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1、BRITISH STANDARD BS ISO 16014-4:2003 Plastics Determination of average molecular mass and molecular mass distribution of polymers using size-exclusion chromatography Part 4: High-temperature method ICS 83.080.01 ? Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:12:36 GMT+00:00 2006, Uncont
2、rolled Copy, (c) BSI BS ISO 16014-4:2003 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 5 June 2003 BSI 5 June 2003 ISBN 0 580 41968 1 National foreword This British Standard reproduces verbatim ISO 16014-4:2003 and implements it as the UK n
3、ational standard. The UK participation in its preparation was entrusted to Technical Committee PRI/21, Plastics test methods, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards whi
4、ch implement international publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does no
5、t purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European co
6、mmittee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii
7、 to iv, pages 1 to 12, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:12:36 GMT+00:00 2006, Uncon
8、trolled Copy, (c) BSI Reference number ISO 16014-4:2003(E) INTERNATIONAL ADNATSDR ISO 141064- tide tsriFino -300251-40 Plastics Determination of average molecular mass and molecular mass distribution of polymers using size- exclusion chromatography Part 4: High-temperature method Plastiques Dtermina
9、tion de la masse molculaire moyenne et de la rpartition des masses molculaires des polymres par chromatographie dexclusion strique Partie 4: Mesurage aux tempratures leves R OSI -4106102:4)E(30 OSI 3002 INTERNATIONAL STANDARD ISO 16014-4 First edition 2003-04-15 scitsalP eteDtanimroifo n avegare cel
10、omussam ral elom dnassam raluc birtsiduitp fo noolyisu sremgn size- isulcxec nohortamargophy :4 traP hgiHet-arepmturtem ehod salPtiuqse D retmanitoied n al samse molcualrie yomnnete e ed al rraptition sed samses omlcualrise sed poylmres apr chrootamrghpaei xedclsuios ntrqi eu raPtie :4 Mesuraeg xua
11、etrpmtaruse lvese BS ISO 160144:2003 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:12:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 16014-4:2003(E) ii BS ISO 160144:2003 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:12:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 160
12、14-4:2003(E) iii Contents Page Forewordiv 1 Scope1 2 Normative references .1 3 Terms and definitions.1 4 Principle.1 5 Reagents1 6 Apparatus.2 7 Procedure.4 8 Data acquisition and processing.6 9 Expression of results6 10 Precision6 11 Test report8 Annex A (informative) Further information on applica
13、bility of method9 Annex B (informative) Further information on reagents 10 Bibliography .12 BS ISO 160144:2003 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:12:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 16014-4:2003(E) iv Foreword ISO (the International Organization for Standardiz
14、ation) 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
15、 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 Standar
16、ds 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 Intern
17、ational Standard requires approval by at least 75 % of the member bodies casting 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 16014-4
18、was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical- chemical properties. ISO 16014 consists of the following parts, under the general title Plastics Determination of average molecular mass and molecular mass distribution of polymers using size-exclusion chromatograp
19、hy: Part 1: General principles Part 2: Universal calibration method Part 3: Low-temperature method Part 4: High-temperature method BS ISO 160144:2003 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:12:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTENRATIONAL TSANDADR IS-41061 O4:(3002E)
20、1 Plastics Determination of average molecular mass and molecular mass distribution of polymers using size-exclusion chromatography Part 4: High-temperature method 1 Scope This part of ISO 16014 specifies a method for determining the average molecular mass and the molecular mass distribution of polym
21、ers by size-exclusion chromatography (SEC) using an organic eluent at temperatures between 60 C and 180 C. The average molecular mass and the molecular mass distribution are calculated from a calibration curve constructed using polymer standards. Therefore, this test method is classified as a relati
22、ve method (see ISO 16014-1:2003, Annex A). 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 amen
23、dments) applies. ISO 16014-1, Plastics Determination of average molecular mass and molecular mass distribution of polymers using size-exclusion chromatography Part 1: General principles ISO 16014-2, Plastics Determination of average molecular mass and molecular mass distribution of polymers using si
24、ze-exclusion chromatography Part 2: Universal calibration method 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 16014-1 apply. 4 Principle See ISO 16014-1:2003, Clause 4. 5 Reagents 5.1 Eluent For a general discussion of eluents, see ISO 16014-1:200
25、3, Subclause 5.1. For examples of eluents used for SEC measurements at temperatures above 60 C, see Annex B. BS ISO 160144:2003 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:12:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 16014-4:2003(E) 2 5.2 Reagent for column evaluation See ISO 1
26、6014-1:2003, Subclause 5.2. There are several low molecular mass compounds that can be used, for example diphenylmethane when 1,2-dichlorobenzene is used as eluent or ethylbenzene when 1,2,4-trichlorobenzene is used as eluent. 5.3 Molecular mass standards See ISO 16014-1:2003, Subclause 5.3. Some ex
27、amples of commercially available molecular mass standards are given in Annex B. 5.4 Reagent for flow rate marker (internal standard) See ISO 16014-1:2003, Subclause 5.4. It is often very difficult to find a low molecular mass compound suitable for use as a flow rate marker because it should not co-e
28、lute with the polymer peak, the system peak or the solvent peak. An example of a compound suitable for use as a flow rate marker is 2,6-di-tert-butyl-4-methylphenol when 1,2-dichlorobenzene or 1,2,4-trichlorobenzene is used as eluent. 5.5 Additives Phenol-type antioxidants such as 2,6-di-tert-butyl-
29、4-methylphenol should preferably be added to avoid degradation of the polymer sample. For further examples of antioxidants, see Annex B. 6 Apparatus 6.1 General A schematic diagram of an SEC system is shown in ISO 16014-1:2003, Figure 1. Either commercially available or assembled SEC systems can be
30、used, provided they meet the component requirements specified and have the capability to maintain a constant column temperature between 60 C and 180 C. However, the temperature of components connected upstream of the injector, such as the eluent reservoir, the pumping system and the tubing, are not
31、kept at the same temperature as the columns. The use of a commercially available SEC system is recommended because of the difficulty involved in assembling a system operating at such high temperatures. 6.2 Eluent reservoir See ISO 16014-1:2003, Subclause 6.2. As mentioned in 6.1 above, it is not nec
32、essary to keep the eluent reservoir at the same temperature as the columns. BS ISO 160144:2003 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:12:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 16014-4:2003(E) 3 6.3 Pumping system See ISO 16014-1:2003, Subclause 6.3. In order to maintain
33、 the flow rate accurate to within 0,3 %, the pumping system shall be kept at a constant temperature. It is, however, not necessary to keep the pumping system at the same temperature as the columns. 6.4 Injector See ISO 16014-1:2003, Subclause 6.4. In order to ensure that the polymer solution remains
34、 clear, without any precipitation, the injector temperature- control equipment shall be capable of keeping the injector at the same temperature, to within 1 C, as the columns. As manual injection is impossible at such temperatures, an automatic injection system shall be used. 6.5 Columns See ISO 160
35、14-1:2003, Subclause 6.5. Organic or inorganic packing materials can be used, and there are no limitations on particle size or shape except that, when analysing high molecular mass and/or shear-sensitive polymers, the particle size shall be large enough for no rupture of the polymer chain to occur d
36、uring elution of the polymers. The set of columns used shall have a theoretical plate number greater than 12 000/m and the resolution factor R shall be greater than 1,5 close to the polymer peak. The asymmetry factor shall be within the range 1,00 0,15. The set of columns used shall cover the whole
37、range of molecular masses being determined and the calibration curve shall be as linear as possible (the correlation factor shall be very close to 1). Determination of the theoretical plate number, the resolution factor and the asymmetry factor of the columns shall be carried out as described in ISO
38、 16014-1:2003, Subclause 6.5. The column temperature-control equipment shall be capable of keeping the columns within 0,5 C of the temperature set to ensure adequate reproducibility of the results. 6.6 Detector See ISO 16014-1:2003, Subclause 6.6. The detector temperature-control equipment shall be
39、capable of keeping the detector within 0,5 C of the temperature set, in order to meet the requirements for flow rate and baseline stability (sensitivity). It is recommended that the columns and detector be kept at the same temperature. 6.7 Tubing See ISO 16014-1:2003, Subclause 6.7. The temperature
40、of the tubing shall be kept constant and high enough to ensure that the column performance requirements are met, but it is not necessary to keep the tubing at the same temperature as the column. 6.8 Temperature-control unit One of the important factors in SEC is that all components need to be kept a
41、t a constant temperature and, with the method described in this part of ISO 16014, some of them need to be kept at a high temperature. Therefore, an accurate temperature-control system is essential to meet the performance requirements for SEC. BS ISO 160144:2003 Licensed Copy: sheffieldun sheffieldu
42、n, na, Mon Nov 27 08:12:36 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 16014-4:2003(E) 4 6.9 Recorder and plotter See ISO 16014-1:2003, Subclause 6.9. 6.10 Data-processing system See ISO 16014-1:2003, Subclause 6.10. 6.11 Other components In addition to the components described above, a column gu
43、ard filter, a pressure monitor, a pulse damper or other related components can be used, if necessary. 7 Procedure 7.1 Preparation of solutions of molecular mass standards The molecular mass standards used to construct the calibration curve shall be selected so as to cover the range of molecular mass
44、es of the polymer being analysed and so that there are at least two standards in each molecular mass decade. Solutions may be prepared which contain more than one narrow molecular mass distribution standard, but only when the standards are perfectly separated from each other on the chromatogram. Sol
45、utions of standards of molecular mass greater than 1 000 000 shall be prepared separately. If molecular mass standards having the same chemical structure as the polymer being analysed are not available, the calibration curve may be constructed using standards consisting of a different type of polyme
46、r and a universal calibration curve constructed for this different type of polymer (see ISO 16014-2). If gentle shaking and/or stirring or heating is required to accelerate dissolution, the time shall be as short as possible to avoid any rupture of the polymer chains. Filtration of the solutions is
47、recommended to protect the column from clogging. In such cases, membrane filters or sintered-metal filters with a pore size between 0,2 m and 1 m shall be used. If solid material is observed on the filter, indicating incomplete dissolution, repeat the dissolution process. If a membrane filter is use
48、d, the membrane and backing shall be inert to the solvent being used. In general, use solutions within 48 h of preparation. However, longer storage times are allowed if the solution is kept in a cool, dark place to prevent polymer degradation and solvent evaporation. Recommended concentrations for s
49、olutions of molecular mass standards are as follows: Mp 5 104 0,4 mg/cm3 5 104 u Mp 106 0,2 mg/cm3 106 u Mp 0,1 mg/cm3 If a viscometric detector is used, higher molecular mass standard concentrations are required in the lower molecular mass region. Sample elution times shall be measured at lower concentrations, however. 7.2 Preparation of sample solutions Prepare sample solutions by weighing accurately 10 mg to 250 mg of samp