1、BRITISH STANDARD BS EN ISO 10304-3:1997 BS 6068-2.59: 1997 Water quality Determination of dissolved anions by liquid chromatography of ions Determination of chromate, iodide, sulfite, thiocyanate and thiosulfate The European Standard EN ISO 10304-3:1997 has the status of a British Standard ICS 13.06
2、0.01BSEN ISO10304-3:1997 This British Standard, having been prepared under the directionof the Health and Environment Sector Board, waspublished under the authorityof the Standards Boardand comes into effect on 15October1997 BSI 04-2000 ISBN 0 580 28485 9 Amendments issued since publication Amd. No.
3、 Date CommentsBSENISO10304-3:1997 BSI 04-2000 i Contents Page National foreword ii Foreword 2 Foreword iv Text of ISO 10304-3 1BSENISO10304-3:1997 ii BSI 04-2000 National foreword This British Standard is the English language version of ENISO10304-3:1997. It is identical with ISO10304-3:1997. The UK
4、 participation in its preparation was entrusted by Technical Committee EH/3, Water quality, to Subcommittee EH/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 enqui
5、ries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international 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. BS EN ISO 10304-3 is o
6、ne of a series of standards on water quality, others of which have been, or will be, published as Sections of BS6068. This standard has therefore been given the secondary identifier BS6068-2.59. The various Sections of BS6068 are comprised within Parts1 to7, which, together with Part0, are listed be
7、low. Part 0: Introduction; Part 1: Glossary; Part 2: Physical, chemical and biochemical methods; Part 3: Radiological methods; Part 4: Microbiological methods; Part 5: Biological methods; Part 6: Sampling; Part 7: Precision and accuracy. NOTEThe tests described in this British Standard should only b
8、e carried out by suitably qualified persons with an appropriate level of chemical expertise. Standard chemical procedures should be followed throughout. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normally include an annex which lists normative references to intern
9、ational publications with their corresponding European publications. The British Standards which implement these international or European publications may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facili
10、ty of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligati
11、ons. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, theEN ISO title page, page 2, the ISO title page, pages ii to iv, pages 1 to 15 and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This wil
12、l be indicated in the amendment table on the inside front cover.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 10304-3 August 1997 ICS 13.060.40 Descriptors: See ISO document English version Water quality Determination of dissolved anions by liquid chromatography of ions Part 3: Determinat
13、ion ofchromate, iodide, sulfite, thiocyanate and thiosulfate (ISO 10304-3:1997) Qualit de leau Dosage des anions dissous par chromatographie des ions en phase liquide Partie 3: Dosage des ions chromate, iodure, sulfite, thiocyanate et thiosulfate (ISO 10304-3:1997) This European Standard was approve
14、d by CEN on 1997-07-18. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standa
15、rds may be obtained on application to the Central Secretariat or to any CEN member. The European Standards exist in three official versions (English, 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 th
16、e Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United
17、Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1997 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 103
18、04-3:1997 EENISO10304-3:1997 BSI 04-2000 2 Foreword The text of the International Standard from Technical Committee ISO/TC147 “Water quality” of the International Organization for Standardization (ISO) has been taken over as an European Standard by Technical Committee CEN/TC230 “Water analysis”, the
19、 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 text or by endorsement, at the latest by month of February1998, and conflicting national standards shall be withdrawn at the latest by February1998. Ac
20、cording to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, CzechRepublic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portug
21、al, Spain, Sweden, Switzerland and theUnitedKingdom. Endorsement notice The text of the International Standard ISO10304-3:1997 has been approved by CEN as a European Standard without any modification.ENISO10304-3:1997 ii BSI 04-2000 Contents Page Foreword iv Introduction 1 1 Scope 1 2 Normative refe
22、rences 1 3 Principle 1 4 Determination of iodide, thiocyanate and thiosulfate 2 4.1 Reagents 2 4.2 Apparatus 5 4.3 Interferences 7 4.4 Sampling and sample pretreatment 7 4.5 Procedure 8 4.6 Calculation 9 4.7 Expression of results 9 4.8 Test report 9 5 Determination of sulfite 9 5.1 Reagents 9 5.2 Ap
23、paratus 11 5.3 Interferences 11 5.4 Sampling and sample pretreatment 11 5.5 Procedure 12 5.6 Calculation 12 5.7 Expression of results 12 5.8 Test report 12 6 Determination of chromate 12 6.1 Reagents 12 6.2 Apparatus 13 6.3 Interferences 13 6.4 Sampling and sample pretreatment 13 6.5 Procedure 13 6.
24、6 Calculation 13 6.7 Expression of results 13 6.8 Test report 13 7 Precision 13 Annex A (informative) Interlaboratory trials 14 Annex B (informative) Bibliography 15 Figure 1 Schematic representation of an ion chromatography system 5 Figure 2 Example of a chromatogram of a column conforming to this
25、part of ISO 10304 6 Figure 3 Graphical representation of the parameters to calculate the peak resolution R 6 Table 1 Applicable working ranges 2 Table 2 Mass portion and pretreatment for stock solutions 4 Table 3 Cross-sensitivity of the anion 11 Table A.1 Description of sample matrix and sample pre
26、treatment 14 Table A.2 Statistical data for iodide (I) 14 Table A.3 Statistical data for thiocyanate (SCN) 14 Table A.4 Statistical data for thiosulfate (S 2 O 3 ) 15 Table A.5 Statistical data for sulfite (SO 3 ) 15 Table A.6 Statistical data for chromate (CrO 4 ) 15ENISO10304-3:1997 BSI 04-2000 ii
27、i Page Table A.7 Estimation of performance characteristics indicated by coefficients of variation of the procedure (V xo ) 15 Descriptors: Water, quality, water pollution, anions, soluble water, water tests, chemical analysis, determination of content, chromates, iodides, sulphites, thiocyanates, th
28、iosulphates, high performance liquid chromatography.ENISO10304-3:1997 iv BSI 04-2000 Foreword ISO (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 thr
29、ough 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 take part in the work. ISO collabo
30、rates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by a
31、t least75% of the member bodies casting a vote. International Standard ISO10304-3 was prepared by Technical Committee ISO/TC147, Water quality, SC 2, Physical, chemical and biochemical methods. ISO 10304 consists of the following parts, under the general title Water quality Determination of dissolve
32、d anions by liquid chromatography of ions: Part 1: Determination of fluoride, chloride, bromide, nitrate, nitrite, orthophosphate and sulfate in water with low contamination; Part 2: Determination of bromide, chloride, nitrate, nitrite, orthophosphate and sulfate in waste water; Part 3: Determinatio
33、n of chromate, iodide, sulfite, thiocyanate and thiosulfate; Part 4: Determination of chlorate, chloride and chlorite in water with low contamination. Annex A and Annex B of this part of ISO10304 are for information only.ENISO10304-3:1997 BSI 04-2000 1 Introduction The essential minimum requirements
34、 of an ion chromatographic system applied within the scope of this part of ISO10304 are the following: The diversity of the appropriate and suitable assemblies and the procedural steps depending on them permit a general description only. For further information on the analytical technique, see refer
35、ence 1. 1 Scope This part of ISO 10304 specifies methods for the determination in aqueous solution of the dissolved anions iodide, thiocyanate and thiosulfate (clause 4); sulfite (clause 5); chromate (clause 6). An appropriate pretreatment of the sample (e.g.dilution) and the application of a conduc
36、tivity detector (CD), UV detector (UV) or amperometric detector (AD) make the working ranges given inTable 1 feasible. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this part of ISO10304. At the time of publication,
37、the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of c
38、urrently valid International Standards. ISO 5667-1:1980, Water quality Sampling Part 1: Guidance on the design of sampling programmes. ISO 5667-2:1991, Water quality Sampling Part 2: Guidance on sampling techniques. ISO 5667-3:1994, Water quality Sampling Part 3: Guidance on the preservation and han
39、dling of samples. ISO 8466-1:1990, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 1: Statistical evaluation of the linear calibration function. ISO 10304-1:1992, Water quality Determination of dissolved fluoride, chloride, nitrite, o
40、rthophosphate, bromide, nitrate, and sulfate ions, using liquid chromatography of ions Part 1: Method for water with low contamination. ISO 10304-2:1995, Water quality Determination of dissolved anions by liquid chromatography of ions Part 2: Determination of bromide, chloride, nitrate, nitrite, ort
41、hophosphate and sulfate in waste water. 3 Principle 3.1 Separation of ions is carried out by liquid chromatography using a separating column. A low capacity anion exchanger is used as the stationary phase, and usually aqueous solutions of salts of weak monobasic and dibasic acids as mobile phases (e
42、luent, see4.1.16, 5.1.4, 6.1.9). 3.2 The addition of organic agents, such as 4-hydroxybenzonitrile (see4.1.16.2.2, 4.3.4), or organic solvents to the eluent can be used to speed up the elution or reduce the tailing effects, especially for the analysis of the more strongly polarizable ions iodide, th
43、iocyanate and thiosulfate. a) Resolution of thecolumn: For the anion to be determined it is essential that the peak resolution does not fall below R = 1,3 (4.2.2, Figure 3) b) Method of detection: 1) measurement of the electrical conductivity with or without suppressor device 2) spectrometric measur
44、ement (UV/VIS), directly or indirectly 3) amperometric direct detection c) Applicability of the method: Working ranges according toTable 1 d) Calibration (4.5.1): Calibration and determination of the linear working range (see ISO 8466-1) Guaranteeing the analytical quality: Validity check of the cal
45、ibration function. Replicate determinations if necessary.ENISO10304-3:1997 2 BSI 04-2000 Table 1 Applicable working ranges 3.3 Detection is by conductivity (CD), UV and amperometric detectors (AD). 3.3.1 When using conductivity detectors it is essential that the eluents have a sufficiently low condu
46、ctivity. For this reason, conductivity detectors are often combined with suppressor devices (cation exchangers) which will reduce the conductivity of the eluents and transform the sample species into their respective acids. 3.3.2 UV detection measures either the absorption directly (seeTable 1) or,
47、in the case of anions which are transparent in the UV-range, the decrease in the background absorption caused by a UV-absorbing eluent is measured (indirect measurement). If indirect UV-detection is used, the measuring wavelength depends on the composition of the eluent. 3.3.3 Amperometric detectors
48、 measure the quantity of current caused by the oxidation of anions. The oxidation voltage required for the anions in question depends on the pH value of the eluent. 3.4 The concentration of the respective anions is determined by a calibration of the overall procedure. Particular cases may require ca
49、libration by means of standard addition (spiking). 4 Determination of iodide, thiocyanate and thiosulfate Follow the instructions given in clause 4 to make the working ranges given inTable 1 feasible. 4.1 Reagents Use only reagents of recognized analytical grade, if commercially available. Carry out weighing with an accuracy of1% of the nominal mass. The water shall have an electrical conductivity of0,454m. An increase of the electrical conductivity due to an upt
