1、BRITISH STANDARD BS ISO 16362:2005 Ambient air Determination of particle-phase polycyclic aromatic hydrocarbons by high performance liquid chromatography ICS 13.040.01 BS ISO 16362:2005 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 10 March
2、 2005 BSI 10 March 2005 ISBN 0 580 45593 9 National foreword This British Standard reproduces verbatim ISO 16362:2005 and implements it as the UK national standard. The UK participation in its preparation was entrusted by Technical Committee EH/2, Air quality, to Subcommittee EH/2/3, Ambient atmosph
3、eres, which has the responsibility to: A list of organizations represented on this subcommittee can be obtained on request to its secretary. Cross-references The British Standards which implement international publications referred to in this document may be found in the BSI Catalogue under the sect
4、ion entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. C
5、ompliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor rel
6、ated international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to v, a blank page, pages 1 to 27 and a back cover. The BSI copyright notice displayed in this document indicates wh
7、en the document was last issued. Amendments issued since publication Amd. No. Date Comments Reference number ISO 16362:2005(E) OSI 5002INTERNATIONAL STANDARD ISO 16362 First edition 2005-02-15 Ambient air Determination of particle- phase polycyclic aromatic hydrocarbons by high performance liquid ch
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13、mail coirypthgiso.o gr We bwww.is.o gro Pulbisdehi n Switlrez dnaii ISO 5002 Allr ithgsr esedevrBSISO16362:2005IS:26361 O5002(E) I SO 5002 All irthgs ersedevr iiiContents Page Foreword iv Introduction v 1 Scope 1 2 Terms and definitions. 1 3 Symbols and abbreviated terms 2 3.1 Symbols . 2 3.2 Abbrev
14、iated terms. 2 4 Principle of the procedure 2 5 Reagents, apparatus and materials 2 6 Measurement procedure 5 6.1 Sampling 5 6.2 Sample preparation. 5 6.3 HPLC analysis . 6 7 Establishment of the calibration function and verification of the measurement values. 6 7.1 Identification 6 7.2 Instrument c
15、alibration 7 7.3 Determination of response factors and quantification . 7 7.4 Determination of the extraction efficiency . 9 8 Calculation of the result . 9 9 Performance characteristics 9 9.1 Standard deviations of the overall measurement procedure. 9 9.2 Detection limits . 9 10 Interferences 11 11
16、 Quality assurance . 11 12 Test report 12 Annex A (informative) General information . 13 Annex B (informative) Examples of operation parameters for HPLC analysis with FLD and DAD in series 14 Annex C (informative) Extraction efficiencies for some PAH compounds. 17 Annex D (informative) Results of du
17、plicate measurements. 18 Annex E (informative) Comparison measurements and invariance test of the PAH profiles. 20 Annex F (informative) Physical constants of PAHs 21 Annex G (informative) List of HPLC columns 25 Bibliography . 26 BSISO16362:2005IS:26361 O5002(E) iv I SO 5002 All irthgs ersedevrFore
18、word ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a techn
19、ical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
20、electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to
21、 the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for
22、identifying any or all such patent rights. ISO 16362 was prepared by Technical Committee ISO/TC 146, Air quality, Subcommittee SC 3, Ambient atmospheres. BSISO16362:2005IS:26361 O5002(E) I SO 5002 All irthgs ersedevr vIntroduction Several polycyclic aromatic hydrocarbons (PAHs) are considered to be
23、potential human carcinogens. PAHs are emitted into the atmosphere primarily through combustion of fossil fuel and wood. Two- and three-ring PAHs are typically present in urban air at concentrations ranging from ten to several hundred nanograms per cubic metre (ng/m 3 ); those with four or more rings
24、 are usually found at concentrations of a few nanograms per cubic metre or lower. PAHs possess saturation vapour pressures at 25 C that range from 10 2kPa to less than 10 13kPa. Those with vapour pressures above 10 8kPa may be substantially distributed between the gas phase and particle-associated (
25、particulate) phase in the atmosphere. The distribution between phases depends on ambient temperature, humidity, types and concentrations of PAHs and particulate matter, and residence time in the air. PAHs, especially those having vapour pressures above 10 8kPa, tend to vaporize from particle filters
26、 during sampling. This International Standard allows the determination of low volatility, particle-bound PAHs, in contrast to ISO 12884 1which allows the measurement of PAHs in the gas phase. This International Standard allows the use of a range of sampler flowrates, and requires the use of high per
27、formance liquid chromatography (HPLC) with the detection carried out by either fluorescence detection or UV absorption. BSISO16362:2005blank 5002:26361OSISBINTENRATIONAL TSANDADR IS:26361 O5002(E)I SO 5002 All irthgs ersedevr 1Ambient air Determination of particle-phase polycyclic aromatic hydrocarb
28、ons by high performance liquid chromatography 1 Scope This International Standard specifies sampling, clean-up and analysis procedures for the quantitative determination of low volatility (particle-bound) polycyclic aromatic hydrocarbons (PAHs) in ambient air. For sampling, a low-volume or a medium/
29、high-volume sampling device may be used. Sampling times between 1 h and 24 h are possible. The sampling volume flowrates can range from 1 m 3 /h to 4 m 3 /h (“low volume sampler”) or from 10 m 3 /h to about 90 m 3 /h (“medium/high-volume sampler”). In any case, the linear face velocity at the collec
30、tion filter should range between about 0,5 m/s and 0,9 m/s. The method has been validated for sampling periods up to 24 h. The detection limits for single PAHs and the standard deviations resulting from duplicate measurements are listed in 9.2 and Annex D respectively. This International Standard de
31、scribes a sampling and analysis procedure for PAH that involves collection from air onto a filter followed by analysis using high performance liquid chromatography usually with fluorescence detector (FLD). The use of a diode array detector (DAD) is possible. The combination of both detector types is
32、 also possible (see Annex B). Total suspended particulate matter is sampled. Generally, compounds having a boiling point above 430 C (vapour pressure less than 10 9kPa at 25 C, e.g. chrysene, benzaanthracene) can be collected efficiently on the filter at low ambient temperatures (e.g. below 10 C). I
33、n contrast, at higher temperatures (above 30 C, see also ISO 12884 1 ), only PAHs having boiling points above 475 C (vapour pressure less than 10 10kPa at 25 C) are determined quantitatively (see Annex F). 2 Terms and definitions For the purposes of this document, the following terms and definitions
34、 apply. 2.1 blank value solution solution which contains the chemicals used in making up the sample solution batch and the constituents influencing the measurement in the same or similar concentration as the sample to be analysed, but to which the compound to be determined has expressly not been add
35、ed 2.2 low-volume sampling device sampling device with a volume flowrate of 1 m 3 /h to 4 m 3 /h 2.3 medium/high-volume sampling device sampling device with a volume flowrate of 10 m 3 /h to about 90 m 3 /h BSISO16362:2005IS:26361 O5002(E) 2 I SO 5002 All irthgs ersedevr3 Symbols and abbreviated ter
36、ms 3.1 Symbols A ipeak area of component i A ISpeak area of internal standard mass concentration f response factors, slope of straight line m imass of component i m ISmass of internal standard M rrelative molecular mass (molecular weight) V volume 3.2 Abbreviated terms ASE accelerated solvent extrac
37、tion b.p. boiling point DAD diode array detector (UV absorption) FLD fluorescence detector HPLC high performance liquid chromatography PAH polycyclic aromatic hydrocarbon SOP standard operating procedure UV ultraviolet WHO World Health Organization 4 Principle of the procedure For sampling, sampling
38、 devices with volume flowrates from 1 m 3 /h to about 90 m 3 /h may be used. The particulate matter, onto which the PAHs are adsorbed, is collected on glass or quartz fibre filters. The PAHs are extracted and the extract concentrated. If necessary, the extracts may be cleaned by column chromatograph
39、y using silica gel. The PAHs are determined by HPLC using DAD or FLD. For quality assurance, internal standards are added. 5 Reagents, apparatus and materials 5.1 Reagents 5.1.1 Solvents for analysis: water, acetonitrile, toluene (all solvents of chromatographic grade). BSISO16362:2005IS:26361 O5002
40、(E) I SO 5002 All irthgs ersedevr 35.1.2 Solvents for sample preparation: chromatographic grade toluene, cyclohexane and acetonitrile. The chromatograms of the solvents obtained under the conditions of the illustrative example shall not exhibit any interfering peaks. 5.1.3 Helium, purity 99,999 %; f
41、or degasification of solvents. To avoid interferences, no plastic hoses shall be employed, preferably metal hoses are recommended. 5.1.4 Internal standard If using DAD: indeno1,2,3-cdfluoranthene dissolved in toluene, mass concentration e.g. 3 g/ml (see 6.2). If using FLD: 6-methylchrysene. 5.1.5 Ca
42、libration standards Cyclopentac,dpyrene CPP Benzaanthracene BaA Chrysene CHR Benzobfluoranthene BbF Benzojfluoranthene BjF Benzokfluoranthene BkF Benzoapyrene BaP Benzoepyrene BeP Indeno1,2,3-cdpyrene INP Dibenza,hanthracene DBahA Dibenza,canthracene DBacA Benzog,h,iperylene BghiP Anthanthrene ANT C
43、oronene COR Dibenzoa,lpyrene DBalP Dibenzoa,ipyrene DBaiP Dibenzoa,epyrene DBaeP Dibenzoa,hpyrene DBahP Benzoachrysene (= picene) BaC 5.2 Apparatus 5.2.1 Sampling device, consisting of the following parts (commercially available). 5.2.1.1 Sampling head, usually containing the filter. BSISO16362:2005
44、IS:26361 O5002(E) 4 I SO 5002 All irthgs ersedevr5.2.1.2 Pumping system, e.g. sliding vane-pump or turbine. 5.2.1.3 Volume meter, for measuring the sample volume or a flowrate-measuring device. 5.2.1.4 Electronic or mechanical device, to establish a constant flow. 5.2.1.5 Timer, for selecting the ti
45、me and duration of the sampling. 5.2.1.6 Blunt tweezers (optional), for handling the filters. 5.2.2 Sample preparation equipment The PAH extraction (see 7.2) is carried out using ordinary laboratory equipment. This may include: 5.2.2.1 Flasks/reflux condenser, round-bottomed flask (e.g. 250 ml, or 1
46、00 ml if the small filter device is used) with matched reflux condenser and heating bath, or 5.2.2.2 Ultrasonic bath, beaker, capacity e.g. 50 ml or 100 ml, or 5.2.2.3 Soxhlet extractor, capacity e.g. 30 ml to 50 ml, cellulose extraction thimble, round-bottomed flask (100 ml) with reflux condenser a
47、nd heating bath, or 5.2.2.4 ASE apparatus, device for extracting samples at elevated temperatures and under high pressure. 5.2.2.5 Vacuum pump, e.g. a membrane or water-jet pump. 5.2.2.6 Centrifuge, with inserts; e.g. of volume 20 ml each. 5.2.2.7 Chromatography column, internal diameter e.g. 10 mm,
48、 length 230 mm (silica gel column). 5.2.3 Analytical apparatus 5.2.3.1 High performance liquid chromatograph, fitted with an isothermal column device, solvent purge system, gradient pump system and a FLD or DAD. 5.2.3.2 Separation columns, reverse phase-sorbent columns optimized for PAH analysis (se
49、e Annex G). 5.2.3.3 Recording equipment, work station with screen and printer/plotter for acquiring, processing, storing and interpreting the data and the possibility of a later baseline correction. 5.2.3.4 GC microliter syringes, suitable for metering aliquots. 5.3 Materials 5.3.1 Collection filter, glass or quartz fibre filters, collection efficiency better than 99,9 % for particles 0,5 m in diame
