1、BRITISH STANDARDBS EN ISO 22478:2006Water quality Determination of certain explosives and related compounds Method using high-performanceliquid chromatography (HPLC) with UV detectionThe European Standard EN ISO 22478:2006 has the status of a British StandardICS 13.060.50g49g50g3g38g50g51g60g44g49g4
2、2g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN ISO 22478:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 10
3、 March 2006 BSI 10 March 2006ISBN 0 580 47943 9National forewordThis British Standard is the official English language version ofEN ISO 22478:2006. It is identical with ISO 22478:2006.The UK participation in its preparation was entrusted by Technical Committee EH/3, Water quality, to Subcommittee EH
4、/3/2, Physical, chemical and biochemical methods, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep UK interests informed; monitor related internati
5、onal and European developments and promulgate them in the UK.A list of organizations represented on this subcommittee can be obtained on request to its secretary.Cross-referencesThe British Standards which implement international or European publications referred to in this document may be found in
6、the BSI Catalogueunder the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online.This publication does not purport to include all the necessary provisions of a contract. Users are responsible
7、for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations.Summary of pagesThis document comprises a front cover, an inside front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii to v, a blank page, pa
8、ges 1 to 24, an inside back cover and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendments issued since publicationAmd. No. Date CommentsEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 22478February 2006ICS 13.060.50English Ver
9、sionWater quality - Determination of certain explosives and relatedcompounds - Method using high-performance liquidchromatography (HPLC) with UV detection (ISO 22478:2006)Qualit de leau - Dosage de certains explosifs et decomposs apparents - Mthode utilisant lachromatographie en phase liquide haute
10、performance(CLHP) avec dtection UV (ISO 22478:2006)Wasserbeschaffenheit - Bestimmung ausgewhlterExplosivstoffe und verwandter Verbindungen - Verfahrenmittels Hochleistungs-Flssigkeitschromatographie (HPLC)mit UV-Detektion (ISO 22478:2006)This European Standard was approved by CEN on 6 February 2006.
11、CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on app
12、lication to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has t
13、he same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,
14、Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2006 CEN All rights of exploitation in any form and by any means reservedworldwid
15、e for CEN national Members.Ref. No. EN ISO 22478:2006: EForeword This document (EN ISO 22478:2006) has been prepared by Technical Committee ISO/TC 147 “Water quality“ in collaboration with Technical Committee CEN/TC 230 “Water analysis“, the secretariat of which is held by DIN.This European Standard
16、 shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by August 2006, and conflicting national standards shall be withdrawn at the latest by August 2006. According to the CEN/CENELEC Internal Regulations, the national standards
17、 organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romani
18、a, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 22478:2006 has been approved by CEN as EN ISO 22478:2006 without any modifications. EN ISO 22478:2006Reference numberISO 22478:2006(E)INTERNATIONAL STANDARDISO22478First edition2006-02-15Water qu
19、ality Determination of certain explosives and related compounds Method using high-performance liquid chromatography (HPLC) with UV detection Qualit de leau Dosage de certains explosifs et de composs apparents Mthode utilisant la chromatographie en phase liquide haute performance (CLHP) avec dtection
20、 UV EN ISO 22478:2006iiEN ISO 22478:2006iiiContents Page Foreword iv Introduction v 1 Scope . 1 2 Normative references . 1 3 Principle. 1 4 Interference . 4 5 Reagents 4 6 Apparatus 5 7 Sampling 6 8 Procedure 6 9 Calibration . 8 10 Evaluation 10 11 Expression of results . 11 12 Test report . 11 Anne
21、x A (informative) Examples of HPLC chromatograms. 12 Annex B (informative) UV spectra of compounds from Table 1 19 Annex C (informative) Interference due to degradation of tetryl (CE) on exposure to daylight 22 Annex D (informative) Precision data. 24 EN ISO 22478:2006iv Foreword ISO (the Internatio
22、nal 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 has been
23、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 electrotechnical standar
24、dization. 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 bodies for v
25、oting. 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 or all s
26、uch patent rights. ISO 22478 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical methods. vIntroduction Explosives and related compounds are frequently encountered in groundwater areas near to soil sites contaminated by armaments waste
27、 and may also be found in drinking water taken from nearby catchment areas. The range of pollutants will depend on the waste concerned, but will not, as a rule, include all the compounds listed in Table 1. Instead, samples of groundwater containing such pollutants may contain numerous other substanc
28、es, such as nitro- and dinitrobenzoic acid, nitrophenols and aromatic amines. The compounds listed in Table 1 are frequently used for exploratory examinations of armaments waste. When using this International Standard, it may be necessary in some cases to determine whether and to what extent particu
29、lar problems will require the specification of additional conditions. EN ISO 22478:2006blank1Water quality Determination of certain explosives and related compounds Method using high-performance liquid chromatography (HPLC) with UV detection WARNING Persons using this International Standard should b
30、e familiar with normal laboratory practice. This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory condition
31、s. IMPORTANT It is absolutely essential that tests conducted in accordance with this International Standard be carried out by suitably trained staff. 1 Scope This International Standard specifies a method for determination of certain explosives, in particular nitrotoluenes, nitroamines and nitrate e
32、sters, and related compounds (by-products and degradation products), such as those listed in Table 1, in drinking water, groundwater and surface water. Depending on the type of sample and the compound to be analysed, the lower limit of the working range for nitroaromatics and nitramines can be assum
33、ed to be between 0,1 g/l and 0,5 g/l (in some cases, the lower limit may be extended down to 0,05 g/l). The lower limit of the working range for nitrate esters may be assumed to be higher (0,5 g/l or more). Similar compounds, in particular other nitroaromatics, may also be determined by this method,
34、 but its applicability will have to be checked in each individual case. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced
35、 document (including any amendments) applies. ISO 3696, Water for analytical laboratory use Specification and test methodsISO 5667-1, Water quality Sampling Part 1: Guidance on the design of sampling programmesISO 5667-2, Water quality Sampling Part 2: Guidance on sampling techniquesISO 5667-3, Wate
36、r quality Sampling Part 3: Guidance on the preservation and handling of water samples3 Principle The substances in the water sample are concentrated by solid-phase extraction using a polystyrene/divinylbenzene-based adsorbent. After elution with a solvent mixture, the eluate is concentrated and the
37、substances are separated by high-performance liquid chromatography (HPLC) and analysed using a UV photodiode array (UV-PDA) detector. EN ISO 22478:20062Table 1 Explosives and related compounds determined by this method (the compounds listed here are particularly likely to be encountered in water sam
38、ples containing armaments waste)Molar massReference No./ letter in example chromatograms in Clause Name AbbreviationaOther name CASbNo. g/mol A.1 A.2 A.3 B.1 2,4,6-Trinitrophenol PA Picric acid 88-89-1 229,1 1 2 1 a 1,3,5,7-Tetranitro-octahydro-1,3,5,7-tetrazocine HMX Octogen 2691-41-0 296,2 2 1 2 b
39、 1,3,5-Trinitro-hexahydro-1,3,5-triazine RDX Hexogen 121-82-4 222,1 3 3 4 d 2,2,4,4,6,6-Hexanitrodiphenylamine Hexyl 131-73-7 439,2 4 19 3 c Ethylene glycol dinitrate EGDN 628-96-6 152,1 5 4 5 e Diethylene glycol dinitrate DEGN 693-21-0 196,1 6 5 6 f 1,3,5-Trinitrobenzene 1,3,5-TNB 99-35-4 213,1 7 6
40、 7 g 1,3-Dinitrobenzene 1,3-DNB 99-65-0 168,1 8 7 9 i N-Methyl-N-2,4,6-tetranitroaniline CE Tetryl 479-45-8 287,2 9 8 8 h Glycerol trinitrate NG Nitroglycerine 55-63-0 227,1 10 9 10 j 2,4,6-Trinitrotoluene 2,4,6-TNT TNT 118-96-7 227,1 11 10 11 k 4-Amino-2,6-dinitrotoluene 4-A-2,6-DNT 19406-51-6 197,
41、1 12 11 12 l 2-Amino-4,6-dinitrotoluene 2-A-4,6-DNT 35572-78-2 197,1 13 12 13 m 2,6-Dinitrotoluene 2,6-DNT 606-20-2 182,1 14 13 14 n 2,4-Dinitrotoluene 2,4-DNT 121-14-2 182,1 15 14 15 o 2-Nitrotoluene 2-NT 88-72-2 137,1 16 15 17 q Pentaerythritol tetranitrate PETN Nitropenta 78-11-5 316,2 17 18 16 p
42、 4-Nitrotoluene 4-NT 99-99-0 137,1 18 16 18 r 3-Nitrotoluene 3-NT 99-08-1 137,1 19 17 19 s Diphenylamine DPA 122-39-4 169,24 20 aStandard abbreviations, some of Anglo-Saxon origin. bChemical Abstracts Service. The structural formulae of selected compounds are given in Figure 1. EN ISO 22478:20063Pic
43、ric acid (PA) Octogen (HMX) Hexogen (RDX) Hexyl Ethylene glycol dinitrate (EGDN) Diethylene glycol dinitrate (DEGN) Tetryl (CE) Nitroglycerine (NG) Nitropenta (PETN) 1,3,5-Trinitrobenzene 1,3-Dinitrobenzene 2,4,6-Trinitrotoluene (TNT) 4-Amino-2,6-dinitrotoluene2-Amino-4,6-dinitrotoluene 2,6-Dinitrot
44、oluene 2,4-Dinitrotoluene 2-Nitrotoluene 4-Nitrotoluene 3-Nitrotoluene Diphenylamine (DPA) Figure 1 Structural formulae of selected explosives EN ISO 22478:200644 Interference 4.1 Sampling To avoid interference, collect samples as specified in Clause 7, observing the instructions given in ISO 5667-1
45、, ISO 5667-2 and ISO 5667-3. 4.2 Filtration If the sample contains suspended matter, first filter it through a borosilicate glass fibre filter to prevent blockage of the solid phase concentrating cartridge and record this operation in the test report. 4.3 Concentration by evaporation Mononitrotoluen
46、es may be lost when the eluates are evaporated as specified in 8.2. 4.4 Chromatography Asymmetrical peaks and peaks that are wider than normal may indicate incompletely resolved peaks or peak overlapping due to compounds with similar retention times and/or absorption at the same or at a similar wave
47、length to those of the compounds being determined. To detect peak overlaps, check the peak purity and compare the UV spectrum with that of a reference material. Interference may also be caused by humic matter eluted in the same range as the analytes being determined. 4.5 Exposure to light Reference
48、solutions, samples and sample extracts may decompose on exposure to light. This is particularly important in the case of tetryl (see Annex C). Therefore a detailed investigation of the recovery of tetryl should be carried out. 4.6 Determination of hexogen When determining small concentrations of hex
49、ogen, interference may be caused by high concentrations of nitroaromatics. 5 Reagents The reagents shall not have blank values that would interfere with the HPLC analysis. If available, use reagents of HPLC grade or residue grade. The solvents shall not contain any measurable UV-absorbing substances that interfere with the method. 5.1 Water, complying with grade 1 as defined in ISO 3696. The water shall not contain any measurable quantities of UV-absorbing substances that interfere with
