BS ISO 11916-2-2013 Soil quality Determination of selected explosives and related compounds Method using gas chromatography (GC) with electron capture detection (ECD) or mass spect.pdf

1、BSI Standards PublicationBS ISO 11916-2:2013Soil quality Determinationof selected explosives andrelated compoundsPart 2: Method using gas chromatography(GC) with electron capture detection (ECD)or mass spectrometric detection (MS)BS ISO 11916-2:2013 BRITISH STANDARDNational forewordThis British Stan

2、dard is the UK implementation of ISO 11916-2:2013.The UK participation in its preparation was entrusted to TechnicalCommittee EH/4, Soil quality.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the neces

3、saryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2013. Published by BSI StandardsLimited 2013ISBN 978 0 580 67545 4ICS 13.080.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was p

4、ublished under the authority of theStandards Policy and Strategy Committee on 30 September 2013.Amendments issued since publicationDate Text affectedBS ISO 11916-2:2013 ISO 2013Soil quality Determination of selected explosives and related compounds Part 2: Method using gas chromatography (GC) with e

5、lectron capture detection (ECD) or mass spectrometric detection (MS)Qualit 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)INTERNATIONAL

6、STANDARDISO11916-2First edition2013-09-01Reference numberISO 11916-2:2013(E)BS ISO 11916-2:2013ISO 11916-2:2013(E)ii ISO 2013 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2013All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise i

7、n any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase pos

8、tale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 11916-2:2013ISO 11916-2:2013(E) ISO 2013 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Principle 24 Interferences 25 Reagents

9、 25.1 General . 25.2 Chemicals . 25.3 Standard substances and solutions . 36 Apparatus . 36.1 General . 36.2 Equipment for extraction . 46.3 Equipment for re-solution (solvent exchange) . 46.4 Gas chromatographic system (GC) with ECD or MS 47 Procedure. 47.1 Sample pretreatment, sample storage and d

10、etermination of water content 47.2 Extraction 57.3 Storage of extract 78 Gas chromatographic analysis 78.1 General . 78.2 Gas chromatographic system 88.3 Calibration 88.4 Identification and quantification . 99 Calculation of results 109.1 General 109.2 Calculation . 1010 Quality assurance .1111 Expr

11、ession of results .1212 Test report 12Annex A (informative) GC/ECD conditions 13Annex B (informative) GC/MS conditions .16Annex C (informative) Precision data .18Bibliography .25BS ISO 11916-2:2013ISO 11916-2:2013(E)ForewordISO (the International Organization for Standardization) is a worldwide fede

12、ration 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 has been established has the right to be represented on that commi

13、ttee. 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 electrotechnical standardization.The procedures used to develop this document and

14、 those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part

15、 2. www.iso.org/directivesAttention 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 or all such patent rights. Details of any patent rights identified during the development of the docum

16、ent will be in the Introduction and/or on the ISO list of patent declarations received. www.iso.org/patentsAny trade name used in this document is information given for the convenience of users and does not constitute an endorsement.The committee responsible for this document is ISO/TC 190, Soil qua

17、lity, Subcommittee SC 3, Chemical methods and soil characteristics.ISO 11916 consists of the following parts, 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

18、 Part 2: Method using gas chromatography (GC) with electron capture detection (ECD) or mass spectrometric detection (MS)iv ISO 2013 All rights reservedBS ISO 11916-2:2013INTERNATIONAL STANDARD ISO 11916-2:2013(E)Soil quality Determination of selected explosives and related compounds Part 2: Method u

19、sing 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 given in Table 1) in soils and soil materials. This part of ISO 11916

20、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 and specific identification of the compounds at low detection levels is

21、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 the substance. Similar compounds may be analysed using this method. Thi

22、s 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 nitroamines) for analysisCompound Abbreviation CAS-RNaNitrobenzene NB 98

23、-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 610-39-92,4,6-Trinitrotoluene 2,4,6-TNT 118-96-74-Amino-2,6-dinitrotoluene 4-A

24、-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 referencesThe following documents, in whole or in part, are normatively reference

25、d 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. ISO 2013 All rights reserved 1BS ISO 11916-2:2013ISO 11916-2:2013(E)ISO 565, T

26、est 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 compounds by gas chromatogr

27、aphy 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 works isothermically at boiling

28、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 dried, reconstituted, dilute

29、d (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 polarities with subsequent detection

30、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 and static electricity shall

31、 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, glassware, and other hardware u

32、sed 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 GeneralAll reagents shall b

33、e 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, C6H5CH3.2 ISO 2013 All rights reservedBS ISO 11916-2:2013ISO 11916-2:2013(E)5.2.5 Sodium chloride, NaCl, for phase separation

34、.5.2.6 Sodium 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 th

35、e sample, e.g. 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

36、stock solutions 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

37、 mark with toluene (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-comp

38、onent stock solutions 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 min

39、imum of 5 concentration 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. ISO 2013 All rights reserved 3BS ISO 11916-2:2013ISO 11916-2:2013(E)6.1.2 Amber glass vials with c

40、aps containing septa with polytetrafluorethene (PTFE) coated 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 a

41、cceleration of at least 1 000g.6.1.7 Filter and suitable 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

42、, 35 Hz, effective HF-power of at least 140 W.Water bath 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 app

43、aratusExtractor, whose extraction chamber and syphon are 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 wi

44、th a hot solvent distillate through complete flooding of 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

45、 this procedure; vials for collection of extracts, 40 ml 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 tolu

46、enic extract.6.4 Gas chromatographic system (GC) with ECD 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 determinatio

47、n of water contentWhile taking a field-moist sample, remove 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.4 ISO 2013 All rights reservedBS ISO 11916-2:2013ISO 11916-2:2013(E)Soil samples shall be an

48、alysed 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 a sieve with an apert

49、ure of 2 mm (6.1.4).For the determination of volatile nitroaromatics (2-NT, 3-NT, 4-NT, NB) a sample withdrawal is to be carried out, in order to minimize evaporative losses.Samples that were primarily taken for the determination of volatile compounds may also be taken by filling them immediately (on-site) in an extraction vial containing methanol. Then, pretreat samples according to 7.2.2 or 7.2.3. These samples have to be considered and reported as non-homogenized unscreened random samples.In order