1、BS ISO13885-1:2008ICS 87.060.20,NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDBinders for paintsand varnishes Gel permeationchromatography (GPC)Part 1: Tetrahydrofuran (THF) aseluentThis British Standardwas published underthe authority of theStandards Policy a
2、ndStrategy Committee on 30November 2008 BSI 2008ISBN 978 0 580 59785 5Amendments/corrigenda issued since publicationDate CommentsBS ISO 13885-1:2008National forewordThis British Standard is the UK implementation of ISO 13885-1:2008. Itsupersedes BS6782-14:1999 and which is withdrawn.The UK participa
3、tion in its preparation was entrusted to TechnicalCommittee STI/3, Paints, media and related products.A list of organizations represented 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 res
4、ponsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.BS ISO 13885-1:2008Reference numberISO 13885-1:2008(E)ISO 2008INTERNATIONAL STANDARD ISO13885-1Second edition2008-08-01Binders for paints and varnishes Gel permeation chromatography (
5、GPC) Part 1: Tetrahydrofuran (THF) as eluent Liants pour peintures et vernis Chromatographie par permation de gel (GPC) Partie 1: Utilisation de ttrahydrofurane (THF) comme luant BS ISO 13885-1:2008ISO 13885-1:2008(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Ad
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8、re has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. COPYRIGHT PROTECTED DOCUMENT ISO 2008 All rights reserved. Unless otherwise specified, n
9、o part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case post
10、ale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2008 All rights reservedBS ISO 13885-1:2008ISO 13885-1:2008(E) ISO 2008 All rights reserved iiiContents Page Foreword iv 1 Scope . 1 2 Normative references .
11、1 3 Terms and definitions. 2 4 Principle. 2 5 Apparatus 2 5.1 General. 2 5.2 Eluent supply 2 5.3 Pump 2 5.4 Injection system 3 5.5 Columns. 3 5.6 Column temperature control . 4 5.7 Detector . 4 5.8 Data acquisition 5 6 Eluent . 5 7 Calibration of the apparatus 5 7.1 General. 5 7.2 Specification for
12、the calibration standard 5 7.3 Preparation of the calibration solutions for injection. 6 7.4 Conditions for calibration runs . 7 7.5 Measurement of retention volume/time 7 7.6 Plotting the calibration curve 7 8 Sampling 7 9 Preparation for the test 8 9.1 Preparation of the injection solution 8 9.2 P
13、reparation of the apparatus. 8 10 Conditions of analysis 8 11 Data acquisition and evaluation 9 11.1 General. 9 11.2 Calculation of the net chromatogram from the raw data 9 11.3 Calculation of the average values. 10 11.4 Calculation of the distribution curves 11 12 Precision 12 12.1 General. 12 12.2
14、 Repeatability 12 12.3 Reproducibility 12 13 Test report . 13 13.1 General. 13 13.2 General data on the equipment and settings. 13 13.3 Special data on the sample 14 Annex A (normative) Calculation of experimental parameters for different column sizes 17 Annex B (informative) Example of a data sheet
15、 for a polymer standard 18 Annex C (informative) Further information 19 Bibliography . 23 BS ISO 13885-1:2008ISO 13885-1:2008(E) iv ISO 2008 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies)
16、. 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 committee. International organizations, governmental and non
17、-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. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part
18、 2. The main task of technical committees 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
19、a vote. 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. ISO 13885-1 was prepared by Technical Committee ISO/TC 35, Paints and varnishes, Subcommittee
20、 SC 10, Test methods for binders for paints and varnishes. This second edition cancels and replaces the first edition (ISO 13885-1:1998), which has been technically revised. In particular, the method has been brought into line with the current state of the art, especially as far as the software used
21、 is concerned, and the procedure for the manual evaluation of the results has been deleted. ISO 13885 consists of the following parts, under the general title Binders for paints and varnishes Gel permeation chromatography (GPC): Part 1: Tetrahydrofuran (THF) as eluent BS ISO 13885-1:2008INTERNATIONA
22、L STANDARD ISO 13885-1:2008(E) ISO 2008 All rights reserved 1Binders for paints and varnishes Gel permeation chromatography (GPC) Part 1: Tetrahydrofuran (THF) as eluent WARNING This part of ISO 13885 may involve hazardous materials, operations or equipment. It does not purport to address all of the
23、 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. A specific hazard statement appears in Clause 6. 1 Scope This part of ISO 13885 describes the
24、 determination of the molar-mass distribution, number-average molar mass Mnand mass-average molar mass Mwof polymers that are soluble in THF (tetrahydrofuran) by gel permeation chromatography (GPC)1). It is possible that, in spite of the good repeatability obtained with this method, it cannot be use
25、d with certain polymer types because of specific interactions, such as adsorption within the sample/eluent/column system. The method is not an absolute one and requires calibration with commercially available unbranched-polystyrene standards that have been characterized by absolute methods. The resu
26、lts for samples of polymers other than polystyrene are therefore only comparable within groups of samples of the same type. The conditions specified in this part of ISO 13885 are not suitable for the GPC analysis of polymer samples with Mwvalues greater than 106(see Annex C). No correction methods,
27、e.g. for the elimination of peak broadening, are included in this part of ISO 13885. If absolute molar-mass values are required, an absolute method, e.g. membrane osmometry for Mnor light scattering for Mw, must be used. 2 Normative references The following referenced documents are indispensable for
28、 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 1513, Paints and varnishes Examination and preparation of samples for testing ISO 5725-1, Accuracy (t
29、rueness and precision) of measurement methods and results Part 1: General principles and definitions ISO 15528, Paints, varnishes and raw materials for paints and varnishes Sampling 1) Also known as size exclusion chromatography (SEC). BS ISO 13885-1:2008ISO 13885-1:2008(E) 2 ISO 2008 All rights res
30、erved3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 gel permeation chromatography chromatographic method in which the completely dissolved molecules of a polymer sample are fractionated on a porous column material, separation taking place ac
31、cording to the size of the molecule (or, more precisely, the size of the polymer coil which forms in this elution solvent) NOTE 1 Small molecules diffuse into the pores of the column material more frequently and are therefore retarded more than large molecules. Thus large molecules are eluted earlie
32、r, small molecules later. Under the test conditions given, the retention volume is solely a function of the size of the molecule. NOTE 2 This is a special form of liquid chromatography. 4 Principle The polymer content of a sample is determined, the sample is then diluted with eluent to give a concen
33、tration of less than 5 g/l and an aliquot of the diluted sample is injected into the GPC system. The concentration of the molecules eluted from the column is measured in order of decreasing coil size with a concentration-sensitive detector, typically a differential refractometer. The molar-mass dist
34、ribution, the quantities Mnand Mwand the heterogeneity or polydispersity Mw/Mnare calculated from the resultant chromatogram with the aid of a calibration curve that has been determined for the particular GPC system. 5 Apparatus 5.1 General The apparatus shall consist of the components shown in Figu
35、re 1, which are described below. It is essential that all components which come into contact with the eluent or the sample solution are resistant to them and do not exhibit adsorption or memory effects in any form. The individual components of the GPC apparatus, which in this case uses THF as eluent
36、, shall be linked with stainless-steel or titanium capillary tubes. 5.2 Eluent supply The eluent reservoir shall provide the eluent with adequate protection against external influences such as the atmosphere and light, if necessary by means of a blanket of inert gas over the surface of the liquid. T
37、he eluent reservoir shall have sufficient capacity to permit equilibrium to be established between the elution solvent and the surface of the column material and several analyses to be conducted. The eluent shall be degassed, either before it is introduced into the reservoir or by use of a device fi
38、tted between the reservoir and the pump, to prevent malfunctions of the pump or the formation of bubbles in the detector. The method of degassing used, e.g. bubble trap, online purging with helium, or vacuum degassing, is open to choice. 5.3 Pump The pump ensures that the eluent flow through the col
39、umn is as smooth and pulse-free as possible. The flow rate shall be 1 ml/min (see, however, Annex A). The maximum permitted variation in the flow rate is 0,1 %. To fulfil these requirements, the pump shall operate at optimum efficiency at this flow rate. BS ISO 13885-1:2008ISO 13885-1:2008(E) ISO 20
40、08 All rights reserved 35.4 Injection system The injection system serves to introduce a predetermined, precise amount of the sample solution into the eluent stream in a rapid and smooth fashion. When filling the sample loop with sample solution and subsequently introducing the sample solution into t
41、he eluent stream, the volume of liquid used shall be great enough to ensure that, even if laminar-flow effects occur, the sample loop is completely filled with the sample solution and subsequently completely flushed out. Memory effects from the previous sample solution in the injection system shall
42、be avoided by suitable design or by adequate flushing. 5.5 Columns The apparatus shall have one or more columns connected in series and packed with spherical porous material, the diameter of the pores corresponding to the size of the polymer molecules being analysed. The packing material typically c
43、onsists of a styrene/divinylbenzene (S/DVB) copolymer, produced by a special polymerization process, which swells only slightly in the solvent and therefore will not normally deform under the pressure developed at the flow rate used. In addition to these macroporous spherical S/DVB particles, packin
44、g materials based on other organic monomers or on silicon dioxide (silica) are also used. The criterion for their use is that no adsorptive interaction shall occur between their surface and the polymer molecules in the sample. Furthermore, the sample being analysed shall not be changed, either chemi
45、cally or structurally, within the chromatographic system. Certain polymers can interact with the surface of the packing material, e.g. by adsorption, and other effects can sometimes interfere with the GPC separation mechanism. Details of such effects and notes on possible remedies are discussed in A
46、nnex C. If it is intended to compare analyses by different laboratories of such polymers, the laboratories shall agree on details of the test conditions that are not covered by this part of ISO 13885. One of the objectives of this part of ISO 13885 is to ensure that results obtained in different lab
47、oratories using different GPC apparatus for the same sample agree as well as possible. In order to meet this objective, it is necessary to adhere to the minimum requirements specified below with regard to peak broadening (expressed in terms of a number of theoretical plates) and separation performan
48、ce. a) Number of theoretical plates The number of theoretical plates N shall be determined, for the apparatus used, from the peak width at half height (see Figure 2). Inject 20 l of a solution of ethylbenzene (concentration 1 g/l) on to the column (see Annex A) and evaluate the chromatogram obtained
49、 under the same conditions as are used for analysing polymers, according to the following equation: 2e1/21005,54VNWL= (1) where Veis the retention volume to the peak maximum; W1/2is the peak width at half height (see Figure 2) use the same units for Veand W; L is the length, in cm, of the column/column system. Express the result as the number of theoretical plates per metre of total column length. To meet the requirements of this part of ISO 13885, the column system shall have at least 20 000 plates/m. Consult Annex C wit
