DIN EN ISO 22892-2011 Soil quality - Guidelines for the identification of target compounds by gas chromatography and mass spectrometry (ISO 22892 2006) German version EN ISO 22892 .pdf

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1、September 2011 Translation by DIN-Sprachendienst.English price group 13No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).

2、ICS 13.080.05!$tU“1815056www.din.deDDIN EN ISO 22892Soil quality Guidelines for the identification of target compounds by gaschromatography and mass spectrometry (ISO 22892:2006)English translation of DIN EN ISO 22892:2011-09Bodenbeschaffenheit Anleitungen fr die Identifizierung von Zielverbindungen

3、 durch Gaschromatographie undMassenspektrometrie (ISO 22892:2006)Englische bersetzung von DIN EN ISO 22892:2011-09Qualit du sol Lignes directrices pour lidentification des composs cibles par chromatographie en phasegazeuse et spectromtrie de masse (ISO 22892:2006)Traduction anglaise de DIN EN ISO 22

4、892:2011-09SupersedesDIN ISO 22892:2006-09www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.2608.11 DIN EN ISO 22892:2011-09 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Comm

5、ittee ISO/TC 190 “Soil quality” in collaboration with Technical Committee CEN/TC 345 “Characterization of soils” (Secretariat: NEN, Netherlands). The responsible German body involved in its preparation was the Normenausschuss Wasserwesen (Water Practice Standards Committee), Working Committee NA 119

6、-01-02-02 UA Chemische und physikalische Verfahren. Expert assistance and specialized laboratories are recommended to perform the procedures described in this standard. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 10382 DIN ISO 10382

7、 ISO 11264 DIN ISO 11264 ISO 15009 DIN ISO 15009 ISO/IEC 17025 DIN EN ISO/IEC 17025 Amendments This standard differs from DIN ISO 22892:2006-09 as follows: a) normative references have been updated; b) the standard has been editorially revised. Previous editions DIN ISO 22892: 2006-09 National Annex

8、 NA (informative) Bibliography DIN ISO 10382, Soil quality Determination of organochlorine pesticides and polychlorinated biphenyls Gas-chromatographic method with electron capture detection DIN ISO 11264, Soil quality Determination of herbicides Method using HPLC with UV-detection DIN ISO 15009, So

9、il quality Gas chromatographic determination of the content of volatile aromatic hydrocarbons, naphthalene and volatile halogenated hydrocarbons Purge-and-trap method with thermal desorption DIN EN ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories EUROPEA

10、N 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 sol - Lignes directrices pour lidentification des composs cibles

11、 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 European Standard was approved by CEN on 10 June 2011. CEN members are

12、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 concerning such national standards may be obtained on application to th

13、e 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 its own language and notified to the CEN-CENELEC Management Cent

14、re 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, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norw

15、ay, 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, B-1000 Brussels 2011 CEN All rights of exploitation in any form

16、and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 22892:2011: EContents EN ISO 22892:2011 (E) DIN EN ISO 22892:2011-09 2 Page Foreword3 Introduction .4 1 Scope 5 2 Principle5 3 Terms and definitions .5 4 Apparatus .6 5 Procedure .7 5.1 Retention times7 5.2 Mass spectra, s

17、election of diagnostic ions 7 6 Qualification .8 6.1 GC-MS procedure 8 6.2 Additional information 9 6.3 Reporting the presence of target compounds11 6.3.1 Identification.11 6.3.2 Indication 12 6.3.3 Absence of the target compound ( detection limit)12 7 Test report 12 Annex A (informative) Diagnostic

18、 ions to be used for identification using GC-MS .13 Annex B (informative) Examples .16 Annex C (informative) Examples of Spectra.22 Bibliography 24 Foreword The text of ISO 22892:2006 has been prepared by Technical Committee ISO/TC 190 “Soil quality” of the International Organization for Standardiza

19、tion (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 the

20、 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 any o

21、r 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, Greece,

22、 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 any mo

23、dification. EN ISO 22892:2011 (E) DIN EN ISO 22892:2011-09 3 Introduction In many analytical standards, use is made of gas chromatography (GC) in combination with mass spectrometric (MS) detection. This detector is a powerful tool provided it is properly used. In this International Standard, guideli

24、nes are given for the identification of target compounds. This International Standard can be used in combination with specific analytical standards or in combination with any GC-MS procedure. The result of the procedure described is: identified, indicated or absent. EN ISO 22892:2011 (E) DIN EN ISO

25、22892:2011-09 4 1 Scope This International Standard gives criteria for gas chromatography and mass spectrometry (GC-MS) identification of target compounds in soil samples. This International Standard is intended for use with standards developed for the determination of specific compounds. The identi

26、fication criteria are based on the comparison of retention times followed by interpretation of the electron ionization mass spectra, or if necessary, additional mass spectrometric techniques and other relevant factors. NOTE This International Standard is also applicable for other environmental sampl

27、es. 2 Principle A target compound is identified if the measured values meet the criteria specified in this International Standard or in the standard in which the procedures are described to analyse the target compound. Criteria are based on the relative retention times and the intensity of diagnosti

28、cs ions selected in the scan mode and measured in the selected ion mode (SIM), and other relevant factors. Additional information regarding diagnostic ions from specific international standards on the analysis of the target compound can be used. The principle of identification points is used. 3 Term

29、s and definitions For the purpose of this document, the following terms and definitions apply. 3.1 target compound selected component, the presence or absence of which is being established NOTE This definition also applies to derivatives of the original compound which are formed during an intentiona

30、l derivatization procedure or on-line derivatization. 3.2 standard compound target compound with the highest possible purity, which can be used as a reference during the analysis NOTE Any impurities should not have any influence on the mass spectrum of the standard compound. 3.3 retention time stand

31、ard compound that is added to the sample (or to the sample extract) and to the calibration standard solution, and used to calculate the relative retention times of the target compounds NOTE The retention time standard may be identical to the internal standard(s). EN ISO 22892:2011 (E) DIN EN ISO 228

32、92:2011-09 5 3.4 relative retention time ratio between the retention time of the target compound and the retention time of the retention time standard 3.5 lowest concentration for identification lowest concentration of the target compound, which, if present in the sample, can be identified using the

33、 identification criteria in this International Standard NOTE 1 It requires that the selected diagnostic ion with the lowest intensity is still present in the mass spectrum with a signal to noise ratio (S/N) higher than 3:1. NOTE 2 This concentration is very dependent on the sensitivity of the instru

34、ment and on the performance characteristics of the analytical method. 3.6 diagnostic ion selected fragment ion, molecular ion or other characteristic ion from the mass spectrum of the target compound with the highest possible specificity 3.7 identification point result of mass spectrometric investig

35、ation or other investigations/information to identify a component in environmental matrices 3.8 selected ion mode SIM measuring the intensity of selected diagnostic ions only 4 Apparatus As this International Standard is complementary to other standards using GC-MS, it is assumed that the instrument

36、ation used meets the requirements of those standards and a detailed description is not within the scope of this International Standard. Suitable quality assurance requirements are set out in ISO/IEC 17025. Minimum requirements are: Ionization mode: Electron ionization. Electron energy: Depending on

37、the application (usually 70 eV). Mass range: Peaks (masses) with a S/N 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 retention time value) Isotope dilution 1 Component spike/standard addition 1 Chromatographic pattern

38、 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 daughters (product ion) HR-MS (high resolution MS) 2 Every ion S/N 3 Expectation, plausibility,

39、 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-xylene).6.2 Additional information Interpretation of environmental data is always a combination of

40、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 stated, a component is identified if 3 identification points are obtained. If only 1 or 2 diagnost

41、ic 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 information about the sample, and interpretation of this information, takes place in Step 3. An extra i

42、dentification 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 obtained in Step 1 and Step 2. They are obtained by interpretation of additional non-analytical in

43、formation. 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 other ions are visible in full scan mode and this is in agreement with the mass spectrum of the

44、 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 specificity of the mass fragments in combination with their retention time will generally be sufficien

45、t. 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 also having similar mass spectra. Step 3: Gathering additional identification points using knowle

46、dge 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 the same site (for instance, if the sample under investigation has a low concentration and one o

47、r 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 identification point EXAMPLE 3 Identification with GC-MS and additional evidence (only 1 diagnost

48、ic 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 EN ISO 22892:2011 (E) DIN EN ISO 22892:2011-09 11 6.3.2 Indication There is an indication for the presence of the analysed t

49、arget 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 Absence 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, providing the proper GC-MS condi