EN ISO 10304-1-2009 en Water quality - Determination of dissolved anions by liquid chromatography of ions - Part 1 Determination of bromide chloride fluoride nitrate nitrite phosph.pdf

1、BS EN ISO10304-1:2009ICS 13.060.50NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDWater quality Determination ofdissolved anions byliquid chromatographyof ionsPart 1: Determination of bromide,chloride, fluoride, nitrate, nitrite,phosphate and sulfate (ISO10304-1

2、:2007)This British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 30 April2009 BSI 2009ISBN 978 0 580 65935 5Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 10304-1:2009National forewordThis British Standard is the UK implementation of E

3、N ISO10304-1:2009. It is identical to ISO 10304-1:2007. It supersedes BS ENISO 10304-1:1995 and BS EN ISO 10304-2:1997 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee EH/3/2, Physical chemical and biochemical methods.A list of organizations represented

4、on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.EUROPEAN STANDARDNORM

5、E EUROPENNEEUROPISCHE NORMEN ISO 10304-1March 2009ICS 13.060.50 Supersedes EN ISO 10304-1:1995, EN ISO 10304-2:1996English VersionWater quality - Determination of dissolved anions by liquidchromatography of ions - Part 1: Determination of bromide,chloride, fluoride, nitrate, nitrite, phosphate and s

6、ulfate (ISO10304-1:2007)Qualit de leau - Dosage des anions dissous parchromatographie des ions en phase liquide - Partie 1:Dosage du bromure, chlorure, fluorure, nitrate, nitrite,phosphate et sulfate (ISO 10304-1:2007)Wasserbeschaffenheit - Bestimmung von gelsen Anionenmittels Flssigkeits-Ionenchrom

7、atographie - Teil 1:Bestimmung von Bromid, Chlorid, Fluorid, Nitrat, Nitrit,Phosphat und Sulfat (ISO 10304-1:2007)This European Standard was approved by CEN on 1 March 2009.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this Europe

8、anStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN Management Centre or to any CEN member.This European Standard exists in three official versions (English, F

9、rench, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus,

10、 Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUR

11、OPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: Avenue Marnix 17, B-1000 Brussels 2009 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 10304-1:2009: EBS EN ISO 10304-1:2009EN ISO 10304-1:2009 (E) 3 Foreword

12、The text of ISO 10304-1:2007 has been prepared by Technical Committee ISO/TC 147 “Water quality” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 10304-1:2009 by Technical Committee CEN/TC 230 “Water analysis” the secretariat of which is held by DIN. This

13、 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 September 2009, and conflicting national standards shall be withdrawn at the latest by September 2009. Attention is drawn to the possibility that some o

14、f the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 10304-1:1995, EN ISO 10304-2:1996. According to the CEN/CENELEC Internal Regulations, the national stan

15、dards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, P

16、ortugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 10304-1:2007 has been approved by CEN as a EN ISO 10304-1:2009 without any modification. BS EN ISO 10304-1:2009ISO 10304-1:2007(E) ISO 2007 All rights reserved iiiContents Page

17、 Foreword iv Introduction v 1 Scope . 1 2 Normative references . 1 3 Interferences . 2 4 Principle. 2 5 Reagents 2 6 Apparatus 4 7 Sampling and sample pre-treatment. 7 8 Procedure 8 9 Calculation. 9 10 Expression of results . 9 11 Test report . 9 Annex A (informative) Performance data. 10 Annex B (i

18、nformative) Checked interferences 14 Bibliography . 15 BS EN ISO 10304-1:2009ISO 10304-1:2007(E) iv ISO 2007 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing Internat

19、ional 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 non-governmental, in liaison with I

20、SO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical c

21、ommittees is to prepare International Standards. 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 least 75 % of the member bodies casting a vote. Attention is drawn to th

22、e 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. ISO 10304-1 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemi

23、cal methods. This second edition of ISO 10304-1 cancels and replaces ISO 10304-1:1992 and ISO 10304-2:1995, which have been technically revised. ISO 10304 consists of the following parts, under the general title Water quality Determination of dissolved anions by liquid chromatography of ions: Part 1

24、: Determination of bromide, chloride, fluoride, nitrate, nitrite, phosphate and sulfate Part 3: Determination of chromate, iodide, sulfite, thiocyanate and thiosulfate Part 4: Determination of chlorate, chloride and chlorite in water with low contamination BS EN ISO 10304-1:2009ISO 10304-1:2007(E) I

25、SO 2007 All rights reserved vIntroduction The user should be aware that particular problems could require the specification of additional conditions not provided for in this part of ISO 10304. BS EN ISO 10304-1:2009BS EN ISO 10304-1:2009INTERNATIONAL STANDARD ISO 10304-1:2007(E) ISO 2007 All rights

26、reserved 1Water quality Determination of dissolved anions by liquid chromatography of ions Part 1: Determination of bromide, chloride, fluoride, nitrate, nitrite, phosphate and sulfate WARNING Persons using this International Standard should be familiar with normal laboratory practice. This standard

27、 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 absolutely essential that tests conduc

28、ted according to this International Standard be carried out by suitably trained staff. 1 Scope This part of ISO 10304 specifies a method for the determination of dissolved bromide, chloride, fluoride, nitrate, nitrite, orthophosphate and sulfate in water, e.g. drinking water, ground water, surface w

29、ater, waste water, leachates and marine water by liquid chromatography of ions. The lower limit of application is W 0,05 mg/l for bromide and for nitrite, and W 0,1 mg/l for chloride, fluoride, nitrate, orthophosphate, and sulfate. The lower limit of application depends on the matrix and the interfe

30、rences encountered. The working range may be expanded to lower concentrations (e.g. W 0,01 mg/l) if an appropriate pre-treatment of the sample (e.g. conditions for trace analyses, pre-concentration technique) is applied, and/or if an ultraviolet (UV) detector (for bromide, nitrate and nitrite) is us

31、ed. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 3696, Water for an

32、alytical laboratory use Specification and test methods ISO 5667-3, Water quality Sampling Part 3: Guidance on the preservation and handling of water samples ISO 8466-1, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 1: Statistical ev

33、aluation of the linear calibration function ISO 8466-2, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 2: Calibration strategy for non-linear second-order calibration functions BS EN ISO 10304-1:2009ISO 10304-1:2007(E) 2 ISO 2007 All

34、 rights reserved3 Interferences 3.1 Organic acids Aliphatic organic acids such as mono- or dicarboxylic acids may interfere with the separation of the anions. 3.2 Sulfite Sulfite may cause a positive bias for sulfate due to autooxidation. In this case the sample may be adjusted to pH 10 and formalde

35、hyde solution is added in order to stabilize sulfite, if necessary. 3.3 Metals The presence of metals (e.g. alkaline earth metals, transition metals, heavy metals) possibly interfering with the anions of interest, should be checked and can be eliminated with the aid of special cation exchangers (e.g

36、. cartridge in the H-form or Na-form). NOTE Depending on the sample matrix, the use of cation exchangers in the H-form can cause losses of fluoride and nitrite. 4 Principle The sample is pretreated in order to remove solids (see Clause 7), sulfite and metal ions, if necessary. The anions of interest

37、 (bromide, chloride, fluoride, nitrate, nitrite, orthophosphate and sulfate), are separated by liquid chromatography, applying an anion exchange resin as stationary phase, and aqueous solutions of salts of weak mono- and dibasic acids as eluents for isocratic or gradient elution (e.g. carbonate, hyd

38、rogencarbonate, hydroxide eluent) (5.10). Detection is carried out using a conductivity detector (CD). When using CDs it is essential that the eluents show a sufficiently low conductivity. For this reason, CDs are usually combined with a suppressor device (cation exchanger), which will reduce the co

39、nductivity of the eluent and transform the sample species into their respective acids. NOTE A UV detector is not required to carry out this analysis, but can be used for bromide, nitrate or nitrite if a higher sensitivity is required and/or in case of a matrix interference to the CD. If used, bromid

40、e, nitrate and nitrite can be measured at = 200 nm to = 215 nm. Check resolution, R, to ensure that it complies with the required separation conditions (6.2). UV may be used in combination with a CD. UV measures the absorption directly. Calibration is carried out as specified in ISO 8466-1 or ISO 84

41、66-2 (8.2). In special cases, extended working ranges (e.g. two concentration decades) may be applied. Control experiments are necessary to check the validity of the calibration function. Replicate determinations may be necessary. Use of the method of standard addition may be required when matrix in

42、terferences are expected (8.3). 5 Reagents Use only reagents of recognized analytical grade. Weigh the reagents with an accuracy of 1 % of the nominal mass, unless stated otherwise. The reagents listed in 5.2 to 5.5 may be considered representative examples for the preparation of eluents (5.10). 5.1

43、 Water, complying with grade 1, as defined in ISO 3696. 5.2 Sodium hydrogencarbonate, NaHCO3. BS EN ISO 10304-1:2009ISO 10304-1:2007(E) ISO 2007 All rights reserved 35.3 Sodium carbonate, Na2CO3. 5.4 Sodium hydroxide, NaOH. 5.5 Potassium hydroxide, KOH. 5.6 Bromide, chloride, fluoride, nitrate, nitr

44、ite, orthophosphate and sulfate stock standard solutions, = 1 000 mg/l each. Single anion and mixed anion stock solutions with adequate and required specification are commercially available. These solutions are considered to be stable for several months. For an alternative preparation of stock solut

45、ions see Table 1. Dissolve the salts accordingly, after appropriate treatment. Table 1 Mass portion and pre-treatment for stock solutions Mass Anion to be determined Salt to be usedag Pre-treatment by drying at (105 5) C for at least Bromide NaBr 1,287 7 6 h Chloride NaCl 1,648 4 2 Fluoride NaF 2,21

46、0 0 1 h Nitrate NaNO31,370 7 24 h Nitrite NaNO21,499 8 1 h Orthophosphate KH2PO41,433 0 1 h Sulfate Na2SO41,478 6 1 h aAlternative salts with adequate and required specification may be used. 5.7 Bromide, chloride, fluoride, nitrate, nitrite, orthophosphate and sulfate standard solutions 5.7.1 Genera

47、l Depending on the concentrations expected, prepare single or mixed standard solutions, of bromide, chloride, fluoride, nitrate, nitrite, orthophosphate and sulfate concentrations from the stock standard solution (5.6). Store the standard solutions in polyethene bottles. 5.7.2 Example for a bromide,

48、 chloride, fluoride, nitrate, nitrite, orthophosphate and sulfate mixed standard solution, = 10 mg/l each. Pipette 1,0 ml of each of the stock standard solutions (5.6) into a 100 ml volumetric flask, and dilute to volume with water (5.1). The solutions are stable for 1 week, if stored in the dark at

49、 2 C to 8 C in polyethene bottles. 5.8 Bromide, chloride, fluoride, nitrate, nitrite, orthophosphate and sulfate calibration solutions Depending on the concentrations expected in the sample, use the standard solution (5.7.2) to prepare e.g. 5 to 10 calibration solutions distributed as evenly as possible over the expected working range. For example, proceed as follows for the range 0,05 mg/l to 0,5 mg/l: BS EN ISO 10304-1:2009ISO 10304-1:2007(E) 4 ISO 2007 All rights reservedPipette, into a series of 20 ml