ASTM D6271-98
(Test Method)Standard Test Method for Estimating Contribution of Environmental Tobacco Smoke to Respirable Suspended Particles Based on Solanesol
Standard Test Method for Estimating Contribution of Environmental Tobacco Smoke to Respirable Suspended Particles Based on Solanesol
SCOPE
1.1 This test method covers the sampling/analysis of respirable suspended particles (RSP) and the estimation of the RSP fraction attributable to environmental tobacco smoke (ETS). The test method is based on collection of total RSP on a membrane filter, extraction of the filter in methanol , and determination of solanesol, a C45 isoprenoid alcohol, by high performance liquid chromatography (HPLC) with ultraviolet (UV) detection.
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Designation: D 6271 – 98
Standard Test Method for
Estimating Contribution of Environmental Tobacco Smoke
to Respirable Suspended Particles Based on Solanesol
This standard is issued under the fixed designation D 6271; 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.
1. Scope 2. Referenced Documents
1.1 This test method covers the sampling/analysis of respi- 2.1 ASTM Standards:
rable suspended particles (RSP) and the estimation of the RSP D 1356 Terminology Relating to Sampling and Analysis of
fraction attributable to environmental tobacco smoke (ETS). Atmospheres
The test method is based on collection of total RSP on a D 1357 Practice for Planning the Sampling of the Ambient
membrane filter, extraction of the filter in methanol, and Atmosphere
determination of solanesol, a C isoprenoid alcohol, by high D 3631 Test Methods for Measuring Surface Atmospheric
performance liquid chromatography (HPLC) with ultraviolet Pressure
(UV) detection. D 5337 Practice for Flow Rate for Calibration of Personal
1.2 This test method is compatible with the determinations Sampling Pumps
of gravimetric RSP, ultraviolet particulate matter (UVPM), and D 5955 Test Methods for Estimating Contribution of Envi-
fluorescent particulate matter (FPM) (see Test Methods ronmental Tobacco Smoke to Respirable Suspended Par-
D 5955), but does not require them. UVPM and FPM, which ticles Based on UVPM and FPM
are based on the ultraviolet absorbance and fluorescence of the
3. Terminology
filter extract, are also used to estimate the contribution of ETS
to RSP. 3.1 Definitions: For definitions of terms used in this test
method, refer to Terminology D 1356.
1.3 The sampling components consist of a 1.0-μm pore size
polytetrafluoroethylene (PTFE) membrane filter in a filter 3.2 Definitions of Terms Specific to This Standard:
3.2.1 environmental tobacco smoke (ETS)—an aged, dilute
cassette connected on the inlet end to a particle size separating
composite of exhaled tobacco smoke (exhaled mainstream
device and, on the outlet end, to a sampling pump. This test
method is applicable to personal and area sampling. smoke) and smoke from tobacco products (sidestream smoke).
3.2.2 respirable suspended particles (RSP)—particles
1.4 This test method is limited in sample duration only by
the capacity of the membrane filter. The test method has been which can be deposited in the gas-exchange region of the lung
and are defined as particles that pass through a sampler having
evaluated up to 24-h sample duration; a minimum sample
duration of1his recommended. a 4.0-μm median cutpoint (1) .
3.2.3 solanesol particulate matter (Sol-PM)—a tobacco-
1.5 Limits of detection (LOD) for this test method at a
sampling rate of 2 L/min are 0.042 μg/m for 1-h sample selective marker for the contribution of ETS particulate matter
to RSP.
duration and 0.005 μg/m for 8-h sample duration.
1.6 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 an inertial
1.7 This standard does not purport to address all the safety
impactor or cyclone assembly separating at 4.0 μm to separate
concerns, if any, associated with its use. It is the responsibility
respirable suspended particles (RSP) from total suspended
of the user of this standard to establish appropriate safety and
particulate matter and then through a filter assembly. Solanesol
health practices and determine the applicability of regulatory
is collected as a component of RSP on a PTFE membrane filter
limitations prior to use. Specific precautionary information is
contained within the filter assembly.
given in 13.6.
This test method is under the jurisdiction of ASTM Committee D22 on
Sampling and Analysis of Atmospheres and is the direct responsibility of Subcom- Annual Book of ASTM Standards, Vol 11.03.
mittee D22.05 on Indoor Air. The boldface numbers in parentheses refer to a list of references at the end of
Current edition approved June 10, 1998. Published September 1998. this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6271–98
4.2 Solanesol is extracted from the filter with methanol in a solansol is a better indicator of the tobacco smoke contribution
4-mL glass vial. to RSP. This test method has been used to apportion RSP into
4.3 An aliquot of the extract is injected into an HPLC ETS and non-ETS components by determining the weight ratio
system equipped with a UV detector (205 nm absorbance). of solanesol to total RSP (2,3,4,7,18,19).
4.4 The area of the resulting solanesol peak is compared to
6. Interferences
areas obtained from the injection of standard solutions of
solanesol, and the weight of solanesol is determined.
6.1 The genus Nicotiana, which includes tobacco as one of
4.5 The concentration of solanesol (μg/m ) is calculated its species, is a member of the Solanaceae family of plants.
from the weight of solanesol and the volume of air sampled. If
Like tobacco, many plants in this family, particularly those
desired, the concentration of RSP can also be calculated which also contain trace amounts of nicotine, contain solane-
according to Test Methods D 5955.
sol. Examples are tomato, potato, eggplant, and pepper. With
4.6 The concentration of RSP attributable to ETS, referred cooking as the only possible source of interference, the
to as Sol-PM, is calculated from the airborne concentration of
potential for interference is negligible. However, if there were
solanesol and the experimentally determined weight ratio of an interference of this type, the weight of solanesol would be
solanesol to RSP in ETS (2,3,4).
biased high and the contribution of ETS to RSP would be
overestimated. It is anticipated that the only measurable
5. Significance and Use
contribution of solanesol to an indoor environment would
5.1 Environmental tobacco smoke consists of both vapor
come from tobacco combustion.
and particulate phase components. Due to the nature of vapor
and particulate phases, they rarely correlate well, and an 7. Apparatus
accurate assessment of ETS levels in indoor air requires
7.1 Sample Collection:
determining good tracers of both phases. Among the attributes
7.1.1 PTFE Filter, membrane filter with 1.0-μm pore size
of an ideal ETS tracer, one critical characteristic is that the
and 37–mm diameter.
tracer should “remain in a fairly consistent ratio to the
7.1.2 Filter Sampling Assembly, consists of monitor case,
individual contaminant of interest or category of contaminants
PTFE membrane filter, and gasket. All connections to the filter
of interest (for example, suspended particulates) under a range
assembly are made with flexible plastic tubing.
of environmental conditions.” (5). Solanesol meets this re-
7.1.3 Barometer and Thermometer, for taking pressure and
quirement, staying in a constant ratio to the RSP contributed by
temperature readings at the sampling site.
tobacco smoke over a variety of ventilation conditions and
7.1.4 Bubble Flowmeter or Mass Flowmeter, for calibration
sampling durations (6). UVPM and FPM, which are the tracers
of the sampling pump.
or markers employed by Test Methods D 5955, also fulfill this
7.1.5 Personal Sampling Pump, portable constant-flow sam-
requirement. Airborne solanesol, however, is unique in that it is
pling pump calibrated for a flow rate dependent upon the
specific to tobacco smoke and is found only in the particulate
separating characteristics of the impactor or cyclone in use (see
phase of ETS. Its high molecular weight and low volatility
7.1.6).
make it extremely unlikely that any solanesol will be lost from
7.1.6 Inertial Impactor or Cyclone, with nominal cutpoint of
the membrane filter used for sample collection. Solanesol
4.0 μm.
constitutes approximately3%by weight of the RSP of ETS
NOTE 1—If alternate definition of RSP is used (see 3.2.2), ensure that
(2,7,8), making it suitable for measurement at realistic smoking
the impactor or cyclone is compatible with this definition.
rates. Of the available ETS particulate phase markers (UVPM,
7.1.7 Stopcock Grease, for coating impactor plates.
FPM, and solanesol), all are currently used and relied upon, but
7.2 Analytical System:
solanesol is considered to be a better marker for the particulate
7.2.1 Liquid Chromatography System, consists of HPLC
phase of ETS and, as a result, provides the best way of
pump, UV detector with deuterium source lamp, autosampler,
quantifying the contribution of ETS particulate matter to RSP
column oven (optional), and data acquisition and peak integra-
(3,4,9,10,11,12,13).
tion system.
5.2 To be able to quantify the contribution of ETS to RSP
7.2.2 HPLC Column, 250 mm by 3.0-mm ID, reversed-
with a tobacco-specific marker is important because RSP is not
phase C column (300-Å pore size; 5-μm particle size). C
specific to tobacco smoke. RSP is a necessary indicator of
18 18
packing material with low carbon loading has been found to be
overall air quality; the Occupational Safety and Health Admin-
preferable.
istration (OSHA) has previously set a PEL (permissible expo-
7.2.3 Guard Cartridge Column, a guard cartridge with
sure level) for respirable dust in the workplace of 5000 μg/m .
packing material and dimensions compatible with the HPLC
However, RSP emanates from numerous sources (14) and has
column in 7.2.2, placed in front of the analytical column for
been shown to be an inappropriate tracer of ETS (7,15,16,17).
protecting and prolonging the life of the column.
UVPM and FPM are used as more selective markers to
estimate the contribution of tobacco smoke to RSP; however,
these markers can overestimate the contribution of tobacco
The sole source of supply of the gasket known to the committee at this time is
smoke to RSP due to potential interference from nontobacco
SKC Inc., 863 Valley View Rd., Eighty Four, PA, 15330. If you are aware of
combustion sources. (Refer to Test Methods D 5955 for the
alternate suppliers, please provide this information to ASTM Headquarters. Your
protocol on determining UVPM and FPM.) Although UVPM
comments will receive careful consideration at a meeting of the responsible
and FPM are useful in investigations of indoor air quality, technical committee, which you may attend.
D6271–98
7.2.4 Sample Containers, low-actinic borosilicate glass au-
where:
tosampler vials, 4-mL capacity, with screw caps and PTFE-
Q = pump flow rate, L/min,
lined septa.
V = volume measured with flowmeter, L, and
7.2.5 Filter Forceps, for handling filters. R = average time for soap-film bubble to flow a known
7.2.6 Wrist-action Shaking Device, for solvent extraction. volume (V) in a flowmeter, min.
9.2.4 Adjust the potentiometer on the sampling pump so
8. Reagents and Materials that the desired flow rate is obtained.
9.2.5 With the filter assembly correctly inserted and posi-
8.1 Purity of Reagents—Reagent grade chemicals shall be
tioned between the impactor or cyclone and pump, turn on the
used in all tests. Unless otherwise indicated, it is intended that
pump power switch to begin sampling; record the start time.
all reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society where
NOTE 3—Most pumps have microprocessing capabilities or built-in
such specifications are available. Other grades may be used, elapsed time meters, or both, for preset sampling periods.
provided it is first ascertained that the reagent is of sufficiently
9.2.6 Record the temperature and barometric pressure of the
high purity to permit its use without lessening the accuracy of
atmosphere being sampled.
the determination.
9.2.7 Acquire samples at the required flow rate for a
8.2 Acetonitrile, HPLC grade, (CAS No. 75-05-8).
minimum sampling period of 1 h. Turn off the pump at the end
8.3 Methanol, HPLC grade, (CAS No. 67-56-1).
of the desired sampling period and record the time elapsed
8.4 Solanesol , 90+ %, (CAS No. 13190-97-1). (See Note
during sample collection.
7.)
9.2.8 Recheck the flow rate of the pump again after sam-
8.5 Helium, 99.995 % grade, (CAS No.7440-59-7), for con-
pling and use the average flow rate (mean of before and after
tinuous purging of mobile phase.
sampling) in later calculations.
9.2.9 Immediately remove the filter assembly from the
9. Sampling
sampling system and seal the filter cassette with plugs pro-
9.1 General—for planning sampling programs, refer to
vided.
Practice D 1357.
9.2.10 Treat a minimum of two filter assemblies in the same
9.2 Procedure:
manner as the samples (remove plugs, measure flow, replace
plugs, and transport). Label and process these filters as field
NOTE 2—If a gravimetric determination of RSP is to be performed, then
blanks.
weigh the filters according to Test Methods D 5955 prior to 9.2.1.
9.2.11 Store all used filter assemblies in a freezer or under
9.2.1 Calibrate the personal sampling pump prior to and
dry ice and transport frozen to the laboratory for analysis.
immediately after sampling. For calibration, connect the flow-
meter to the inlet of the inertial impactor or cyclone. Measure NOTE 4—If the samples are not prepared and analyzed immediately,
then store them at 0°C or less. Analyze all the filters within six weeks after
the flow with the prepared filter assembly in place between the
sample collection. It has been established that samples are stable for at
pump and the impactor or cyclone. Refer to Practice D 5337
least six weeks at -10°C storage conditions (20).
for standard practice in calibrating personal sampling pumps.
9.2.2 Record the barometric pressure and ambient tempera-
10. Analysis
ture.
10.1 System Description:
9.2.3 If using a mass flowmeter, record the volumetric flow
10.1.1 Perform analysis using an HPLC system equipped
rate, Q. If using a bubble flowmeter, generate several soap-film
with a UV detector at a wavelength setting of 205 nm.
bubbles in the flowmeter and allow them to thoroughly wet the
surface before recording any actual measurements. Measure
NOTE 5—A UV detector with a deuterium source is required. A detector
the time for a soap-film bubble to travel a known volume with with a xenon source is not acceptable because of insufficient lamp energy
at 205 nm.
a stopwatch. Obtain five replicate measurements and compute
the mean time. Calculate the volumetric flow rate, Q,in
10.1.2 The HPLC column and guard column are as listed in
accordance with Eq 1:
7.2.2 and 7.2.3.
V
10.1.3 The mobile phase consists of 95:5 (v/v) acetonitrile:
Q5 (1)
R
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