1、Designation: D 4600 95 (Reapproved 2005)Standard Test Method forDetermination of Benzene-Soluble Particulate Matter inWorkplace Atmospheres1This standard is issued under the fixed designation D 4600; the number immediately following the designation indicates the year oforiginal adoption or, in the c
2、ase 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 describes the sampling and gravimetricdetermination of benzene-soluble
3、particulate matter that hasbecome airborne as a result of certain industrial processes. Thistest method can be used to determine the total weight ofbenzene-soluble materials and to provide a sample that may beused for specific and detailed analyses of the soluble compo-nents.1.2 The limit of detecti
4、on is 0.05 mg/m3by sampling a 1-m3volume of air.NOTE 1Other volatile organic solvents have been used for thisdetermination and whereas a less toxic solvent for this analysis might bedesirable, the substitution of a solvent other than benzene is unwise at thistime. A tremendous volume of environmenta
5、l sampling data based onbenzene-soluble determinations has been accumulated over many years inseveral industries.2Some of the determinations have been used inepidemiological studies. Furthermore, the use of benzene is specified inexisting federal standards.3As a result, it appears imprudent to use a
6、different solvent until the qualitative and quantitative relationship ofanalyses derived from benzene and a substitute solvent is established.With proper care, benzene can be safely used in the laboratory.1.3 This standard does not purport to address all of thesafety concerns, if any, associated wit
7、h its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:4D 1356 Terminology Relating to Sampling and Analysis ofAtmospheres3
8、. Terminology3.1 Definitions:3.1.1 For definitions of terms used in this test method, referto Terminology D 1356.4. Summary of Test Method4.1 By the use of a personal sampling pump, air is pulledthrough a glass-fiber filter held in a sampling cassette. The filteris extracted ultrasonically with benz
9、ene. After filtration, analiquot of the total extract is evaporated to dryness and theresidue weighed.5. Significance and Use5.1 This test method provides a means of evaluating expo-sures to benzene-soluble particulate matter in a concentrationrange that can be related to occupational exposures.6. I
10、nterferences6.1 This test method is, by definition, free of interferences.However, this test method is nonspecific. It supplies noinformation on the composition of the soluble material. Itmeasures all those substances in the sample that are soluble inbenzene. The composition must be determined by so
11、me inde-pendent means.6.2 The greatest errors most likely to be incurred in the useof this test method are associated with the sample collection orhigh blanks from solvent and filter. Avoid contamination fromextraneous material by using high-purity solvents for the finalcleaning of all apparatus. Th
12、e use of plastic containers otherthan TFE-fluorocarbon for any organic solvent is unacceptable,and the evaporation step should be conducted in a clean hood.7. Apparatus7.1 Personal Sampling Pumps, any pump capable of sam-pling at a calibration rate of about 2 L/min for 8 h.7.2 Glass-Fiber Filters, 3
13、7-mm, free of organic binder, heldin a two- or three-piece polystyrene cassette having a rigidfilter support. Filters should be pre-extracted or preheated at400C for a minimum of 1 h.1This test method is under the jurisdiction of ASTM Committee D22 on AirQuality and is the direct responsibility of S
14、ubcommittee D22.04 on WorkplaceAtmospheres.Current edition approved Oct. 1, 2005. Published January 2006. Originallyapproved in 1986. Last previous edition approved in 2000 as D 4600 - 95(2000)e1.2“Benzene-Soluble Compounds in Air, P Gelman Acrodisc CR disposable syringefilter (0.45 to 1.0 m pore si
15、ze) attached toa5to10-mLsyringe having a Luer tip; or other equivalent suitable media.NOTE 2When using a disposable syringe filter, prewash with 10 mLof acetonitrile.NOTE 3Placing a pre-extracted filter (37-mm glass fiber) ahead of thefritted glass in the Allihn tube will increase the life of the fr
16、it.7.6 Microbalance, capable of weighing to 1 g. (If entiresample is to be used for the benzene-soluble determination, afive-place balance is acceptable.)7.7 Weighing Cups, aluminum or TFE-fluorocarbon of suit-able capacity with a weight not to exceed 500 mg.7.8 Vacuum Oven.8. Reagent8.1 BenzeneThe
17、benzene used should be of sufficientpurity so that the residue weight following evaporation of 5 mLof the solvent is less than 10 g.9. Safety Precautions9.1 To minimize the exposure hazard to benzene, analystsshould avoid inhalation of solvent vapors and, if indicated, bemonitored to determine the m
18、agnitude of their exposures.Transfer and evaporation of the solvent should be carried out ina properly ventilated fume hood (150-fpm face velocity).Protective gloves should be used to minimize the possibility ofabsorbing benzene through the skin.9.2 The extract must be handled with proper caution be
19、-cause some polycyclic aromatic hydrocarbons are potentialcarcinogens.10. Sampling10.1 Place the cassette assembly, in the closed face mode, inthe breathing zone of the employee and for the entire shift,draw air through the filter using a calibrated sampling pump.The pump should be operated at a rat
20、e of about 2 L/min andshould be checked periodically to ensure maintenance of thisrate.10.2 Upon completion of sampling, seal the cassette withthe plugs provided and send it to the laboratory for analysis.The cassette must be protected from exposure to heat and light.To minimize deterioration of sam
21、ples prior to analysis, theymay be stored in a freezer.10.3 Field blanks are treated in the same manner as samples.They are opened in the environment to be sampled andimmediately closed and placed with the samples to be sent tothe laboratory for analysis. An unopened, unused cassetteassembly is used
22、 as a laboratory blank. At least one laboratoryblank and one field blank should be submitted with each set ofsamples collected.11. Calibration and Standardization11.1 No standards are required for this test method.12. Procedure12.1 Remove the filter from the cassette and, using forceps,insert into t
23、he extraction vessel. Treat the blanks in the samemanner as the samples.12.2 Pipet 5.0 mLof benzene into the extraction vessel. Sealimmediately with a TFE-fluorocarbon-lined cap if an aliquot ofthe sample is to be used for analysis.12.3 Place the extraction vessel in the ultrasonic bath for 5min and
24、 then allow the vessel to stand for 30 min. If the entiresample is to be used for the benzene-soluble determination,proceed to 12.8.12.4 Decant the solution into the filter vessel. Immediatelypressure or vacuum filter the solution through the filter into aclean, dry collection vessel. The entire 5-m
25、L volume ofbenzene solution need not be recovered; however, evaporationlosses must be minimized. On completion of filtration, seal thevessel immediately.12.5 Weigh the weighing cup to the nearest microgram onthe microbalance. Store the weighed cup in a covered glasspetri dish.12.6 Pipet an aliquot n
26、o less than 0.5 mL of the solutionfrom 12.4 into the tared weighing cup. Evaporate the solvent ina preheated vacuum oven at 40C and 26.66 kPa and continuedrying for a total of 3 h.NOTE 4It is recommended to air evaporate benzene to dryness undera hood before transferring to the preheated vacuum oven
27、. This willminimize benzene exposures in the laboratory.12.7 After cooling, reweigh the cup against the same tareused in 12.5. The difference between the weight obtained andthe tare obtained in 12.5 is the residue weight for the aliquot.12.8 When entire sample is to be used for the benzene-soluble d
28、etermination, decant the solution into the filteringvessel. Pressure filter the solution into a preweighed (60.01mg) 50-mL beaker. Rinse filtration apparatus with three 1-mLwashes of benzene, directly into the beaker.12.9 Evaporate the solvent in a preheated vacuum oven at40C and 26.66 kPa and conti
29、nue drying for a total of 3 h.Reweigh the beaker after cooling. The difference between thefinal weight and the tare weight of the beaker is the residueweight of the sample.13. Calculation13.1 Calculate the air concentration of soluble particulateorganic matter as follows:C 5A 2 B!V5F(1)where:C = con
30、centration, mg/m3,A = residue weight of sample, mg,B = residue weight of blank, mg,V = volume of air sample, m3, andF = volume of aliquot, mL.D 4600 95 (2005)214. Precision and Bias514.1 Precision, Repeatability (Both Single Analyst andOverall)A high-volume air sample was collected on a filterat a c
31、oke oven battery and extracted with benzene. The extractwas used to generate four levels of benzene soluble material:0.09, 0.18, 0.36, and 0.72 mg/sample. Each concentration wasanalyzed in triplicate by nine participating laboratories. Thesingle operator relative standard deviation (RSD) varied from
32、25 % to 5 % with a pooled relative standard deviation of 13 %.The overall relative standard deviation for the nine laboratoriesvaried from 47 % to 10 % with a pooled RSD of 32 %.14.2 BiasThe bias of this method has not been determinedbecause the reference values were established by the methoditself.
33、15. Keywords15.1 air monitoring; benzene-soluble particulate matter;coal tar pitch volatiles; sampling and analysis; workplaceatmospheresASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this sta
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36、which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-295
37、9,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).5Supporting data are available on loan from ASTM Headquarters, 100 BarrHarbor Drive, PO Box C700, West Conshohocken, PA 194282959. Request RR:D22-1016.D 4600 95 (2005)3
