1、BRITISH STANDARDBS EN ISO 16703:2011Soil quality Determination of content of hydrocarbon in the range C10to C40by gas chromatographyICS 13.080.10g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g
2、37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58National forewordThis British Standard is the UK implementation of EN ISO 16703:2011. It is identical to ISO 16703:2004. It supersedes BS ISO 16703:2004, which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee EH/4,
3、 Soil quality.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.Compliance with a British Standard cannot conf
4、er immunity from legal obligations.BS EN ISO 16703:2011This British Standard was published under the authority of the Standards Policy and Strategy Committee on 22 November 2004 BSI 2011Amendments/corrigenda issued since publicationDate Comments 31 August 2011 This corrigendum renumbers BS ISO 16703
5、:2004 as BS EN ISO 16703:2011ISBN 978 0 580 73155 6EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 16703 June 2011 ICS 13.080.10 English Version Soil quality - Determination of content of hydrocarbon in the range C10to C40by gas chromatography (ISO 16703:2004) Qualit du sol - Dosage des hyd
6、rocarbures de C10 C40par chromatographie en phase gazeuse (ISO 16703:2004)Bodenbeschaffenheit - Gaschromatographische Bestimmung des Gehalts an Kohlenwasserstoffen von C10bis C40(ISO 16703:2004) This European Standard was approved by CEN on 10 June 2011. CEN members are bound to comply with the CEN/
7、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 the CEN-CENELEC Management Cent
8、re 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 Centre has the same status as the
9、 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, Norway, Poland, Portugal, Romania
10、, 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 and by any means reserved wor
11、ldwide for CEN national Members. Ref. No. EN ISO 16703:2011: E3 Foreword The text of ISO 16703:2004 has been prepared by Technical Committee ISO/TC 190 “Soil quality” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 16703:2011 by Technical Committee CEN/T
12、C 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 latest by December 2011, and conflicting national standards shall be withdrawn at t
13、he 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 or all such patent rights. According to the CEN/CENELEC Internal Regulations, the nat
14、ional 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, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands
15、, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 16703:2004 has been approved by CEN as a EN ISO 16703:2011 without any modification. BS EN ISO 16703:2011EN ISO 16703:2011 (E)I SO 4002 All irthgs ersedevr i
16、iiContents Page Foreword iv 1 Scope 1 2 Normative references . 1 3 Terms and definitions. 2 4 Interferences 2 5 Principle . 2 6 Reagents 2 6.7 Hydrocarbon standard solution for calibration . 3 6.8 Control solution 3 6.9 System-performance standard solution. 3 7 Apparatus 3 8 Sampling, sample conserv
17、ation and pretreatment . 4 9 Procedure 5 9.1 Preparation of the clean-up column 5 9.2 Blank. 5 9.3 Extraction and clean-up . 5 9.4 Determination by gas chromatography 5 9.5 Quality control. 7 10 Precision 8 11 Test report . 8 Annex A (informative) Examples of gas chromatograms of mineral oil hydroca
18、rbon standard and soil samples. 10 Annex B (informative) Determination of the boiling range of mineral oil hydrocarbons from the gas chromatogram 16 Annex C (informative) Precision data. 17 Bibliography . 18 BS EN ISO 16703:2011EN ISO 16703:2011 (E)iv I SO 4002 All irthgs ersedevrForeword ISO (the I
19、nternational 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 technical committee
20、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 electrotechnica
21、l 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 the member bod
22、ies 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 identifying any
23、 or all such patent rights. ISO 16703 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical methods and soil characteristics. BS EN ISO 16703:2011EN ISO 16703:2011 (E)INTENRATIONAL TSANDADR IS:30761 O4002(E)I SO 4002 All irthgs ersedevr 1Soil quality Determination
24、 of content of hydrocarbon in the range C10to C40by gas chromatography 1 Scope This International Standard specifies a method for the quantitative determination of the mineral oil (hydrocarbon) content in field-moist soil samples by gas chromatography. The method is applicable to mineral oil content
25、s (mass fraction) between 100 mg/kg and 10 000 mg/kg soil, expressed as dry matter, and can be adapted to lower limits of detection. This International Standard is applicable to the determination of all hydrocarbons with a boiling range of 175 C to 525 C, of n-alkanes from C10H22to C40H82, of isoalk
26、anes, cycloalkanes, alkylbenzenes, alkylnaphthalenes and polycyclic aromatic compounds, provided that they are not absorbed on the specified column during the clean-up procedure. This International Standard is not applicable to the quantitative determination of hydrocarbons C40) compounds in the chr
27、omatogram; f) any details not specified in this International Standard or which are optional, as well as any other factor that might have affected the results. BS EN ISO 16703:2011EN ISO 16703:2011 (E)IS:30761 O4002(E) 10 I SO 4002 All irthgs ersedevrAnnex A (informative) Examples of gas chromatogra
28、ms of mineral oil hydrocarbon standard and soil samples Figure A.1 shows the gas chromatogram of the calibration mixture of mineral oil consisting of equal parts of a diesel fuel and a lubricating oil. Figure A.2 shows the gas chromatogram of the “column bleed” after injection of n-heptane, and Figu
29、re A.3 shows the integrated gas chromatogram of the calibration mixture of mineral oil corrected for the “column bleed”. The total peak area between n-decane (C10) and n-tetracontane (C40) used for quantification is indicated as hatched area. The Figures A.4 and A.5 show integrated gas chromatograms
30、 corrected for the “column bleed” of low and highly contaminated soil samples, respectively. Figure A.6 shows a chromatogram of a system-performance standard solution. Examples of chromatograms of soil samples with representative characteristics are given in Figures A.7 to A.10. The gas chromatogram
31、s were recorded under the following conditions: Injection technique: on-column Injection volume: 1 l to 3 l Column type: WCOT fused silica Column length: 12 m Internal diameter: 0,32 mm Liquid phase: BPX-5 Film thickness: 1,0 m Pre-column: deactivated fused silica capillary, 2 m x 0,53 mm Carrier ga
32、s: helium Pressure: 100 kPa Detector: flame ionization detector Detector temperature: 360 C Temperature programme: 80 C for 1 min; 20C/min to 360 C; 360 C for 15 min BS EN ISO 16703:2011EN ISO 16703:2011 (E)IS:30761 O4002(E) I SO 4002 All irthgs ersedevr 11Key 1 n-decane 2 n-tetracontane Figure A.1
33、Gas chromatogram of the calibration mixture consisting of equal parts of diesel fuel and lubricating oil Figure A.2 Gas chromatogram of the “column bleed” BS EN ISO 16703:2011EN ISO 16703:2011 (E)IS:30761 O4002(E) 12 I SO 4002 All irthgs ersedevrKey 1 n-decane 2 n-tetracontane Figure A.3 Integrated
34、gas chromatogram of the calibration mixture of mineral oil corrected for the “column bleed” Key 1 n-decane 2 n-tetracontane Figure A.4 Integrated gas chromatogram of a low-contaminated soil sample corrected for the “column bleed” BS EN ISO 16703:2011EN ISO 16703:2011 (E)IS:30761 O4002(E) I SO 4002 A
35、ll irthgs ersedevr 13Key 1 n-decane 2 n-tetracontane Figure A.5 Integrated gas chromatogram of a highly contaminated soil sample corrected for the “column bleed” Figure A.6 Gas chromatogram of a system-performance standard solution BS EN ISO 16703:2011EN ISO 16703:2011 (E)IS:30761 O4002(E) 14 I SO 4
36、002 All irthgs ersedevrFigure A.7 Gas chromatogram Sample 3 GC Soil 1 (sufficient clean-up for PAHs) Figure A.8 Gas chromatogram Sample 3 GC Soil 1 (insufficient clean-up for PAHs) BS EN ISO 16703:2011EN ISO 16703:2011 (E)IS:30761 O4002(E) I SO 4002 All irthgs ersedevr 15Figure A.9 Sample 3 GC Soil
37、1 (acetone content about 2,5 % in extract) with insufficient clean-up of PAHs) Figure A.10 Sample 3 GC Soil 1 (acetone content less than 0,1 % in extract) with sufficient clean-up of PAHs BS EN ISO 16703:2011EN ISO 16703:2011 (E)IS:30761 O4002(E) 16 I SO 4002 All irthgs ersedevrAnnex B (informative)
38、 Determination of the boiling range of mineral oil hydrocarbons from the gas chromatogram Using the data from Table B.1, the approximate boiling range of the hydrocarbons in the sample can be estimated by comparison of the peak pattern of the sample chromatogram and that of the n-alkane mixture. Tab
39、le B.1 Boiling points of the n-alkanes with from 6 to 44 carbon atoms Number of carbon atoms Boiling point C 6 69 7 98 8 126 9 151 10 175 11 196 12 216 13 235 14 253 15 271 16 287 17 302 18 317 19 331 20 344 21 356 22 369 23 380 24 391 25 402 26 412 27 422 28 432 29 441 30 450 31 459 32 468 33 476 3
40、4 483 35 491 36 498 37 505 38 512 39 518 40 525 41 531 42 537 43 543 44 548 BS EN ISO 16703:2011EN ISO 16703:2011 (E)IS:30761 O4002(E) I SO 4002 All irthgs ersedevr 17Annex C (informative) Precision data An interlaboratory comparison was carried out in 2003. The precision data from this interlaborat
41、ory comparison are given in Table C.1. Table C.1 Precision data for ISO 16703 Sample Matrix L X CVRCVrGC Soil 1 Soil 23 697 44,86 9,14 GC Soil 2 Soil 24 1 818 28,52 8,31 GC Waste 2 Waste 19 780 26,91 3,88 GC Waste 2 Rubble 19 7841 25,53 6,05 20 2 848 mg/l HC solution Hydrocarbon standard solution Gr
42、avimetric reference value 2 842 mg/l 8,62 4,94 L is the number of laboratories; X is the mean value of all results after elimination of outliers, in milligrams per kilogram; CVRis the coefficient of variation of the reproducibility, in percent (%); CVris the coefficient of variation of the repeatabi
43、lity, in percent (%). BS EN ISO 16703:2011EN ISO 16703:2011 (E)IS:30761 O4002(E) 18 I SO 4002 All irthgs ersedevrBibliography 1 ISO/TR 11046, Soil quality Determination of mineral oil content Method by infrared spectrometry and gas chromatographic method 2 ISO 11464:1994, Soil quality Pretreatment o
44、f samples for physico-chemical analyses 3 ISO 15009, Soil quality Gas chromatographic determination of the content of volatile aromatic hydrocarbons, naphthalene and volatile halogenated hydrocarbons Purge-and-trap method with thermal desorption 4 ISO 9377-2, Water quality Determination of hydrocarb
45、on oil index Part 2: Method using solvent extraction and gas chromatography 5 prEN 14039:2000, Characterization of waste Determination of hydrocarbon content in the range of C10to C40by gas chromatography BS EN ISO 16703:2011EN ISO 16703:2011 (E)blankBSI GroupHeadquarters 389 Chiswick High Road, Lon
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