1、Designation: D6271 10 (Reapproved 2016)Standard Test Method forEstimating Contribution of Environmental Tobacco Smoketo Respirable Suspended Particles Based on Solanesol1This standard is issued under the fixed designation D6271; the number immediately following the designation indicates the year ofo
2、riginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the sampling/analysis of respi-rable
3、 suspended particles (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
4、 liquid chromatography (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 MethodsD5955), but does not require them. UVPM and FPM, whichare based o
5、n the ultraviolet 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 separat
6、ingdevice and, 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 of1h
7、isrecommended.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. No other units of measurement are included in thisstandard.1.7 Thi
8、s standard does not purport to address all the safetyconcerns, if any, associated 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 infor
9、mation isgiven in 13.6.2. Referenced Documents2.1 ASTM Standards:2D1356 Terminology Relating to Sampling and Analysis ofAtmospheresD1357 Practice for Planning the Sampling of the AmbientAtmosphereD3631 Test Methods for Measuring Surface AtmosphericPressureD5337 Practice for Flow Rate Adjustment of P
10、ersonal Sam-pling PumpsD5955 Test Methods for Estimating Contribution of Envi-ronmental Tobacco Smoke to Respirable Suspended Par-ticles Based on UVPM and FPM3. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, refer to Terminology D1356.3.2 Definitions of Terms Specific to
11、 This Standard:3.2.1 environmental tobacco smoke (ETS)an aged, dilutecomposite of exhaled tobacco smoke (exhaled mainstreamsmoke) and smoke from tobacco products (sidestream smoke).3.2.2 respirable suspended particles (RSP)particles whichcan be deposited in the gas-exchange region of the lung and ar
12、edefined as particles that pass through a sampler having a4.0-m median cutpoint (1).33.2.3 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 c
13、yclone assembly separating at 4.0 m to separate1This test method is under the jurisdiction of ASTM Committee D22 on AirQuality and is the direct responsibility of Subcommittee D22.05 on Indoor Air.Current edition approved March 1, 2016. Published March 2016. Originallyapproved in 1998. Last previous
14、 edition approved in 2010 as D6271 10. DOI:10.1520/D6271-10R16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM websit
15、e.3The boldface numbers in parentheses refer to a list of references at the end ofthis standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1respirable suspended particles (RSP) from total suspendedparticulate matter and then throu
16、gh a filter assembly. Solanesolis collected as a component of RSP on a PTFE membrane filtercontained within the filter assembly.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 n
17、m absorbance).4.4 The area of the resulting solanesol peak is 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. I
18、fdesired, the concentration of RSP can also be calculatedaccording to Test Methods D5955.4.6 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 (2-4).5.
19、 Significance and Use5.1 Environmental tobacco smoke consists 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
20、attributesof an ideal ETS tracer, one critical characteristic 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
21、meets thisrequirement, staying in a constant ratio to the RSP contributedby tobacco smoke over a variety of ventilation conditions andsampling durations (6). UVPM and FPM, which are the tracersor markers employed by Test Methods D5955, also fulfill thisrequirement.Airborne solanesol, however, is uni
22、que in that it isspecific to tobacco smoke and is found 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
23、the RSP of ETS(2,7,8), making it suitable for measurement 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, pr
24、ovides the best way ofquantifying the contribution of ETS particulate matter to RSP(3, 4, 9-13).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 Oc
25、cupational Safety and Health Admin-istration (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, 15-17).UVPM and FPM are used as mor
26、e selective markers toestimate the contribution 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 D5955 for theprotocol on determining UVPM and FPM.) Although
27、 UVPMand FPM are useful in investigations of 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 (2-4, 7, 18, 19).6. Inter
28、ferences6.1 The genus Nicotiana, which includes 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 so-lanesol. Examples are tomato, potato, eggplant, and pepper
29、.With cooking as the only likely source of interference, thepotential for interference is negligible. However, if there werean interference 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 measurableco
30、ntribution of solanesol to an indoor environment 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 i
31、mprove durability and handling ease.7.1.2 Filter Sampling Assembly, consists of the PTFE mem-brane filter and a black, opaque, conductive polypropylenefilter cassette in a three-piece configuration with a 1.3-cmspacer ring inserted between the top (inlet) and bottom (outlet)pieces.4The filter casset
32、te holds the PTFE membrane duringsampling. 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
33、 Personal Sampling Pump, portable constant-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.
34、2), ensure thatthe impactor or cyclone is compatible with this definition.7.1.7 Stopcock Grease, for coating impactor plates.7.2 Analytical System:4The three-piece filter cassette (with a spacer ring in the center) is not alwaysneeded. A two-piece filter cassette may be substituted.D6271 10 (2016)27
35、.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 Column, 250 mm by 3.0-mm ID, reversed-phase C18column (30-nm pore size; 5-m particle size). C18packing mat
36、erial with low carbon loading has been found to bepreferable.7.2.3 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 Containe
37、rs, low-actinic borosilicate glass au-tosampler vials, 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 t
38、ests. Unless otherwise indicated, it is intended thatall 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 sufficientl
39、yhigh purity to permit its use without lessening the 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 Solanesol, 90+ %, (CAS No. 13190-97-1).8.5 Helium, 99.995 % grade, (CAS No.7440-59-7), for con-tinuous purging of mobile p
40、hase.9. Sampling9.1 Generalfor planning sampling programs, refer toPractice D1357.9.2 Procedure:NOTE 2If a gravimetric determination of RSP is to be performed, thenweigh the filters according to Test Methods D5955 prior to 9.2.1.9.2.1 Calibrate the personal sampling pump prior to andimmediately afte
41、r sampling. For calibration, connect 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 D5337 forstandard practice in calibrating personal sampling pumps.9.2.2 Reco
42、rd the barometric pressure and ambient 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 tim
43、e for a soap-film bubble to travel a known volume witha stopwatch. Obtain five replicate measurements and computethe mean time. Calculate the volumetric flow rate, Q,inaccordance with Eq 1:Q 5VR(1)where:Q = pump flow rate, L/min,V = volume measured with flowmeter, L, andR = average time for soap-fil
44、m bubble to flow a knownvolume (V) in 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 sampli
45、ng; record the start time.NOTE 3Most 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
46、period of 1 h. Turn off the pump at 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
47、the filter assembly from thesampling 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 us
48、ed filter assemblies in a freezer or 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
49、 stable for atleast six weeks at -10C 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 5AUV detector with a deuterium source is required.Adetectorwith 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 Pu
