DIN ISO 11916-2-2014 Soil quality - Determination of selected explosives and related compounds - Part 2 Method using gas chromatography (GC) with electron capture detection (ECD) o.pdf

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1、November 2014 Translation by DIN-Sprachendienst.English price group 14No 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).I

2、CS 13.080.10!%=cG“2266436www.din.deDDIN ISO 11916-2Soil quality Determination of selected explosives and related compounds Part 2: Method using gas chromatography (GC) with electron capturedetection (ECD) or mass spectrometric detection (MS)(ISO 11916-2:2013),English translation of DIN ISO 11916-2:2

3、014-11Bodenbeschaffenheit Bestimmung von ausgewhlten Explosivstoffen und verwandten Verbindungen Teil 2: Verfahren mittels Gaschromatographie (GC) undElektronen-Einfang-Detektion (ECD) oder massenspektrometrischer Detektion (MS)(ISO 11916-2:2013),Englische bersetzung von DIN ISO 11916-2:2014-11Quali

4、t du sol Dosage dune slection dexplosifs et de composs apparents Partie 2: Mthode utilisant la chromatographie en phase gazeuse (CG) avec dtection capture dlectrons (DCE) ou dtection par spectromtrie de masse (SM)(ISO 11916-2:2013),Traduction anglaise de DIN ISO 11916-2:2014-11www.beuth.deDocument c

5、omprises 29 pagesIn case of doubt, the German-language original shall be considered authoritative.10.14 Contents PageNational foreword 31 Scope . 52 Normative references 53 Principle 64 Interferences 65 Reagents 65.1 General . 65.2 Chemicals . 65.3 Standard substances and solutions . 76 Apparatus .

6、76.1 General . 76.2 Equipment for extraction . 86.3 Equipment for re-solution (solvent exchange) . 86.4 Gas chromatographic system (GC) with ECD or MS 87 Procedure. 87.1 Sample pretreatment, sample storage and determination of water content 87.2 Extraction 97.3 Storage of extract . 118 Gas chromatog

7、raphic analysis. 118.1 General .118.2 Gas chromatographic system. 128.3 Calibration . 128.4 Identification and quantification 139 Calculation of results 149.1 General 149.2 Calculation . 1410 Quality assurance .1511 Expression of results .1612 Test report 16Annex A (informative) GC/ECD conditions 17

8、Annex B (informative) GC/MS conditions .20Annex C (informative) Precision data .22Bibliography .29A comma is used as the decimal marker. DIN ISO 11916-2:2014-11 2National Annex NA (informative) Bibliography .4DIN ISO 11916-2:2014-11 3National foreword This document (ISO 11916-2:2013) has been prepar

9、ed by Technical Committee ISO/TC 190 “Soil quality” (Secretariat: NEN, Netherlands). The responsible German body involved in its preparation was the DIN-Normenausschuss Wasserwesen (DIN Standards Committee Water Practice), Working Group NA 119-01-02-02-53 AK Sprengstofftypische Verbindungen of Worki

10、ng Committee NA 119-01-02 AA Boden- und Abfalluntersuchung. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. DIN shall not be held responsible for identifying any or all such patent rights. ISO 11916 consists of the following parts

11、, under the general title Soil quality Determination of selected explosives and related compounds: Part 1: Method using high-performance liquid chromatography (HPLC) with ultraviolet detection Part 2: Method using gas chromatography (GC) with electron capture detection (ECD) or mass spectrometric de

12、tection (MS) As a result of national implementation in Germany, the following should be noted: A shaking width of about 10 cm of the horizontal mechanical shaker as given in Subclause 6.2.2 is not realistic. Conventional horizontal mechanical shakers are preset according to type and are not adjustab

13、le. Experience has shown that shaking widths between 5 cm and 7 cm are adequate. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 565 DIN ISO 565 ISO 5725-2 DIN ISO 5725-2 ISO 11465 DIN EN 15934 ISO 11916-1 DIN ISO 11916-1 ISO 14507 DIN

14、19747 ISO 22892 DIN EN ISO 22892 WARNING Users of this Standard should be familiar with normal laboratory practice. This standard does not purport to address all the safety aspects, if any, associated with its use. It is the responsibility of the employer to establish appropriate safety and protecti

15、ve practices and to ensure compliance with any national regulatory conditions. IMPORTANT Expert assistance and specialized laboratories will be required to perform the analyses described in this standard. DIN ISO 11916-2:2014-11 4National Annex NA (informative) Bibliography DIN 19747, Investigation

16、of solids Pretreatment, preparation and processing of samples for chemical, biological and physical investigations DIN EN 15934, Sludge, treated biowaste, soil and waste Calculation of dry matter fraction after determination of dry residue or water content DIN EN ISO 22892, Soil quality Guidelines f

17、or the identification of target compounds by gas chromatography and mass spectrometry DIN ISO 565, Test sieves Metal wire cloth, perforated metal plate and electroformed sheet Nominal sizes of openings DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic

18、 method for the determination of repeatability and reproducibility of a standard measurement method DIN ISO 11916-1, Soil quality Determination of selected explosives and related compounds Part 1: Method using high-performance liquid chromatography (HPLC) with ultraviolet detection Soil quality Dete

19、rmination of selected explosives and related compounds Part 2: Method using gas chromatography (GC) with electron capture detection (ECD) or mass spectrometric detection (MS)1 ScopeThis part of ISO 11916 specifies the measurement of explosive and related compounds (nitroaromatics and nitroamines, as

20、 given in Table 1) in soils and soil materials. This part of ISO 11916 is intended for the trace analysis of explosives and related compounds by gas chromatography (GC) using electron capture detector(s) (ECD) or a mass spectrometer (MS) as detector.This part of ISO 11916 can be used when reliable a

21、nd specific identification of the compounds at low detection levels is required, e.g. for the evaluation of the toxic potential of soils contaminated with 2,6-DNT.Under the conditions specified in this part of ISO 11916, concentrations as low as 0,05 mg/kg dry matter can be determined, depending on

22、the substance. Similar compounds may be analysed using this method. This is, however, to be verified experimentally.This method is not suitable for the analysis of hexogen (RDX), octogen (HMX), hexyl, tetryl and nitropenta (PETN).Table 1 Selected explosive and related compounds (nitroaromatics and n

23、itroamines) for analysisCompound Abbreviation CAS-RNaNitrobenzene NB 98-95-31,3,5-Trinitrobenzeneb1,3,5-TNB 99-35-42-Nitrotoluene 2-NT 88-72-23-Nitrotoluene 3-NT 99-08-14-Nitrotoluene 4-NT 99-99-02,4-Dinitrotoluene 2,4-DNT 121-14-22,6-Dinitrotoluene 2,6-DNT 606-20-23,4-Dinitrotoluene 3,4-DNT 610-39-

24、92,4,6-Trinitrotoluene 2,4,6-TNT 118-96-74-Amino-2,6-dinitrotoluene 4-A-2,6-DNT 1946-51-02-Amino-4,6-dinitrotoluene 2-A-4,6-DNT 35572-78-2aCAS-RN: Chemical Abstract Service-Registry Number.b1,3,5-TNB gave poor interlaboratory trial results and its analysis could be problematic.2 Normative references

25、The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.DIN ISO

26、11916-2:2014-11 5 ISO 565, Test sieves Metal wire cloth, perforated metal plate and electroformed sheet Nominal sizes of openingsISO 11465, Soil quality Determination of dry matter and water content on a mass basis Gravimetric methodISO 22892, Soil quality Guidelines for the identification of target

27、 compounds by gas chromatography and mass spectrometry3 PrincipleExplosive materials in soils are extracted with methanol, using one of the following techniques: ultrasonic bath with ultrasonic waves as medium (USE); horizontal mechanical shaker at room temperature (MSE); Soxhlet apparatus that work

28、s isothermically at boiling temperature (SOX); pressurized liquid extraction (PLE).By means of a liquid/liquid extraction, the analytes are re-solved from the methanolic extract into toluene. Traces of methanol in the organic phase are then washed out with water and discarded. The toluenic phase is

29、dried, reconstituted, diluted (if necessary) and injected directly into a capillary gas chromatograph (GC). The analytes are detected by means of electron capture detection (ECD) or by mass spectrometry (MS).Substances are verified either by running samples through two columns of different polaritie

30、s with subsequent detection through ECD (simultaneous injection and operating with two ECD is recommended), or through MS detection utilizing known mass spectra and typical fragmentary ions.WARNING Take care when transporting, storing or treating explosive materials. High temperature, high pressure

31、and static electricity shall be prevented when storing explosive materials. Small amounts of explosive materials should be kept moist in a cool, dark place. Soil samples containing explosives with a mass fraction of less than 1 % do not have a risk of explosion.4 InterferencesSolvents, reagents, gla

32、ssware, and other hardware used for sample processing may yield artefacts and/or elevated baselines, causing misinterpretation of the chromatograms. All of these materials shall therefore be demonstrated to be free of contaminants and interferences through the analysis of method blanks.5 Reagents5.1

33、 GeneralAll reagents shall be blank-free and of recognized analytical grade.5.2 Chemicals5.2.1 Water.5.2.2 Acetone, C3H6O, for the cleaning of containers and devices.5.2.3 Methanol, CH3OH.5.2.4 Toluene, C6H5CH3.DIN ISO 11916-2:2014-11 6 5.2.5 Sodium chloride, NaCl, for phase separation.5.2.6 Sodium

34、sulfate, Na2SO4,anhydrous.5.2.7 Diatomaceous earth or sea sand, pelletized and calcinated (for PLE).5.3 Standard substances and solutions5.3.1 Standard substances5.3.1.1 Reference substancesCompounds listed in Table 1.5.3.1.2 Method-checking standardSuitable compound(s) not found in the sample, e.g.

35、 2,5-DNT.5.3.2 Standard solutions5.3.2.1 GeneralAll standard solutions used in this method shall be prepared as described below.NOTE If commercially available certified standard stock solutions (Table 1) are used, calibration solutions are prepared in volumetric flasks by diluting the stock solution

36、s with toluene (5.2.4) or methanol (5.2.3), for 5.3.1.2 respectively.All dilution steps shall not exceed the factor 100.5.3.2.2 Single-substance stock solutionsFor the preparation, weigh 50 mg 0,1 mg of the reference substances into 50 ml measuring flasks (scale: mg/ml), fill up to the mark with tol

37、uene (5.2.4) and let them dissolve completely.Transfer the stock solutions to amber-glass flasks and seal with PTFE-coated screw caps.The stock solutions can be kept in the refrigerator at 2 C to 6 C in the dark for up to 1 year.5.3.2.3 Multi-component stock solutionsPrepare multi-component stock so

38、lutions of different concentrations from the various single-substance stock solutions (5.3.2.2) by mixing and diluting with toluene (5.2.4).At concentrations below 1 mg/ml, solutions should be checked after one week as reference substances may decompose.For calibration standards, a minimum of 5 conc

39、entration levels is needed.6 Apparatus6.1 GeneralUsual laboratory apparatus and the following.6.1.1 Amber glass containers with caps containing polytetrafluoroethene (PTFE) coated lining.DIN ISO 11916-2:2014-11 7 6.1.2 Amber glass vials with caps containing septa with polytetrafluorethene (PTFE) coa

40、ted lining.6.1.3 Amber glass conical bottles with ground-in stopper.6.1.4 Perforated metal plate sieve, complying with ISO 565.6.1.5 Analytical balance, with a precision of at least 0,1 mg.6.1.6 Laboratory centrifuge, capable of producing an acceleration of at least 1 000g.6.1.7 Filter and suitable

41、filter discs, 0,45 m pore size.Any adsorption of the target analytes shall be avoided. No interfering material shall be eluated. PTFE or polyamide material is recommended.6.2 Equipment for extraction6.2.1 Temperature-controlled ultrasonic bath, 35 Hz, effective HF-power of at least 140 W.Water bath

42、capable of maintaining the temperature at (30 5) C or at (50 5) C during ultrasonic extraction.6.2.2 Horizontal mechanical shakerThe shaker shall maintain a frequency of 100 cycles/min and offer a shaking width of about 10 cm.6.2.3 Soxhlet apparatusExtractor, whose extraction chamber and syphon are

43、placed inside the steam chamber and suitably covered, or extractor with additionally heated extraction chamber, complete with boiling vessel, suitable heating mantle and reflux condenser, suitable for the extraction of a 50 g sample of soil with a hot solvent distillate through complete flooding of

44、the extractive.6.2.4 Pressurized liquid extractor (PLE)Pressurized liquid extraction device, equipped with extraction cells made of stainless steel or other material capable of withstanding the pressure levels (890 hPa/2 000 psi) necessary for this procedure; vials for collection of extracts, 40 ml

45、or 60 ml, pre-cleaned, open-top screw-cap with polytetrafluoroethylene (PTFE)-lined septum; filter disc, cellulose or glass fibre; cell cap sealing disc.6.3 Equipment for re-solution (solvent exchange)Microseparator, for the uptake of the toluenic extract.6.4 Gas chromatographic system (GC) with ECD

46、 or MSGas chromatograph, equipped with a non-discriminating injection system, suitable capillary columns and electron-capture detector(s) (ECD) or mass selective detector (MS).7 Procedure7.1 Sample pretreatment, sample storage and determination of water contentWhile taking a field-moist sample, remo

47、ve coarse impurities, e.g. plant residues and stones. Put the sample in an amber glass flask and store immediately in a cool, dark transport container.DIN ISO 11916-2:2014-11 8 Soil samples shall be analysed as soon as possible.When sample treatment is proceeded within 1 week after sampling, store the sample in a dark place at (4 2) C. Samples that are stored for longer periods (i.e. 1 week) prior to analysis, shall be stored at -20 C.Homogenize the sample by sieving through