1、BSI Standards PublicationBS ISO 16560:2015Surface active agents Determination of polyethyleneglycol content in nonionicethoxylated surfactants HPLC methodBS ISO 16560:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 16560:2015.The UK participation in its pr
2、eparation 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. Users are responsib
3、le for its correctapplication. The British Standards Institution 2015. Published by BSI StandardsLimited 2015ISBN 978 0 580 77090 6ICS 71.100.40Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Poli
4、cy and Strategy Committee on 30 April 2015.Amendments issued since publicationDate Text affectedBS ISO 16560:2015 ISO 2015Surface active agents Determination of polyethylene glycol content in nonionic ethoxylated surfactants HPLC methodAgents de surface tensioactifs Dosage de la teneur en polythylne
5、 glycol dans les surfactants thoxyls non ioniques Mthode par CLHPINTERNATIONAL STANDARDISO16560First edition2015-04-15Reference numberISO 16560:2015(E)BS ISO 16560:2015ISO 16560:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2015All rights reserved. Unless otherwise specified
6、, 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 requested from either ISO at the address below or ISOs m
7、ember 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 16560:2015ISO 16560:2015(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Ter
8、ms and definitions . 14 Principle 15 Reagents 16 Apparatus . 27 Sampling 27.1 Preparation of the test sample 27.2 Preparation of test solutions . 28 Procedure. 38.1 Apparatus settings . 38.2 Calibration 38.2.1 Preparation of calibration solutions . 38.2.2 Calibration curve . 48.3 Determination . 49
9、Expression of results 510 Precision . 510.1 Repeatability . 510.2 Reproducibility . 511 Test report . 5Annex A (informative) Results of interlaboratory tests for fatty alcohol ethoxylate . 6 ISO 2015 All rights reserved iiiContents PageBS ISO 16560:2015ISO 16560:2015(E)ForewordISO (the International
10、 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 body interested in a subject for which a technical committee has been est
11、ablished 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 Electrotechnical Commission (IEC) on all matters of electrotechnical standardiz
12、ation.The procedures used to develop this document 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 wi
13、th the editorial rules of the ISO/IEC Directives, 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
14、patent rights identified during the development 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.F
15、or an explanation on the meaning of ISO specific 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 information .The committee responsible fo
16、r this document is ISO/TC 91, Surface active agents.iv ISO 2015 All rights reservedBS ISO 16560:2015ISO 16560:2015(E)IntroductionThis International Standard was developed based on EN 12582. ISO 2015 All rights reserved vBS ISO 16560:2015BS ISO 16560:2015Surface active agents Determination of polyeth
17、ylene glycol content in nonionic ethoxylated surfactants HPLC method1 ScopeThis International Standard specifies a method for the determination of the polyethylene glycol (PEG) content in aromatic and aliphatic non-ionic surface active agents of the type R-(O-C2H4) nOH; where n is the mean ethylene
18、oxide (EO) value. It is applicable to all ethoxylated products soluble in methanol or methanol/water mixture. This method applies to PEG concentrations as mass fraction greater than or equal to 0,1 %. This International Standard is not applicable to PEG whose molar mass is lower than 400 g/mol. Mono
19、meric ethylene glycol, diethylene glycol, triethylene glycol, and glycerol are not detected.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.
20、 For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 3696, Water for analytical laboratory use Specification and test methodsISO 607, Surface active agents and detergents Methods of sample divisionISO 5725-2, Accuracy (trueness and precision)
21、measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1polyethylene glycol contentamount of polyethylene gly
22、col, expressed as a percentage by mass, calculated from the calibration curve in accordance with this International Standard4 PrinciplePolyethylene glycol is separated from the polyethoxylated surface active agents by means of reversed phase liquid chromatography. In this process PEG is eluted in th
23、e first minutes while the non-ionic surface active agents are retarded. Evaporative light scattering detector (ELSD) or charged aerosol detector (CAD) does not detect volatile materials such as the sample solvent; interferences with the PEG peak are limited. The sample is dissolved in an 80/20 (V/V)
24、 mixture of methanol/water or in another methanol/water mixture to obtain a clear solution. A portion of the sample solution is then analysed by high performance liquid chromatography (HPLC). Quantification of PEG content is achieved by external calibration with PEG molar mass equal to 1 000 g/mol.5
25、 ReagentsDuring the analysis, use only reagents of recognized analytical grade and the water used shall conform to grade 3 in accordance with ISO 3696.5.1 Polyethylene glycol, with molar mass of 1 000 g/mol, gel permeation chromatography (GPC) grade.INTERNATIONAL STANDARD ISO 16560:2015(E) ISO 2015
26、All rights reserved 1BS ISO 16560:2015ISO 16560:2015(E)5.2 Methanol, HPLC grade, filtered before use with filter unit (6.5).5.3 Water, HPLC grade, filtered before use with filter unit (6.5).5.4 Helium gas, chromatography grade, for degassing eluent.5.5 Nitrogen or air, dry, and without dust.5.6 Mobi
27、le phase, either of the following:a) 80/20 (V/V) mixture of methanol and water;b) methanol.6 ApparatusOrdinary laboratory apparatus and glassware with the following.6.1 HPLC unit, equipped with gradient pump.6.2 Evaporative light scattering detector (ELSD), or charged aerosol detector (CAD).6.3 Chro
28、matography column, octadecyl C18 bonded phase silica gel; 5 m; 250 mm length and 4,6 mm internal diameter.6.4 Data logger/plotter, capable of recording and displaying the chromatographic peak area.6.5 Filter unit, for solvent (0,45 m).7 Sampling7.1 Preparation of the test samplePrepare and store the
29、 test sample in accordance with ISO 607.7.2 Preparation of test solutionsWeigh, to the nearest 0,1 mg, the test sample mass given in Table 1 for the expected PEG content into a 100 ml volumetric flask. Fill to the mark with the mobile phase 5.6 a) or other suitable mixture of methanol/water and diss
30、olve to obtain a clear solution. If necessary, filter through 0,45 m filter unit.2 ISO 2015 All rights reservedBS ISO 16560:2015ISO 16560:2015(E)Table 1Expected PEG content, % Sample mass, ga10,1 to 2 12 to 5 0,55 to 10 0,2510 to 25 0,1aSample mass can be adjusted depending on the detector sensitivi
31、ty.8 Procedure8.1 Apparatus settingsSet the HPLC unit according to the following conditions.8.1.1 Gradienta) t = 0 min 0 % methanol 5.6 b);b) t = 6 min 0 % methanol 5.6 b);c) t = 7 min 100 % methanol 5.6 b);d) t = 30 min 100 % methanol 5.6 b);e) t = 35 min 0 % methanol 5.6 b).NOTE Going from mobile
32、phase 5.6 a) to mobile phase 5.6 b) is done in order to elute the ethoxylated products more rapidly.8.1.2 Flow rate: 1,0 ml/min.8.1.3 Temperature: room temperature.8.1.4 Injection volume: 20 l.8.1.5 Detector: evaporative light scattering detector (ELSD), or charged aerosol detector (CAD).Optimize th
33、e working conditions, depending on the apparatus in use and the physical parameters.8.2 Calibration8.2.1 Preparation of calibration solutionsWeigh, to the nearest 0,1 mg, 0,1 g of polyethylene glycol (PEG 1 000) (5.1) into a 100 ml volumetric flask, dissolve with the mobile phase 5.6 a) and make up
34、to the mark. Quantitatively transfer 1,0 ml, 5,0 ml, 10 ml, 25 ml of this solution each into 100 ml volumetric flasks and make up to the volume with the mobile phase. The concentrations of PEG in these solutions respectively are 0,01 g/l, 0,05 g/l, 0,1 g/l, 0,25 g/l. Mix the solution thoroughly. If
35、necessary, filter through a 0,45 m filter unit.NOTE Mass of polyethylene glycol can be adjusted depending on the detector sensitivity. ISO 2015 All rights reserved 3BS ISO 16560:2015ISO 16560:2015(E)8.2.2 Calibration curveAnalyse, at least twice, calibration solutions prepared in 8.2.1, in accordanc
36、e with the chromatographic conditions given in 8.1. Construct a graph: log of peak area (y-axis) versus log PEG weight in 100 ml (x-axis) and draw a calibration curve.NOTE For ELSD, calibration curves give similar results when molar masses of PEG are less than or equal to 4 000, and curve shift is o
37、bserved when the molar mass of PEG is greater than 4 000. For CAD, calibration curves give similar results when molar masses of PEG are less than or equal to 10 000, and curve shift is observed when the molar mass of PEG is greater than 10 000.8.3 DeterminationTake the test solution as prepared in 7
38、.2 and carry out the analysis in accordance with the chromatographic conditions given in 8.1. Typical chromatograms are shown in Figure 1 and Figure 2.Figure 1 Chromatogram of fatty alcohol ethoxylate (near 3 EO) by ELSDFigure 2 Chromatogram of fatty alcohol ethoxylate (near 25EO) by CAD4 ISO 2015 A
39、ll rights reservedBS ISO 16560:2015ISO 16560:2015(E)NOTE In this reversed phase HPLC method, polyethylene glycol elutes quickly in the first minutes, in only one peak. When the molar mass distribution of PEG is large, it is possible to observe several peaks or shoulders corresponding to different mo
40、lar masses of PEG. Sum the peak areas of the chromatogram corresponding to PEG.9 Expression of resultsUse the calibration curve in 8.2.2 to obtain the PEG mass corresponding to the area given by the integrator. Express the PEG content as mass fraction in percent as follows:PEG,%=mm1000(1)wherem0is t
41、he mass of sample to be analysed (7.2), in grams;m is the mass of PEG determined by means of the calibration curve, in grams.10 Precision10.1 RepeatabilityThe absolute difference between the results of two determinations carried out simultaneously or in rapid succession by the same operator on the s
42、ame sample using the same equipment according to ISO 5725-2 shall not be greater than 0,2 % with a probability of 95 %.Results of an interlaboratory test carried out in accordance with ISO 5725-2 are given in Annex A.10.2 ReproducibilityThe absolute difference between two results obtained in differe
43、nt laboratories on the same sample according to ISO 5725-2 shall not be greater than 0,8 % with a probability of 95 %.Results of an interlaboratory test carried out in accordance with ISO 5725-2 are given in Annex A.11 Test reportThe test report shall include the following information:a) all informa
44、tion necessary for the complete identification of the sample;b) a reference to this International Standard, i.e. ISO 16560;c) the results with their units (see Clause 9);d) room temperature for each liquid chromatographic determination and all information about ELSD or CAD;e) details of any operatio
45、ns not specified in this International Standard or in the International Standards to which reference is made, and any operations regarded as optional, as well as any incidents likely to have affected the results. ISO 2015 All rights reserved 5BS ISO 16560:2015ISO 16560:2015(E)Annex A (informative) R
46、esults of interlaboratory tests for fatty alcohol ethoxylateTable A.1 Fatty alcohol ethoxylate (near 3 EO)LaboratoryNumber of single valuesMean value (g/100 g sample)Standard deviationDetector1 6 0,36 0,018 ELSD2 6 0,38 0,002 ELSD3 6 0,40 0,023 ELSD4 5 6 0,38 0,014 ELSD6 6 0,39 0,014 CAD7 6 0,39 0,0
47、19 CAD8 6 0,33 0,018 CAD9 6 0,34 0,016 CAD10 6 0,38 0,005 CAD11 6 0,39 0,006 CADNumber of laboratories retained after eliminating outliers 11Number of outliers (laboratories) 1Number of accepted results 60Mean value (g/100 g sample) 0,37Repeatability standard deviation sr(g/100 g sample) 0,015 0Repe
48、atability limit: r = 2,83 sr(g/100 g sample) 0,042 4Repeatability relative standard deviation (%) 4,05Reproducibility standard deviation sR(g/100 g sample) 0,028 6Reproducibility limit: R = 2,83 sR(g/100 g sample) 0,080 9Reproducibility relative standard deviation (%) 7,736 ISO 2015 All rights reser
49、vedBS ISO 16560:2015ISO 16560:2015(E)Table A.2 Fatty alcohol ethoxylate (near 25 EO)LaboratoryNumber of single valuesMean value (g/100 g sample)Standard deviationDetector1 6 3,21 0,064 ELSD2 6 3,68 0,074 ELSD3 6 3,30 0,075 ELSD4 6 3,64 0,087 CAD5 6 3,50 0,055 CAD6 6 3,91 0,092 CADNumber of laboratories retained after eliminating outliers 6Number of outliers (laboratories) 0Number of accepted results 36Mean value (g/100 g sample) 3,54Repeatability standard deviation sr(g/100 g sample) 0,
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