outside
ETS as measured by CO and FID response (3). It is for these
diameter and 4-mm inside diameter, containing two sections of
reasons that 3-ethenylpyridine may be a better tracer of ETS
20/40 mesh XAD-4 resin. The front section contains 80 mg of
(1,4,5). The ETS at high concentrations is known to be
resin, the backup section contains 40 mg of resin. A glass wool
annoying and irritating to individuals, and concerns over
plug is located at each end of the tube and between the front
potential health effects have also been expressed. There is a
and backup sections. The front plug is held in place with a
definite need to have reliable methods for the estimation of
metal lockspring (see Fig. 1).
ETS levels in order to evaluate its effect. The NIOSH has
7.1.3 Tube Holder, with clip attachment for attaching tube
previously set a threshold limit value (TLV) for nicotine in the
to clothing or objects.
workplace of 0.5 mg/m .
7.1.4 Tube Breaker, to break sealed ends from sample
5.2 Studies show that more than 90 % of nicotine in indoor
tubes.
air is found in the vapor phase (6,7). The described test method
7.1.5 NIOSH-approved Plastic Caps, for capping tubes after
collects vapor-phase nicotine quantitatively. Early studies on
sampling.
freshly generated ETS indicated that some but not all of the
particulate phase was trapped on the XAD-4 resin (7). A more
recent investigation of the trapping of particulate materials by 5
XAD-4 sorbent tubes for nicotine and 3-EP, Cat. No. 226-93, available from
sorbent beds suggests that the trapping of the particles from
SKC, Inc., 863 Valley View Rd., Eighty Four, PA 15330-9614, or equivalent, have
been found suitable for this purpose.
indoor air may be nearly quantitative (8). 3-Ethenylpyridine is
Tube holders available from SKC, Inc., Cat. No. 222-3-1, or equivalent, have
found exclusively in the vapor phase.
been found suitable for this purpose.
5.3 Nicotine concentrations typically range from ND (not
Tube breaker, Cat. No. 2-0596, available from Supelco, Inc., Supelco Park,
detected) to 70 μg/m in various indoor environments with Bellefonte, PA 16823-0048, or equivalent, has been found suitable for this purpose.
D 5075
7.1.6 Barometer and Thermometer, for taking pressure and 8.6 4-Ethenylpyridine (4-EP), 95 %, commercially avail-
temperature readings at the sampling site (optional). able isomer of 3-ethenylpyridine.
7.1.7 Bubble Flowmeter, for sample pump calibration. 8.7 Helium Cylinders, for carrier or detector makeup gas, or
7.1.8 Personal Sampling Pump, portable constant-flow both, 99.995 % grade.
sampling pump calibrated for the flow rate desired (up to 1.5 8.8 Hydrogen Cylinders, for detector gas, 99.995 % grade.
L/min). 8.9 Air, for detector gas (<0.1 ppm hydrocarbon).
7.2 Analytical System:
9. Sampling
7.2.1 Gas Chromatograph, with a nitrogen-phosphorus
10 11
(thermionic) detector and autosampler.
9.1 General—For planning sampling programs, refer to
7.2.2 GC Column —A 30-m by 0.32-mm inside diameter
Practice D 1357.
fused silica capillary column, coated with a 1.0-μm film of 5 %
9.2 Procedure:
phenyl methylpolysiloxane (DB-5).
9.2.1 Prepare XAD-4 sampling tubes immediately before
7.2.3 Chromatography Data Acquisition System, for mea-
sampling. Break both ends of the sealed sorbent tube using a
suring peak areas electronically.
tube breaker tool. The opening should measure at least 2 mm
7.2.4 Sample Containers, borosilicate glass autosampler
in diameter.
vials, 2-mL capacity, with PTFE-lined septum closures.
9.2.2 Connect the sorbent tube to the personal sampling
7.2.5 Dispensing Pipets, 1.25-mL.
pump with tubing. Position the sorbent tube so that the air
7.2.6 Triangular File, for scoring and breaking open sample
being sampled will pass first through the front section of resin
tubes.
and then through the backup section. The inlet end of the tube
7.2.7 Forceps, for assisting transfer of sorbent tube contents
is exposed directly to the atmosphere, and the outlet end is
from tube to autosampler vial.
inserted in the tubing; or the tube itself is put into a safety
7.2.8 Glass Wool Removal Tool, for assisting transfer of
casing in the personal sampling setup and attached accordingly.
sorbent tube contents from tube to autosampler vial.
Adjust the potentiometer on the sampling pump until the
7.2.9 Wrist-action Shaking Device, for solvent extraction.
desired flow rate (#1.5 L/min) is obtained. With the bubble
flowmeter connected to the inlet end of the sorbent tube,
8. Reagents and Materials
measure and record the rate of airflow through the sorbent tube
8.1 Purity of Reagents—Reagent grade chemicals shall be
in litres per minute. Refer to Practice D 5337 for standard
used in all tests. Unless otherwise indicated, it is intended that
practice in calibrating personal sampling pumps.
all reagents conform to the specifications of the Committee on
9.2.3 After the XAD-4 sorbent tube is correctly inserted and
Analytical Reagents of the American Chemical Society where
positioned, turn on the power switch for the pump to begin
such specifications are available. Other grades may be used,
sampling. Record the start time.
provided it is first ascertained that the reagent is of sufficiently
NOTE 1—Most pumps have microprocessing capabilities for preset
high purity to permit its use without lessening the accuracy of
sampling periods.
the determination.
9.2.4 Record the barometric pressure and ambient tempera-
8.2 Ethyl Acetate, chromatographic quality.
ture (optional).
8.3 Quinoline (internal standard), 99+ %.
9.2.5 Turn off the pump at the end of the desired sampling
8.4 Triethylamine, 99+ %.
period, and record the elapsed time in minutes.
8.5 Nicotine, 99+ %.
9.2.6 Measure and record the flow rate after sampling so
that an average of initial and final flow rates can be used in
subsequent calculations.
The Gilibrator primary standard airflow calibrator manufactured by Gilian
Instrument Corp., 35 Fairfield Place, W. Caldwell, NJ 07006-6206, or equivalent,
9.2.7 Remove the sorbent tube from the sampling system
has been found suitable for this purpose.
and place plastic caps over both ends of the tube.
Personal sampling pump available from SKC, Inc., Model No. 224-50, or
9.2.8 Treat a minimum of two sorbent tubes in the same
equivalent, has been found suitable for this purpose.
GC system, Model 5890, available from Hewlett-Packard Co., 2850 Center- manner as the sample tubes (break, measure flows, cap, and
ville Rd., Wilmington, DE 19808-1610, or equivalent, has been found suitable for
transport). Label and process these tubes as flow blanks.
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