1、BRITISH STANDARD BS EN ISO 14911:1999 Water quality Determination of dissolved Li + , Na + , NH 4 + , K + , Mn 2+ , Ca 2+ , Mg 2+ , Sr 2+and Ba 2+using ion chromatography Method for water and waste water The European Standard ENISO14911:1999 has the status of a British Standard ICS 13.060.50BSEN ISO
2、 14911:1999 This British Standard, having been prepared under the directionof the Health and Environment Sector Committee,was published underthe authority of theStandards Committee andcomes into effect on 15October1999 BSI 04-2000 ISBN 0 580 35020 7 National foreword This British Standard is the Eng
3、lish language version of ENISO14911:1999. It is identical with ISO14911:1998. The UK 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 unders
4、tand the text; present to the responsible international/European committee any enquiries 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 t
5、his subcommittee can be obtained on request to its secretary. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normally include an annex which lists normative references to international publications with their corresponding European publications. The British Standards
6、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” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to includ
7、e 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 obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i
8、 and ii, theEN ISO title page, page 2, the ISO title page, pages ii to iv, pages 1 to 16, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Amen
9、dments issued since publication Amd. No. Date CommentsBSEN ISO 14911:1999 BSI 04-2000 i Contents Page National foreword Inside front cover Foreword 2 Foreword iii Text of ISO 14911 1ii blankEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 14911 August 1999 ICS 13.060.01 English version Water
10、 quality Determination of dissolved Li + , Na + , NH 4 + , K + , Mn 2+ , Ca 2+ , Mg 2+ , Sr 2+and Ba 2+using ion chromatography Method for water and waste water (ISO14911:1998) Qualit de leau Dosage, par chromatographie ionique, des ions Li + , Na + , NH 4 + , K + , Mn 2+ , Ca 2+ , Mg 2+ , Sr 2+et B
11、a 2+dissous Mthode applicable pour leau et les eaux rsiduaires (ISO14911:1998) Wasserbeschaffenheit Bestimmung der gelsten Kationen Li + , Na + , NH 4 + , K + , Mn 2+ , Ca 2+ , Mg 2+ , Sr 2+und Ba 2+mittels Ionenchromatographie Verfahren fr Wasser und Abwasser (ISO14911:1998) This European Standard
12、was approved by CEN on 7 July 1999. 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 nat
13、ional standards may be obtained on application 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 translation under the responsibility of a CEN member into its own language and n
14、otified to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, CzechRepublic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland
15、 and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1999 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No
16、. EN ISO 14911:1999 EEN ISO 14911:1999 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 anal
17、ysis”, 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 text or by endorsement, at the latest by February2000, and conflicting national standards shall be withdrawn at the latest by February2000. A
18、ccording 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, Portu
19、gal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard ISO14911:1998 has been approved by CEN as a European Standard without any modification. NOTENormative references to International Standards are listed inAnnex ZA (normative).EN ISO 14911
20、:1999 ii BSI 04-2000 Contents Page Foreword iii Introduction 1 1 Scope 1 2 Normative references 1 3 Interferences 2 4 Principle 2 5 Essential minimum requirements 2 6 Reagents 2 7 Apparatus 6 8 Quality requirements for the separator column 6 9 Sampling and sample pretreatment 8 10 Procedure 9 11 Cal
21、culation 10 12 Expression of results 10 13 Test report 11 Annex A (informative) Interlaboratory trial 12 Annex B (informative) Bibliography 16 Annex ZA (normative) Normative references t o international publications with their relevant European publications Inside back cover Figure 1 Schematic repre
22、sentation of an ion chromatography system 6 Figure 2 Example of a chromatogram of a column conforming to this International Standard 7 Figure 3 Graphical representation of the parameters to calculate the peak resolutionR 8 Table 1 Working ranges of the analytical method 1 Table 2 Mass of portion and
23、 suggestions how to store stock solutions 4 Table 3 Volumes of stock solutions for the preparation of the mixed standard solution 5 Table 4 Concentrations of the calibration solutions 5 Table A.1 Description of sample matrix 12 Table A.2 Statistical data for ammonium 13 Table A.3 Statistical data fo
24、r barium 13 Table A.4 Statistical data for potassium 13 Table A.5 Statistical data for calcium 14 Table A.6 Statistical data for lithium 14 Table A.7 Statistical data for magnesium 14 Table A.8 Statistical data for manganese 14 Table A.9 Statistical data for sodium 15 Table A.10 Statistical data for
25、 strontium 15 Table A.11 Estimation of performance characteristics indicated by coefficients of variation of the procedure (V xo ) 15 Descriptors: Water, quality, water pollution, soluble matter, water tests, chemical analysis, determination of content, cations, lithium, sodium potassium, manganese,
26、 calcium.EN ISO 14911:1999 BSI 04-2000 iii 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 through ISO technical committees. Each member
27、 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 collaborates closely with the International Elect
28、rotechnical 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 at least75% of the member bodies casting a
29、vote. International Standard ISO14911 was prepared by Technical Committee TC147, Water quality, SubcommitteeSC2, Physical, chemical, biochemical methods. Annex A andAnnex B of this International Standard are for information only.iv blankEN ISO 14911:1999 BSI 04-2000 1 Introduction The essential mini
30、mum requirements of an ion chromatographic system applied within the scope of this International Standard are given inclause5. The diversity of the appropriate and suitable assemblies and the procedural steps depending on them permit a general description only. Further information on the analytical
31、technique is given in the normative references (seeclause2) and the bibliography. 1 Scope This International Standard specifies a method for the determination of the dissolved cations Li + , Na + , NH 4 + , K + , Mn 2+ , Ca 2+ , Mg 2+ , Sr 2+and Ba 2+in water (e.g.drinking water, surface water, wast
32、e water). An appropriate pretreatment of the sample (e.g.dilution) and the application of a conductivity detector (CD) make the working ranges given inTable 1 feasible. The applicability of the method for waste water samples should be proved in each case. Table 1 Working ranges of the analytical met
33、hod 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on
34、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 currently valid International Standards. ISO 5667-1:1980, Water quality Sampling Part1: Guidance on the design
35、 of sampling programmes. ISO 5667-2:1991, Water quality Sampling Part2: Guidance on sampling techniques. ISO 5667-3:1994, Water quality Sampling Part3: Guidance on the preservation and handling of samples. ISO 6058:1984, Water quality Determination of calcium content EDTA titrimetric method. ISO 605
36、9:1984, Water quality Determination of the sum of calcium and magnesium EDTA titrimetric method. ISO 6333:1986, Water quality Determination of manganese Formaldoxime spectrometric method. ISO 7980:1986, Water quality Determination of calcium and magnesium Atomic absorption spectrometric method. ISO
37、8466-1:1990, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part1: Statistical evaluation of the linear calibration function. Cation Typical working range with10 4l loop mg/l a Lithium 0,01 to 1 Sodium 0,1 to 10 Ammonium 0,1 to 10 Potassi
38、um 0,1 to 10 Manganese 0,5 to 50 Calcium 0,5 to 50 Magnesium 0,5 to 50 Strontium 0,5 to 50 Barium 1 to 100 a The working range is limited by the ion-exchange capacity of the separator column. If necessary, the sample shall be diluted to meet the working range, or use a1004l loop for lower working ra
39、nges.EN ISO 14911:1999 2 BSI 04-2000 ISO 8466-2:1993, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part2: Calibration strategy for non-linear second order calibration functions. 3 Interferences 3.1 Organics such as amino acids and aliph
40、atic amines can interfere with the determination of inorganic cations. 3.2 If a strong complexing agent such as pyridine-2,6-dicarboxylic acid (PDA) is not present in the mobile phase, and if the suppressor technique is not used, cross interferences from other cations like Zn 2+ , Ni 2+ , Cd 2+etc.c
41、an Occur. 3.3 Cross-sensitivities with other cations, e.g.manganese, are dependent on the selectivity of the separator column used. If the quality requirements inclause8 are not achieved, the sample shall be diluted. 3.4 Cross-sensitivities in the determination of NH 4 +and Na +can occur when there
42、are large differences in concentration. 3.5 Solid material and organic compounds (such as mineral oils, detergents and humic acids) shorten the lifetime of the separator column. They are therefore eliminated from the sample (9.3). 4 Principle Liquid chromatographic separation of Li + , Na + , NH 4 +
43、 , K + , Mn 2+ , Ca 2+ , Mg 2+ , Sr 2+and Ba 2+by means of a separator column. A low-capacity cation exchanger is used as the stationary phase, and usually, aqueous solutions of mono- and dibasic acids as mobile phases (eluent, see6.16). These cations are detected by conductivity. It is essential th
44、at the eluents have a sufficiently low conductivity. For this reason, a conductivity detector (CD) is often combined with a suppressor device (e.g.an anion exchanger) which will reduce the conductivity of the eluent and transform the separated cations into their corresponding bases. In the conductiv
45、ity detection without chemical suppression, the difference between the ion equivalent conductivities is measured directly after the column. This difference should be as high as possible and the detector cell temperature should be stabilized within 0,1 C. The concentration of the respective cations i
46、s determined by a calibration of the overall procedure. Particular cases can require calibration by means of standard addition (spiking). 5 Essential minimum requirements The essential minimum requirements of an ion chromatographic system applied within the scope of this International Standard are t
47、he following: 6 Reagents Use only reagents of recognized analytical grade. Carry out weighing with an accuracy of 1% of the nominal mass. The water shall have an electrical conductivity of0,454m. 6.1 DL-2,3-Diaminopropionic acid monohydrochloride (DAP), C 3 H 8 N 2 O 2 HCl. 6.2 Hydrochloric acid sol
48、ution, c(HCl)=7,7mol/l. 6.3 Methanesulfonic acid, CH 4 O 3 S (U 99%). a) Resolution power (R) of the column: For the cation to be determined it is essential that the peak resolution does not fall below R = 1,3 (seeclause8,Figure 3). b) Method of detection: Measurement of the electrical conductivity
49、with or without suppressor device. c) Applicability of the method: Working ranges according toTable 1. d) Calibration (10.2): Calibration and determination of the linear (seeISO8466-1) or quadratic (see ISO8466-2) working range. Use of the method of standard addition to special cases of application (see10.3). e) Guaranteeing the analytical quality (10.3.2): Validity check of the calibration function. Replicate determinations, if necessary.EN ISO 14911:1999 BSI 04-20
