BS EN ISO 22892-2011 Soil quality Guidelines for the identification of target compounds by gas chromatography and mass spectrometry《土质 用气相色谱法和质谱法对靶子化合物识别的指南》.pdf

1、Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 24/11/2011 06:42, Uncontrolled Copy, (c) BSIg49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58c

2、ompounds by gas chromatography and mass spectrometryICS 13.080.05Soil quality Guidelines for the identification of target BRITISH STANDARDBS EN ISO22892:2011National forewordThis British Standard is the UK implementation of EN ISO 22892:2011. It is identical to ISO 22892:2006. It supersedes BS ISO 2

3、2892:2006, which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee EH/4, Soil quality.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of

4、 a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunity from legal obligations.BS EN ISO 22892:2011This British Standard was published under the authority of the Standards Policy and Strategy Committee on 28 April 2006 BSI 2011Amendmen

5、ts/corrigenda issued since publicationDate Comments 31 August 2011 This corrigendum renumbers BS ISO 22892:2006 as BS EN ISO 22892:2011ISBN 978 0 580 73160 0Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 24/11/2011 06:42, Uncontrolled Copy, (c) BSIEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE

6、 NORM EN ISO 22892 June 2011 ICS 13.080.05 English Version Soil quality - Guidelines for the identification of target compounds by gas chromatography and mass spectrometry (ISO 22892:2006) Qualit du sol - Lignes directrices pour lidentification de composs cibles par chromatographie en phase gazeuse

7、et spectromtrie de masse (ISO 22892:2006) Bodenbeschaffenheit - Anleitungen fr die Identifizierung von Zielverbindungen durch Gaschromatographie und Massenspektrometrie (ISO 22892:2006) This European Standard was approved by CEN on 10 June 2011. CEN members are bound to comply with the CEN/CENELEC I

8、nternal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to

9、any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official

10、 versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovaki

11、a, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitation in any form and by any means reserved worldwide fo

12、r CEN national Members. Ref. No. EN ISO 22892:2011: ELicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 24/11/2011 06:42, Uncontrolled Copy, (c) BSIForeword The text of ISO 22892:2006 has been prepared by Technical Committee ISO/TC 190 “Soil quality” of the International Organization for Standar

13、dization (ISO) and has been taken over as EN ISO 22892:2011 by Technical Committee CEN/TC 345 “Characterization of soils” the secretariat of which is held by NEN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at

14、 the latest by December 2011, and conflicting national standards shall be withdrawn at the latest by December 2011. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying a

15、ny or all such patent rights. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Gre

16、ece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 22892:2006 has been approved by CEN as a EN ISO 22892:2011 without an

17、y modification. BS EN ISO 22892:2011EN ISO 22892:2011 (E)iiLicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 24/11/2011 06:42, Uncontrolled Copy, (c) BSIiiiContents Page Foreword iv Introduction v 1 Scope . 1 2 Principle. 1 3 Terms and definitions. 1 4 Apparatus 2 5 Procedure 3 5.1 Retention ti

18、mes . 3 5.2 Mass spectra, selection of diagnostic ions . 3 6 Qualification 4 6.1 GC-MS procedure . 4 6.2 Additional information 5 6.3 Reporting the presence of target compounds. 7 6.3.1 Identification 7 6.3.2 Indication . 8 6.3.3 Absence of the target compound ( 3 Absence of any other ions in full s

19、can 1 Diagnostic ions in full scan S/N 3 Column with other polarity a 1 GC-criterion (extra retention time value) Isotope dilution 1 Component spike/standard addition 1 Chromatographic pattern 1 i.e. PCB, PAH, dioxins Other analytical techniques 1 Every other selective detector (i.e. ECD) or techniq

20、ue (i.e. LC) GC-MS (EI and CI; positive/negative) 3 1 (EI) + 2 (CI) GC-MS-MS 4 1 precursor and 2 daughters (product ion) HR-MS (high resolution MS) 2 Every ion S/N 3 Expectation, plausibility, earlier investigations 1 See 6.2 NOTE More examples with different techniques are found in Reference 1. aNo

21、t valid for non-separated compounds (isomers) with the same mass (chrysene/triphenylene, m/p-xylene).6.2 Additional information Interpretation of environmental data is always a combination of data analyses, knowledge about the origin of the sample, knowledge on the behaviour of contaminants and proc

22、esses that occur or may occur. This is also true for the interpretation of GC-MS analysis. As stated, a component is identified if 3 identification points are obtained. If only 1 or 2 diagnostic ions are present, additional identification points are necessary. In this International Standard, gatheri

23、ng additional identification points using analytical procedures is part of Step 2. Using information about the sample, and interpretation of this information, takes place in Step 3. An extra identification point is obtained if one or more of the following criteria is fulfilled. NOTE Strictly taken,

24、an identification point obtained in Step 3 is of another order than the identification points obtained in Step 1 and Step 2. They are obtained by interpretation of additional non-analytical information. In this International Standard, the term “identification point“ (3.7) is used for the points obta

25、ined in all three steps. Step 2: Gathering identification points using analytical procedures. No other ions are visible in full scan mode and this is in agreement with the mass spectrum of the pure component (for instance, PAH). Identification is in agreement with the chromatographic pattern normall

26、y present or present on that site (for instance, PCB or PAH). For volatile compounds, the specificity of the mass fragments in combination with their retention time will generally be sufficient. Their volatility corresponds to a low molecular mass, limiting the number of possible false positive resu

27、lts: there are no low molecular mass compounds with the same retention time on a GC column and also having similar mass spectra. Step 3: Gathering additional identification points using knowledge and interpretation of this knowledge about the sample or sampling site. If identification points are obt

28、ained using Step 3, this shall be reported. The component is identified in earlier samples from the same site (for instance, if the sample under investigation has a low concentration and one or two diagnostic ions have S/N 3 bOnly allowed if the missing ion has the smallest intensity and S/N 3) 1 id

29、entification point Column with other polarity (Step 1) 1 identification point Expected value 1 identification point EXAMPLE 3 Identification with GC-MS and additional evidence (only 1 diagnostic ion, for instance PAH). Diagnostic ion with S/N 3 is present 1 identification point Pattern of PAH recogn

30、ized 1 identification point Result of LC-FLD 1 identification point BS EN ISO 22892:2011EN ISO 22892:2011 (E)Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 24/11/2011 06:42, Uncontrolled Copy, (c) BSI8 6.3.2 Indication There is an indication for the presence of the analysed target compound i

31、n the sample if: Step 1 The criteria given in 6.3.1 Step 1 are met. Step 2 and Step 3 Only one or two identification points are obtained. At least one must be based on the GC-MS data. 6.3.3 Absence of the target compound ( detection limit) The target compound is absent in the sample (not identified

32、and no indication for its presence), if: Step 1 The criteria given in 6.3.1 Step 1 are not met. Step 2 The criteria given in 6.3.1 Step 1 are met and no identification points are obtained with MS, providing the proper GC-MS conditions have been used. 7 Test report The test report in addition to the

33、specifications given in the analytical International Standard, shall contain the following information: a) a reference to this International Standard, i.e. “ISO 22892:2006“; b) complete identification of the sample; c) the results of the identification procedure, i.e. identification, indication or a

34、bsence as performed according to 6.3 of this International Standard; d) the source of the additional non-analytical identification points (Step 3) which have been used; e) any details not specified in this International Standard or which are optional, as well as any factor, which may have affected t

35、he results. BS EN ISO 22892:2011EN ISO 22892:2011 (E)Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 24/11/2011 06:42, Uncontrolled Copy, (c) BSI9Annex A (informative) Diagnostic ions to be used for identification using GC-MS Table A.1 gives a list of recommended diagnostic ions. The relative

36、 intensities are given in parentheses when ion trap detection is used. These ratios depend on the equipment used and can only be used as an indication. Therefore the ratios are to be determined on each single machine by the user. The precision of the masses used depends on the equipment, and more di

37、gits can be necessary. Table A.1 List of recommended diagnostic ions Compound CAS RN aDiagnostic ion 1m/z Diagnostic ion 2 m/z Diagnostic ion 3 bm/z Volatile compounds MTBE 1634-04-4 73 (100) 57 (9 ) TAME 994-05-08 73 (100) 55 (24) 87 (23) Dichloromethane 75-09-2 84 (33) 86 (7) 49 (100) Dichlorodifl

38、uoromethane 75-01-04 85 (100) 87 (31) Vinylchloride 75-71-8 62 (100) 64 (32) 1,1-Dichloroethane 75-34-3 63 (100) 65 (36) 83 (25) 1,2-Dichloroethane 107-06-2 62 (100) 64 (34) 98 (8) 1,1-Dichloroethene 75-35-4 96 (75) 98 (45) 61(100) Z-1,2-Dichloroethene 156-59-2 96 (91) 98 (63) 61 (100) E-1,2-Dichlor

39、oethene 156-60-5 96 (94) 98 (63) 61 (100) 1,1-Dichloropropane 78-99-9 77 (100) 79 (33) 78 (10) 1,2-Dichloropropane 78-87-5 62 (85) 63 (76) 76 (100) 1,3-Dichloropropane 142-28-9 76 (100) 78 (33) 63 (7) 2,2-Dichloropropane 594-20-7 77 (100) 79 (33) 97 (27) 1,1-Dichloropropene 563-58-6 75 (100) 110 (45

40、) 77 (31) Z-1,3-Dichloropropene 10061-01-5 75 (100) 110 (7) 77 (36) E-1,3-Dichloropropene 10061-02-6 75 (100) 110 (7) 77 (36) 2,3-Dichloropropene-1 78-88-6 75 (100) 110 (23) 77 (33) Benzene 71-43-2 78 (100) 77 (41) Toluene 108-88-3 91 (100) 92 (32) Ethylbenzene 100-41-4 91 (100) 106 (21) o-Xylene 95

41、-47-6 91 (100) 106 (33) 105 (16) m-Xylene 108-38-3 91 (100) 106 (33) 105 (20) p-Xylene 106-42-3 91 (100) 106 (33) 105 (20) BS EN ISO 22892:2011EN ISO 22892:2011 (E)Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 24/11/2011 06:42, Uncontrolled Copy, (c) BSI10 Table A.1 (continued) Compound CAS

42、 RN aDiagnostic ion 1m/z Diagnostic ion 2 m/z Diagnostic ion 3 bm/z Polycyclic aromatic hydrocarbons (PAH) Naphthalene 91-20-3 128 (100) 102 (11) - Acenaphthene 83-32-9 154 (70) 153 (100) 76 (10) Acenaphthylene 208-96-8 152 (100) Fluorene 86-73-7 166 (81) 165 (100) Anthracene 120-12-7 178 (100) 152

43、(12) Phenanthrene 85-01-8 178 (100) 152 (9) Fluoranthene 206-44-0 202 (100) 200 (31) Pyrene 129-00- 202 (100) Benzaanthracene 56-55-3 228 (100) Chrysene 218-01-9 228 (100) 226 (6) Benzobfluoranthene 205-99-2 252 (100) 250 (22) Benzokfluoranthene 207-08-9 252 (100) 250 (22) Benzoapyrene 50-32-8 252 (

44、100) 250 (18) 113 (11) Indeno1,2,3-cdpyrene 193-39-5 276 (100) 138 (12) Dibenza,hanthracene 53-70-3 278 (100) 139 (9) Benzoghiperylene 191-24-2 276 (100) 138 (12) Organochlorine pesticides (OCP) -Endosulfan 33213-65-9 195 (100) 241 (85) 159 (56) Mirex 2385-85-5 272 (100) 237 (88) 119 (37) Hexachloro

45、benzene (HCB) 118-74-1 284 (100) 142 (22) 249 (24) -Hexachlorocyclohexane (-HCH) 319-84-6 181 (100) 219 (33) 109 (29) -Hexachlorocyclohexane (-HCH) 319-85-7 181 (97) 219 (54) 109 (49) -Hexachlorocyclohexane (-HCH) 58-89-9 181 (97) 219 (34) 109 (33) Aldrin 309-00-2 66 (100) 263 (78) 293 (41) Dieldrin

46、 60-57-1 79 (100) 263 (70) 277 (18) Endrin 72-20-8 81 (100) 263 (70) 245 (55) Heptachlor 76-44-8 100 (100) 65 (65) 272 (89) cis-Heptachloro epoxide 28044-83-9 253 (100) 183 (90) 289 (85) trans-Heptachloro epoxide 1024-57-3 353 (100) 81 (67) 263 (26) -Endosulfan 959-98-7 195 (100) 159 (93) 265 (55) p

47、,p-DDE 72-55-9 246 (100) 318 (37) 176 (36) o,p-DDD 53-19-0 235 (100) 165 (66) 199 (29) o,p-DDT 789-02-6 235 (100) 165 (67) 199 (27) p,p-DDD 72-54-8 235 (100) 165 (66) 199 (20) o,p-DDE 3424-82-6 246 (100) 318 (37) 176 (27) p,p-DDT 50-29-3 235 (100) 165 (68) 199 (20) BS EN ISO 22892:2011EN ISO 22892:2

48、011 (E)Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 24/11/2011 06:42, Uncontrolled Copy, (c) BSI11Table A.1 (continued) Compound CAS RN aDiagnostic ion 1m/z Diagnostic ion 2 m/z Diagnostic ion 3 bm/z Polychlorinated biphenyls (PCB) PCB 28 7012-37-5 186 (100) 258 (74) 256 (82) PCB 52 35693-

49、99-3 292 (100) 294 (49) 220 (95) PCB101 37680-73-2 326 (100) 328 (65) 256 (62) PCB 118 31508-00-6 326 (100) 328 (62) 254 (57) PCB 138 35065-28-2 290 (100) 358 (42) 360 (94) PCB 153 35065-27-1 360 (100) 362 (92) 290 (73) PCB 180 35065-29-3 394 (100) 396 (96) 324 (84) Herbicides Atrazine 1912-24-9 200 (100) 202 (36) 215 (41) Simazine 122-34-9 138 (62) 186 (66) 201 (100) Acylated chlorophenols cMono 128 (100) 170 (6) 100 (13) Di 162 (100) 133 (10) Tri 196 (100) 238 (6) 160 (25) Tetra 230 (100) 194 (15) Penta 264 (100) aCAS RN: Chem