IEC TS 62607-6-19:2021

IEC TS 62607-6-19 ®
Edition 1.0 2021-10
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –
Part 6-19: Graphene-based material – Elemental composition: CS analyser,
ONH analyser
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IEC TS 62607-6-19 ®
Edition 1.0 2021-10
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –

Part 6-19: Graphene-based material – Elemental composition: CS analyser,

ONH analyser
INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
ICS 07.120 ISBN 978-2-8322-1033-0

– 2 – IEC TS 62607-6-19:2021 © IEC 2021
CONTENTS
FOREWORD . 4
INTRODUCTION . 6
1 Scope . 7
2 Normative references . 7
3 Terms and definitions . 7
3.1 General terms . 7
3.2 Key control characteristics measured according to this document . 9
3.3 Terms related to the measurement method . 10
4 General . 10
4.1 Measurement principle . 10
4.2 Sample preparation method . 11
4.3 Description of measurement equipment / apparatus . 11
4.4 Supporting materials . 11
4.5 Ambient conditions during measurement . 12
5 Measurement procedure . 12
5.1 Calibration of measurement equipment . 12
5.2 Detailed protocol of the measurement procedure . 12
5.3 Measurement accuracy . 13
6 Data analysis / interpretation of results . 13
7 Results to be reported . 13
7.1 General . 13
7.2 Product / sample identification . 13
7.3 Test conditions . 13
7.4 Measurement specific information . 13
7.5 Test results . 13
Annex A (informative) Test report . 14
A.1 Recommended format of the test report . 14
Annex B (informative) Case study: Comparative results between CS/ONH analyser
and EA . 16
B.1 Measurement sample . 16
B.2 Measurement equipment . 16
B.3 Measurement results . 16
B.3.1 General . 16
B.3.2 Measuring samples with low C content (mass fraction (%)): . 16
B.3.3 Measuring samples with high C content (mass fraction (%)): . 17
B.3.4 Measuring samples with low S content (mass fraction (%)): . 17
B.3.5 Measuring samples with high S content (mass fraction (%)): . 18
B.3.6 Measuring samples with low O content (mass fraction (%)): . 18
B.3.7 Measuring samples with high O content (mass fraction (%)): . 19
B.3.8 Measuring samples with low N content (mass fraction (%)): . 20
B.3.9 Measuring samples with high N content (mass fraction (%)): . 20
Bibliography . 23

Figure B.1 – Measurement results of samples with low C content . 16
Figure B.2 – Measurement results of samples with high C content . 17

Figure B.3 – Measurement results of samples with low S content. 18
Figure B.4 – Measurement results of samples with high S content . 18
Figure B.5 – Measurement results of samples with low O content . 19
Figure B.6 – Measurement results of samples with high O content . 20
Figure B.7 – Measurement results of samples with low N content . 20
Figure B.8 – Measurement results of samples with high N content . 21
Figure B.9 – A summary of SD of all measurements . 22

Table A.1 – Product identification . 14
Table A.2 – General material description . 14
Table A.3 – Information relating to test . 15
Table A.4 – Measurement results . 15
Table B.1 – Measurement results of samples with low C content. 16
Table B.2 – Measurement results of samples with high C content . 17
Table B.3 – Measurement results of samples with low S content . 17
Table B.4 – Measurement results of samples with high S content . 18
Table B.5 – Measurement results of samples with low O content . 19
Table B.6 – Measurement results of samples with high O content . 19
Table B.7 – Measurement results of samples with low N content. 20
Table B.8 – Measurement results of samples with high N content . 21

– 4 – IEC TS 62607-6-19:2021 © IEC 2021
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
NANOMANUFACTURING – KEY CONTROL CHARACTERISTICS –

Part 6-19: Graphene-based material –
Elemental composition: CS analyser, ONH analyser

FOREWORD
1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising
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rights. IEC shall not be held responsible for identifying any or all such patent rights.
IEC 62607-6-19 has been prepared by IEC technical committee 113: Nanotechnology for
electrotechnical products and systems. It is a Technical Specification.
The text of this Technical Specification is based on the following documents:
Draft Report on voting
113/557/DTS 113/599/RVDTS
Full information on the voting for its approval can be found in the report on voting indicated in
the above table.
The language used for the development of this Technical Specification is English.
This document was drafted in accordance with ISO/IEC Directives, Part 2, and developed in
accordance with ISO/IEC Directives, Part 1 and ISO/IEC Directives, IEC Supplement, available
at www.iec.ch/members_experts/refdocs. The main document types developed by IEC are
described in greater detail at www.iec.ch/standardsdev/publications.

A list of all parts of the IEC TS 62607 series, published under the general title
Nanomanufacturing – Key control characteristics, can be found on the IEC website.
The committee has decided that the contents of this document will remain unchanged until the
stability date indicated on the IEC website under "http://webstore.iec.ch" in the data related to
the specific document. At this date, the document will be
• reconfirmed,
• withdrawn,
• replaced by a revised edition, or
• amended.
IMPORTANT – The "colour inside" logo on the cover page of this document indicates that it
contains colours which are considered to be useful for the correct understanding of its
contents. Users should therefore print this document using a colour printer.

– 6 – IEC TS 62607-6-19:2021 © IEC 2021
INTRODUCTION
In recent decades, graphene has attracted extensive attention from academy and industry,
because of its extraordinary physical and chemical properties for promising applications in
energy storage, electronics, composites, etc. For most graphene powder available either in the
laboratory or on the market, apart from carbon, the presence of other elements (e.g. sulfur,
oxygen, nitrogen, hydrogen) is inevitable in the course of graphene fabrication. Heteroatoms in
graphene can change the material's energy band at different levels, thus affecting its electrical
properties and thermal conductivity [1],[2] . Therefore, the heteroatom content is a key control
characteristic which helps to ascertain the structure and purity of graphene powder, and its
determination is significant for the production and application of graphene.
A method used to determine the elemental composition in graphene is the combustion/pyrolysis
method, which infers the elemental composition in a sample by analysing the content of the
combustion or pyrolysis gases. This method has high analysis efficiency and convenience of
operation, but different instruments will provide different levels of measurement uncertainty.
In general, the combustion/pyrolysis method is established on an organic elemental analyser
(EA), which uses a thermal conductivity detector (TCD) to analyse the components of the
combustion or pyrolysis gases. But for graphene powder, EA is not an excellent tool to access
the heteroatom content. One reason for this is that graphene has low density and sputtering
happens during combustion. Another reason is that the pyrolysis temperature in EA is set at a
relatively low value (e.g. 1 150 °C), which is sufficient for organics but not high enough to
completely release oxygen or other atoms in graphene.
The use of a carbon/sulfur analyser (CS analyser) and an oxygen/nitrogen/hydrogen analyser
(ONH analyser) can circumvent the above-mentioned problems and provide an efficient and
well repeatable method for determining heteroatom content in graphene [3]. The CS analyser
quantitatively analyses the combustion gas components using the infrared gas detector (IGD),
while the ONH analyser quantitatively analyses the pyrolysis gas components using the TCD
and IGD. The instrument has a higher pyrolysis temperature and the measurement of target
gases is also completely different.
This document focuses on the determination of chemical composition in graphene powder and
standardization of the procedures.

___________
Numbers in square brackets refer to the Bibliography.

NANOMANUFACTURING – KEY CONTROL CHARACTERISTICS –

Part 6-19: Graphene-based material –
Elemental composition: CS analyser, ONH analyser

1 Scope
This part of IEC TS 62607 establishes a standardized method to determine the chemical key
control characteristic
• elemental composition
for powder consisting of graphene-based material by
• CS analyser and ONH analyser.
The method as described in this document determines the content of carbon (C), sulfur (S),
oxygen (O), nitrogen (N) and hydrogen (H).
The carbon (C) and sulfur (S) content in graphene powder is derived by the content of converted
CO, CO and SO , which is determined by infrared gas detector (IGD) using a non-dispersive
2 2
infrared adsorption method in CS analyser.
The content of oxygen (O), nitrogen (N) and hydrogen (H) in graphene powder is derived by
ONH analyser using pyrolysis method. The O content is obtained according to the content of
, which is determined by IGD using a non-dispersive infrared adsorption
converted CO and CO
method. The N content is obtained according to the content of converted N , which is
determined by a thermal conductivity detector (TCD) method. The H content is obtained by
measuring converted H or H O, corresponding to TCD or IGD method.
2 2
• The method is applicable for graphene, graphene oxide (GO) and reduced graphene oxide
(rGO) in powder form.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions 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 http://www.iso.org/obp
3.1 General terms
3.1.1
two-dimensional material
2D material
material, consisting of one or several layers with the atoms in each layer strongly bonded to
neighbouring atoms in the same layer, which has one dimension, its thickness, in the nanoscale
or smaller and the other two dimensions generally at larger scales
Note 1 to entry: The number of layers when a two-dimensional material becomes a bulk material varies depending
on both the material being measured and its properties. In the case of graphene layers, it is a two-dimensional
material up to 10 layers thick for electrical measurements, beyond which the electrical properties of the material are
not distinct from those for the bulk [also known as graphite].
Note 2 to entry: Interlayer bonding is distinct from and weaker than intralayer bonding.

– 8 – IEC TS 62607-6-19:2021 © IEC 2021
Note 3 to entry: Each layer may contain more than one element.
Note 4 to entry: A two-dimensional material can be a nanoplate.
[SOURCE: ISO/TS 80004-13:2017, 3.1.1.1]
3.1.2
graphene
graphene layer
single-layer graphene
monolayer graphene
single layer of carbon atoms with each atom bound to three neighbours in a honeycomb
structure
Note 1 to entry: It is an important building block of many carbon nano-objects.
Note 2 to entry: As graphene is a single layer, it is also sometimes called monolayer graphene or single-layer
graphene and abbreviated as 1LG to distinguish it from bilayer graphene (2LG) and few-layer graphene (FLG).
Note 3 to entry: Graphene has edges and can have defects and grain boundaries where the bonding is disrupted.
[SOURCE: ISO/TS 80004-13:2017, 3.1.2.1]
3.1.3
graphene-based material
GBM
graphene material
grouping of carbon-based 2D materials that include one or more of graphene, bilayer graphene,
few-layer graphene, graphene nanoplate, and functionalized variations thereof as well as
graphene oxide and reduced graphene oxide.
Note 1 to entry: "Graphene material" is a short name for graphene-based material.
3.1.4
graphene oxide
GO
chemically modified graphene prepared by oxidation and exfoliation of graphite, causing
extensive oxidative modification of the basal plane
Note 1 to entry: Graphene oxide is a single-layer material with a high oxygen content, typically characterized by
C/O atomic ratios of approximately 2,0 depending on the method of synthesis.
[SOURCE: ISO/TS 80004-13:2017, 3.1.2.13]
3.1.5
reduced graphene oxide
rGO
reduced oxygen content form of graphene oxide
Note 1 to entry: This can be produced by chemical, thermal, microwave, photo-chemical, photo-thermal or
microbial/bacterial methods or by exfoliating reduced graphite oxide.
Note 2 to entry: If graphene oxide was fully reduced, then graphene would be the product. However, in practice,
3 2
some oxygen containing functional groups will remain and not all sp bonds will return back to sp configuration.
Different reducing agents will lead to different carbon to oxygen ratios and different chemical compositions in reduced
graphene oxide.
Note 3 to entry: It can take the form of several morphological variations such as platelets and worm-like structures.
[SOURCE: ISO/TS 80004-13:2017, 3.1.2.14]
3.1.6
blank detail specification
BDS
structured generic specification of the set of key control characteristics which are needed to
describe a specific nano-enabled product without assigning specific values and/or attributes
Note 1 to entry: The templates defined in a blank detail specification list the key control characteristics for the nano-
enabled material or product without assigning specific values to it.
Note 2 to entry: Examples of nano-enabled products are: nanomaterials, nanocomposites and nano-subassemblies.
Note 3 to entry: Blank detail specifications are intended to be used by industrial users to prepare their detail
specifications used in bilateral procurement contracts. A blank detail specification facilitates the comparison and

benchmarking of different materials. Furthermore, a standardized format makes procurement more efficient and more
error robust.
3.1.7
sectional blank detail specification
SBDS
specification based on a blank detail specification adapted for a subgroup of the nano-enabled
product
Note 1 to entry: In general the sectional blank detail specification contains a subset of those key control
characteristics (KCCs) listed in
...