ASTM D5075-01(2007)
(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/m3 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.
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Designation:D5075–01 (Reapproved 2007)
Standard Test Method for
Nicotine and 3-Ethenylpyridine in Indoor Air
This standard is issued under the fixed designation D5075; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 This test method covers the sampling/analysis of nico- 2.1 ASTM Standards:
tine and 3-ethenylpyridine (3-EP) in indoor air. This test D1356 Terminology Relating to Sampling and Analysis of
method is based upon the collection of nicotine and 3-EP by Atmospheres
adsorption on a sorbent resin, extraction of nicotine and 3-EP D1357 Practice for Planning the Sampling of the Ambient
from the sorbent resin, and determination by gas chromatog- Atmosphere
raphy (GC) with nitrogen selective detection. (1) D3631 Test Methods for Measuring Surface Atmospheric
1.2 The active samplers consist of an XAD-4 sorbent tube Pressure
attached to a sampling pump.This test method is applicable to D5337 Practice for Flow Rate Calibration of Personal
personal or area sampling. Sampling Pumps
1.3 This test method is limited in sample duration by the E260 Practice for Packed Column Gas Chromatography
capacity of the XAD-4 tube for nicotine (about 300 µg). This E355 Practice for Gas Chromatography Terms and Rela-
test method has been evaluated up to 24-h sample duration; tionships
however, samples are typically acquired for at least 1h
3. Terminology
(sometimes only 1 h). (2)
1.4 For this test method, limits of detection (LOD) and 3.1 Definitions—For definitions of terms used in this test
method, refer to Terminology D1356 and Practice E355.
quantitation(LOQ)fornicotineatasamplingrateof1.5L/min
3 3
are, respectively, 0.11 µg/m and 0.37 µg/m for 1-h sample 3.2 Definitions of Terms Specific to This Standard:
3 3
3.2.1 environmental tobacco smoke (ETS)—an aged, dilute
duration and 0.01 µg/m and 0.05 µg/m for 8-h sample
duration.TheLODandLOQfor3-EPatasamplingrateof1.5 composite of exhaled tobacco smoke and smoke from tobacco
3 3
products.
L/min are, respectively, 0.06 µg/m and 0.19 µg/m for 1-h
3 3
3.2.2 nitrogen-phosphorus detector (NPD)—a highly sensi-
sampledurationand0.01µg/m and0.02µg/m for8-hsample
duration (2).BothLODandLOQcanbereducedbyincreasing tivedeviceselectivefordetectionofnitrogen-andphosphorus-
containing organic compounds.
the sensitivity of the thermionic specific detector.
1.5 The values stated in SI units are to be regarded as 3.2.3 XAD-4 resin—macroreticular polystyrene-
divinylbenzene copolymer beads.
standard.
1.6 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
4.1 A known volume of air is drawn through a sorbent
responsibility of the user of this standard to establish appro-
sampling tube containing XAD-4 resin to adsorb the nicotine
priate safety and health practices and determine the applica-
and 3-EP present.
bility of regulatory limitations prior to use. Specific precau-
4.2 The XAD-4 sorbent tube contents are transferred to a
tionary information is given in 13.6.
2-mLautosamplervial,andthenicotineand3-EParedesorbed
with ethyl acetate containing 0.01% triethylamine and a
This test method is under the jurisdiction of ASTM Committee D22 on Air
known quantity of quinoline, the internal standard.
Quality and is the direct responsibility of Subcommittee D22.05 on Indoor Air.
Current edition approved April 1, 2007. Published June 2007. Originally
approved in 1990. Last previous edition approved in 2001 as D5075-01. DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/D5075-01R07. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
The boldface numbers in parentheses refer to a list of references at the end of Standards volume information, refer to the standard’s Document Summary page on
the text. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5075–01 (2007)
4.3 An aliquot of the desorbed sample is injected into a gas (6,10,11,12). 3-Ethenylpyridine concentrations typically are
chromatograph equipped with a thermionic-specific (nitrogen- about one third the concentrations of nicotine in real-world
phosphorus) detector. environments (13).
4.4 The areas of the resulting nicotine and 3-EP peaks are
6. Interferences
each divided by the area of the internal standard peak and
6.1 UseofpackedGCcolumnsmayresultinreadingslower
compared with area ratios obtained from the injection of
than expected because nicotine can adsorb onto undeactivated
standards.
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
collectedbytheXAD-4resin.If>10µgnicotineiscollectedon
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
concentrationof167µg/m wassampledat1L/minfor1h.)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
usedtoextracttheoriginalsample;thatis,decreasetheamount
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
concentrations. Although this is true in many environments
prevent significant interference, the nicotine concentration in
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-ethylnornico-
overestimationofETSconcentrations.Thus,measuredconcen-
tine is recommended (14)].
trations of nicotine precisely assess only airborne nicotine and
7. Apparatus
indicate only that smoking has taken place; they do not
necessarilyindicatethepresence,andcertainlynottheconcen- 7.1 Sample Collection:
trations, of other ETS constituents. 3-Ethenylpyridine, on the 7.1.1 XAD-4 Sorbent Tube—Glass tube with both ends
otherhand,hasbeenshowntotrackexactlythevaporphaseof 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 one section of
reasons that 3-ethenylpyridine may be a better tracer of ETS 120 mg of 20/40 mesh XAD-4 resin. A glass wool plug is
(1,4,5). The ETS at high concentrations is known to be located at the front end (inlet) and back end of the tube. The
annoying and irritating to individuals, and concerns over glasswoolplugattheinletendofthetubeisheldinplacewith
potential health effects have also been expressed. There is a a metal lockspring.
definite need to have reliable methods for the estimation of 7.1.2 Tube Holder, with clip attachment for attaching tube
ETS levels in order to evaluate its effect. The NIOSH has to clothing or objects.
previously set a threshold limit value (TLV) for nicotine in the 7.1.3 Tube Breaker, to break sealed ends from sample
workplace of 0.5 mg/m . tubes.
5.2 Studies show that more than 90% of nicotine in indoor 7.1.4 NIOSH-approvedPlasticCaps,forcappingtubesafter
airisfoundinthevaporphase (6,7).Thedescribedtestmethod sampling.
collects vapor-phase nicotine quantitatively. Early studies on 7.1.5 Barometer and Thermometer, for taking pressure and
freshly generated ETS indicated that some but not all of the temperature readings at the sampling site (optional).
particulate phase was trapped on the XAD-4 resin (7). Amore 7.1.6 Bubble Flowmeter, for sample pump calibration.
recent investigation of the trapping of particulate materials by 7.1.7 Personal Sampling Pump, portable constant-flow
sorbent beds suggests that the trapping of the particles from sampling pump calibrated for the flow rate desired (up to 1.5
indoor air may be nearly quantitative (8). 3-Ethenylpyridine is L/min).
found exclusively in the vapor phase. 7.2 Analytical System:
5.3 Nicotine concentrations typically range from ND (not 7.2.1 Gas Chromatograph, with a nitrogen-phosphorus
detected) to 70 µg/m in various indoor environments with (thermionic) detector and autosampler.
values usually at the lower end of this range (9). Because such 7.2.2 GC Column—A 30-m by 0.32-mm inside diameter
low concentrations of nicotine are often encountered, sophis- fusedsilicacapillarycolumn,coatedwitha1.0-µmfilmof5%
ticated analytical procedures and equipment are required for phenyl methylpolysiloxane (DB-5).
quantifying nicotine in indoor air. Other methods for the 7.2.3 Chromatography Data Acquisition System, for mea-
determination of nicotine in indoor air have also been reported suring peak areas electronically.
D5075–01 (2007)
7.2.4 Sample Containers, borosilicate glass autosampler 9.2.4 Record the barometric pressure and ambient tempera-
vials, 2-mL capacity, with PTFE-lined septum closures. ture (optional).
9.2.5 Turn off the pump at the end of the desired sampling
7.2.5 Dispensing Pipets, 1.25-mL.
period, and record the elapsed time in minutes.
7.2.6 Triangular File,forscoringandbreakingopensample
9.2.6 Measure and record the flow rate after sampling so
tubes.
that an average of initial and final flow rates can be used in
7.2.7 Forceps,forassistingtransferofsorbenttubecontents
subsequent calculations.
from tube to autosampler vial.
9.2.7 Remove the sorbent tube from the sampling system
7.2.8 Glass Wool Removal Tool, for assisting transfer of
and place plastic caps over both ends of the tube.
sorbent tube contents from tube to autosampler vial.
9.2.8 Treat a minimum of two sorbent tubes in the same
7.2.9 Wrist-action Shaking Device, for solvent extraction.
manner as the sample tubes (break, measure flows, cap, and
transport). Label and process these tubes as flow blanks.
8. Reagents and Materials
9.2.9 Transport capped sorbent tubes to the laboratory for
8.1 Purity of Reagents—Reagent grade chemicals shall be
analysis.
used in all tests. Unless otherwise indicated, it is intended that
NOTE 2—If the samples are not prepared and analyzed immediately,
all reagents conform to the specifications of the Committee on
they should be stored at 0°C or less. All sorbent tube samples should be
Analytical Reagents of theAmerican Chemical Society where
analyzed within eight weeks after sample collection. It has been estab-
such specifications are available. Other grades may be used,
lished that samples are stable for at least eight weeks at−10°C.
provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
10. Analysis
the determination.
10.1 System Description:
8.2 Ethyl Acetate, chromatographic quality.
10.1.1 Analysis is performed using a GC fitted with a
8.3 Quinoline (internal standard), 99+%.
nitrogen-phosphorus detector and an autosampler equipped for
8.4 Triethylamine, 99+%.
split/splitless injection.
8.5 Nicotine, 99+%.
10.1.2 The GC column is as listed in 7.2.2.
8.6 4-Ethenylpyridine (4-EP), 95%, commercially avail-
10.1.3 The GC conditions are as listed in Table 1.
able isomer of 3-ethenylpyridine.
10.1.4 The autosampler uses default settings for the injec-
8.7 Helium Cylinders,forcarrierordetectormakeupgas,or
tion sequence, and 1 or 2 µL of sample is injected with a 30-s
both, 99.995% grade.
splitless period.
8.8 Hydrogen Cylinders, for detector gas, 99.995% grade.
10.1.5 Peak areas are measured electronically with a chro-
8.9 Air, for detector gas (<0.1 ppm hydrocarbon). matography data acquisition system.
10.2 Systems Performance Criteria:
9. Sampling 10.2.1 Approximate retention times for 3-EP, 4-EP, quino-
line, and nicotine are listed in Table 1.
9.1 General—For planning sampling programs, refer to
10.2.2 Desorption efficiency should be determined for each
Practice D1357.
new lot of sorbent tubes. Failure to determine the desorption
9.2 Procedure:
efficiency and adjust results may impair the accuracy of the
9.2.1 Prepare XAD-4 sampling tubes immediately before
test.
sampling. Break both ends of the sealed sorbent tube using a
tube breaker tool. The opening should measure at least 2 mm
in diameter.
TABLE 1 Summary of Gas Chromatograph Conditions
9.2.2 Connect the sorbent tube to the personal sampling
Temperatures
pump with tubing. Position the sorbent tube so that the air Injector 225°C
Oven
being sampled will pass first through the front section of resin
Initial temperature 50°C
and then through the backup section. The inlet end of the tube
Hold time 1 min
is exposed directly to the atmosphere, and the outlet end is Program Step 1
Rate 10°C/min
inserted in the tubing; or the tube itself is put into a safety
Final temperature 215°C
casinginthepersonalsamplingsetupandattachedaccordingly.
Hold time 0 min
Program Step 2
Adjust the potentiometer on the sampling pump until the
Rate 20°C/min
desired flow rate (#1.5 L/min) is obtained. With the bubble
Final temperature 295°C
flowmeter connected to the inlet end of the sorbent tube,
Hold time 1 min
Detector 300°C
measureandrecordtherateofairflowthroughthesorbenttube
Gas flows
in litres per minute. Refer to Practice D5337 for standard
He, carrier 4 mL/min (15 psig)
practice in calibrating personal samp
...
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