1、BSI Standards PublicationBS ISO 11916-1:2013Soil quality Determinationof selected explosives andrelated compoundsPart 1: Method using high-performanceliquid chromatography (HPLC) withultraviolet detectionBS ISO 11916-1:2013 BRITISH STANDARDNational forewordThis British Standard is the UK implementat
2、ion of ISO 11916-1:2013.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 necessaryprovisions of a contra
3、ct. Users are responsible for its correctapplication. The British Standards Institution 2013. Published by BSI StandardsLimited 2013ISBN 978 0 580 66864 7ICS 13.080.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authori
4、ty of theStandards Policy and Strategy Committee on 30 September 2013.Amendments issued since publicationDate Text affectedBS ISO 11916-1:2013 ISO 2013Soil quality Determination of selected explosives and related compounds Part 1: Method using high-performance liquid chromatography (HPLC) with ultra
5、violet detectionQualit du sol Dosage dune slection dexplosifs et de composs apparents Partie 1: Mthode utilisant la chromatographie liquide haute performance (CLHP) avec dtection ultravioletINTERNATIONAL STANDARDISO11916-1First edition2013-09-01Reference numberISO 11916-1:2013(E)BS ISO 11916-1:2013I
6、SO 11916-1:2013(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 in any form or by any means, electronic or mechanical, including photocopying, or posting on the
7、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 postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb w
8、ww.iso.orgPublished in SwitzerlandBS ISO 11916-1:2013ISO 11916-1:2013(E) ISO 2013 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Principle 24 Interferences 25 Reagents 25.1 General . 25.2 Chemicals . 25.3 Standard substances and solutions . 36 Apparatus . 36.1 Ge
9、neral . 36.2 Equipment for extraction . 46.3 High-performance liquid chromatography (HPLC) system with DAD 47 Procedure. 47.1 Sample pretreatment, sample storage and determination of water content 47.2 Extraction 57.3 Storage of extract 78 High-performance liquid chromatographic analysis . 78.1 Gene
10、ral . 78.2 High-performance liquid chromatographic system 78.3 Calibration 88.4 Identification and quantification . 99 Calculation of results . 910 Quality assurance 911 Expression of results .1012 Test report 10Annex A (informative) Method-checking standard recovery limit 11Annex B (informative) HP
11、LC-UV-DAD conditions .12Annex C (informative) Precision data .16Bibliography .25BS ISO 11916-1:2013ISO 11916-1:2013(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Stand
12、ards 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 committee. International organizations, governmental and non-governmental, in liaison with ISO, also ta
13、ke 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 those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In pa
14、rticular 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 2. www.iso.org/directivesAttention is drawn to the possibility that some of the elements of this
15、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 document will be in the Introduction and/or on the ISO list of patent declarations received. www.iso.or
16、g/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 quality, Subcommittee SC 3, Chemical methods and soil characteristics.ISO 11916 consists of the follo
17、wing 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 Part 2: Method using gas chromatography (GC) with electron capture detection (ECD) or mass spectr
18、ometric detection (MS)iv ISO 2013 All rights reservedBS ISO 11916-1:2013INTERNATIONAL STANDARD ISO 11916-1:2013(E)Soil quality Determination of selected explosives and related compounds Part 1: Method using high-performance liquid chromatography (HPLC) with ultraviolet detection1 ScopeThis part of I
19、SO 11916 specifies the measurement of explosive and related nitrocompounds (as 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 high-performance liquid chromatography (HPLC) using an ultraviolet (UV) detec
20、tor.Under the conditions specified in this part of ISO 11916, concentrations as low as 0,1 mg/kg to 1 mg/kg dry matter can be determined, depending on the substance. Similar compounds, in particular various nitroaromatics, by-products and degradation products of explosive compounds may be analysed u
21、sing this method. However, the applicability should be checked on a case-by-case basis.Table 1 Explosive and related nitrocompounds for analysisCompound Abbreviation CAS-RNaNitrobenzene NB 98-95-31,3-Dinitrobenzene 1,3-DNB 99-65-01,3,5-Trinitrobenzeneb1,3,5-TNB 99-35-42-Nitrotoluene 2-NT 88-72-23-Ni
22、trotoluene 3-NT 99-08-14-Nitrotoluene 4-NT 99-99-02,4-Dinitrotoluene 2,4-DNT 121-14-22,6-Dinitrotoluene 2,6-DNT 606-20-22,4,6-Trinitrotoluene 2,4,6-TNT 118-96-74-Amino-2,6-dinitrotoluene 4-A-2,6-DNT 19406-51-62-Amino-4,6-dinitrotoluene 2-A-4,6-DNT 35572-78-2N-Methyl-N-2,4,6-tetranitroanilinebTetryl
23、479-45-82,4,6-Trinitro-N-(2,4,6-trinitrophenyl)aniline Hexyl 131-73-71,3,5-Trinitrohexahydro-1,3,5-triazine RDX 121-82-41,3,5,7-Tetranitrooctahydro-1,3,5,7-tetrazocine HMX 2691-41-0PentaerythrityltetranitratebPETN 78-11-5aCAS-RN: Chemical Abstract Service-Registry NumberbPETN, 1,3,5-TNB and tetryl g
24、ave poor interlaboratory trial results and their analysis could be problematic2 Normative referencesThe 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 r
25、eferences, the latest edition of the referenced document (including any amendments) applies. ISO 2013 All rights reserved 1BS ISO 11916-1:2013ISO 11916-1:2013(E)ISO 565, Test sieves Metal wire cloth, perforated metal plate and electroformed sheet Nominal sizes of openingsISO 11465, Soil quality Dete
26、rmination of dry matter and water content on a mass basis Gravimetric methodISO 22478, Water quality Determination of certain explosives and related compounds Method using high-performance liquid chromatography (HPLC) with UV detection3 PrincipleExplosive materials in soils are extracted with aceton
27、itrile or 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 temperature (SOX); pressurized liquid extraction (PLE).The extract containi
28、ng the analytes is either injected directly, or if necessary diluted prior to injection, into a reversed-phase high-performance liquid chromatography system (HPLC) and the analytes are detected by means of a diode array detector (DAD).WARNING Take care when transporting, storing or treating explosiv
29、e materials. High temperature, high pressure 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 exp
30、losion.4 InterferencesSolvents, reagents, glassware, 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 throug
31、h the analysis of method blanks.Tetryl may decompose in methanol or water at (or above) room temperature. Degradation products of tetryl appear as a shoulder of 2,4,6-TNT when a C18column is used. In this case, evaluation of 2,4,6-TNT should be based on peak height rather than peak area.Samples cont
32、aining 2,4,6-trinitrobenzoic acid should not be extracted with acetonitrile as it may result in the overestimation of 1,3,5-TNB, due to decarboxylation.5 Reagents5.1 GeneralAll reagents shall be blank-free and of recognized analytical grade. They shall not contain any measurable quantities of UV-abs
33、orbing substances that may interfere with the determination.5.2 Chemicals5.2.1 Water.5.2.2 Acetone, C3H6O, for the cleaning of containers and devices.5.2.3 Acetonitrile, CH3CN, HPLC grade or equivalent.2 ISO 2013 All rights reservedBS ISO 11916-1:2013ISO 11916-1:2013(E)5.2.4 Methanol, CH3OH, HPLC gr
34、ade or equivalent.5.2.5 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. 2,5-DNT
35、.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 solutions with a
36、cetonitrile (5.2.3) or methanol (5.2.4), 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 acetonitrile (5.2.
37、3) or methanol (5.2.4), respectively 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
38、multi-component stock solutions of different concentrations from the various single-substance stock solutions (5.3.2.2) by mixing and diluting with acetonitrile (5.2.3) or methanol (5.2.4), respectively.At concentrations below 1 mg/ml, solutions should be checked after one week as reference substanc
39、es may decompose.For calibration standards, a minimum 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.6.1.2 Amber glass vials with caps containing septa
40、 with polytetrafluorethene (PTFE) coated lining. ISO 2013 All rights reserved 3BS ISO 11916-1:2013ISO 11916-1:2013(E)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
41、 Laboratory centrifuge, capable of producing an acceleration of at least 1 000g.6.1.7 pH-meter, to adjust the pH of the mobile phase for HPLC.6.1.8 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. PTF
42、E 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 capable of maintaining the temperature at (30 5) C or at (50 5) C during ultrasonic extraction.6.2.2 Horizontal mechanical shakerThe
43、 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 placed inside the steam chamber and suitably covered, or extractor with additionally heated extraction chamber, complete with boilin
44、g 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 the extractive.6.2.4 Pressurized liquid extractor (PLE)Pressurized liquid extraction device, equipped with extraction cells made of
45、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 or 60 ml, pre-cleaned, open-top screw-cap with polytetrafluoroethylene (PTFE)-lined septum; filter disc, cellulose or glass fibre; c
46、ell cap sealing disc.6.3 High-performance liquid chromatography (HPLC) system with DADHPLC system, consisting of a pump which supports a pressure of at least 40 MPa (400 bar), an injection system with a loop capacity of 100 l and a diode array detector (DAD) with wavelength range of 200 nm to 400 nm
47、 (or higher).Other specifications of the HPLC system should be in accordance with ISO 22478.7 Procedure7.1 Sample pretreatment, sample storage and determination of water contentWhile taking a field-moist sample, remove coarse impurities, e.g. plant residues and stones. Put the sample in an amber gla
48、ss flask and store immediately in a cool, dark transport container.Soil samples shall be analysed as soon as possible.4 ISO 2013 All rights reservedBS ISO 11916-1:2013ISO 11916-1:2013(E)When sample treatment is proceeded within 1 week after sampling, store the sample in a dark place at (4 2) C. Samp
49、les 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 aperture 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 methano
