07-30169420-DC.pdf

a date: 20 july 2007 origin: international latest date for receipt of comments: 31 october 2007 project no.: 2007/02008 responsible committee: sti/3 paints, media and related products interested committees: title: draft bs iso 13885-1 binders for paints and varnishes - gel permeation chromatography (gpc) part 1: tetrahydrofuran (thf) as eluent supersession information: if this document is published as a standard, the uk implementation of it will supersede bs6782-14 : 1999 and partially supersede. none if you are aware of a current national standard which may be affected, please notify the secretary (contact details below). warning: this is a draft and must not be regarded or used as a british standard. this draft is not current beyond 31 october 2007. this draft is issued to allow comments from interested parties; all comments will be given consideration prior to publication. no acknowledgement will normally be sent. see overleaf for information on commenting. no copying is allowed, in any form, without prior written permission from bsi except as permitted under the copyright, designs and patent act 1988 or for circulation within a nominating organization for briefing purposes. electronic circulation is limited to dissemination by e-mail within such an organization by committee members. further copies of this draft may be purchased from bsi customer services, tel: +44(0) 20 8996 9001 or email . british, international and foreign standards are also available from bsi customer services. british standards on cd or online are available from british standards publishing sales limited. tel: 01344 404409 or email bsonlinetechindex.co.uk. information on the co-operating organizations represented on the committees referenced above may be obtained from the responsible committee secretary. cross-references the british standards which implement international or european publications referred to in this draft may be found via the british standards online service on the bsi web site . direct tel: 020 8996 7009 responsible committee secretary: committee service centre (bsi) e-mail: draft for public comment head office 389 chiswick high road london w4 4al telephone: +44(0)20 8996 9000 fax: +44(0)20 8996 7001 form 36 version 7.0 dpc: 07/30169420 dc licensed copy: london south bank university, london south bank university, wed aug 08 04:06:00 gmt+00:00 2007, uncontrolled copy, (c) bsi b introduction this draft standard is based on international discussions in which the uk has taken an active part. your comments on this draft are invited and will assist in the preparation of the consequent standard. comments submitted will be reviewed by the relevant bsi committee before sending the consensus uk vote and comments to the international secretariat, which will then decide appropriate action on the draft and the comments received. if no comments are received to the contrary, then the uk will approve this draft. if the international standard is approved, it is possible the text will be published as an identical british standard. uk vote please indicate whether you consider the uk should submit a negative (with reasons) or positive vote on this draft. submission the guidance given below is intended to ensure that all comments receive efficient and appropriate attention by the responsible bsi committee. annotated drafts are not acceptable and will be rejected. all comments must be submitted, preferably electronically, to the responsible committee secretary at the address given on the front cover. comments should be compatible with version 6.0 or version 97 of microsoft word for windows, if possible; otherwise comments in ascii text format are acceptable. any comments not submitted electronically should still adhere to these format requirements. all comments submitted should be presented as given in the example below. further information on submitting comments and how to obtain a blank electronic version of a comment form are available from the bsi web site at: /en/standards-and-publications/current-work/dpcs/ template for comments and secretariat observations date: xx/xx/200x document: iso/dis xxxxx 1 2 (3) 4 5 (6) (7) mb clause no./ subclause no./ annex (e.g. 3.1) paragraph/ figure/table/ note (e.g. table 1) type of com- ment comment (justification for change) by the mb proposed change by the mb secretariat observations on each comment submitted 3.1 definition 1 ed definition is ambiguous and needs clarifying. amend to read . so that the mains connector to which no connection . 6.4 paragraph 2 te the use of the uv photometer as an alternative cannot be supported as serious problems have been encountered in its use in the uk. delete reference to uv photometer. microsoft and ms-dos are registered trademarks, and windows is a trademark of microsoft corporation. licensed copy: london south bank university, london south bank university, wed aug 08 04:06:00 gmt+00:00 2007, uncontrolled copy, (c) bsi this document is a draft circulated for comment and approval. it is therefore subject to change and may not be referred to as an international standard until published as such. in addition to their evaluation as being acceptable for industrial, technological, commercial and user purposes, draft international standards may on occasion have to be considered in the light of their potential to become standards to which reference may be made in national regulations. recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are aware and to provide supporting documentation. draft international standard iso/dis 13885-1 international organization for standardization, 2007 international organization for standardization organisation internationale de normalisation iso/tc 35/sc 10 voting begins on: 2007-07-17 secretariat: din voting terminates on: 2007-12-17 binders for paints and varnishes gel permeation chromatography (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 revision of first edition (iso 13885-1:1998) ics 87.060.20 in accordance with the provisions of council resolution 15/1993 this document is circulated in the english language only. conformment aux dispositions de la rsolution du conseil 15/1993, ce document est distribu en version anglaise seulement. to expedite distribution, this document is circulated as received from the committee secretariat. iso central secretariat work of editing and text composition will be undertaken at publication stage. pour acclrer la distribution, le prsent document est distribu tel quil est parvenu du secrtariat du comit. le travail de rdaction et de composition de texte sera effectu au secrtariat central de liso au stade de publication. licensed copy: london south bank university, london south bank university, wed aug 08 04:06:00 gmt+00:00 2007, uncontrolled copy, (c) bsi iso/dis 13885-1 ii iso 2007 all rights reserved pdf disclaimer this pdf file may contain embedded typefaces. in accordance with adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. in downloading this file, parties accept therein the responsibility of not infringing adobes licensing policy. the iso central secretariat accepts no liability in this area. adobe is a trademark of adobe systems incorporated. details of the software products used to create this pdf file can be found in the general info relative to the file; the pdf-creation parameters were optimized for printing. every care 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 notice this iso document is a draft international standard and is copyright-protected by iso. except as permitted under the applicable laws of the users country, neither this iso draft nor any extract from it may be reproduced, stored in a retrieval system or transmitted in any form or by any means, electronic, photocopying, recording or otherwise, without prior written permission being secured. requests for permission to reproduce should be addressed to either iso at the address below or isos member body in the country of the requester. iso copyright office case postale 56 ch-1211 geneva 20 tel. + 41 22 749 01 11 fax + 41 22 749 09 47 e-mail web reproduction may be subject to royalty payments or a licensing agreement. violators may be prosecuted. licensed copy: london south bank university, london south bank university, wed aug 08 04:06:00 gmt+00:00 2007, uncontrolled copy, (c) bsi iso/dis 13885-1 iso 2007 all rights reserved iii contents page foreword iv 1 scope1 2 normative references1 3 terms and definitions.1 4 principle .2 5 apparatus.2 5.1 general .2 5.2 eluent supply.2 5.3 pump.2 5.4 injection system 2 5.5 columns .3 5.6 column temperature control4 5.7 detector4 5.8 data acquisition.5 6 reagent (eluent) 5 7 calibration of the apparatus.5 7.1 general .5 7.2 specification for the calibration standard 5 7.3 preparation of the calibration solutions for injection6 7.4 conditions for calibration runs7 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 preparation of the apparatus .8 10 conditions of analysis8 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 repeatability12 12.3 reproducibility 12 13 test report13 13.1 general .13 13.2 general data on the equipment and settings .13 annex a (normative) conversion of experimental parameters for variant column combinations.17 annex b (informative) example of a data sheet for a polymer standard.19 annex c (informative) further information.20 bibliography25 licensed copy: london south bank university, london south bank university, wed aug 08 04:06:00 gmt+00:00 2007, uncontrolled copy, (c) bsi iso/dis 13885-1 iv iso 2007 all rights reserved foreword iso (the international 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 established 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 standardization. international standards are drafted in accordance with the rules given in the iso/iec directives, part 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 a vote. iso 13885-1 was prepared by technical committee iso/tc 35, paints and varnishes, subcommittee sc 10, binders for paints and varnishes. this second edition cancels and replaces the first edition (iso 13885-1:1998), which has been technically revised. the main technical changes are: a) the standard has been adapted to the actual state-of-the-art especially of the software; b) the manual evaluation of results has been deleted; c) references to astm standards were 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 licensed copy: london south bank university, london south bank university, wed aug 08 04:06:00 gmt+00:00 2007, uncontrolled copy, (c) bsi iso/dis 13885-1 iso 2007 all rights reserved v introduction warning this standard may involve hazardous materials, operations and equipment. this standard does not purport to address all of the safety problems associated with its use. it is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. a specific hazard statement appears in note 5. licensed copy: london south bank university, london south bank university, wed aug 08 04:06:00 gmt+00:00 2007, uncontrolled copy, (c) bsi licensed copy: london south bank university, london south bank university, wed aug 08 04:06:00 gmt+00:00 2007, uncontrolled copy, (c) bsi draft international standard iso/dis 13885-1 iso 2007 all rights reserved 1 binders for paints and varnishes gel permeation chromatography (gpc) part 1: tetrahydrofuran (thf) as eluent 1 scope this international standard describes the determination of the molar mass distribution, number-average molar mass mn and weight-average molar mass mw of 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 used 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 results for samples of polymers other than polystyrene are therefore only comparable within groups of samples of the same type. the conditions specified in this standard are not suitable for the gpc analysis of polymer samples with mw values greater than 106 (see annex c). no correction methods, e.g. for the elimination of peak broadening, are included in this standard. if absolute molar mass values are required, an absolute method, e.g. membrane osmometry for mn or light scattering for mw, must be used. 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 1513, paints and varnishes examination and preparation of samples for testing iso 5725-1, accuracy (trueness 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 of products in liquid, paste and solid form 3 terms and definitions for the purposes of this document, the following terms and definitions apply. 1) also known as size exclusion chromatography (sec). licensed copy: london south bank university, london south bank university, wed aug 08 04:06:00 gmt+00:00 2007, uncontrolled copy, (c) bsi iso/dis 13885-1 2 iso 2007 all rights reserved 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 according to the size of the molecule (or more precisely the polymer coil size which forms in this elution solvent). 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 earlier, small molecules later. under the test conditions given, the retention volume is solely a function of the size of the molecule note 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 concentration 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 distribution, the quantities mn and mw and the heterogeneity or polydispersity mw/mn are 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 figure 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, 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. the eluent reservoir shall have sufficient capacity for the apparatus to be brought to the equilibrium between elution solvent and the surface of separating 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 fitted 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