ISO 2561:2006
(Main)Plastics — Determination of residual styrene monomer in polystyrene (PS) and impact-resistant polystyrene (PS-I) by gas chromatography
Plastics — Determination of residual styrene monomer in polystyrene (PS) and impact-resistant polystyrene (PS-I) by gas chromatography
ISO 2561:2006 specifies a method for the determination of the residual styrene monomer in polystyrene (PS) and impact-resistant polystyrene (PS-I) by gas chromatography. It may also be used for the simultaneous determination of other volatile aromatic hydrocarbons in PS and PS-I.
Plastiques — Détermination du styrène monomère résiduel dans le polystyrène (PS) et le polystyrène résistant au choc (PS-I) par chromatographie en phase gazeuse
General Information
Relations
Standards Content (Sample)
INTERNATIONAL ISO
STANDARD 2561
Second edition
2006-03-01
Plastics — Determination of residual
styrene monomer in polystyrene (PS)
and impact-resistant polystyrene (PS-I)
by gas chromatography
Plastiques — Détermination du styrène monomère résiduel dans le
polystyrène (PS) et le polystyrène résistant au choc (PS-I) par
chromatographie en phase gazeuse
Reference number
ISO 2561:2006(E)
©
ISO 2006
---------------------- Page: 1 ----------------------
ISO 2561:2006(E)
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's 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 Adobe's 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.
© ISO 2006
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 2006 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 2561:2006(E)
Contents Page
Foreword. iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions. 1
4 Principle. 1
5 Reagents and materials . 1
5.1 Internal standard. 1
5.2 Solvent . 1
5.3 Precipitator . 2
5.4 Aromatic hydrocarbons . 2
5.5 Carrier gases and fuel gases for gas chromatograph . 2
6 Apparatus . 2
6.1 General. 2
6.2 Gas chromatograph. 2
6.3 Data processor. 2
6.4 Sample injection syringe . 2
6.5 Analytical balance. 2
7 Preparation of sample . 2
8 Procedure . 3
8.1 General. 3
8.2 Preparation of internal-standard solution. 3
8.3 Preparation of sample solution for method A . 3
8.4 Preparation of sample solution for method B . 3
8.5 Preparation of calibration solutions . 3
8.6 Gas-chromatographic procedure. 4
9 Expression of results . 6
9.1 Calculation of results from a calibration graph.6
9.2 Acceptability of results and measurement sensitivity. 7
10 Test report . 7
Annex A (informative) Typical analytical conditions. 8
Annex B (informative) Correlation between mass of aromatic hydrocarbon in calibration solution
and concentration of aromatic hydrocarbon in sample solution for typical calibration
solutions used in method A and method B. 11
© ISO 2006 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 2561:2006(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 2561 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 9, Thermoplastic
materials.
This second edition cancels and replaces the first edition (ISO 2561:1974), which has been technically revised.
iv © ISO 2006 – All rights reserved
---------------------- Page: 4 ----------------------
INTERNATIONAL STANDARD ISO 2561:2006(E)
Plastics — Determination of residual styrene monomer in
polystyrene (PS) and impact-resistant polystyrene (PS-I) by gas
chromatography
1 Scope
This International Standard specifies a method for the determination of the residual styrene monomer in
polystyrene (PS) and impact-resistant polystyrene (PS-I) by gas chromatography. It may also be used for the
simultaneous determination of other volatile aromatic hydrocarbons in PS and PS-I.
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 apply.
4 Principle
The polymer sample is dissolved in solvent, which for polystyrene contains an internal standard. Either a small
volume of the polymer solution is injected directly into a gas chromatograph (method A) or a small volume of
the supernatant solution remaining after precipitation of polymer by addition of a precipitator is injected
(method B), in order to obtain separation of styrene and other volatile materials. Method A is simple and has
much the same accuracy as method B. However, there is a possibility that contamination of the injector with
polymer and oligomers will occur over time, leading to erroneous results.
5 Reagents and materials
5.1 Internal standard
The internal standard shall be selected based on consideration of the retention times of the materials
contained in the polymer sample and solvent. Recommended candidates are n-butylbenzene, cyclopentanol
and 1,2,4-trimethylbenzene, of sufficient purity for analytical use.
5.2 Solvent
Use analytical-grade dimethylformamide, butanone or dichloromethane.
© ISO 2006 – All rights reserved 1
---------------------- Page: 5 ----------------------
ISO 2561:2006(E)
5.3 Precipitator
Use analytical-grade 2,2,4-trimethylpentane or ethanol.
5.4 Aromatic hydrocarbons
Use analytical-grade styrene and (if required) other aromatic hydrocarbons such as ethylbenzene, cumene or
α-methylstyrene. Styrene shall give a clear mixture when mixed with an equal volume of ethanol.
5.5 Carrier gases and fuel gases for gas chromatograph
Use helium or nitrogen as carrier gas. Use hydrogen and air as fuel gases.
6 Apparatus
6.1 General
Normal laboratory equipment and the following apparatus are required. Typical operating conditions are
described in Annex A.
6.2 Gas chromatograph
6.2.1 Injection port: Use an injection port for liquid samples. When using an open tubular column
(hereafter called an OT column), an injection port with splitter may be applicable.
6.2.2 Column: The column diameter and length, as well as the packing material and liquid phase, shall be
selected based on consideration of column resolution and calibration curve linearity. Both packed columns
and OT columns are acceptable.
6.2.3 Detector: Use a hydrogen flame ionization detector (FID).
6.3 Data processor
Use a recorder or microcomputer to record the signals from the detector.
6.4 Sample injection syringe
Use a micro-syringe of the 1 µl to 50 µl type. A micro-syringe forming part of the auto-injector may also be
used.
6.5 Analytical balance
A balance capable of measuring to 0,1 mg is required.
7 Preparation of sample
The sample can be taken from material in the form of powder, pellets or moulded parts. In order to ensure the
desired accuracy of the sample mass, large pieces of sample shall be reduced to smaller fragments.
2 © ISO 2006 – All rights reserved
---------------------- Page: 6 ----------------------
ISO 2561:2006(E)
8 Procedure
8.1 General
During the dilution processes described below, the temperature of each solution shall remain under 25 °C.
8.2 Preparation of internal-standard solution
Weigh 200 mg of internal standard (5.1), to the nearest 1 mg, into a 1 000 ml volumetric flask. Then add
solvent (5.2) to make exactly 1 000 ml, stopper tightly and mix well.
8.3 Preparation of sample solution for method A
Weigh 0,5 g of sample, to the nearest 1 mg, into a 20 ml volumetric flask. Then add the internal standard
solution prepared in 8.2 to make exactly 20 ml, stopper tightly and mix until dissolved.
8.4 Preparation of sample solution for method B
Weigh 0,5 g of sample, to the nearest 1 mg, into a 100 ml volumetric flask. Using either a syringe or a pipette,
add 20 ml of the internal standard solution prepared in 8.2. Then stopper tightly and dissolve the sample
(shake well, if necessary). After completely dissolving the sample, add 10 ml of precipitator (5.3) with a pipette.
After vigorous shaking, allow the precipitate to settle. The supernatant solution is used for injection into the
gas chromatograph using a micro-syringe.
8.5 Preparation of calibration solutions
8.5.1 General
The range of conc
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.