1、BSI Standards PublicationBS ISO 17293-2:2014Surface active agents Determination of chloroaceticacid (chloroacetate) insurfactantsPart 2: Ionic chromatographic methodBS ISO 17293-2:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 17293-2:2014.The UK particip
2、ation in its preparation was entrusted to TechnicalCommittee CII/34, Methods of test for surface active agents.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 contract. User
3、s are responsible for its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 76728 9ICS 71.100.40Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of th
4、eStandards Policy and Strategy Committee on 31 March 2014.Amendments issued since publicationDate Text affectedBS ISO 17293-2:2014 ISO 2014Surface active agents Determination of chloroacetic acid (chloroacetate) in surfactants Part 2: Ionic chromatographic methodAgents de surface Dtermination de lac
5、ide chloroactique (chloroactate) dans les agents tensioactifs Partie 2: Mthode par chromatographie ioniqueINTERNATIONAL STANDARDISO17293-2First edition2014-04-01Reference numberISO 17293-2:2014(E)BS ISO 17293-2:2014ISO 17293-2:2014(E)ii ISO 2014 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 20
6、14All 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 can be request
7、ed 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 17293-2:2014ISO 17293-2:2014(E) ISO 2014 Al
8、l rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Principle 14 Reagents 14.1 General . 15 Apparatus . 26 Procedure. 36.1 General . 36.2 Ion chromatographic condition 36.3 Calibration 36.4 Sampling and analysis 37 Results and calculation 47.1 General . 47.2 Content of
9、monochloroacetic acid 47.3 Content of dichloroacetic acid . 48 Precision . 48.1 Repeatability limit 48.2 Reproducible limit . 59 Test report . 5Annex A (informative) Typical chromatograms 6BS ISO 17293-2:2014ISO 17293-2:2014(E)ForewordISO (the International Organization for Standardization) is a wor
10、ldwide 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 interested in a subject for which a technical committee has been established has the right to be represented on
11、 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 Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this d
12、ocument 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 documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Direc
13、tives, 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 for identifying any or all such patent rights. Details of any patent rights identified during the develo
14、pment 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 the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO s
15、pecific 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: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 91, Surface acti
16、ve agents.ISO 17293 consists of the following parts, under the general title Surface active agents Determination of chloroacetic acid (chloroacetate) in surfactants: Part 1: HPLC method Part 2: Ionic chromatographic methodiv ISO 2014 All rights reservedBS ISO 17293-2:2014INTERNATIONAL STANDARD ISO 1
17、7293-2:2014(E)Surface active agents Determination of chloroacetic acid (chloroacetate) in surfactants Part 2: Ionic chromatographic method1 ScopeThis part of ISO 17293 specifies a method for the determination of monochloroacetic acid (monochloroacetate) and dichloroacetic acid (dichloroacetate) in s
18、urfactants by ion chromatographic method.The method applies for anionic surfactants such as alkyl (phenyl) ethoxylated carboxylate (AEC) or amphoteric surfactants such as alkyl imidazoline carboxylate, alkyl dimethyl betaine, and fatty acetyl propyl dimethyl betaine.The limit of detection (LOD) is 0
19、,01 g/ml for monochloroacetic acid and 0,05 g/ml for dichloroacetic acid; and the limit of quantification (LOQ) is 0,1 g/ml for each standard (using a standard solution).The LOD, at 1 g of sample weight, is 1 mg/kg for monochloroacetic acid and 5 mg/kg for dichloroacetic acid; and the LOQ is 10 mg/k
20、g for each acid.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 the edition cited applies. For undated references, the latest edition of the referenced document (incl
21、uding any amendments) applies.ISO 607, Surface active agents and detergents Methods of sample divisionISO 3696, Water for analytical laboratory use Specification and test methodsISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determinatio
22、n of repeatability and reproducibility of a standard measurement method3 PrincipleThe sample solution is diluted to a proper concentration and flows through an anionic ion exchange column. The monochloroacetic acid (monochloroacetate) and dichloroacetic acid (dichloroacetate) are adsorbed in the col
23、umn then eluted by the mobile phase and detected by an electrical conductivity detector.The contents of monochloroacetic acid and dichloroacetic acid in the sample are achieved by the external calibration method.4 Reagents4.1 GeneralDuring the analysis, use only reagents of recognized analytical gra
24、de and the water used shall conform to grade 1 in accordance with ISO 3696, unless otherwise specified. ISO 2014 All rights reserved 1BS ISO 17293-2:2014ISO 17293-2:2014(E)4.2 Monochloroacetic acid (ClCH2COOH), purity 99 % (w/w)4.3 Dichloroacetic acid (Cl2CHCOOH), purity 99 % (w/w)4.4 Sulfuric acid
25、(H2SO4)4.5 Sodium carbonate (Na2CO3)4.6 Sodium hydrogen carbonate (NaHCO3)4.7 Sodium hydroxide (NaOH)4.8 Sodium carbonate/sodium hydrogen carbonate eluent stock solution, containing 0,32 mol/l sodium carbonate and 0,1 mol/l sodium hydrogen carbonate.Dissolve 3,39 g of sodium carbonate (4.5) and 0,84
26、 g of sodium hydrogen carbonate (4.6) in 30 ml of water and swirl to mix. Quantitatively transfer the solution to a 100 ml volumetric flask (5.8), make up to the mark with water, stopper, and mix thoroughly.4.9 Sodium carbonate/sodium hydrogen carbonate eluent solution, containing 3,2 mmol/l sodium
27、carbonate and 1 mmol/l sodium hydrogen carbonate.Quantitatively transfer 10 ml of sodium carbonate/sodium hydrogen carbonate stock solution (4.8) to a 1 000 ml volumetric flask (5.8), dilute to the mark with water, stopper, and mix thoroughly.4.10 Sulfuric acid solution, 50 mmol/lDilute 3,0 ml of su
28、lfuric acid (4.4) in 1 000 ml of water, mix thoroughly.4.11 Sodium hydroxide solution, 15 mmol/lDissolve 0,6 g of sodium hydroxide (4.7) in 30 ml of water and swirl to mix. Quantitatively transfer the solution to a 1 000 ml volumetric flask (5.8), dilute to the mark with water, stopper, and mix thor
29、oughly.5 ApparatusUse usual laboratory apparatus and, in particular, the following.5.1 Ion chromatography instrument, equipped with pump, separator column, guard column, appropriate suppressor, data process system, and electrical conductivity detector.5.2 Separator column, anionic ion exchange colum
30、n, suitable for resolving monochloroacetic acid and dichloroacetic acid from sample, 4 mm 250 mm, with appropriate guard column.5.3 Filter syringe, of capacity 2 ml or 5 ml.5.4 Injection syringe, of capacity 25 l.5.5 Analytical balance, accurate to 0,1 mg.5.6 Filters, with suitable porosity (0,2 m o
31、r 0,45 m) for the filtration of reagents and sample.5.7 Vacuum pump.5.8 Volumetric flasks, of capacity 100 ml and 1 000 ml.5.9 Glass beakers, of capacity 25 ml and 100 ml.2 ISO 2014 All rights reservedBS ISO 17293-2:2014ISO 17293-2:2014(E)6 Procedure6.1 GeneralThe choice of chromatographic condition
32、s depends on the apparatus in use and can be varied from those given below, provided that suitable separation of the compounds of interest is maintained. The following conditions have been found to be suitable for the column recommended.6.2 Ion chromatographic conditionTwo kinds of ion chromatograph
33、ic conditions can be used in this part of ISO 17293, depending on the apparatus selected.6.2.1 Ion chromatographic condition 1a) Eluent solution (4.9)b) Flow rate: 0,70 ml/minc) Column temperature: room temperatured) Injection volume: 20 le) Regeneration solution (4.10)Based on the above conditions,
34、 a typical chromatogram can be found in Figure A.1.6.2.2 Ion chromatographic condition 2a) Eluent solution (4.11)b) Flow rate: 0,85 ml/minc) Column temperature: room temperatured) Injection volume: 20 lBased on the above conditions, a typical chromatogram can be found in Figure A.2.6.3 Calibration1)
35、 Dissolve 0,1 g of monochloroacetic acid (4.2) and 0,1 g of dichloroacetic acid (4.3), accurate to 0,1 mg, in 20 ml of water. Transfer quantitatively to a 1 000 ml volumetric flask(5.8), make up to the mark with water and completely homogenize.Store this solution in a refrigerator at (4 2) C and ren
36、ew it every 7 d.Quantitatively dilute 0,1 ml, 0,5 ml, 1,0 ml, 5,0 ml, and 10,0 ml of this solution to 100 ml with water, respectively. These standards shall be freshly prepared before analysis.2) Filter (5.6) the diluted solutions and inject 20 l each to equipment for analysis. The analysis must be
37、done at least twice in accordance with the chromatographic conditions given in 6.2.1 or 6.2.2. The obtained linear correlation coefficient (R) shall be 0,999 or above.6.4 Sampling and analysisPrepare and store the test sample in accordance with ISO 607. ISO 2014 All rights reserved 3BS ISO 17293-2:2
38、014ISO 17293-2:2014(E)Add approximately 1 g of sample, accurate to 0,1 mg, in 30 ml of water, and stir until the sample is dissolved completely. Transfer into a 100 ml volumetric flask, make up to the mark with water. Filter (5.6) the solution and inject 20 l for analysis on the appropriate chromato
39、graphic condition.If necessary, pretreatment should be done to remove surfactant in order to protect the ion exchange column. Reversed phase ODS can be used before injection.7 Results and calculation7.1 GeneralDetermine the monochloroacetic acid and dichloroacetic acid contents in the test sample us
40、ing the procedure according to 6.4. Calculate the results in milligrams per kilogram (mg/kg) according to Formula (1) and Formula (2). Under given experimental conditions, no hydrolysis of chloroacetic acid has been observed.7.2 Content of monochloroacetic acidXmgkgAVm1(/)=(1)whereX1is the content o
41、f monochloroacetic acid, in milligrams per kilogram;A is the calculated concentration of monochloroacetic acid in the test sample solution, in micro-grams per millilitre;V is the volume of test sample, in millilitres;m is the mass of the test sample, in grams.7.3 Content of dichloroacetic acidXmgkgB
42、Vm2(/)=(2)whereX2is the content of dichloroacetic acid, in milligrams per kilogram;B is the calculated concentration of dichloroacetic acid in the test sample solution, in micro-grams per millilitre.8 Precision8.1 Repeatability limitThe absolute difference between two independent single test results
43、, obtained using the same method on identical test material in the same laboratory by the same operator using the same equipment within a short interval of time, shall not exceed the repeatability limit (r) in more than 5 % of cases.According to ISO 5725-2, r can be expected to be: 10 % for contents
44、 greater than or equal to 50 mg/kg;4 ISO 2014 All rights reservedBS ISO 17293-2:2014ISO 17293-2:2014(E) 15 % for contents less than 50 mg/kg.8.2 Reproducible limitThe absolute difference between two single test results, obtained using the same method on identical test material in different laborator
45、ies by different operators using different equipment, shall not exceed the reproducibility limit (R) in more than 5 % of cases. R can be expected to be 35 %.9 Test reportThe test report shall include the following information:a) the test method used, with a reference to this part of ISO 17293 (i.e.
46、part of ISO 17293-2);b) all information necessary for the complete identification of the test compound;c) all the data (e.g. in tabular form) obtained and the calibration curve;d) all operating details not specified in this part of ISO 17293, or regarded as optional, together with details of any inc
47、idents which may have influenced the test result(s). ISO 2014 All rights reserved 5BS ISO 17293-2:2014ISO 17293-2:2014(E)Annex A (informative) Typical chromatogramsFigure A.1 A typical IC chromatogram for monochloroacetic acid and dichloroacetic acid (on IC condition 1)Figure A.2 A typical IC chroma
48、togram for monochloroacetic acid and dichloroacetic acid (on IC condition 2)6 ISO 2014 All rights reservedBS ISO 17293-2:2014BS ISO 17293-2:2014ISO 17293-2:2014(E) ISO 2014 All rights reservedICS 71.100.40Price based on 6 pagesThis page deliberately left blankBSI is the national body responsible for
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