EN ISO 22892-2011 en Soil quality - Guidelines for the identification of target compounds by gas chromatography and mass spectrometry《土壤质量准则 目标化合物的气相色谱和质谱鉴定》.pdf

《EN ISO 22892-2011 en Soil quality - Guidelines for the identification of target compounds by gas chromatography and mass spectrometry《土壤质量准则 目标化合物的气相色谱和质谱鉴定》.pdf》由会员分享，可在线阅读，更多相关《EN ISO 22892-2011 en Soil quality - Guidelines for the identification of target compounds by gas chromatography and mass spectrometry《土壤质量准则 目标化合物的气相色谱和质谱鉴定》.pdf（30页珍藏版）》请在麦多课文档分享上搜索。

1、BRITISH STANDARDSoil quality Guidelines for the identification of target compounds by gas chromatography and mass spectrometryICS 13.080.05g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g

2、3g38g50g51g60g53g44g42g43g55g3g47g36g58BS 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 It supersedes BS ISO 22892:2006, which is withdrawn.The UK participation in its preparation was entrusted to Technical Co

3、mmittee 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 a contract. Users are responsible for its correct application.Compliance with a British Standard c

4、annot 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 2011Amendments/corrigenda issued since publicationDate Comments 31 August 2011 This corrigendum renumbers BS IS

5、O 22892:2006 as BS EN ISO 22892:2011ISBN 978 0 580 73160 0EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE 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

6、 sol - Lignes directrices pour lidentification de composs cibles par chromatographie en phase gazeuse et spectromtrie de masse (ISO 22892:2006) Bodenbeschaffenheit - Anleitungen fr die Identifizierung von Zielverbindungen durch Gaschromatographie und Massenspektrometrie (ISO 22892:2006) This Europea

7、n Standard was approved by CEN on 10 June 2011. CEN members are bound to comply with the CEN/CENELEC Internal 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 concern

8、ing such national standards may be obtained on application to the CEN-CENELEC Management Centre or to 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

9、its own language and notified to the CEN-CENELEC Management Centre has the same status as the official 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

10、, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17,

11、B-1000 Brussels 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 22892:2011: EForeword The text of ISO 22892:2006 has been prepared by Technical Committee ISO/TC 190 “Soil quality” of the International Organization for Stan

12、dardization (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,

13、 at 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 identifyin

14、g any 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,

15、Greece, 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

16、 any modification. BS EN ISO 22892:2011EN ISO 22892:2011 (E)iiiiiContents 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 times . 3 5.2 Mass spectra, selection of diagnostic ions . 3 6 Qualification 4 6.1 GC-MS procedure

17、 . 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 scan 1 Diagnostic ions in full scan S/N 3 Column with other polarity a 1 GC-criterion (extra rete

18、ntion 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 technique (i.e. LC) GC-MS (EI and CI; positive/negative) 3 1 (EI) + 2 (CI) GC-MS-MS 4 1 precursor and 2

19、 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. aNot valid for non-separated compounds (isomers) with the same mass (chrysene/triphenylene, m/p-xyl

20、ene).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 processes that occur or may occur. This is also true for the interpretation of GC-MS analysis. As st

21、ated, 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, gathering additional identification points using analytical procedures is part of Step 2. Using informa

22、tion 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, an identification point obtained in Step 3 is of another order than the identification points ob

23、tained 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 obtained in all three steps. Step 2: Gathering identification points using analytical procedures. No

24、 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 normally present or present on that site (for instance, PCB or PAH). For volatile compounds, the specif

25、icity 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 results: there are no low molecular mass compounds with the same retention time on a GC column and a

26、lso 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 obtained using Step 3, this shall be reported. The component is identified in earlier samples from

27、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 identification point Column with other polarity (Step 1) 1 identification point Expected value 1 i

28、dentification 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 recognized 1 identification point Result of LC-FLD 1 identification point BS EN ISO 22892:2011EN ISO 2

29、2892:2011 (E)8 6.3.2 Indication There is an indication for the presence of the analysed target compound in 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 Absen

30、ce of the target compound ( detection limit) The target compound is absent in the sample (not identified 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

31、, providing the proper GC-MS conditions have been used. 7 Test report The test report in addition to the 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 identific

32、ation of the sample; c) the results of the identification procedure, i.e. identification, indication or absence 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 specifi

33、ed in this International Standard or which are optional, as well as any factor, which may have affected the results. BS EN ISO 22892:2011EN ISO 22892:2011 (E)9Annex A (informative) Diagnostic ions to be used for identification using GC-MS Table A.1 gives a list of recommended diagnostic ions. The re

34、lative 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 m

35、ore digits 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) Dichlo

36、rodifluoromethane 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-D

37、ichloroethene 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) 1

38、10 (45) 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-Xyl

39、ene 95-47-6 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)10 Table A.1 (continued) Compound CAS RN aDiagnostic ion 1m/z Diagnostic ion 2 m/z Diagnostic ion 3 bm/z Polycyclic aromatic hydro

40、carbons (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 (12) Phenanthrene 85-01-8 178 (100) 152 (9) Fluoranthene 206-44-0 202 (100) 200 (31) Pyrene 1

41、29-00- 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 (100) 250 (18) 113 (11) Indeno1,2,3-cdpyrene 193-39-5 276 (100) 138 (12) Dibenza,hanthracene 5

42、3-70-3 278 (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) Hexachlorobenzene (HCB) 118-74-1 284 (100) 142 (22) 249 (24) -Hexachlorocyclohexane (-HCH) 319-84-6 181

43、 (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 60-57-1 79 (100) 263 (70) 277 (18) Endrin 72-20-8 81 (100) 263 (70) 245 (55) Heptachlor 76-4

44、4-8 100 (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,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-DD

45、T 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 22892:2011 (E)11Table A.1 (continued) Compound CAS RN aDiagnostic ion 1m/z Diagnostic ion 2 m/z Diag

46、nostic ion 3 bm/z Polychlorinated biphenyls (PCB) PCB 28 7012-37-5 186 (100) 258 (74) 256 (82) PCB 52 35693-99-3 292 (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

47、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 (1

48、00) 194 (15) Penta 264 (100) aCAS RN: Chemical Abstracts Service Registration Number. bThe choice of ion 3 (m/z) depends on the applied mass spectrometric method: quadrupole or ion trap detection, because of the formation of different fragment ions. cTaken from Reference 4. The relative intensities

49、may vary between mass isomers. BS EN ISO 22892:2011EN ISO 22892:2011 (E)12 Annex B (informative) Examples B.1 Example 1, -endosulfan Compound: -endosulfan, diagnostic ions 195, 241, 159. The three selected diagnostic ions have the following relative intensities: 100 %, 80 % and 56 %. B.1.1 Identification B.1.1.1 Example based on relative retention time Table B.1 Retention times and relative retention times Calibration standard 1 Sample 1 Retention time s Relative retention time Retention times Relative retention timeRetent