1、BSI Standards PublicationBS ISO 17378-1:2014Water quality Determinationof arsenic and antimonyPart 1: Method using hydride generationatomic fluorescence spectrometry (HG-AFS)BS ISO 17378-1:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 17378-1:2014.The UK
2、 participation in its preparation was entrusted to TechnicalCommittee 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 contr
3、act. Users are responsible for its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 70963 0ICS 13.060.50Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the author
4、ity of theStandards Policy and Strategy Committee on 28 February 2014.Amendments issued since publicationDate Text affectedBS ISO 17378-1:2014 ISO 2014Water quality Determination of arsenic and antimony Part 1: Method using hydride generation atomic fluorescence spectrometry (HG-AFS)Qualit de leau D
5、osage de larsenic et de lantimoine Partie 1: Mthode par spectromtrie de fluorescence atomique gnration dhydrures (HG-AFS)INTERNATIONAL STANDARDISO17378-1First edition2014-02-01Reference numberISO 17378-1:2014(E)BS ISO 17378-1:2014ISO 17378-1:2014(E)ii ISO 2014 All rights reservedCOPYRIGHT PROTECTED
6、DOCUMENT 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
7、 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 www.iso.orgPublished in SwitzerlandBS ISO 17378-1:2014ISO 17378-1:2014
8、(E) ISO 2014 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Principle 24 Interferences 25 Reagents 45.1 General requirements . 46 Apparatus . 97 Sampling and sample preparation .117.1 Sampling techniques . 117.2 Pre-reduction 118 Instrumental set-up
9、 .119 Procedure1210 Calibration and data analysis .1310.1 General requirements 1310.2 Calculation using the calibration curve 1311 Expression of results .1312 Test report 14Annex A (informative) Additional information 15Annex B (informative) Figures .16Annex C (informative) Performance data .18BS IS
10、O 17378-1:2014ISO 17378-1:2014(E)ForewordISO (the International 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 inter
11、ested 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 take part in the work. ISO collaborates closely with the International Electrotechnical
12、 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 particular the different approval criteria needed for the different types of ISO docume
13、nts 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 to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible
14、 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 (see www.iso.org/patents).Any trade name used in this document is information given for th
15、e 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, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Fo
16、reword - Supplementary informationThe committee responsible for this document is ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical methods.ISO 17378 consists of the following parts, under the general title Water quality Determination of arsenic and antimony: Part 1: Me
17、thod using hydride generation atomic fluorescence spectrometry (HGAFS) Part 2: Method using hydride generation atomic absorption spectrometry (HGAAS)iv ISO 2014 All rights reservedBS ISO 17378-1:2014ISO 17378-1:2014(E)IntroductionThis part of ISO 17378 should be used by analysts experienced in the h
18、andling 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 parts of Asia, South America, and the USA, notably in the Ganges delta where arsenic poisoning from contaminated tube well
19、s is a serious problem. Antimony concentrations in natural waters are generally well below 10 g/l. Arsenic or antimony occur naturally in organic and inorganic compounds, and can have oxidation states III, 0, III, and V.In order to fully decompose all of the arsenic or antimony compounds, a digestio
20、n 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-oxidation step.The user should be aware that particular problems can require the specification of additional marginal conditi
21、ons.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 text refers to both arsenic and antimony where the text is equally applicable to both instances. The subclause dealing
22、 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 reserved vBS ISO 17378-1:2014BS ISO 17378-1:2014Water quality Determination of arsenic and antimony Part 1: Method using hydr
23、ide generation atomic fluorescence spectrometry (HG-AFS)WARNING Persons using this document should be familiar with normal 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 app
24、ropriate safety and health practices and to ensure compliance with any national regulatory conditions.IMPORTANT It is absolutely 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
25、 determination of arsenic and antimony. The method is applicable to drinking water, surface water, ground water and rain water. The linear application range of this part of ISO 17378 is from 0,02 g/l to 100 g/l. Samples containing arsenic or antimony at higher concentrations than the application ran
26、ge can be analysed following appropriate dilution.Generally sea water is outside the scope of this part of ISO 17378. 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 com
27、pounds or organo-antimony compounds.The sensitivity of this method is dependent on the selected operating conditions.2 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 t
28、he edition cited applies. For undated references, the latest edition of the referenced 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 programmes and
29、sampling techniquesISO 5667-3, Water quality Sampling Part 3: Preservation and handling of water samplesISO 5667-5, Water 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
30、 of rivers and streamsISO 5667-8, Water quality Sampling Part 8: Guidance on the sampling of wet depositionISO 5667-11, Water quality Sampling Part 11: Guidance on sampling of groundwatersISO 8466-1, Water quality Calibration and evaluation of analytical methods and estimation of performance charact
31、eristics Part 1: Statistical evaluation of the linear calibration functionISO 15587-1, Water quality Digestion for the determination of selected elements in water Part 1: Aqua regia digestionINTERNATIONAL STANDARD ISO 17378-1:2014(E) ISO 2014 All rights reserved 1BS ISO 17378-1:2014ISO 17378-1:2014(
32、E)3 PrincipleAn aliquot of sample is acidified with hydrochloric acid (7.2.1). Potassium iodideascorbic acid reagent (5.9) is added to ensure quantified reduction of the arsenic(V) to arsenic(III) and antimony(V) to antimony(III). The subsequent sample solutions are then treated with sodium tetrahyd
33、roborate (5.7) to generate the covalent gaseous hydride (AsH3) or (SbH3). The hydride and excess hydrogen are swept out of the generation vessel in case of the batch mode and out of the gas/liquid separator in the case of the continuous mode into an atomizer suited for atomic fluorescence measuremen
34、ts (e.g. a chemically generated hydrogen diffusion flame). The hydride is atomized and the resulting atoms excited by an intense arsenic or antimony light source, the resulting fluorescence is detected by atomic fluorescence spectrometry after isolation by an interference filter that transmits the a
35、rsenic or antimony resonance line at 193,7 nm (for arsenic) or 206,8 nm and 217,6 nm (for antimony). The procedure is automated by means of auto-sampler and control software.4 InterferencesThe hydride generation technique is prone to interferences by transition and easily reducible metals. For the m
36、ajority of natural water samples, this type of interference should not be significant. The user should carry out recovery tests on typical waters and also determine the maximum concentrations of potentially interfering elements, using appropriate methods. If such interferences are indicated, the lev
37、el of interferences should be assessed by performing spike recoveries. However, the atomic fluorescence technique has a high linear dynamic range and a very low detection limit. In most cases, many interferences can be removed by a simple dilution step as long as the final antimony and arsenic conce
38、ntrations are above the LOQ.The reaction conditions set out in this part of ISO 17378 have been chosen so that any interference is reduced to a minimum.It is important that the light source does not contain any significant amount of other hydride-forming elements (e.g. antimony when analysing for ar
39、senic or arsenic when analysing for antimony) that emit fluorescent radiation over the band pass of the interference filter used in the detector, if these elements are present in the sample.Measurements carried out using the procedures in this part of ISO 17378 generally do not suffer from interfere
40、nces due to quenching within the ranges of interest.Interference studies on a number of elements have been conducted and are shown in Tables 1 and 2 for arsenic and antimony, respectively. Easily reducible elements such as gold and mercury cause a significant negative bias, especially for antimony.
41、A significant positive bias is caused by bismuth for both arsenic and low levels of antimony. However, these elements are unlikely to be present at the tested levels in the vast majority of water samples. Arsenic causes a large positive bias for antimony.Interference can be indicated by the irregula
42、rity of the signal peak shape. Usually the interference can be removed by diluting the samples; this dilution should not reduce the concentration of the analyte lower than the LOQ.2 ISO 2014 All rights reservedBS ISO 17378-1:2014ISO 17378-1:2014(E)Table 1 Interference study for arsenicInterfering su
43、bstanceConcentration of interfering sub-stanceAs recovery, %mg/l 2 g/l As 10 g/l AsThallium nitrate Tl(III) 20 94,8 0,9 89,9 2,8Strontium nitrate Sr(II) 20 107,3 5,9 100,0 2,5Zinc nitrate Zn(II) 1 101,7 5,5 91,0 3,1di(Ammonium)silicon hexafluoride Si(IV) 1 94,4 3,7 102,4 1,7Aluminium nitrate Al(III)
44、 1 104,6 0,8 98,9 0,8Calcium chloride Ca(II) 200 101,8 1,3 103,3 1,3Sodium chloride Na(I) 200 104,2 1,6 100,6 1,8Potassium bromide K(I) 200 96,3 0,7 97,6 0,7Indium nitrate In(III) 1 99,4 1,4 99,1 1,5Barium nitrate Ba(II) 1 95,2 3,1 105,9 1,4Magnesium oxide Mg(II) 1 99,7 3,5 97,2 1,5Cadmium nitrate C
45、d(II) 1 100,4 0,9 97,2 0,2Ammonium dihydrogenphosphate P(V) 1 100,3 1,3 100,5 2,1Sodium fluoride F(I) 1 113,3 2,6 109,4 1,0Gold chloride Au(III) 0,1 97,8 6,4 103,2 1,4Gold chloride Au(III) 1 80,9 1,9 93,8 1,5Orthoboric acid B(III) 1 99,5 3,0 99,7 3,4Iron(II) nitrate Fe(II) 1 99,0 0,9 100,2 0,7Lead(I
46、I) nitrate Pb(II) 1 87,0 4,1 95,3 0,7Bismuth nitrate Bi(III) 1 121,4 0,9 107,0 0,2Tin nitrate Sn(IV) 1 95,1 1,9 104,8 1,8Germanium chloride Ge(IV) 1 104,4 3,0 102,1 1,1Mercury Hg(II) 1 100,7 0,7 98,1 0,4Chromium(III) nitrate Cr(III) 1 101,0 1,2 98,4 0,6Cobalt nitrate Co(II) 1 103,1 0,7 99,9 2,0Silve
47、r nitrate Ag(I) 1 97,9 1,8 95,9 2,3Nickel(II) nitrate Ni(II) 1 100,2 0,4 98,8 1,2Telluric acid Te(IV) 0,01 90,7 2,9 99,3 0,7Telluric acid Te(IV) 0,1 100,1 1,2 98,0 0,9Telluric acid Te(IV) 1 101,5 0,6 100,3 1,0Antimony oxide Sb(III) 0,01 101,0 0,8 102,1 1,1Antimony oxide Sb(III) 0,05 107,3 1,8 97,5 1
48、,7Antimony oxide Sb(III) 0,1 118,3 1,0 96,7 2,7Copper(II) sulfate Cu(II) 0,1 101,8 1,9 102,7 2,4Copper(II) sulfate Cu(II) 0,2 100,5 2,8 101,4 0,1Copper(II) sulfate Cu(II) 0,5 99,8 1,1 99,0 1,0Copper(II) sulfate Cu(II) 1 94,0 4,7 100,7 1,9Copper(II) sulfate Cu(II) 2 98,8 1,1 99,0 1,0Iron(IIl) nitrate
49、 Fe(III) 200 114,3 0,7 105,0 0,6 ISO 2014 All rights reserved 3BS ISO 17378-1:2014ISO 17378-1:2014(E)Table 2 Interference study for antimonyInterfering substanceConcentration of interfering sub-stanceSb recovery, %mg/l 2 g/l Sb 10 g/l SbThallium nitrate Tl(llI) 20 100,9 1,6 93,5 2,1Strontium nitrate Sr(II) 20 99,7 4,5 99,6
