ASTM D5075-01(2017)e1
(Test Method)Standard Test Method for Nicotine and 3-Ethenylpyridine in Indoor Air
Standard Test Method for Nicotine and 3-Ethenylpyridine in Indoor Air
SIGNIFICANCE AND USE
5.1 In order to estimate ETS concentrations, there needs to be a marker or tracer for ETS that is unique or highly specific to tobacco smoke, in sufficient concentrations in air to be measured easily at realistic smoking rates, and in constant proportion to the other components of ETS for a variety of tobacco blends and environmental conditions. Nicotine and 3-ethenylpyridine have been used as tracers of the vapor phase of ETS. Nicotine is the major alkaloid of tobacco and a major constituent of ETS. The determination of nicotine concentration has often been used to estimate the concentration of ETS; however, due to its unpredictable decay kinetics, nicotine may not be an ideal tracer. Because nicotine readily adsorbs to building materials and room furnishings and is depleted from ETS at a rate faster than most other components, some have suggested that nicotine concentrations underestimate ETS concentrations. Although this is true in many environments during the generation of smoke, the converse is true in environments with a recent past history of smoking. The adsorbed nicotine slowly desorbs over time, resulting in an overestimation of ETS concentrations. Thus, measured concentrations of nicotine precisely assess only airborne nicotine and indicate only that smoking has taken place; they do not necessarily indicate the presence, and certainly not the concentrations, of other ETS constituents. 3-Ethenylpyridine, on the other hand, has been shown to track exactly the vapor phase of ETS as measured by CO and FID response (3). It is for these reasons that 3-ethenylpyridine may be a better tracer of ETS (1, 4, 5). The ETS at high concentrations is known to be annoying and irritating to individuals, and concerns over potential health effects have also been expressed. There is a definite need to have reliable methods for the estimation of ETS levels in order to evaluate its effect. The NIOSH has previously set a recommended exposure limit (REL) for nicotine in the workp...
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)2
1.2 The active samplers consist of an macroreticular polystyrene-divinylbenzene copolymer (for example, XAD-4) sorbent tube attached to a sampling pump. Macroreticular polystyrene-divinylbenzene copolymer is referred to “sorbent resin” throughout this method. 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 sorbent tube for nicotine (about 300 μg). 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 μg/m3 and 0.37 μg/m 3 for 1-h sample duration and 0.01 μg/m3 and 0.05 μg/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 μg/m 3 and 0.19 μg/m3 for 1-h sample duration and 0.01 μg/m3 and 0.02 μg/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 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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...
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´1
Designation: D5075 − 01 (Reapproved 2017)
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.
ε NOTE—Reapproved with editorial changes throughout in March 2017.
1. Scope priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific precau-
1.1 This test method covers the sampling/analysis of nico-
tionary information is given in 13.6.
tine and 3-ethenylpyridine (3-EP) in indoor air. This test
method is based upon the collection of nicotine and 3-EP by 1.7 This international standard was developed in accor-
adsorption on a sorbent resin, extraction of nicotine and 3-EP dance with internationally recognized principles on standard-
from the sorbent resin, and determination by gas chromatog-
ization established in the Decision on Principles for the
raphy (GC) with nitrogen selective detection (1).
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
1.2 The active samplers consist of an macroreticular
Barriers to Trade (TBT) Committee.
polystyrene-divinylbenzene copolymer (for example, XAD-4)
sorbent tube attached to a sampling pump. Macroreticular
2. Referenced Documents
polystyrene-divinylbenzene copolymer is referred to “sorbent
resin”throughoutthismethod.Thistestmethodisapplicableto
2.1 ASTM Standards:
personal or area sampling.
D1356Terminology Relating to Sampling and Analysis of
1.3 This test method is limited in sample duration by the
Atmospheres
capacity of the sorbent tube for nicotine (about 300 µg). This
D1357Practice for Planning the Sampling of the Ambient
test method has been evaluated up to 24-h sample duration;
Atmosphere
however, samples are typically acquired for at least 1h
D3631Test Methods for Measuring Surface Atmospheric
(sometimes only1h) (2).
Pressure
D5337Practice for Flow RateAdjustment of Personal Sam-
1.4 For this test method, limits of detection (LOD) and
quantitation(LOQ)fornicotineatasamplingrateof1.5L/min pling Pumps
3 3
are, respectively, 0.11 µg/m and 0.37 µg/m for 1-h sample
E260Practice for Packed Column Gas Chromatography
3 3
duration and 0.01 µg/m and 0.05 µg/m for 8-h sample
E355PracticeforGasChromatographyTermsandRelation-
duration.TheLODandLOQfor3-EPatasamplingrateof1.5
ships
3 3
L/min are, respectively, 0.06 µg/m and 0.19 µg/m for 1-h
3 3
sampledurationand0.01µg/m and0.02µg/m for8-hsample
3. Terminology
duration (2).BothLODandLOQcanbereducedbyincreasing
3.1 Definitions—For definitions of terms used in this test
the sensitivity of the thermionic specific detector.
method, refer to Terminology D1356 and Practice E355.
1.5 Units—The values stated in SI units are to be regarded
3.2 Definitions of Terms Specific to This Standard:
asstandard.Nootherunitsofmeasurementareincludedinthis
3.2.1 environmental tobacco smoke (ETS)—an aged, dilute
standard.
composite of exhaled tobacco smoke (exhaled mainstream
1.6 This standard does not purport to address all of the
smoke) and smoke from tobacco products (sidestream smoke).
safety concerns, if any, associated with its use. It is the
3.2.2 nitrogen-phosphorus detector (NPD)—a highly sensi-
responsibility of the user of this standard to establish appro-
tivedeviceselectivefordetectionofnitrogen-andphosphorus-
containing organic compounds.
This test method is under the jurisdiction of ASTM Committee D22 on Air
Quality and is the direct responsibility of Subcommittee D22.05 on Indoor Air.
Current edition approved March 1, 2017. Published March 2017. Originally
ɛ1
approved in 1990. Last previous edition approved in 2012 as D5075–01 (2012) . For referenced ASTM standards, visit the ASTM website, www.astm.org, or
DOI: 10.1520/D5075-01R17E01. 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
´1
D5075 − 01 (2017)
4. Summary of Test Method beds suggests that the trapping of the particles from indoor air
may be nearly quantitative (8). 3-Ethenylpyridine is found
4.1 A known volume of air is drawn through a sorbent
exclusively in the vapor phase.
samplingtubecontainingresintoadsorbthenicotineand3-EP
present.
5.3 Nicotine concentrations typically range from ND (not
detected) to 70 µg/m in various indoor environments with
4.2 The sorbent tube contents are transferred to a 2-mL
values usually at the lower end of this range (9). Because such
autosampler vial, and the nicotine and 3-EP are desorbed with
low concentrations of nicotine are often encountered, sophis-
ethyl acetate containing 0.01% triethylamine and a known
ticated analytical procedures and equipment are required for
quantity of quinoline, the internal standard.
quantifying nicotine in indoor air. Other methods for the
4.3 An aliquot of the desorbed sample is injected into a gas
determination of nicotine in indoor air have also been reported
chromatograph equipped with a thermionic-specific (nitrogen-
(6, 10, 11, 12). 3-Ethenylpyridine concentrations typically are
phosphorus) detector.
about one third the concentrations of nicotine in real-world
4.4 The areas of the resulting nicotine and 3-EP peaks are environments (13).
each divided by the area of the internal standard peak and
compared with area ratios obtained from the injection of
6. Interferences
standards.
6.1 UseofpackedGCcolumnsmayresultinreadingslower
than expected because nicotine can adsorb onto undeactivated
5. Significance and Use
glass, metal, and solid support particles. Fused silica capillary
5.1 In order to estimate ETS concentrations, there needs to
columns and the modified extraction solvent prescribed here
be a marker or tracer for ETS that is unique or highly specific
can circumvent this problem.
to tobacco smoke, in sufficient concentrations in air to be
6.2 Quinoline (internal standard) is present in ETS at a
measured easily at realistic smoking rates, and in constant
proportion to the other components of ETS for a variety of concentration approximately 1% of that for nicotine and is
collected by the resin. If >10 µg nicotine is collected on the
tobacco blends and environmental conditions. Nicotine and
3-ethenylpyridine have been used as tracers of the vapor phase resin, there will be sufficient quinoline present to cause a
detectable bias in results (approximately 1%). (For example,
of ETS. Nicotine is the major alkaloid of tobacco and a major
constituent of ETS. The determination of nicotine concentra- this quantity of nicotine would be collected if a nicotine
concentrationof167µg/m wassampledat1L/minfor1h.)In
tion has often been used to estimate the concentration of ETS;
these cases, one of the following alternative procedures should
however, due to its unpredictable decay kinetics, nicotine may
be followed:
not be an ideal tracer. Because nicotine readily adsorbs to
building materials and room furnishings and is depleted from
6.2.1 Quantitatively dilute the sample with the same modi-
ETS at a rate faster than most other components, some have fied solvent containing internal standard (described in 11.2)
suggested that nicotine concentrations underestimate ETS
usedtoextracttheoriginalsample;thatis,decreasetheamount
concentrations. Although this is true in many environments of quinoline (and also nicotine) present in the sample while
during the generation of smoke, the converse is true in
keeping the quinoline concentration in the solvent constant.To
environments with a recent past history of smoking. The prevent significant interference, the nicotine concentration in
adsorbed nicotine slowly desorbs over time, resulting in an
the most concentrated sample should be less than or equal to
overestimationofETSconcentrations.Thus,measuredconcen- the quinoline concentration in the solvent.
trations of nicotine precisely assess only airborne nicotine and
6.2.2 Use an alternate internal standard [N'-ethylnornico-
indicate only that smoking has taken place; they do not
tine is recommended (14)].
necessarily indicate the presence, and certainly not the
concentrations, of other ETS constituents. 3-Ethenylpyridine,
7. Apparatus
on the other hand, has been shown to track exactly the vapor
7.1 Sample Collection:
phase of ETS as measured by CO and FID response (3).Itis
7.1.1 Sorbent Tube—Glass tube with both ends flame-
for these reasons that 3-ethenylpyridine may be a better tracer
sealed, approximately 7 cm long with 6-mm outside diameter
of ETS (1, 4, 5). The ETS at high concentrations is known to
and4-mminsidediameter,containingonesectionof120mgof
be annoying and irritating to individuals, and concerns over
20/40 mesh resin.Aglass wool plug is located at the front end
potential health effects have also been expressed. There is a
(inlet)andbackendofthetube.Theglasswoolplugattheinlet
definite need to have reliable methods for the estimation of
end of the tube is held in place with a metal lockspring.
ETS levels in order to evaluate its effect. The NIOSH has
7.1.2 Tube Holder,withclipattachmentforattachingtubeto
previously set a recommended exposure limit (REL) for
clothing or objects.
nicotine in the workplace of 0.5 mg/m .
7.1.3 Tube Breaker,tobreaksealedendsfromsampletubes.
5.2 Studies show that more than 90% of nicotine in indoor
7.1.4 NIOSH-approved Plastic Caps,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 resin (7). A more recent
investigationofthetrappingofparticulatematerialsbysorbent 7.1.6 Bubble Flowmeter, for sample pump calibration.
´1
D5075 − 01 (2017)
7.1.7 Personal Sampling Pump,portableconstant-flowsam- casinginthepersonalsamplingsetupandattachedaccordingly.
pling pump calibrated for the flow rate desired (up to 1.5 Adjust the potentiometer on the sampling pump until the
L/min). desired flow rate (≤1.5 L/min) is obtained. With the bubble
flowmeter connected to the inlet end of the sorbent tube,
7.2 Analytical System:
measureandrecordtherateofairflowthroughthesorbenttube
7.2.1 Gas Chromatograph, with a nitrogen-phosphorus
in litres per minute. Refer to Practice D5337 for standard
(thermionic) detector and autosampler.
practice in calibrating personal sampling pumps.
7.2.2 GC Column—A 30-m by 0.32-mm inside diameter
9.2.3 After the sorbent tube is correctly inserted and
fusedsilicacapillarycolumn,coatedwitha1.0-µmfilmof5%
positioned, turn on the power switch for the pump to begin
phenyl methylpolysiloxane (DB-5).
sampling. Record the start time.
7.2.3 Chromatography Data Acquisition System, for mea-
suring peak areas electronically.
NOTE 1—Most pumps have microprocessing capabilities for preset
sampling periods.
7.2.4 Sample Containers, borosilicate glass autosampler
vials, 2-mL capacity, with PTFE-lined septum closures.
9.2.4 Record the barometric pressure and ambient tempera-
7.2.5 Dispensing Pipets, 1.25-mL.
ture (optional).
7.2.6 Triangular File,forscoringandbreakingopensample
9.2.5 Turn off the pump at the end of the desired sampling
tubes.
period, and record the elapsed time in minutes.
7.2.7 Forceps,forassistingtransferofsorbenttubecontents
9.2.6 Measure and record the flow rate after sampling so
from tube to autosampler vial.
that an average of initial and final flow rates can be used in
7.2.8 Glass Wool Removal Tool, for assisting transfer of
subsequent calculations.
sorbent tube contents from tube to autosampler vial.
9.2.7 Remove the sorbent tube from the sampling system
7.2.9 Wrist-action Shaking Device, for solvent extraction.
and place plastic caps over both ends of the tube.
9.2.8 Treat a minimum of two sorbent tubes in the same
8. Reagents and Materials
manner as the sample tubes (break, measure flows, cap, and
8.1 Purity of Reagents—Reagent grade chemicals shall be transport). Label and process these tubes as flow blanks.
used in all tests. Unless otherwise indicated, it is intended that 9.2.9 Transport capped sorbent tubes to the laboratory for
all reagents conform to the specifications of the Committee on analysis.
Analytical Reagents of theAmerican Chemical Society where
NOTE 2—If the samples are not prepared and analyzed immediately,
such specifications are available. Other grades may be used,
they should be stored at 0°C or less. All sorbent tube samples should be
provided it is first ascertained that the reagent is of sufficiently
analyzed within eight weeks after sample collection. It has been estab-
lished that samples are stable for at least eight weeks at−10°C.
high purity to permit its use without lessening the accuracy of
the determination.
10. Analysis
8.2 Ethyl Acetate, chromatographic quality.
10.1 System Description:
8.3 Quinoline (internal standard), 99+%.
10.1.1 Analysis is performed using a GC fitted with a
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.
TABLE 1 Summary of Gas Chromatograph Conditions
8.7 Helium Cylinders,forcarrierordetectormakeupgas,or
both, 99.995% grade.
Temperatures
Injector 225°C
8.8 Hydrogen Cylinders, for detector gas, 99.995% grade.
Oven
Initial temperature 50°C
8.9 Air, for detector gas (<0.1 ppm hydrocarbon).
Hold time 1 min
Program Step 1
9. Sampling Rate 10°C/min
Final temperature 215°C
9.1 General—For planning sampling programs, refer to
Hold time 0 min
Program Step 2
Practice D1357.
Rate 20°C/min
9.2 Procedure: Final temperature 295°C
Hold time 1 min
9.2.1 Prepare sampling tubes immediately before sampling.
Detector 300°C
Breakbothendsofthesealedsorbenttubeusingatubebreaker
Gas flows
tool. The opening should measure at least 2 mm in diameter. He, carrier 4 mL/min (15 psig)
H , detector 3 mL/min
9.2.2 Connect the sorbent tube to the personal sampling
Air, detector 75 mL/min
pump with tubing. Posi
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1 ´1
Designation: D5075 − 01 (Reapproved 2012) D5075 − 01 (Reapproved 2017)
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Reapproved with editorial change tochanges throughout 1.5in April 2012.March 2017.
1. 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 macroreticular polystyrene-divinylbenzene copolymer (for example, XAD-4)
sorbent tube attached to a sampling pump. Macroreticular polystyrene-divinylbenzene copolymer is referred to “sorbent resin”
throughout this method. 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-4sorbent tube for nicotine (about 300 μg). 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,
3 3 3 3
respectively, 0.11 μg/m and 0.37 μg/m for 1-h sample duration and 0.01 μg/m and 0.05 μg/m for 8-h sample duration. The LOD
3 3
and LOQ for 3-EP at a sampling rate of 1.5 L/min are, respectively, 0.06 μg/m and 0.19 μg/m for 1-h sample duration and 0.01
3 3
μg/m and 0.02 μg/m for 8-h sample duration (2). Both LOD and LOQ can be reduced by increasing the sensitivity of the
thermionic specific detector.
1.5 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this
standard.
1.6 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.
2. Referenced Documents
2.1 ASTM Standards:
D1356 Terminology Relating to Sampling and Analysis of Atmospheres
D1357 Practice for Planning the Sampling of the Ambient Atmosphere
D3631 Test Methods for Measuring Surface Atmospheric Pressure
D5337 Practice for Flow Rate Adjustment of Personal Sampling Pumps
E260 Practice for Packed Column Gas Chromatography
E355 Practice for Gas Chromatography Terms and Relationships
3. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to Terminology D1356 and Practice E355.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 environmental tobacco smoke (ETS)—an aged, dilute composite of exhaled tobacco smoke (exhaled mainstream smoke)
and smoke from tobacco products. products (sidestream smoke).
This test method is under the jurisdiction of ASTM Committee D22 on Air Quality and is the direct responsibility of Subcommittee D22.05 on Indoor Air.
Current edition approved April 1, 2012March 1, 2017. Published July 2012March 2017. Originally approved in 1990. Last previous edition approved in 20072012 as
ɛ1
D5075 - 01D5075 – 01 (2012) (2007). DOI: 10.1520/D5075-01R12E01.10.1520/D5075-01R17E01.
The boldface numbers in parentheses refer to a list of references at the end of the text.
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 standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D5075 − 01 (2017)
3.2.2 nitrogen-phosphorus detector (NPD)—a highly sensitive device selective for detection of nitrogen- and phosphorus-
containing organic compounds.
3.2.3 XAD-4 resin—macroreticular polystyrene-divinylbenzene copolymer beads.
4. Summary of Test Method
4.1 A known volume of air is drawn through a sorbent sampling tube containing XAD-4 resin to adsorb the nicotine and 3-EP
present.
4.2 The XAD-4 sorbent tube contents are transferred to a 2-mL autosampler vial, and the nicotine and 3-EP are desorbed with
ethyl acetate containing 0.01 % triethylamine and a known quantity of quinoline, the internal standard.
4.3 An aliquot of the desorbed sample is injected into a gas chromatograph equipped with a thermionic-specific (nitrogen-
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 standards.
5. Significance and Use
5.1 In order to estimate ETS concentrations, there needs to be a marker or tracer for ETS that is unique or highly specific to
tobacco smoke, in sufficient concentrations in air to be measured easily at realistic smoking rates, and in constant proportion to
the other components of ETS for a variety of tobacco blends and environmental conditions. Nicotine and 3-ethenylpyridine have
been used as tracers of the vapor phase of ETS. Nicotine is the major alkaloid of tobacco and a major constituent of ETS. The
determination of nicotine concentration has often been used to estimate the concentration of ETS; however, due to its unpredictable
decay kinetics, nicotine may not be an ideal tracer. Because nicotine readily adsorbs to building materials and room furnishings
and is depleted from ETS at a rate faster than most other components, some have suggested that nicotine concentrations
underestimate ETS concentrations. Although this is true in many environments during the generation of smoke, the converse is true
in environments with a recent past history of smoking. The adsorbed nicotine slowly desorbs over time, resulting in an
overestimation of ETS concentrations. Thus, measured concentrations of nicotine precisely assess only airborne nicotine and
indicate only that smoking has taken place; they do not necessarily indicate the presence, and certainly not the concentrations, of
other ETS constituents. 3-Ethenylpyridine, on the other hand, has been shown to track exactly the vapor phase of ETS as measured
by CO and FID response (3). It is for these reasons that 3-ethenylpyridine may be a better tracer of ETS (1, 4, 5). The ETS at high
concentrations is known to be annoying and irritating to individuals, and concerns over potential health effects have also been
expressed. There is a definite need to have reliable methods for the estimation of ETS levels in order to evaluate its effect. The
NIOSH has previously set a threshold limit value (TLV) recommended exposure limit (REL) for nicotine in the workplace of 0.5
mg/m .
5.2 Studies show that more than 90 % of nicotine in indoor air is found in the vapor phase (6, 7). The described test method
collects vapor-phase nicotine quantitatively. Early studies on 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
sorbent beds suggests that the trapping of the particles from indoor air may be nearly quantitative (8). 3-Ethenylpyridine is found
exclusively in the vapor phase.
5.3 Nicotine concentrations typically range from ND (not detected) to 70 μg/m in various indoor environments with values
usually at the lower end of this range (9). Because such low concentrations of nicotine are often encountered, sophisticated
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
glass, metal, and solid support particles. Fused silica capillary columns and the modified extraction solvent prescribed here can
circumvent this problem.
6.2 Quinoline (internal standard) is present in ETS at a concentration approximately 1 % of that for nicotine and is collected
by the XAD-4 resin. If >10 μg nicotine is collected on the resin, there will be sufficient quinoline present to cause a detectable bias
in results (approximately 1 %). (For example, this quantity of nicotine would be collected if a nicotine concentration of 167 μg/m
was sampled at 1 L/min for 1 h.) In these cases, one of the following alternative procedures should be followed:
6.2.1 Quantitatively dilute the sample with the same modified solvent containing internal standard (described in 11.2) used to
extract the original sample; that is, decrease the amount of quinoline (and also nicotine) present in the sample while keeping the
quinoline concentration in the solvent constant. To prevent significant interference, the nicotine concentration in the most
concentrated sample should be less than or equal to the quinoline concentration in the solvent.
´1
D5075 − 01 (2017)
6.2.2 Use an alternate internal standard [N'-ethylnornico-
tine is recommended (14)].
7. Apparatus
7.1 Sample Collection:
7.1.1 XAD-4 Sorbent Tube—Glass tube with both ends flame-sealed, approximately 7 cm long with 6-mm outside diameter and
4-mm inside diameter, containing one section of 120 mg of 20/40 mesh XAD-4 resin. A glass wool plug is located at the front end
(inlet) and back end of the tube. The glass wool plug at the inlet end of the tube is held in place with a metal lockspring.
7.1.2 Tube Holder, with clip attachment for attaching tube to clothing or objects.
7.1.3 Tube Breaker, to break sealed ends from sample tubes.
7.1.4 NIOSH-approved Plastic Caps, for capping tubes after sampling.
7.1.5 Barometer and Thermometer, for taking pressure and temperature readings at the sampling site (optional).
7.1.6 Bubble Flowmeter, for sample pump calibration.
7.1.7 Personal Sampling Pump, portable constant-flow sampling pump calibrated for the flow rate desired (up to 1.5 L/min).
7.2 Analytical System:
7.2.1 Gas Chromatograph, with a nitrogen-phosphorus (thermionic) detector and autosampler.
7.2.2 GC Column—A 30-m by 0.32-mm inside diameter fused silica capillary column, coated with a 1.0-μm film of 5 % phenyl
methylpolysiloxane (DB-5).
7.2.3 Chromatography Data Acquisition System, for measuring peak areas electronically.
7.2.4 Sample Containers, borosilicate glass autosampler vials, 2-mL capacity, with PTFE-lined septum closures.
7.2.5 Dispensing Pipets, 1.25-mL.
7.2.6 Triangular File, for scoring and breaking open sample tubes.
7.2.7 Forceps, for assisting transfer of sorbent tube contents from tube to autosampler vial.
7.2.8 Glass Wool Removal Tool, for assisting transfer of sorbent tube contents from tube to autosampler vial.
7.2.9 Wrist-action Shaking Device, for solvent extraction.
8. Reagents and Materials
8.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such
specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity
to permit its use without lessening the accuracy of the determination.
8.2 Ethyl Acetate, chromatographic quality.
8.3 Quinoline (internal standard), 99+ %.
8.4 Triethylamine, 99+ %.
8.5 Nicotine, 99+ %.
8.6 4-Ethenylpyridine (4-EP), 95 %, commercially available isomer of 3-ethenylpyridine.
8.7 Helium Cylinders, for carrier or detector makeup gas, or both, 99.995 % grade.
8.8 Hydrogen Cylinders, for detector gas, 99.995 % grade.
8.9 Air, for detector gas (<0.1 ppm hydrocarbon).
9. Sampling
9.1 General—For planning sampling programs, refer to Practice D1357.
9.2 Procedure:
9.2.1 Prepare XAD-4 sampling tubes immediately before sampling. Break both ends of the sealed sorbent tube using a tube
breaker tool. The opening should measure at least 2 mm in diameter.
9.2.2 Connect the sorbent tube to the personal sampling pump with tubing. Position the sorbent tube so that the air being
sampled will pass first through the front section of resin and then through the backup section. The inlet end of the tube is exposed
directly to the atmosphere, and the outlet end is inserted in the tubing; or the tube itself is put into a safety casing in the personal
sampling setup and attached accordingly. Adjust the potentiometer on the sampling pump until the desired flow rate (≤1.5 L/min)
is obtained. With the bubble flowmeter connected to the inlet end of the sorbent tube, measure and record the rate of airflow
through the sorbent tube in litres per minute. Refer to Practice D5337 for standard practice in calibrating personal sampling pumps.
9.2.3 After the XAD-4 sorbent tube is correctly inserted and positioned, turn on the power switch for the pump to begin
sampling. Record the start time.
NOTE 1—Most pumps have microprocessing capabilities for preset sampling periods.
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9.2.4 Record the barometric pressure and ambient temperature (optional).
9.2.5 Turn off the pump at the end of the desired sampling period, and record the elapsed time in minutes.
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.
9.2.7 Remove the sorbent tube from the sampling system and place plastic caps over both ends of the tube.
9.2.8 Treat a minimum of two sorbent tubes in the same manner as the sample tubes (break, measure flows, cap, and transport).
Label and process these tubes as flow blanks.
9.2.9 Transport capped sorbent tubes to the laboratory for analysis.
NOTE 2—If the samples are not prepared and analyzed immedia
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