1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationDD ISO/TS 11251:2010Nanotechnologies Characterization of volatilecomponents in single-wallcarbon nanotube samplesusing evolved gas analysis/gas chromatograph-massspectrometryDD I
2、SO/TS 11251:2010 DRAFT FOR DEVELOPMENTNational forewordThis Draft for Development is the UK implementation of ISO/TS11251:2010.This publication is not to be regarded as a British Standard.It is being issued in the Draft for Development series of publicationsand is of a provisional nature. It should
3、be applied on thisprovisional basis, so that information and experience of its practicalapplication can be obtained.Comments arising from the use of this Draft for Developmentare requested so that UK experience can be reported to theinternational organization responsible for its conversion toan inte
4、rnational standard. A review of this publication willbe initiated not later than 3 years after its publication by theinternational organization so that a decision can be taken on itsstatus. Notification of the start of the review period will be made inan announcement in the appropriate issue of Upda
5、te Standards.According to the replies received by the end of the review period,the responsible BSI Committee will decide whether to support theconversion into an international Standard, to extend the life of theTechnical Specification or to withdraw it. Comments should be sentto the Secretary of the
6、 responsible BSI Technical Committee at BritishStandards House, 389 Chiswick High Road, London W4 4AL.The UK participation in its preparation was entrusted to TechnicalCommittee NTI/1, Nanotechnologies.A list of organizations represented on this committee can beobtained on request to its secretary.T
7、his publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2010ISBN 978 0 580 61386 9ICS 07.030Compliance with a British Standard cannot confer immunity fromlegal obligations.This Draft for Development was published un
8、der the authority ofthe Standards Policy and Strategy Committee on 31 December 2010.Amendments issued since publicationDate Text affectedDD ISO/TS 11251:2010Reference numberISO/TS 11251:2010(E)ISO 2010TECHNICAL SPECIFICATION ISO/TS11251First edition2010-12-01Nanotechnologies Characterization of vola
9、tile components in single-wall carbon nanotube samples using evolved gas analysis/gas chromatograph-mass spectrometry Nanotechnologies Caractrisation des composants volatiles dans les nanotubes de carbone paroi simple (SWCNT) utilisant lanalyse des gaz mis par chromatographie en phase gazeuse/spectr
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13、he Central Secretariat at the address given below. COPYRIGHT PROTECTED DOCUMENT ISO 2010 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 per
14、mission in writing from 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 copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2010 All rights res
15、ervedDD ISO/TS 11251:2010ISO/TS 11251:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normative references1 3 Terms and definitions .1 4 Principle .2 5 Apparatus.2 6 Sample preparation.3 7 Measurement procedures for EGA/MS and EGA/GCMS .3 7.1 General .3 7.2 Measurement p
16、rocedure of EGA/MS.3 7.3 Measurement procedure of EGA/GCMS4 8 Data analysis and interpretations of results 4 8.1 Qualitative analysis.4 8.2 Mass loss analysis 4 9 Precision and uncertainties .5 10 Test report5 Annex A (informative) Case study.6 Bibliography10 DD ISO/TS 11251:2010ISO/TS 11251:2010(E)
17、 iv ISO 2010 All rights reservedForeword 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 inter
18、ested 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
19、 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 te
20、chnical 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. In other circumstances, particularly when there is an urgent market requirement for such documents, a technical committe
21、e may decide to publish other types of document: an ISO Publicly Available Specification (ISO/PAS) represents an agreement between technical experts in an ISO working group and is accepted for publication if it is approved by more than 50 % of the members of the parent committee casting a vote; an I
22、SO Technical Specification (ISO/TS) represents an agreement between the members of a technical committee and is accepted for publication if it is approved by 2/3 of the members of the committee casting a vote. An ISO/PAS or ISO/TS is reviewed after three years in order to decide whether it will be c
23、onfirmed for a further three years, revised to become an International Standard, or withdrawn. If the ISO/PAS or ISO/TS is confirmed, it is reviewed again after a further three years, at which time it must either be transformed into an International Standard or be withdrawn. Attention is drawn to th
24、e 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/TS 11251 was prepared by Technical Committee ISO/TC 229, Nanotechnologies. DD ISO/TS 11251:2010TECHNICAL SPECIFICATION IS
25、O/TS 11251:2010(E) ISO 2010 All rights reserved 1Nanotechnologies Characterization of volatile components in single-wall carbon nanotube samples using evolved gas analysis/gas chromatograph-mass spectrometry 1 Scope This Technical Specification specifies a method for the characterization of volatile
26、 components in single-wall carbon nanotubes (SWCNTs) samples using evolved gas analysis/gas chromatograph mass spectrometry (EGA/GCMS). 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited appli
27、es. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO/TS 27687, Nanotechnologies Terminology and definitions for nano-objects Nanoparticle, nanofibre and nanoplate 3 Terms and definitions For the purposes of this document, the terms and def
28、initions given in ISO/TS 27687 and the following apply. 3.1 evolved gas analysis EGA technique in which the nature and/or amount of volatile product(s) released by a substance subjected to a controlled temperature program is(are) determined NOTE The method of analysis should always be clearly stated
29、 (Reference 1 in the Bibliography). 3.2 evolved gas analysis/mass spectrometry EGA/MS technique using mass spectrometry to analyse gaseous components evolved from a sample as a function of temperature NOTE Although the gases evolved at any particular temperature are detected simultaneously, it might
30、 not be possible to uniquely identify the different components using MS alone. 3.3 evolved gas analysis/gas chromatograph mass spectrometry EGA/GCMS technique combining a gas chromatograph and a mass spectrometer to identify the chemical composition of gases evolved from a sample as a function of te
31、mperature NOTE The evolved gases are passed through a gas chromatograph (GC) to separate each component so that it can be identified in the MS unit. DD ISO/TS 11251:2010ISO/TS 11251:2010(E) 2 ISO 2010 All rights reserved3.4 volatile compounds compounds that are evolved from a sample at the temperatu
32、re under consideration 4 Principle EGA/MS and EGA/GCMS are used to characterize volatile impurities in samples of SWCNT. Volatile compounds are identified by measuring the mass spectra of the gaseous component evolved from the heated samples in a furnace or other suitable heating device, such as tha
33、t used for programmed temperature pyrolysis or thermogravimetric analysis. EGA/MS is used to determine the temperature range over which the release of volatile components occurs. EGA/GCMS analysis is used to identify each component separately by the use of a capillary column. Quantitative informatio
34、n can additionally be obtained by the sample mass loss in thermogravimetric analysis (TGA) and the peak area in EGA/MS. NOTE Some details of the technique are described in References 2 to 6 in the Bibliography. EGA/GCMS plays a complementary role to TGA, which is mainly devoted to quantifying the ma
35、ss of the volatile components. 5 Apparatus Figure 1 shows a schematic diagram of EGA/MS which is composed of a furnace, a heating unit without a separation column and a MS unit. In the EGA/MS, evolved gas from the furnace is led to the MS unit directly through a capillary tube without a separation p
36、rocess. Figure 2 shows a schematic diagram of an EGA/GCMS which is composed of a furnace, a GC with a separation column and an MS unit. In the EGA/GCMS, all compounds evolved from the sample within the furnace are captured by the cooling trap and are then introduced to the GC unit by heating the tra
37、p. The compounds are separated by the column in the GC unit. Key 1 furnace 2 heating unit 3 MS unit Figure 1 Schematic diagram of EGA/MS DD ISO/TS 11251:2010ISO/TS 11251:2010(E) ISO 2010 All rights reserved 3Key 1 furnace 2 cooling trap 3 capillary column 4 GC unit 5 MS unit Figure 2 Schematic diagr
38、am of EGA/GCMS 6 Sample preparation Sample preparation, such as dissolution or dispersion, is not required. For a qualitative analysis, the sample shall be introduced into the EGA/MS or EGA/GCMS as it is. In order to avoid the vaporization of any volatiles that might be present, samples shall not be
39、 dried before analysis. 7 Measurement procedures for EGA/MS and EGA/GCMS 7.1 General Load the SWCNT sample into the furnace and heat it up to identify the temperature range of gasification using EGA/MS measurement, and use the EGA/GCMS to identify each component at the designated temperature range.
40、7.2 Measurement procedure of EGA/MS Weigh between 0,5 mg and 2 mg of the SWCNT sample, to the nearest 0,01 mg, using a calibrated mass balance. Load the weighed sample into the furnace, including the sample cup used when weighing. Heat the sample at a constant rate until gas evolution stops. Measure
41、 the total ions from volatile components. Determine the start temperature and the end-point of gasification using the EGA curve. Compare the observed MS spectrum with the MS spectral database and determine each component in the evolved gas species. For appropriate comparison of MS spectra, an ioniza
42、tion voltage shall be in accordance with the voltage of the spectral database. DD ISO/TS 11251:2010ISO/TS 11251:2010(E) 4 ISO 2010 All rights reservedPerform EGA/GCMS if the measured spectrum cannot be identified using the MS spectral database due to its mixed components (see 7.3). Weigh the sample
43、after EGA/MS measurement, to the nearest 0,01 mg. NOTE The rate of heating depends on the calorific capacity of the sample. Generally a range of 15 to 25 C/min is used for EGA/MS. 7.3 Measurement procedure of EGA/GCMS Weigh between 0,5 mg and 2 mg of SWCNT from the same sample as that used in 7.2, t
44、o the nearest 0,01 mg. Load the sample into the furnace. Heat up the sample at a constant rate to the lower temperature of either the end-point of the gasification or upper limit of the instrument. Compare the observed MS spectrum with the mass spectral database and determine each component of the e
45、volved gas species. An ionization voltage shall be in accordance with the voltage of the standard spectra. The MS detector shall be calibrated by using a calibration reference material. NOTE The rate of heating depends on the sample. Generally, a range of 45 to 65 C/min is used for EGA/GCMS to short
46、en the analytical time. 8 Data analysis and interpretations of results 8.1 Qualitative analysis The qualitative analysis shall be based upon the standard spectral information of compounds. Components from evolved gas shall be determined by comparing the measured MS spectra with a mass spectral datab
47、ase. a) Choose the component that needs to be identified. b) Subtract the background from the targeted MS spectrum. c) Search for similar spectra from within the spectral database. d) Select the probable components in the sample from the candidates identified using the standard spectra. NOTE 1 Many
48、kinds of software for searching and a mass spectral database are available, as an example, NIST/EPA/NIH Mass Spectral Library with Search Program. NOTE 2 Using this method, n-hexane, benzene and toluene were identified in the example shown in Annex A and Figure A.4. 8.2 Mass loss analysis The volati
49、le components in SWCNT samples are determined using the following formula: 0t0100WWPW= DD ISO/TS 11251:2010ISO/TS 11251:2010(E) ISO 2010 All rights reserved 5where P is the volatile impurity content, expressed as a percentage; W0is the sample mass, in milligrams, before heating; Wtis the sample mass, in milligrams, after heating. NOTE Normally, quantitative analysis by GC/MS needs calibration curves, which show the relationship of the signal intensity and the concentration of each component. It is impossible to prepa
