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1、BRITISH STANDARD BS EN ISO 14911:1999 Water quality Determination of dissolved Li+, Na+, NH4+, K+, Mn2+, Ca2+, Mg2+, Sr2+ and Ba2+ using ion chromatography Method for water and waste water The European Standard EN ISO 14911:1999 has the status of a British Standard ICS 13.060.50 Licensed Copy: sheff
2、ieldun sheffieldun, na, Sat Nov 18 01:48:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 14911:1999 This British Standard, having been prepared under the direction of the Health and Environment Sector Committee, was published under the authority of the Standards Committee and comes into effe
3、ct on 15 October 1999 BSI 04-2000 ISBN 0 580 35020 7 National foreword This British Standard is the English language version of EN ISO 14911:1999. It is identical with ISO 14911:1998. The UK participation in its preparation was entrusted by Technical Committee EH/3, Water quality, to Subcommittee EH
4、/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 enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related inter
5、national 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. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normally include an annex which lists normative refer
6、ences to international 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 th
7、e “Find” facility 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
8、 legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN 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
9、 had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Amendments issued since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 14911:1999 BSI 04-2000i
10、 Contents Page National forewordInside front cover Foreword2 Forewordiii Text of ISO 149111 Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii blank Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:29 GMT+00:00 2006, Uncontrolled
11、 Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 14911 August 1999 ICS 13.060.01 English version Water quality Determination of dissolved Li+, Na+, NH4+, K+, Mn2+, Ca2+, Mg2+, Sr2+ and Ba2+ using ion chromatography Method for water and waste water (ISO 14911:1998) Qualit de le
12、au Dosage, par chromatographie ionique, des ions Li+, Na+, NH4+, K+, Mn2+, Ca2+, Mg2+, Sr2+ et Ba2+ dissous Mthode applicable pour leau et les eaux rsiduaires (ISO 14911:1998) Wasserbeschaffenheit Bestimmung der gelsten Kationen Li+, Na+, NH4+, K+, Mn2+, Ca2+, Mg2+, Sr2+ und Ba2+ mittels Ionenchroma
13、tographie Verfahren fr Wasser und Abwasser (ISO 14911:1998) This European Standard 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
14、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, French, German). A version in any other language made
15、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, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, I
16、reland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland 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 exploitati
17、on in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 14911:1999 E Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 14911:1999 BSI 04-2000 2 Foreword The text of the International Standard from Te
18、chnical Committee ISO/TC 147 “Water quality” of the International Organization for Standardization (ISO) has been taken over as an European Standard by 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 nati
19、onal standard, either by publication of an identical text or by endorsement, at the latest by February 2000, and conflicting national standards shall be withdrawn at the latest by February 2000. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
20、countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the Internationa
21、l Standard ISO 14911:1998 has been approved by CEN as a European Standard without any modification. NOTENormative references to International Standards are listed in Annex ZA (normative). Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licen
22、sed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 14911:1999 ii BSI 04-2000 Contents Page Forewordiii Introduction1 1Scope1 2Normative references1 3Interferences2 4Principle2 5Essential minimum requirements2 6Reagents2 7Apparatus6 8Quality r
23、equirements for the separator column6 9Sampling and sample pretreatment8 10Procedure9 11Calculation10 12Expression of results10 13Test report11 Annex A (informative) Interlaboratory trial12 Annex B (informative) Bibliography16 Annex ZA (normative) Normative references t o international publications
24、with their relevant European publicationsInside back cover Figure 1 Schematic representation of an ion chromatography system6 Figure 2 Example of a chromatogram of a column conforming to this International Standard7 Figure 3 Graphical representation of the parameters to calculate the peak resolution
25、 R8 Table 1 Working ranges of the analytical method1 Table 2 Mass of portion and suggestions how to store stock solutions4 Table 3 Volumes of stock solutions for the preparation of the mixed standard solution5 Table 4 Concentrations of the calibration solutions5 Table A.1 Description of sample matri
26、x12 Table A.2 Statistical data for ammonium13 Table A.3 Statistical data for barium13 Table A.4 Statistical data for potassium13 Table A.5 Statistical data for calcium14 Table A.6 Statistical data for lithium14 Table A.7 Statistical data for magnesium14 Table A.8 Statistical data for manganese14 Tab
27、le A.9 Statistical data for sodium15 Table A.10 Statistical data for strontium15 Table A.11 Estimation of performance characteristics indicated by coefficients of variation of the procedure (Vxo)15 Descriptors: Water, quality, water pollution, soluble matter, water tests, chemical analysis, determin
28、ation of content, cations, lithium, sodium potassium, manganese, calcium. Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 14911:1999 BSI 04-2000iii Foreword ISO (the International Organization for Standardization) is a worldwide feder
29、ation of national standards bodies (ISO member bodies). 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 commit
30、tee. International organizations, governmental and 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. Draft International Standards adopted by the tec
31、hnical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. International Standard ISO 14911 was prepared by Technical Committee TC 147, Water quality, Subcommittee SC 2, Physical,
32、chemical, biochemical methods. Annex A and Annex B of this International Standard are for information only. Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv blank Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:29 GMT+00:00 20
33、06, Uncontrolled Copy, (c) BSI EN ISO 14911:1999 BSI 04-20001 Introduction The essential minimum requirements of an ion chromatographic system applied within the scope of this International Standard are given in clause 5. The diversity of the appropriate and suitable assemblies and the procedural st
34、eps depending on them permit a general description only. Further information on the analytical technique is given in the normative references (see clause 2) and the bibliography. 1 Scope This International Standard specifies a method for the determination of the dissolved cations Li+, Na+, NH4+, K+,
35、 Mn2+, Ca2+, Mg2+, Sr2+ and Ba2+ in water (e.g. drinking water, surface water, waste water). An appropriate pretreatment of the sample (e.g. dilution) and the application of a conductivity detector (CD) make the working ranges given in Table 1 feasible. The applicability of the method for waste wate
36、r samples should be proved in each case. Table 1 Working ranges of the analytical method 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 w
37、ere 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 currently valid Internati
38、onal 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 handling of samples. ISO 60
39、58:1984, Water quality Determination of calcium content EDTA titrimetric method. ISO 6059:1984, 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 qua
40、lity Determination of calcium and magnesium Atomic absorption spectrometric method. 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. Cation Typical working
41、range with 10 4l loop mg/la Lithium0,01 to 1 Sodium0,1 to 10 Ammonium0,1 to 10 Potassium0,1 to 10 Manganese0,5 to 50 Calcium0,5 to 50 Magnesium0,5 to 50 Strontium0,5 to 50 Barium1 to 100 a The working range is limited by the ion-exchange capacity of the separator column. If necessary, the sample sha
42、ll be diluted to meet the working range, or use a 100 4l loop for lower working ranges. Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 14911:1999 2 BSI 04-2000 ISO 8466-2:1993, Water quality Calibration and evaluation of analytical m
43、ethods and estimation of performance characteristics Part 2: Calibration strategy for non-linear second order calibration functions. 3 Interferences 3.1 Organics such as amino acids and aliphatic amines can interfere with the determination of inorganic cations. 3.2 If a strong complexing agent such
44、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 Zn2+, Ni2+, Cd2+ etc. can Occur. 3.3 Cross-sensitivities with other cations, e.g. manganese, are dependent on the selectivity of the se
45、parator column used. If the quality requirements in clause 8 are not achieved, the sample shall be diluted. 3.4 Cross-sensitivities in the determination of NH4+ and Na+ can occur when there are large differences in concentration. 3.5 Solid material and organic compounds (such as mineral oils, deterg
46、ents 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+, NH4+, K+, Mn2+, Ca2+, Mg2+, Sr2+ and Ba2+ by means of a separator column. A low-capacity cation exchanger is used as the
47、 stationary phase, and usually, aqueous solutions of mono- and dibasic acids as mobile phases (eluent, see 6.16). These cations are detected by conductivity. It is essential that the eluents have a sufficiently low conductivity. For this reason, a conductivity detector (CD) is often combined with a
48、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 conductivity detection without chemical suppression, the difference between the ion equivalent conductivities is measured directly a
49、fter 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 is 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