EN ISO 12010-2014 en Water quality - Determination of short-chain polychlorinated alkanes (SCCPs) in water - Method using gas chromatography-mass spectrometry (GC-MS) and negative-.pdf

1、BSI Standards PublicationWater quality Determinationof short-chain polychlorinatedalkanes (SCCPs) in water Method using gaschromatography-massspectrometry (GC-MS)and negative-ion chemicalionization (NCI)BS EN ISO 12010:2014Incorporating corrigendum June 2014BS EN ISO 12010:2014National forewordThis

2、British Standard is the UK implementation of EN ISO 12010:2014. It is identical to ISO 12010:2012. It supersedes BS ISO 12010:2012, which is withdrawn.The UK participation in its preparation was entrusted by Technical Committee EH/3, Water quality to Subcommittee EH/3/2, Physical chemical and bioche

3、mical methods.A list of organizations represented on this subcommittee 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. The British Standards Institution 2014. Publi

4、shed by BSI Standards Limited 2014ISBN 978 0 580 84022 7ICS 13.060.50Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 May 2012.Amendments/corrigenda issued sinc

5、e publicationDate Text affected30 June 2014 This corrigendum renumbers BS ISO 12010:2012 as BS EN ISO 12010:201430 June 2014 Implementation of CEN correction notice 14 May 2014: Preparation statement in EN foreword addedBRITISH STANDARDEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 12010 A

6、pril 2014 ICS 13.060.50 English Version Water quality - Determination of short-chain polychlorinated alkanes (SCCPs) in water - Method using gas chromatography-mass spectrometry (GC-MS) and negative-ion chemical ionization (NCI) (ISO 12010:2012) Qualit de leau - Dtermination des alcanes polychlors c

7、hane courte (SCCP) dans leau - Mthode par chromatographie gazeuse-spectromtrie de masse (CG-SM) avec ionisation chimique ngative (ICN) (ISO 12010:2012) Wasserbeschaffenheit - Bestimmung von kurzkettigen Chloralkanen (SCCP) in Wasser - Verfahren mittels Gaschromatographie-Massenspektrometrie (GC-MS)

8、und negativer chemischer Ionisation (NCI) (ISO 12010:2012) This European Standard was approved by CEN on 11 April 2014. 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

9、 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 any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other lan

10、guage 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 versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denma

11、rk, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE

12、FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 12010:2014 Eii ISO 2012 All

13、 rights reservedBS EN ISO 12010:2014 EN ISO 12010:2014 (E)Foreword The text of ISO 12010:2012 has been prepared by Technical Committee ISO/TC 147 “Water quality” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 12010:2014 by Technical Committee CEN/TC 230

14、 “Water analysis” the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by October 2014, and conflicting national standards shall be withdrawn at the latest by Octo

15、ber 2014. 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 or all such patent rights. This document has been prepared under a mandate given to CEN by the European

16、 Commission and the European Free Trade Association. 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, Finlan

17、d, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO

18、 12010:2012 has been approved by CEN as EN ISO 12010:2014 without any modification. ISO 2012 All rights reserved iiiContents Page. ivIntroduction1 Scope 12 Normative references . 13 Principle . 14 Interferences . 25 Reagents and standards . 26 Apparatus 67 Sampling and sample pretreatment . 78 Proce

19、dure 78.1 Extraction with liquid-liquid extraction method 78.2 Extraction of samples with higher content of suspended matter 78.3 Extract clean-up . 88.4 Measurement and integration of the chromatogram . 98.5 Calibration . 99 Expression of results .1210 Test report .12Annex A (informative) Additiona

20、l quality control check solutions 13Annex B (informative) Explanation of the calibration of the sum of SCCPs with multiple linear regression 14Annex C (informative) Typical GC-MS conditions 19Annex D (informative) Typical chromatograms of standard solutions 1 g/ml .22Annex E (informative) Presentati

21、on of goodness of fit 23Annex F (informative) Example for recoveries of quality assurance solutions .24Annex G (informative) Chromatogram of a real water sample with a sum of SCCPs concentration of 2,59 g/l 25Annex H (informative) Precision data27Bibliography .28BS EN ISO 12010:2014 ISO 12010:2012 (

22、E)iv ISO 2012 All rights reservedIntroductionThe user should be aware that particular problems might require the specifications of additional marginal conditions.BS EN ISO 12010:2014 ISO 12010:2012 (E)Water quality Determination of short-chain polychlorinated alkanes (SCCPs) in water Method using ga

23、s chromatography-mass spectrometry (GC-MS) and negative-ion chemical ionization (NCI)WARNING Persons using this International Standard should be familiar with normal laboratory practice. This International Standard does not purport to address all of the safety problems, if any, associated with its u

24、se. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.IMPORTANT It is absolutely essential that tests conducted in accordance to this International Standard be carried out by suitably qualified s

25、taff.1 ScopeThis International Standard specifies a method for the quantitative determination of the sum of short-chain polychlorinated n-alkanes, also known as short-chain polychlorinated paraffins (SCCPs), in the carbon bond range n-C10to n-C13inclusive, in mixtures with chlorine mass fractions (“

26、contents”) between 49 % and 67 %, including approximately 6 300 of approximately 8 000 congeners.This method is applicable to the determination of the sum of SCCPs in unfiltered surface water, ground water, drinking water and waste water using gas chromatography-mass spectrometry with electron captu

27、re negative ionization (GC-ECNI-MS).The method can be applied to samples containing 0,1 g/l to 10 g/l. Depending on the waste water matrix, the lowest detectable concentration is estimated to be 0,1 g/l.2 Normative referencesThe following referenced documents are indispensable for the application of

28、 this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 5667-1, Water quality Sampling Part 1: Guidance on the design of sampling programmes and sampling techniquesISO 5667-3, W

29、ater quality Sampling Part 3: Preservation and handling of water samplesISO 8466-1, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 1: Statistical evaluation of the linear calibration functionISO/TS 13530, Water quality Guidance on an

30、alytical quality control for chemical and physicochemical water analysis3 PrincipleDetermination of the sum of SCCPs in the carbon bond range n-C10to n-C13inclusive, in technical and environmental transposed mixtures with chlorine mass fractions (“contents”) between 49 % and 67 % (e.g. approximately

31、 3 to 10 chlorine atoms per molecule) and independent of the C-number distribution pattern of the congeners. No recognition of the chlorine content is necessary.SCCPs in whole water samples are fortified with an internal standard and extracted using liquid-liquid extraction with an organic solvent.

32、The sample enrichment procedure is followed by a clean-up procedure to eliminate interfering compounds. Gas chromatography (GC) is undertaken using a short capillary column within a short INTERNATIONAL STANDARD ISO 12010:2012(E) ISO 2012 All rights reserved 1BS EN ISO 12010:2014 retention time range

33、. The detection of selected mass fragments is carried out using mass spectrometry (MS) in selected ion-monitoring mode using electron capture negative ionization mode (ECNI). The selection of the mass fragments is specific for the variety of technical mixtures as well as for their chlorine content a

34、nd C-number distribution patterns. Alternative mass fragment combinations for qualification are also given in this International Standard.The selected ion chromatogram is integrated over the full retention time range of the SCCPs. The quantification of the sum of SCCPs is carried out after establish

35、ing a calibration by multiple linear regression, measuring solutions of different technical mixtures fortified with an internal standard.The calibration requires a minimum of three different composed standard mixtures, each of which resembles the C-number distribution pattern and chlorine content of

36、 different technical mixtures. This is to reflect the variety of chlorine contents and C-number distribution patterns of technical SCCP mixtures and SCCP levels found in environmental samples, which cannot be described by a single defined standard substance.The method allows a quantification of the

37、sum of SCCPs expected to be within an expanded measurement uncertainty of less than 50 %.4 InterferencesNon-specific matrix interferences, as well as interferences from other environmental situations, are dealt with using the given clean-up procedure. Following the entire procedure, including the co

38、ncentration factor of approximately 5 000, the following pollutants have been tested and found not to cause interferences below the following concentrations.Potential interfering compounds Highest concentration level at which no interferences higher than the limit of detection are detectedAroclor 12

39、62a0,5 g/lAroclor 1242a0,5 g/lAroclor 1221a1 g/lCampheclor 0,2 g/lHalowax 1014a1 g/lHalowax 1051a1 g/lTechnical chlordane 0,5 g/lMCCP (medium-chain chlorinated n-alkanes) 42 % 0,2 g/lMCCP (medium-chain chlorinated n-alkanes) 52 % 0,2 g/lMCCP (medium-chain chlorinated n-alkanes) 57 % 0,2 g/laProduct

40、available commercially. This information is given for the convenience of users of this document and does not constitute an endorsement by ISO of this product.If the clean-up procedure is repeated, interferences can be further reduced.5 Reagents and standardsUse solvents and reagents of sufficient pu

41、rity, i.e. with negligibly low concentrations of SCCPs (e.g. lower than the limit of detection of the method).NOTE Check blanks regularly over the entire procedure to ensure they are suitable and establish proper analytical control.2 ISO 2012 All rights reservedBS EN ISO 12010:2014 ISO 12010:2012 (E

42、)5.1 Solvents for extraction and preparation of stock solutions. The solvent for extraction is n-heptane. Other non-polar solvents, e.g. n-hexane (C6H14) or cyclohexane (C6H12), can be used if the extraction efficiency is comparable with those of n-heptane.Use 2,2,4-trimethylpentane (C8H18, isooctan

43、e) for conditioning of the glass bottles (6.1).For preparation of the stock solutions, use dilutions in propanone (acetone), C3H6O.For conditioning of the clean-up columns, use mixtures of n-heptane and propanone (acetone).For the first elution step of the filtrated suspended matter, use methanol (C

44、H3OH).5.2 Reference SCCP stock solutions. Use commercially available solutions, e.g. in cyclohexane or n-hexane, of the single mixtures of SCCP congeners with a defined carbon chain length and with different defined chlorine contents (see Table 1, first two columns). Alternatively, use commercially

45、available ready-mixed solutions as described in Table 1.Prepare the solutions Hordalub 171)-s1, SCCP 51,5 % -s1, Hordalub 801)-s1, Cereclor 601)-s1, Hordalub 5001)-s1, and Cereclor 701)-s1 according to Table 1. The suffix “-s1” denotes synthetically mixed standard solutions, which resemble the techn

46、ical mixtures.The chlorine content (third row) of the mixtures is calculated as the weighted mean.Store the prepared solutions in a refrigerator at a temperature of 2 C to 6 C.5.3 Internal standard stock solutions from individual congeners. Use commercially available individual congener standard sol

47、utions and prepare a stock solution in propanone (acetone) (5.1) at a concentration of, for example, 1 g/ml.Individual SCCP congeners with chlorine contents of between 49 % and 67 % are suitable as internal standards, e.g. 1,1,1,3,10,11-hexachloroundecane, with e.g. 0,1 g/ml; 1,1,1,3,11,13,13,13-oct

48、achlorotridecane, with e.g. 0,1 g/ml; 1,2,5,5,6,9,10-heptachlorodecane, with e.g. 0,01 g/ml.NOTE 1 The different individual SCCP congeners used as internal standard substances probably contribute to the sum of SCCPs in environmental samples. Nevertheless, the contribution is approximately 0,15 mm; s

49、urface area, determined according to the BET method, 170 m2/g to 300 m2/g; pH 9 to pH 10.Activate the magnesium silicate by heating, for example, 200 g in a shallow dish at 140 C for at least 4 h. Allow the activated magnesium silicate to cool to room temperature in a desiccator. Activated magnesium silicate can be stored in a closed bottle at room temperature for up to 1 month.Table 1 Reference substances stock solutionsStandard solutionsSynthetic mixed standard solutions, which resemble technical mix