1、 DEUTSCHE NORM July 2006DIN EN ISO 22478 ICS 13.060.45 Supersedes DIN 38407-21:2001-12 Water quality Determination of certain explosives and related compounds Method using high-performance liquid chromatography (HPLC) with UV detection (ISO 22478:2006) English version of DIN EN ISO 22478:2006-07 Was
2、serbeschaffenheit Bestimmung ausgewhlter Explosivstoffe und verwandter Verbindungen Verfahren mittels Hochleistungs-Flssigkeitschromatographie (HPLC) mit UV-Detektion (ISO 22478:2006) Englische Fassung DIN EN ISO 22478:2006-07 Document comprises 31 pages No part of this standard may be reproduced wi
3、thout prior permission of DIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany, has the exclusive right of sale for German Standards (DIN-Normen). English price group 13 www.din.de www.beuth.de !,p#“11.06 9770090DIN EN ISO 22478:2006-07 2 This standard is part of
4、 the series Deutsche Einheitsverfahren zur Wasser-, Abwasser- und Schlammunter-suchung Gemeinsam erfassbare Stoffgruppen (Gruppe F) (German standard methods for the examination of water, waste water and sludge Substance group analysis (group F). National foreword This standard has been prepared by T
5、echnical Committee ISO/TC 147 Water quality in collaboration with Technical Committee CEN/TC 230 Water analysis (Secretariat: Germany). The responsible German body involved in its preparation was the Normenausschuss Wasserwesen (Water Practice Standards Committee), Technical Committee NA 119-01-03 A
6、A Wasseruntersuchung. Expert assistance and specialized laboratories will be required to perform the analysis described in this standard. Depending on the objective of the analysis, a check shall be made on a case-by-case basis as to whether and to what extent additional conditions will have to be s
7、pecified. Standard methods published as DIN Standards are obtainable from Beuth Verlag GmbH, either individually or grouped in volumes. The standard methods included in the loose-leaf publication entitled Deutsche Einheits-verfahren zur Wasser-, Abwasser- und Schlammuntersuchung will continue to be
8、published by Wiley-VCH Verlag and Beuth Verlag GmbH. All standard methods relevant to the Abwasserverordnung (Waste Water Regulation) (AbwV) included in the new Regulation on Section 7a of the Gesetz zur Ordnung des Wasserhaushalts (German Water Management Act together with the Abwasserverordnung an
9、d the Gesetz zur Ordnung des Wasserhaushalts and other valid administrative regulations on waste water have been published as a loose-leaf collection “Analysenver-fahren in der Abwasserverordnung Rechtsvorschriften und Normen” *), with Supplement 1 (DIN Standards, Supplement 2 (DIN EN and DIN EN ISO
10、 Standards) and 3 (DIN, DIN EN and DIN EN ISO Standards). Standard methods or draft standards bearing the group title German standard methods for the examination of water, waste water and sludge are classified under the following categories (main titles): General information (group A) (DIN 38402) Se
11、nsory analysis (group B) (DIN 38403) Physical and physicochemical parameters (group C) (DIN 38404) Anions (group D) (DIN 38405) Cations (group E) (DIN 38406) Substance group analysis (group F) (DIN 38407) Gaseous constituents (group G) (DIN 38408) Parameters characterizing effects and substances (gr
12、oup H) (DIN 38409) Biological-ecological methods of analysis (group M) (DIN 38410) Microbiological methods (group K) (DIN 38411) Test methods using water organisms (group L) (DIN 38412) *) Available in German. DIN EN ISO 22478:2006-07 3 Individual constituents (group P) (DIN 38413) Sludge and sedime
13、nts (group S) (DIN 38414) Bio-assays with microorganisms (group T) (DIN 38415) In addition to the methods described in the DIN 38402 to DIN 38415 series of standards, there are a number of European and International Standards available as DIN EN, DIN EN ISO and DIN ISO Standards, which also form par
14、t of the collection of German standard methods. Information on Parts of these series of standards that have already been published can be obtained from the offices of the Normenausschuss Wasserwesen, telephone (030) 2601-2448, or from Beuth Verlag GmbH, Burggrafenstrae 6, 10787 Berlin, Germany. The
15、DIN Standards corresponding to the International Standards referred to in clause 2 of the EN are as follows: ISO 3696 DIN ISO 3696 ISO 5667-1 DIN EN 25667-1 ISO 5667-2 DIN EN 25667-2 ISO 5667-3 DIN EN ISO 5667-3 Amendments This standard differs from DIN 38407-21:2001-12 as follows: a) The number of
16、the standard has been changed. b) Details of the test set-up, procedure and evaluation have been changed. c) The standard has been editorially revised. Previous editions DIN 38407-21: 2001-12 National Annex NA (informative) Bibliography DIN EN 25667-1, Water quality Sampling Part 1: Guidance on the
17、design of sampling programmes DIN EN 25667-2, Water quality Sampling Part 2: Guidance on sampling techniques DIN EN ISO 5667-3, Water quality Sampling Part 3: Guidance on the preservation and handling of water samples DIN ISO 3696, Water for analytical laboratory use Specification and test methods D
18、IN EN ISO 22478:2006-07 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 22478 February 2006 ICS 13.060.50 English Version Water quality - Determination of certain explosives and related compounds - Method using high-performance liquid chromatography (HPLC)
19、 with UV detection (ISO 22478:2006) Qualit de leau - Dosage de certains explosifs et de composs apparents - Mthode utilisant la chromatographie en phase liquide haute performance (CLHP) avec dtection UV (ISO 22478:2006) Wasserbeschaffenheit - Bestimmung ausgewhlter Explosivstoffe und verwandter Verb
20、indungen - Verfahren mittels Hochleistungs-Flssigkeitschromatographie (HPLC) mit UV-Detektion (ISO 22478:2006) This European Standard was approved by CEN on 6 February 2006. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this Europ
21、ean 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 Central Secretariat or to any CEN member. This European Standard exists in three official versions (English,
22、 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 Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech
23、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 United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPE
24、N DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2006 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 22478:2006: EEN ISO 22478:2006 (E) 2 Foreword This document (EN ISO 22
25、478:2006) 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 shall be given the status of a national standard, either by publication of an identical
26、 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 organizations of the following countries are bound to implement this European Standard:
27、 Austria, Belgium, 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 United Kingdom. Endorsement notice
28、 The text of ISO 22478:2006 has been approved by CEN as EN ISO 22478:2006 without any modifications. EN ISO 22478:2006 (E) 3 Contents Page Foreword .2 Introduction.4 1 Scope5 2 Normative references5 3 Principle .5 4 Interference 8 5 Reagents 8 6 Apparatus.9 7 Sampling 10 8 Procedure.10 9 Calibration
29、12 10 Evaluation 14 11 Expression of results15 12 Test report15 Annex A (informative) Examples of HPLC chromatograms .16 Annex B (informative) UV spectra of compounds from Table 1.23 Annex C (informative) Interference due to degradation of tetryl (CE) on exposure to daylight.26 Annex D (informative)
30、 Precision data .28 EN ISO 22478:2006 (E) 4 Introduction Explosives and related compounds are frequently encountered in groundwater areas near to soil sites contaminated by armaments waste and may also be found in drinking water taken from nearby catchment areas. The range of pollutants will depend
31、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 substances, such as nitro- and dinitrobenzoic acid, nitrophenols and aromatic amines. The compounds listed in Table 1 ar
32、e 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 particular problems will require the specification of additional conditions. EN ISO 22478:2006 (E) 5 WARNING Persons us
33、ing this International Standard should be 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 complianc
34、e with any national regulatory conditions. 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
35、nitrotoluenes, nitroamines and nitrate esters, 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 ni
36、troaromatics and nitramines can be assumed 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
37、, may also be determined by this method, 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 referenc
38、es, the latest edition of the referenced document (including any amendments) applies. ISO 3696, Water for analytical laboratory use Specification and test methods ISO 5667-1, Water quality Sampling Part 1: Guidance on the design of sampling programmes ISO 5667-2, Water quality Sampling Part 2: Guida
39、nce on sampling techniques ISO 5667-3, Water quality Sampling Part 3: Guidance on the preservation and handling of water samples 3 Principle The substances in the water sample are concentrated by solid-phase extraction using a polystyrene/divinylbenzene-based adsorbent. After elution with a solvent
40、mixture, the eluate is concentrated and the substances are separated by high-performance liquid chromatography (HPLC) and analysed using a UV photodiode array (UV-PDA) detector. EN ISO 22478:2006 (E) 6 Table 1 Explosives and related compounds determined by this method (the compounds listed here are
41、particularly likely to be encountered in water samples containing armaments waste) Molar mass Reference 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
42、,5,7-tetrazocine HMX Octogen 2691-41-0 296,2 2 1 2 b 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
43、 f 1,3,5-Trinitrobenzene 1,3,5-TNB 99-35-4 213,1 7 6 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-
44、Amino-2,6-dinitrotoluene 4-A-2,6-DNT 19406-51-6 197,1 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 t
45、etranitrate PETN Nitropenta 78-11-5 316,2 17 18 16 p 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 a Standard abbreviations, some of Anglo-Saxon origin. bChemical Abstracts Service. The structural formulae of selected c
46、ompounds are given in Figure 1. EN ISO 22478:2006 (E) 7 Picric 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-Amin
47、o-2,6-dinitrotoluene2-Amino-4,6-dinitrotoluene 2,6-Dinitrotoluene 2,4-Dinitrotoluene 2-Nitrotoluene 4-Nitrotoluene 3-Nitrotoluene Diphenylamine (DPA) Figure 1 Structural formulae of selected explosives EN ISO 22478:2006 (E) 8 4 Interference 4.1 Sampling To avoid interference, collect samples as spec
48、ified in Clause 7, observing the instructions given in ISO 5667-1, 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
49、the test report. 4.3 Concentration by evaporation Mononitrotoluenes 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 wavelength to those of the compounds being determined. To detect peak overlaps, check the peak purity and com
