ISO/TS 11251:2019

TECHNICAL ISO/TS
SPECIFICATION 11251
Second edition
2019-09
Nanotechnologies — Characterization
of volatile components in single-
wall carbon nanotube samples
using evolved gas analysis/gas
chromatograph-mass spectrometry
Nanotechnologies — Caractérisation des composés volatils dans les
nanotubes de carbone à simple paroi (SWCNT) utilisant l'analyse
des gaz émis par chromatographie en phase gazeuse couplée à la
spectrométrie de masse
Reference number
ISO/TS 11251:2019(E)
©
ISO 2019

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ISO/TS 11251:2019(E)

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ii © ISO 2019 – All rights reserved

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ISO/TS 11251:2019(E)

Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Apparatus . 2
6 Sample preparation . 4
7 Measurement procedures for EGA/MS and EGA/GCMS. 4
7.1 General . 4
7.2 Measurement procedure of EGA/MS . 4
7.3 Measurement procedure of EGA/GCMS . 4
8 Data analysis and interpretations of results . 5
8.1 Qualitative analysis . 5
8.2 Mass loss analysis . 5
9 Accuracy and uncertainties . 5
10 Test report . 5
Annex A (informative) Case study. 7
Bibliography .12
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ISO/TS 11251:2019(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
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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. 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 elements of this document may be the subject of
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on the ISO list of patent declarations received (see www .iso .org/patents).
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.org/iso/foreword .html.
This document was prepared by Technical Committee ISO/TC 229, Nanotechnologies.
This second edition cancels and replaces the first edition (ISO/TS 11251:2010), which has been
technically revised.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/members .html.
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TECHNICAL SPECIFICATION ISO/TS 11251:2019(E)
Nanotechnologies — Characterization of volatile
components in single-wall carbon nanotube samples
using evolved gas analysis/gas chromatograph-mass
spectrometry
1 Scope
This document specifies a method for the characterization of evolved gas components in single-wall
carbon nanotube (SWCNT) samples using evolved gas analysis/gas chromatograph mass spectrometry
(EGA/GCMS).
NOTE Some difference could appear between qualitative and quantitative results of emitted gas and gas
content in the sample due to the heating and the possible presence of catalysts.
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/TS 80004-3, Nanotechnologies — Vocaburlary — Part 3: Carbon nano-objects
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO/TS 80004-3 and the
following apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https: //www .iso .org/obp
— IEC Electropedia: available at http: //www .electropedia .org/
3.1
single-wall carbon nanotube
SWCNT
carbon nanotube consisting of cylindrical graphene layer
3.2
evolved gas analysis
EGA
technique in which the nature and/or amount of evolved gas product(s) released by a sample subjected
to a controlled temperature program is(are) determined
Note 1 to entry: The method of analysis should always be clearly stated (Reference [1] in the Bibliography).
3.3
EGA/MS
evolved gas analysis/mass spectrometry
technique using mass spectrometry to analyse gaseous components evolved from a sample as a function
of temperature
Note 1 to entry: Although the gases evolved at any particular temperature are detected simultaneously, it might
not be possible to uniquely identify the different components using MS alone.
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ISO/TS 11251:2019(E)

3.4
EGA/GCMS
evolved gas analysis/gas chromatography coupled to mass spectrometry
technique combining a gas chromatograph and a mass spectrometer to identify the chemical
composition of gases evolved from a sample as a function of temperature
Note 1 to entry: The evolved gases are passed through a gas chromatograph (GC) to separate each component so
that it can be identified in the MS unit.
3.5
volatile compounds
compounds that are evolved from a sample at the temperature under consideration
4 Principle
EGA/MS and EGA/GCMS are used to characterize evolved gas impurities in samples of SWCNT. Evolved
gas 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 that used for programmed
temperature pyrolysis or thermogravimetric analysis. EGA/MS is used to determine the temperature
range over which the release of evolved gas components occurs. EGA/GCMS analysis is used to
identify each component separately by the use of a GC capillary column. Quantitative information 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 mass of the evolved gas
components.
5 Apparatus
Figure 1 shows a schematic diagram of EGA/MS
...