1、BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06Plastics - Determination of the molecular mass and molecular mass distribution of polymer species by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS)BS EN ISO 10927:2018Nationa
2、l forewordThis British Standard is the UK implementation of EN ISO 10927:2018. It is identical to ISO 10927:2018. It supersedes BS EN ISO 10927:2011, which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee PRI/21, Testing of plastics.A list of organizations re
3、presented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2018 Published by BSI Standards Limited 2018ISBN 978 0
4、 580 96208 0ICS 83.080.01Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 July 2018.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STA
5、NDARDBS EN ISO 10927:2018EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 10927July 2018ICS 83.080.01 Supersedes EN ISO 10927:2011EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGCEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 20
6、18 CEN Ref. No. EN ISO 10927:2018: EAll rights of exploitation in any form and by any means reserved worldwide for CEN national MembersPlastics - Determination of the molecular mass and molecular mass distribution of polymer species by matrix-assisted laser desorption/ionization time-of-flight mass
7、spectrometry (MALDI-TOF-MS) (ISO 10927:2018)Plastiques - Dtermination de la masse molculaire et de la distribution des masses molculaires des polymres par spectromtrie de masse, temps de vol, aprs dsorption/ionisation laser assiste par matrice (SM-MALDI-TOF) (ISO 10927:2018)Kunststoffe - Bestimmung
8、der Molmasse und Molmassenverteilung von polymeren Species durch matrixuntersttze Laser-Desorptions/Ionisations-Flugzeit-Massenspektrometrie (MALDI-TOF-MS) (ISO 10927:2018)This European Standard was approved by CEN on 28 June 2018.CEN members are bound to comply with the CEN/CENELEC Internal Regulat
9、ions which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member.
10、This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions.CEN me
11、mbers are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Port
12、ugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.English VersionEN ISO 10927:2018 (E)European forewordThis document (EN ISO 10927:2018) has been prepared by Technical Committee ISO/TC 61 “Plastics“ in collaboration with Technical Committee CEN/TC 139 “
13、Paints and varnishes” the secretariat of which is held by DIN.This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by January 2019, and conflicting national standards shall be withdrawn at the latest by J
14、anuary 2019.Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights.This document supersedes EN ISO 10927:2011.According to the CEN-CENELEC Internal Regulatio
15、ns, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy,
16、 Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.Endorsement noticeThe text of ISO 10927:2018 has been approved by CEN as EN ISO 10927:2018 without any modification.iiBS EN ISO
17、 10927:2018ISO 10927:2018Foreword ivIntroduction v1 Scope .12 Normative references 13 Terms and definitions .14 Principle 25 Reagents 25.1 Matrices . 25.2 Solvents . 25.3 Salts 35.4 Molecular mass standards 36 Apparatus . 36.1 General . 36.2 Sample introduction chamber/target . 36.3 Laser source 46.
18、4 Flight tube . 46.5 Detector . 46.6 Data recording . 46.7 Data handling . 57 Procedure. 57.1 General . 57.2 Sample preparation 57.2.1 General 57.2.2 Preparation of polymer/matrix/salt solutions . 57.2.3 Deposition of the sample on the sample plate (target) 57.2.4 Preparation and spotting of biopoly
19、mer/matrix solutions 67.3 Instrument settings . 67.4 Recording spectra . 78 Data acquisition and processing 78.1 General . 78.2 Calibration 88.2.1 General 88.2.2 Calibration of mass axis using synthetic-polymer standards . 88.2.3 Calibration of mass axis using biopolymer standards . 88.2.4 Self-cali
20、bration method . 88.3 Generation of calibration curve 88.4 Signal intensity axis calibration . 89 Expression of results 99.1 Calculation of molecular mass distribution . 99.2 Calculation of the average molecular masses . 910 Precision .911 Test report .9Annex A (normative) Calibrants .11Annex B (inf
21、ormative) Precision data 12Bibliography .13 ISO 2018 All rights reserved iiiContents PageBS EN ISO 10927:2018ISO 10927:2018ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International
22、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, al
23、so 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 document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1.
24、 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 Directives, Part 2 (see www.iso.org/directives).Attention is drawn to the possibility that some of the eleme
25、nts 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 development of the document will be in the Introduction and/or on the ISO list of patent declarations received
26、 (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 voluntary nature of standards, the meaning of ISO specific terms and expressions related to conformity assessment, as we
27、ll as information about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www.iso.org/iso/foreword.html.This document was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-chemical properties
28、.This second edition cancels and replaces the first edition (ISO 10927:2011), which has been technically revised to update Figure 1 and 6.7 on data handling.iv ISO 2018 All rights reservedBS EN ISO 10927:2018ISO 10927:2018IntroductionThe molecular mass and molecular mass distribution of a synthetic
29、polymer are fundamental characteristics that result from the polymerization process. They may be used for a wide variety of correlations for fundamental studies and for processing and product applications. Determination of the molecular mass and molecular mass distribution is used for quality contro
30、l of polymers and for specification purposes in the commerce of polymers. The comparability of MALDI-TOF-MS results obtained in different laboratories can be ensured by using standardized conditions of measurement, identical samples and identical matrix preparation methods. The classification of MAL
31、DI-TOF-MS as an equitable (standardized) method compared with other established methods of polymer characterization could result in a significant increase in the use of MALDI-TOF-MS. ISO 2018 All rights reserved vBS EN ISO 10927:2018This page deliberately left blankPlastics - Determination of the mo
32、lecular mass and molecular mass distribution of polymer species by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS)1 ScopeThis document specifies a general method for determining the average molecular mass and molecular mass distribution of polymers (see Re
33、ference 1) from 2 000 g mol1to 20 000 g mol1by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS).The average molecular masses and molecular mass distributions are calculated from a calibration curve constructed using synthetic-polymer and/or biopolymer stand
34、ards. This method is therefore classified as a relative method.The method is not applicable to polyolefins or to polymers with a polydispersity 1,2.2 Normative referencesThe following documents are referred to in the text in such a way that some or all of their content constitutes requirements of th
35、is document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 472, Plastics Vocabulary3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 472
36、 and the following apply.ISO and IEC maintain terminological databases for use in standardization at the following addresses: IEC Electropedia: available at http:/www.electropedia.org/ ISO Online browsing platform: available at https:/www.iso.org/obp3.1matrix-assisted laser desorption/ionization tim
37、e-of-flight-mass spectrometryMALDI-TOF-MSmass-spectrometric technique in which the separation is based on different flight times in a field free flight tube depending on the mass of formed polymer ions after ionization by a laser, desorption and acceleration by high voltage3.2number-average molecula
38、r massMnMNMNiiiiin=11()where Niis the number of molecules of species i of molecular mass MiINTERNATIONAL STANDARD ISO 10927:2018 ISO 2018 All rights reserved 1BS EN ISO 10927:2018ISO 10927:20183.3mass-average molecular massMwMNMNMmMmiiiiiiiiiiiw=()()=12111whereNiis the number of molecules of species
39、 i of molecular mass Mi;miis the mass of the ithspecies (i.e. mi= NiMi)3.4z-average molecular massMzMNMNMmMmMiiiiiiiiiiiiiz=()()=()=13121211=zMziiii1whereNiis the number of molecules of species i of molecular mass Mi;miis the mass of the ithspecies (i.e. mi= NiMi);zi= miMi/mi4 PrincipleThe MALDI pro
40、cess involves the desorption and the ionization of an analyte dispersed in an organic small-molecule matrix. The matrix shall be able to absorb the laser energy. A metal salt may be added to cationize the analyte. A polymer is co-crystallized or co-mixed with the matrix molecule and deposited on the
41、 target. A short-duration UV laser pulse is used to desorb the matrix and the analyte. The laser energy is transferred to the matrix molecules, causing them to vaporize. Analyte and matrix molecules leave the target surface in a plume. Due to the very short desorption time, polymer molecules do not
42、degrade. The polymer in the desorption plume gains a cation and is accelerated by a high voltage, drifts down the field-free flight tube and is detected at the end of the flight tube. The time of flight of the species is a measure of its mass. From the distribution of arrival times and the calibrati
43、on of the arrival times with known mass standards, the mass distribution of the polymer is determined.5 Reagents5.1 Matrices2,5-dihydroxybenzoic acid (gentisic acid, DHB), trans-2-3-(4-tert-butylphenyl)-2-methyl-2-propenylidenemalononitrile (DCTB), and 1,8,9-trihydroxyanthracene (dithranol) are the
44、recommended matrices for this method. All of these materials shall be at least 97 % pure. They shall be stored in a freezer and warmed to room temperature immediately before use.5.2 SolventsThe recommended solvent is tetrahydrofuran (THF) with the purity more than 99 %. THF with an antioxidant, such
45、 as 2,6-di-tert-butyl-4-methylphenol (dibutylated hydroxytoluene, BHT) at a concentration of 0,025 % to 0,1 % (m/V), shall be stored in an amber container. If THF without an 2 ISO 2018 All rights reservedBS EN ISO 10927:2018ISO 10927:2018antioxidant is used, it shall be stored in an amber container
46、under an inert gas. Otherwise, it will react with oxygen to form peroxides which are hazardous on evaporative concentration.Depending on the solubility of the polymer being investigated, toluene, methanol and acetone may also be used.High-purity solvents are recommended.5.3 SaltsLithium, sodium, pot
47、assium, cesium and silver trifluoroacetate are recommended since they are soluble in THF and toluene. AgNO3with ethanol as solvent may be used with the polymer and matrix in THF.The salts shall be soluble in the solvent chosen for the polymer and the matrix. When silver nitrate is used, relevant saf
48、ety aspects should be borne in mind.5.4 Molecular mass standardsThe calibration of the mass spectrometer shall be carried out using biopolymers and/or synthetic polymers with known repeating units and end groups. The molecular masses of the standards shall lie within the range of the molecular mass
49、of the polymer being investigated. The software of the mass spectrometer shall be used for calibration. A list of recommended biopolymers and their molecular masses is given in Annex A.6 Apparatus6.1 GeneralA schematic diagram of a MALDI-TOF mass spectrometer is shown in Figure 1. The main components are a sample introduction chamber, a laser source, an ion source (target), a flight tube with an acceleration region and an ion detector (linear detector). The instruments may have additionally an i
