SIST EN ISO 10927:2011

SLOVENSKI STANDARD
SIST EN ISO 10927:2011
01-november-2011
Polimerni materiali - Ugotavljanje molekularne mase in porazdelitev molekularne
mase z ionizacijo v nosilcu (matriksu) z lasersko desorpcijo (MALDITOF-MS) (ISO
10927:2011)
Plastics - 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) (ISO 10927:2011)
Kunststoffe - Bestimmung der Molmasse und Molmassenverteilung von polymeren
Species durch matrixunterstütze Laser-Desorptions/Ionisations-Flugzeit-
Massenspektrometrie (MALDI-TOF-MS) (ISO 10927:2011)
Plastiques - Détermination de la masse moléculaire et de la distribution des masses
moléculaires des polymères par spectrométrie de masse, à temps de vol, après
désorption/ionisation laser assistée par matrice (SM-MALDI-TOF) (ISO 10927:2011)
Ta slovenski standard je istoveten z: EN ISO 10927:2011
ICS:
83.080.01 Polimerni materiali na Plastics in general
splošno
SIST EN ISO 10927:2011 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 10927:2011

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SIST EN ISO 10927:2011


EUROPEAN STANDARD
EN ISO 10927

NORME EUROPÉENNE

EUROPÄISCHE NORM
April 2011
ICS 83.080.01
English Version
Plastics - 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) (ISO 10927:2011)
Plastiques - Détermination de la masse moléculaire et de la Kunststoffe - Bestimmung der Molmasse und
distribution des masses moléculaires des polymères par
Molmassenverteilung von polymeren Species durch
spectrométrie de masse, à temps de vol, après matrixunterstütze Laser-Desorptions/Ionisations-Flugzeit-
désorption/ionisation laser assistée par matrice (SM- Massenspektrometrie (MALDI-TOF-MS) (ISO 10927:2011)
MALDI-TOF) (ISO 10927:2011)
This European Standard was approved by CEN on 14 April 2011.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations 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.

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 members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.





EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2011 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 10927:2011: E
worldwide for CEN national Members.

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SIST EN ISO 10927:2011
EN ISO 10927:2011 (E)
Contents Page
Foreword .3

2

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SIST EN ISO 10927:2011
EN ISO 10927:2011 (E)
Foreword
This document (EN ISO 10927:2011) has been prepared by Technical Committee ISO/TC 61 "Plastics" in
collaboration with Technical Committee CEN/TC 139 “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 October 2011, and conflicting national standards shall be withdrawn at
the latest by October 2011.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
According to the CEN/CENELEC Internal Regulations, 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland and the United Kingdom.
Endorsement notice
The text of ISO 10927:2011 has been approved by CEN as a EN ISO 10927:2011 without any modification.

3

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SIST EN ISO 10927:2011

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SIST EN ISO 10927:2011

INTERNATIONAL ISO
STANDARD 10927
First edition
2011-04-15

Plastics — 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)
Plastiques — Détermination de la masse moléculaire et de la
distribution des masses moléculaires des polymères par spectrométrie
de masse, à temps de vol, après désorption/ionisation laser assistée
par matrice (SM-MALDI-TOF)





Reference number
ISO 10927:2011(E)
©
ISO 2011

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SIST EN ISO 10927:2011
ISO 10927:2011(E)


COPYRIGHT PROTECTED DOCUMENT


©  ISO 2011
All rights reserved. Unless otherwise specified, no 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
ISO's 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 copyright@iso.org
Web www.iso.org
Published in Switzerland

ii © ISO 2011 – All rights reserved

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SIST EN ISO 10927:2011
ISO 10927:2011(E)
Contents Page
Foreword .iv
Introduction.v
1 Scope.1
2 Normative references.1
3 Terms and definitions .1
4 Principle .2
5 Reagents .3
5.1 Matrices .3
5.2 Solvents.3
5.3 Salts .3
5.4 Molecular mass standards .3
6 Apparatus.3
6.1 General .3
6.2 Sample introduction chamber/target.3
6.3 Laser source .4
6.4 Flight tube .4
6.5 Detector .5
6.6 Data recording .5
6.7 Data handling.5
7 Procedure.5
7.1 General .5
7.2 Sample preparation.5
7.3 Instrument settings .6
7.4 Recording spectra.7
8 Data acquisition and processing.8
8.1 General .8
8.2 Calibration.8
8.3 Generation of calibration curve .9
8.4 Signal intensity axis calibration.9
9 Expression of results.9
9.1 Calculation of molecular mass distribution.9
9.2 Calculation of the average molecular masses .9
10 Precision .9
11 Test report.10
Annex A (normative) Calibrants .11
Annex B (informative) Precision data .12
Bibliography.13

© ISO 2011 – All rights reserved iii

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SIST EN ISO 10927:2011
ISO 10927:2011(E)
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.
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 10927 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-
chemical properties.
iv © ISO 2011 – All rights reserved

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SIST EN ISO 10927:2011
ISO 10927:2011(E)
Introduction
The molecular mass and molecular mass distribution of a synthetic 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 control 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 MALDI-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 2011 – All rights reserved v

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SIST EN ISO 10927:2011

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SIST EN ISO 10927:2011
INTERNATIONAL STANDARD ISO 10927:2011(E)

Plastics — 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)
1 Scope
This International Standard specifies a general method for determining the average molecular mass and
−1 −1
molecular mass distribution of polymers (see Reference [1]) from 2 000 g⋅mol to 20 000 g⋅mol by 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 standards. 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 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 472, Plastics — Vocabulary
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 472 and the following apply.
3.1
matrix-assisted laser desorption/ionization time-of-flight-mass spectrometry
MALDI-TOF-MS
a mass-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 voltage
3.2
molecular mass
M
sum of the masses of the atoms making up a molecule
NOTE Molecular weight is also used for molecular mass.
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SIST EN ISO 10927:2011
ISO 10927:2011(E)
3.3
average molecular mass
Three possible types of average molecular mass are defined by the following equations, where
N is the number of molecules of species i of molecular mass M ;
i i
m is the mass of the ith species (i.e. m = N M );
i i i i
z = m M /Σm .
i i i i
3.3.1
number-average molecular mass
M
n
∞
()NM×
∑ ii
i=1
M = (1)
n
∞
N
i
∑
i=1
3.3.2
mass-average molecular mass
M
w
∞∞
2
()NM××m M
∑∑ii ii
ii==11
M== (2)
w
∞∞
()NM× m
ii i
∑∑
ii==11
3.3.3
z-average molecular mass
M
z
∞∞ ∞
32
()NM××m M z×M
∑∑ii ()i i∑ii
ii==11 i=1
M== = (3)
z
∞∞ ∞
2
()NM××m M z
∑∑ii i i∑i
ii==11 i=1
4 Principle
The MALDI process involves the desorption and the ionization of an analyte dispersed in an organic small-
molecule matrix. The matrix must 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 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 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 calibration of the arrival times with known mass standards, the mass
distribution of the polymer is determined.
2 © ISO 2011 – All rights reserved

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SIST EN ISO 10927:2011
ISO 10927:2011(E)
5 Reagents
5.1 Matrices
2,5-dihydroxybenzoic acid (gentisic acid, DHB) and 1,8,9-trihydroxyanthracene (dithranol) are the
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 Solvents
The recommended solvent is tetrahydrofuran (THF). THF with an antioxidant, such 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 antioxidant is used, it shall be stored in an amber container
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 Salts
Lithium, sodium, potassium and silver trifluoroacetate are recommended since they are soluble in THF and
toluene. AgNO with ethanol as solvent may be used with the polymer and matrix in THF.
3
The salts shall be soluble in the solvent chosen for the polymer and the matrix. When silver nitrate is used,
relevant safety aspects should be borne in mind.
5.4 Molecular mass standards
The 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 sh
...