1、Designation: D 6271 04Standard Test Method forEstimating Contribution of Environmental Tobacco Smoketo Respirable Suspended Particles Based on Solanesol1This standard is issued under the fixed designation D 6271; the number immediately following the designation indicates the year oforiginal adoption
2、 or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the sampling/analysis of respi-rable suspended part
3、icles (RSP) and the estimation of the RSPfraction attributable to environmental tobacco smoke (ETS).The test method is based on collection of total RSP on amembrane filter, extraction of the filter in methanol, anddetermination of solanesol, a C45isoprenoid alcohol, by highperformance liquid chromat
4、ography (HPLC) with ultraviolet(UV) detection.1.2 This test method is compatible with the determinationsof gravimetric RSP, ultraviolet particulate matter (UVPM), andfluorescent particulate matter (FPM) (see Test MethodsD 5955), but does not require them. UVPM and FPM, whichare based on the ultravio
5、let absorbance and fluorescence of thefilter extract, are also used to estimate the contribution of ETSto RSP.1.3 The sampling components consist of a 1.0-m pore sizepolytetrafluoroethylene (PTFE) membrane filter in a filtercassette connected on the inlet end to a particle size separatingdevice and,
6、 on the outlet end, to a sampling pump. This testmethod is applicable to personal and area sampling.1.4 This test method is limited in sample duration only bythe capacity of the membrane filter. The test method has beenevaluated up to 24-h sample duration; a minimum sampleduration of1hisrecommended.
7、1.5 Limits of detection (LOD) for this test method at asampling rate of 2 L/min are 0.042 g/m3for 1-h sampleduration and 0.005 g/m3for 8-h sample duration.1.6 The values stated in SI units are to be regarded asstandard.1.7 This standard does not purport to address all the safetyconcerns, if any, ass
8、ociated with its use. It is the responsibilityof the user of this standard to establish appropriate safety andhealth practices and determine the applicability of regulatorylimitations prior to use. Specific precautionary information isgiven in 13.6.2. Referenced Documents2.1 ASTM Standards:2D 1356 T
9、erminology Relating to Sampling and Analysis ofAtmospheresD 1357 Practice for Planning the Sampling of the AmbientAtmosphereD 3631 Test Methods for Measuring Surface AtmosphericPressureD 5337 Practice for Flow Rate for Calibration of PersonalSampling PumpsD 5955 Test Methods for Estimating Contribut
10、ion of Envi-ronmental Tobacco Smoke to Respirable Suspended Par-ticles Based on UVPM and FPM3. Terminology3.1 Definitions: For definitions of terms used in this testmethod, refer to Terminology D 1356.3.2 Definitions of Terms Specific to This Standard:3.2.1 environmental tobacco smoke (ETS)an aged,
11、dilutecomposite of exhaled tobacco smoke (exhaled mainstreamsmoke) and smoke from tobacco products (sidestream smoke).3.2.2 respirable suspended particles (RSP)particleswhich can be deposited in the gas-exchange region of the lungand are defined as particles that pass through a sampler havinga 4.0-m
12、 median cutpoint (1)3.3.2.3 solanesol particulate matter (Sol-PM)a tobacco-selective marker for the contribution of ETS particulate matterto RSP.4. Summary of Test Method4.1 A known volume of air is drawn through an inertialimpactor or cyclone assembly separating at 4.0 m to separaterespirable suspe
13、nded particles (RSP) from total suspendedparticulate matter and then through a filter assembly. Solanesolis collected as a component of RSP on a PTFE membrane filtercontained within the filter assembly.1This test method is under the jurisdiction of ASTM Committee D22 onSampling and Analysis of Atmos
14、pheres and is the direct responsibility of Subcom-mittee D22.05 on Indoor Air.Current edition approved April 1, 2004. Published May 2004. Originallyapproved in 1998. Last previous edition approved in 1998 as D 6271 - 98.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact
15、ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The boldface numbers in parentheses refer to a list of references at the end ofthis standard.1Copyright ASTM International, 100 Barr Harbor
16、Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4.2 Solanesol is extracted from the filter with methanol in a4-mL glass vial.4.3 An aliquot of the extract is injected into an HPLCsystem equipped with a UV detector (205 nm absorbance).4.4 The area of the resulting solanesol peak i
17、s compared toareas obtained from the injection of standard solutions ofsolanesol, and the weight of solanesol is determined.4.5 The concentration of solanesol (g/m3) is calculatedfrom the weight of solanesol and the volume of air sampled. Ifdesired, the concentration of RSP can also be calculatedacc
18、ording to Test Methods D 5955.4.6 The concentration of RSP attributable to ETS, referredto as Sol-PM, is calculated from the airborne concentration ofsolanesol and the experimentally determined weight ratio ofsolanesol to RSP in ETS (2,3,4).5. Significance and Use5.1 Environmental tobacco smoke cons
19、ists of both vaporand particulate phase components. Due to the nature of vaporand particulate phases, they rarely correlate well, and anaccurate assessment of ETS levels in indoor air requiresdetermining good tracers of both phases. Among the attributesof an ideal ETS tracer, one critical characteri
20、stic is that thetracer should “remain in a fairly consistent ratio to theindividual contaminant of interest or category of contaminantsof interest (for example, suspended particulates) under a rangeof environmental conditions.” (5). Solanesol meets this re-quirement, staying in a constant ratio to t
21、he RSP contributed bytobacco smoke over a variety of ventilation conditions andsampling durations (6). UVPM and FPM, which are the tracersor markers employed by Test Methods D 5955, also fulfill thisrequirement. Airborne solanesol, however, is unique in that it isspecific to tobacco smoke and is fou
22、nd only in the particulatephase of ETS. Its high molecular weight and low volatilitymake it extremely unlikely that any solanesol will be lost fromthe membrane filter used for sample collection. Solanesolconstitutes approximately 3 % by weight of the RSP of ETS(2,7,8), making it suitable for measure
23、ment at realistic smokingrates. Of the available ETS particulate phase markers (UVPM,FPM, and solanesol), all are currently used and relied upon, butsolanesol is considered to be a better marker for the particulatephase of ETS and, as a result, provides the best way ofquantifying the contribution of
24、 ETS particulate matter to RSP(3,4,9,10,11,12,13).5.2 To be able to quantify the contribution of ETS to RSPwith a tobacco-specific marker is important because RSP is notspecific to tobacco smoke. RSP is a necessary indicator ofoverall air quality; the Occupational Safety and Health Admin-istration (
25、OSHA) has previously set a PEL (permissible expo-sure level) for respirable dust in the workplace of 5000 g/m3.However, RSP emanates from numerous sources (14) and hasbeen shown to be an inappropriate tracer of ETS (7,15,16,17).UVPM and FPM are used as more selective markers toestimate the contribut
26、ion of tobacco smoke to RSP; however,these markers can overestimate the contribution of tobaccosmoke to RSP due to potential interference from nontobaccocombustion sources. (Refer to Test Methods D 5955 for theprotocol on determining UVPM and FPM.) Although UVPMand FPM are useful in investigations o
27、f indoor air quality,solanesol is a better indicator of the tobacco smoke contribu-tion to RSP. This test method has been used to apportion RSPinto ETS and non-ETS components by determining the weightratio of solanesol to total RSP (2,3,4,7,18,19).6. Interferences6.1 The genus Nicotiana, which inclu
28、des tobacco as one ofits species, is a member of the Solanaceae family of plants.Like tobacco, many plants in this family, particularly thosewhich also contain trace amounts of nicotine, contain solane-sol. Examples are tomato, potato, eggplant, and pepper. Withcooking as the only likely source of i
29、nterference, the potentialfor interference is negligible. However, if there were aninterference of this type, the weight of solanesol would bebiased high and the contribution of ETS to RSP would beoverestimated. It is anticipated that the only measurablecontribution of solanesol to an indoor environ
30、ment wouldcome from tobacco combustion.7. Apparatus7.1 Sample Collection:7.1.1 PTFE Filter, membrane filter with 1.0-m pore sizeand 37mm diameter. The PTFE membrane is bonded to a highdensity polyethylene support net, referred to as the filterbacking, to improve durability and handling ease.7.1.2 Fi
31、lter Sampling Assembly, consists of the PTFE mem-brane filter and a black, opaque, conductive polypropylenefilter cassette in a three-piece configuration with a 0.5-in.spacer ring inserted between the top (inlet) and bottom (outlet)pieces.4The filter cassette holds the PTFE membrane duringsampling.
32、All connections to the filter assembly are made withflexible plastic tubing.7.1.3 Barometer and Thermometer, for taking pressure andtemperature readings at the sampling site.7.1.4 Bubble Flowmeter or Mass Flowmeter, for calibrationof the sampling pump.7.1.5 Personal Sampling Pump, portable constant-
33、flow sam-pling pump calibrated for a flow rate dependent upon theseparating characteristics of the impactor or cyclone in use (see7.1.6).7.1.6 Inertial Impactor or Cyclone, with nominal cutpoint of4.0 m.NOTE 1If alternate definition of RSP is used (see 3.2.2), ensure thatthe impactor or cyclone is c
34、ompatible with this definition.7.1.7 Stopcock Grease, for coating impactor plates.7.2 Analytical System:7.2.1 Liquid Chromatography System, consists of HPLCpump, UV detector with deuterium source lamp, autosampler,column oven (optional), and data acquisition and peak integra-tion system.7.2.2 HPLC C
35、olumn, 250 mm by 3.0-mm ID, reversed-phase C18column (300- pore size; 5-m particle size). C18packing material with low carbon loading has been found to bepreferable.4The three-piece filter cassette (with a spacer ring in the center) is not alwaysneeded. A two-piece filter cassette may be substituted
36、.D62710427.2.3 Guard Cartridge Column, a guard cartridge withpacking material and dimensions compatible with the HPLCcolumn in 7.2.2, placed in front of the analytical column forprotecting and prolonging the life of the column.7.2.4 Sample Containers, low-actinic borosilicate glass au-tosampler vial
37、s, 4-mL capacity, with screw caps and PTFE-lined septa.7.2.5 Filter Forceps, for handling filters.7.2.6 Wrist-action Shaking Device, for solvent extraction.8. Reagents and Materials8.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended tha
38、tall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.5Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the
39、 accuracy ofthe determination.8.2 Acetonitrile, HPLC grade, (CAS No. 75-05-8).8.3 Methanol, HPLC grade, (CAS No. 67-56-1).8.4 Solanesol6, 90+ %, (CAS No. 13190-97-1). (See Note6.)8.5 Helium, 99.995 % grade, (CAS No.7440-59-7), for con-tinuous purging of mobile phase.9. Sampling9.1 Generalfor plannin
40、g sampling programs, refer toPractice D 1357.9.2 Procedure:NOTE 2If a gravimetric determination of RSP is to be performed, thenweigh the filters according to Test Methods D 5955 prior to 9.2.1.9.2.1 Calibrate the personal sampling pump prior to andimmediately after sampling. For calibration, connect
41、 the flow-meter to the inlet of the inertial impactor or cyclone. Measurethe flow with the prepared filter assembly in place between thepump and the impactor or cyclone. Refer to Practice D 5337for standard practice in calibrating personal sampling pumps.9.2.2 Record the barometric pressure and ambi
42、ent tempera-ture.9.2.3 If using a mass flowmeter, record the volumetric flowrate, Q. If using a bubble flowmeter, generate several soap-filmbubbles in the flowmeter and allow them to thoroughly wet thesurface before recording any actual measurements. Measurethe time for a soap-film bubble to travel
43、a known volume witha stopwatch. Obtain five replicate measurements and computethe mean time. Calculate the volumetric flow rate, Q,inaccordance with Eq 1:Q5VR(1)where:Q = pump flow rate, L/min,V = volume measured with flowmeter, L, andR = average time for soap-film bubble to flow a knownvolume (V) i
44、n a flowmeter, min.9.2.4 Adjust the potentiometer on the sampling pump sothat the desired flow rate is obtained.9.2.5 With the filter assembly correctly inserted and posi-tioned between the impactor or cyclone and pump, turn on thepump power switch to begin sampling; record the start time.NOTE 3Most
45、 pumps have microprocessing capabilities or built-inelapsed time meters, or both, for preset sampling periods.9.2.6 Record the temperature and barometric pressure of theatmosphere being sampled.9.2.7 Acquire samples at the required flow rate for aminimum sampling period of 1 h. Turn off the pump at
46、the endof the desired sampling period and record the time elapsedduring sample collection.9.2.8 Recheck the flow rate of the pump again after sam-pling and use the average flow rate (mean of before and aftersampling) in later calculations.9.2.9 Immediately remove the filter assembly from thesampling
47、 system and seal the filter cassette with plugs pro-vided.9.2.10 Treat a minimum of two filter assemblies in the samemanner as the samples (remove plugs, measure flow, replaceplugs, and transport). Label and process these filters as fieldblanks.9.2.11 Store all used filter assemblies in a freezer or
48、 underdry ice and transport frozen to the laboratory for analysis.NOTE 4If the samples are not prepared and analyzed immediately,then store them at 0C or less. Analyze all the filters within six weeks aftersample collection. It has been established that samples are stable for atleast six weeks at -1
49、0C storage conditions (20).10. Analysis10.1 System Description:10.1.1 Perform analysis using an HPLC system equippedwith a UV detector at a wavelength setting of 205 nm.NOTE 5A UV detector with a deuterium source is required. A detectorwith a xenon source is not acceptable because of insufficient lamp energyat 205 nm.10.1.2 The HPLC column and guard column are as listed in7.2.2 and 7.2.3.10.1.3 The mobile phase consists of 95:5 (v/v) acetonitrile:methanol.10.1.4 Use helium for the continuous purging of the mobilephase.10.1.5 Pump flow is 0.5 mL/min.10.1.6 Injecti
