1、BSI Standards PublicationBS ISO 17378-2:2014Water quality Determinationof arsenic and antimonyPart 2: Method using hydride generationatomic absorption spectrometry (HG-AAS)Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Not for ResaleNo reproduction
2、 or networking permitted without license from IHS-,-,-BS ISO 17378-2:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 17378-2:2014.It supersedes BS EN ISO 11969:1996 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommit
3、tee EH/3/2, Physical chemical and biochemical methods.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 contract. Users are responsible for its correctapplication. The British
4、 Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 70964 7ICS 13.060.50Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 28 February 2
5、014.Amendments issued since publicationDate Text affectedCopyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Not for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS ISO 17378-2:2014 ISO 2014Water quality Determination of ar
6、senic and antimony Part 2: Method using hydride generation atomic absorption spectrometry (HG-AAS)Qualit de leau Dosage de larsenic et de lantimoine Partie 2: Mthode par spectromtrie dabsorption atomique gnration dhydrures (HG-AAS)INTERNATIONAL STANDARDISO17378-2First edition2014-02-01Reference numb
7、erISO 17378-2:2014(E)Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Not for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS ISO 17378-2:2014ISO 17378-2:2014(E)ii ISO 2014 All rights reservedCOPYRIGHT PROTECTED DOCUMENT
8、 ISO 2014All 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 internet or an intranet, without prior written permission. Permission can be
9、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 www.iso.orgPublished in SwitzerlandCopyright British Standards Institution Pro
10、vided by IHS under license with BSI - Uncontrolled Copy Not for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS ISO 17378-2:2014ISO 17378-2:2014(E) ISO 2014 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Principle 23.1
11、Arsenic . 23.2 Antimony 24 Interferences 24.1 General . 24.2 Arsenic . 34.3 Antimony 35 Reagents 35.1 General requirements . 36 Apparatus . 87 Sampling and sample preparation 97.1 Sampling technique 97.2 Pre-reduction . 98 Instrumental set up 109 Procedure109.1 General requirements 109.2 Analysis us
12、ing the method of standard calibration 119.3 Analysis using the standard addition method of calibration .1110 Calibration and data analysis .1210.1 General requirements 1210.2 Calculation using the calibration curve 1210.3 Calculation using the standard addition method .1311 Expression of results .1
13、312 Test report 13Annex A (informative) Additional information 14Annex B (informative) Schematic flow diagram and signal response 15Annex C (informative) Example of enrichment technique 17Annex D (informative) Performance data 19Bibliography .22Copyright British Standards Institution Provided by IHS
14、 under license with BSI - Uncontrolled Copy Not for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS ISO 17378-2:2014ISO 17378-2:2014(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bod
15、ies). 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 committee. International organizations, governmental and
16、 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 those intended for its further maintenance are des
17、cribed 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 2 (see www.iso.org/directives).Attention is drawn
18、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 document will be in the Introduction and/or on the
19、 ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment,
20、as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical method
21、s.This first edition of ISO 17378-2 cancels and replaces ISO 11969:1996, which has been technically revised.ISO 17378 consists of the following parts, under the general title Water quality Determination of arsenic and antimony: Part 1: Method using hydride generation atomic fluorescence spectrometry
22、 (HGAFS) Part 2: Method using hydride generation atomic absorption spectrometry (HGAAS)iv ISO 2014 All rights reservedCopyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Not for ResaleNo reproduction or networking permitted without license from IHS-,-,-
23、BS ISO 17378-2:2014ISO 17378-2:2014(E)IntroductionThis part of ISO 17378 should be used by analysts experienced in the handling of trace elements at very low concentrations.Arsenic concentrations in natural waters are highly variable, from 10 g/l to as high as several milligrams per litre in some pa
24、rts of Asia, South America and the USA, notable in the Ganges delta where arsenic poisoning from contaminated tube wells is a serious problem. Antimony concentrations in natural waters are generally well below 10 g/l. Arsenic and antimony occur naturally in organic and inorganic compounds and may ha
25、ve oxidation states III, 0, III and V.In order to fully decompose all of the arsenic or antimony compounds, a digestion procedure is necessary. Digestion can only be omitted if it is certain that the arsenic or antimony in the sample can form a covalent hydride without the necessity of a pre-oxidati
26、on step.The user should be aware that particular problems could require the specification of additional marginal conditions.The method for determining arsenic or antimony is identical in all aspects except for the preparation of standard solutions to be tested. To avoid repetition or duplication the
27、 text refers to both arsenic and antimony where the text is equally applicable to both instances. The subclause dealing with preparation of standard solutions is divided into 5.11.1, which deals with solutions of arsenic, and 5.11.2, which deals with solutions of antimony. ISO 2014 All rights reserv
28、ed vCopyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Not for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS ISO 17378-2:2014Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled C
29、opy Not for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS ISO 17378-2:2014Water quality Determination of arsenic and antimony Part 2: Method using hydride generation atomic absorption spectrometry (HG-AAS)WARNING Persons using this document should be familiar with nor
30、mal laboratory practice. This document 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 conditions.IMPORTANT It is a
31、bsolutely essential that tests conducted according to this document be carried out by suitably trained and experienced staff.1 ScopeThis part of ISO 17378 specifies a method for the determination of arsenic and antimony. The method is applicable to drinking water, surface water, ground water, and ra
32、in water. The approximate linear application range of this part of ISO 17378 for both elements is from 0,5 g/l to 20 g/l. Samples containing higher concentrations than the application range can be analysed following appropriate dilution.Generally sea water is outside the scope of this part of ISO 17
33、378. Sea water samples can be analysed using a standard additions approach providing that this is validated for the samples under test. The method is unlikely to detect organo-arsenic and organo-antimony compounds.The sensitivity of this method is dependent on the selected operating conditions.2 Nor
34、mative 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 references, the latest edition of the referenced document (including any amendments)
35、 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 programmes and sampling techniquesISO 5667-3, Water quality Sampling Part 3: Preservation and handling of water samplesISO 5667-5, Water
36、quality Sampling Part 5: Guidance on sampling of drinking water from treatment works and piped distribution systemsISO 5667-6, Water quality Sampling Part 6: Guidance on sampling of rivers and streamsISO 5667-8, Water quality Sampling Part 8: Guidance on the sampling of wet depositionISO 5667-11, Wa
37、ter quality Sampling Part 11: Guidance on sampling of groundwatersISO 8466-1, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 1: Statistical evaluation of the linear calibration functionISO 8466-2, Water quality Calibration and evalua
38、tion of analytical methods and estimation of performance characteristics Part 2: Calibration strategy for non-linear second-order calibration functionsINTERNATIONAL STANDARD ISO 17378-2:2014(E) ISO 2014 All rights reserved 1Copyright British Standards Institution Provided by IHS under license with B
39、SI - Uncontrolled Copy Not for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS ISO 17378-2:2014ISO 17378-2:2014(E)ISO 15587-1, Water quality Digestion for the determination of selected elements in water Part 1: Aqua regia digestion3 PrincipleNOTE Other measurement techn
40、iques can be applicable providing the performance criteria are adequately demonstrated to be fulfilled or exceeded by the user laboratory. (See Annex C.)3.1 ArsenicAn aliquot of sample is acidified with hydrochloric acid (5.3). Potassium iodideascorbic acid reagent (5.9) is added to ensure quantifie
41、d reduction of arsenic(V) to arsenic(III). The sample solutions are treated with sodium tetrahydroborate (5.5) to generate the covalent gaseous arsenic trihydride (arsine, AsH3). The hydride and excess hydrogen are swept out of the generation vessel in case of batch mode and out of the gas/liquid se
42、parator in case of the continuous mode into a heated silica cell. After atomization, the absorbance of arsenic is determined at a wavelength = 193,7 nm. The procedure is automated by means of auto-sampler and control software.3.2 AntimonyAn aliquot of sample is digested with hydrochloric acid (5.3).
43、 Potassium iodideascorbic acid reagent (5.9) is added to ensure quantified reduction of the antimony(V) to antimony(III). The sample solutions are then treated with sodium tetrahydroborate (5.5) to generate the covalent gaseous antimony trihydride (stibane, SbH3). The hydride and excess hydrogen are
44、 swept out of the generation vessel in case of batch mode and out of the gas/liquid separator in case of continuous mode. After atomization, the absorbance of antimony is determined at a wavelength = 217,6 nm. The procedure is automated by means of auto-sampler and control software.4 Interferences4.
45、1 GeneralThe hydride generation technique is prone to interferences by transition and easily reducible metals. For the majority of natural water samples, this type of interference shall not be significant. The user should carry out recovery tests on typical waters and also determine the maximum conc
46、entrations of potentially interfering elements, using appropriate methods. If such interferences are indicated, the level of interferences should be assessed by performing spike recoveries.Metals which are readily reduced by sodium tetrahydroborate may also cause interferences. In particular, these
47、include chromium, iron, copper, nickel, and lead. If the concentrations of these elements specified in Table 1 are exceeded, a significant decrease of absorption may occur.Table 1 Maximum mass concentration in test solution of interfering heavy metals (valid for flow systems)Interfering elementCr Fe
48、 Cu Ni Pbmg/l500 500 500 250 100The reaction conditions in this part of ISO 17378 have been chosen to minimize these interferences.Further information on these interferences and the technique are given in References.12NOTE If batch systems are used, mass concentrations which are appreciably lower than those specified in Table 1, Table 2 and Table 3 can cause interferences.2 ISO 2014 All rights reservedCopyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Not for ResaleNo r
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