DIN EN ISO 16703-2011 Soil quality - Determination of content of hydrocarbon in the range C to C by gas chromatography (ISO 16703 2004) German version EN ISO 16703 2011《土质 用气相色谱法测定.pdf

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1、September 2011 Translation by DIN-Sprachendienst.English price group 12No 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 13.080.10!$tT“1814957www.din.deDDIN EN ISO 16703Soil quality Bodenbeschaffenheit Gaschromatographische Bestimmung des Gehalts an Kohlenwasserstoffen vonEnglische bersetzung von DIN EN ISO 16703:2011-09Qualit du sol phase gazeuse (ISO 16703:2004)Traduction anglaise de DIN EN ISO 16703:2011-09Supe

3、rsedesDIN ISO 16703:2005-12www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.25Determination of content of hydrocarbon in the range C10to C40by gas chromatography (ISO 16703:2004) English translation of DIN EN ISO 16703:2011-09 C10bi

4、s C40(ISO 16703:2004) Dosage des hydrocarbures de C10 40par chromatographie en C08.11 DIN EN ISO 16703:2011-09 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee ISO/TC 190 “Soil quality” in collaboration with Technical Committee CEN/TC

5、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 119-01-02-02 UA Chemische und physikalische Verfahren. Expert assistance and special

6、ized laboratories are recommended to perform the sampling procedures described in this standard. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 8466-1 DIN 38402-51 ISO 9377-2 DIN EN ISO 9377-2 ISO 10381-1 DIN ISO 10381-1 ISO 11464 DIN

7、19747 ISO 11465 DIN ISO 11465 ISO 14507 DIN ISO 14507 ISO 15009 DIN ISO 15009 Amendments This standard differs from DIN ISO 16703:2005-12 as follows: a) normative references have been updated; b) the standard has been editorially revised. Previous editions DIN ISO 16703: 2005-12 DIN EN ISO 16703:201

8、1-09 3 National Annex NA (informative) Bibliography DIN 19747, Investigation of solids Pre-treatment, preparation and processing of samples for chemical, biological and physical investigations DIN 38402-51, German standard methods for the examination of water, waste water and sludge General informat

9、ion (group A) Calibration of analytical methods, evaluation of analytical results and linear calibration functions used to determine the performance characteristics of analytical methods (A 51) DIN EN ISO 9377-2, Water quality Determination of hydrocarbon oil index Part 2: Method using solvent extra

10、ction and gas chromatography DIN ISO 10381-1, Soil quality Sampling Part 1: Guidance on the design of sampling programmes DIN ISO 11465, Soil quality Determination of dry matter and water content on a mass basis Gravimetric method DIN ISO 14507, Soil quality Pretreatment of samples for determination

11、 of organic contaminants DIN 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 DIN EN ISO 16703:2011-09 4 This page is intentionally blank EUROPEA

12、N 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 hydrocarbures de C10 C40par chromatographie en phase gazeuse

13、(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/CENELEC Internal Regulations which stipulate the condition

14、s 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 any CEN member. This European Standard exists in

15、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 versions. CEN members are the national standards

16、 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, Slovakia, Slovenia, Spain, Sweden, Switzerland and Unite

17、d 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 for CEN national Members. Ref. No. EN ISO 16703:201

18、1: EContents DIN EN ISO 16703:2011-09 EN ISO 16703:2011 (E) 2 Page Foreword3 1 Scope 4 2 Normative references 4 3 Terms and definitions .5 4 Interferences 5 5 Principle5 6 Reagents.5 7 Apparatus .6 8 Sampling, sample conservation and pretreatment 7 9 Procedure .8 9.1 Preparation of the clean-up colu

19、mn 8 9.2 Blank .8 9.3 Extraction and clean-up 8 9.4 Determination by gas chromatography.8 9.5 Quality control10 10 Precision.11 11 Test report 11 Annex A (informative) Examples of gas chromatograms of mineral oil hydrocarbon standard and soil samples .13 Annex B (informative) Determination of the bo

20、iling range of mineral oil hydrocarbons from the gas chromatogram.19 Annex C (informative) Precision data20 Bibliography 21 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

21、taken over as EN ISO 16703:2011 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 latest by December 2011

22、, 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 or all such patent rights

23、. 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, Hungary, Iceland, Irela

24、nd, 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 16703:2004 has been approved by CEN as a EN ISO 16703:2011 without any modification. DIN EN ISO 1

25、6703:2011-09 EN ISO 16703:2011 (E) 3 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 contents (mass fraction) between 100 mg/k

26、g 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 isoalkanes, cycloalkanes, alkylbenzenes,

27、 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 chromatogram; f) any details not spec

28、ified in this International Standard or which are optional, as well as any other factor that might have affected the results. DIN EN ISO 16703:2011-09 EN ISO 16703:2011 (E) 12 Annex A (informative) Examples of gas chromatograms of mineral oil hydrocarbon standard and soil samples Figure A.1 shows th

29、e 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 Figure A.3 shows the integrated gas chromatogram of the calibration mixture of

30、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 corrected for the “column bleed” of low and highly contaminated soil sampl

31、es, 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 chromatograms were recorded under the following conditions: Injection technique: on-col

32、umn 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 gas: helium Pressure: 100 kPa Detector: flame ionization detector Detector te

33、mperature: 360 C Temperature programme: 80 C for 1 min; 20C/min to 360 C; 360 C for 15 min DIN EN ISO 16703:2011-09 EN ISO 16703:2011 (E) 13 Key 1 n-decane 2 n-tetracontane Figure A.1 Gas chromatogram of the calibration mixture consisting of equal parts of diesel fuel and lubricating oil Figure A.2

34、Gas chromatogram of the “column bleed” DIN EN ISO 16703:2011-09 EN ISO 16703:2011 (E) 14 Key 1 n-decane 2 n-tetracontane Figure A.3 Integrated 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 chromat

35、ogram of a low-contaminated soil sample corrected for the “column bleed” DIN EN ISO 16703:2011-09 EN ISO 16703:2011 (E) 15 Key 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 sys

36、tem-performance standard solution DIN EN ISO 16703:2011-09 EN ISO 16703:2011 (E) 16 Figure 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) DIN EN ISO 16703:2011-09 EN ISO 16703:2011 (E) 17 Figure A

37、.9 Sample 3 GC Soil 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 DIN EN ISO 16703:2011-09 EN ISO 16703:2011 (E) 18 Annex B (informative) Determination of the

38、 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. Table B.1 Boiling points

39、 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 34 483 35 491 36 498 3

40、7 505 38 512 39 518 40 525 41 531 42 537 43 543 44 548 DIN EN ISO 16703:2011-09 EN ISO 16703:2011 (E) 19 Annex C (informative) Precision data An interlaboratory comparison was carried out in 2003. The precision data from this interlaboratory comparison are given in Table C.1. Table C.1 Precision dat

41、a 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 Gravimetric reference value 2 842 mg/l 8,62 4,94 L is the number

42、 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 repeatability, in percent (%). DIN EN ISO 16703:2011-09 EN ISO 16703:20

43、11 (E) 20 Bibliography 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 of samples for physico-chemical analyses 3 ISO 15009, Soil quality Gas chromatographic determination of

44、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 hydrocarbon 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 DIN EN ISO 16703:2011-09 EN ISO 16703:2011 (E) 21