IEC TS 62607-6-22:2022

IEC TS 62607-6-22 ®
Edition 1.0 2022-11
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –
Part 6-22: Graphene-based material – Ash content: incineration
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IEC TS 62607-6-22 ®
Edition 1.0 2022-11
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –

Part 6-22: Graphene-based material – Ash content: incineration

INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
ICS 07.120 ISBN 978-2-8322-6003-6

– 2 – IEC TS 62607-6-22:2022  IEC 2022
CONTENTS
FOREWORD . 4
INTRODUCTION . 6
1 Scope . 7
2 Normative references . 7
3 Terms, definitions, symbols and abbreviated terms . 7
3.1 General terms . 7
3.2 Key control characteristics measured in accordance with this document . 8
4 General . 9
4.1 Measurement principle . 9
4.1.1 Incineration principle . 9
4.1.2 Operation principle of this method . 9
4.2 Sample preparation method . 10
4.3 Description of measurement equipment . 10
4.4 Supporting materials . 11
4.5 Ambient conditions during measurement . 11
5 Measurement procedure . 11
5.1 Pre-treatment of sample . 11
5.1.1 Powder . 11
5.1.2 Dispersion . 12
5.2 Preparation of the crucible . 12
5.3 Incineration of sample . 12
5.3.1 Graphene and rGO . 12
5.3.2 GO and graphite oxide . 12
5.4 Weighing. 13
5.5 Completion of ashing . 13
6 Data analysis . 13
6.1 Ash content . 13
6.2 Repeatability . 13
7 Results to be reported . 13
7.1 General . 13
7.2 Product or sample identification . 14
7.3 Test conditions . 14
7.4 Test results . 14
Annex A (informative) Format of the test report . 15
Annex B (informative) Worked examples . 17
B.1 rGO powder prepared by thermal exfoliation of graphite oxide: sample 1 . 17
B.2 rGO powder prepared by thermal exfoliation of graphite oxide: sample 2 . 18
B.3 Graphene powder prepared by liquid phase exfoliation: sample 3 . 19
B.4 GO dispersion: sample 4 . 19
B.5 Graphite oxide powder: sample 5 . 20
Bibliography . 22

Figure 1 – TG-DSC of graphite oxide and rGO in air with 2 °C/min heating speed . 10
Figure B.1 – Press and shape the sample 1 powder into a cylindrical pellet . 17
Figure B.2 – Incineration of sample 1 . 17

Figure B.3 – Pre-treatment of sample 2 . 18
Figure B.4 – Sample 4 dispersion becomes GO film after drying . 19

Table A.1 – Product identification (in accordance with the relevant blank detail
specification) . 15
Table A.2 – General material description (in accordance with the relevant blank detail
specification) . 15
Table A.3 – Measurement related information and results . 15
Table A.4 – Measurement results . 16
Table B.1 – Measurement results of sample 1 . 18
Table B.2 – Measurement results of sample 2 . 18
Table B.3 – Measurement results of sample 3 . 19
Table B.4 – Measurement results of sample 4 . 20
Table B.5 – Measurement results of sample 5 . 21

– 4 – IEC TS 62607-6-22:2022  IEC 2022
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
NANOMANUFACTURING – KEY CONTROL CHARACTERISTICS –

Part 6-22: Graphene-based material – Ash content: incineration

FOREWORD
1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising
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IEC TS 62607-6-22 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
113/704/DTS 113/681/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/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 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
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contents. Users should therefore print this document using a colour printer.

– 6 – IEC TS 62607-6-22:2022  IEC 2022
INTRODUCTION
Impurity, which is inevitable because of the production process, often has significant influence
on the performance of graphene in energy conversion and storage, electronics, composites
and catalysis, etc. The ash content can quickly provide an indication of impurity to some
extent.
Determination of ash content of graphene is essential for manufacturers to perform quality
control. It is also important for users to choose suitable product.
Incineration, the most common method of testing ash content, is a low cost, good repeatable
and easy to operate method. Some unique properties of graphene-based material, such as
ultra-low bulk density, relative high oxygen content and thermal exfoliation, make it impossible
to follow existing incineration standards to determine the ash content of graphene-based
material correctly. With the development of the graphene industry, it is important to establish
a specific standard method for graphene to determine the ash content correctly. In this
method, the two key objectives are to increase the bulk density of ultra-low density reduced
graphene oxide through press or impregnation and to avoid instant exfoliation of high oxygen
content graphene oxide through low-speed heating during heating at 130 °C to 200 °C.
This document introduces a reliable method for determining the ash content of graphene with
incineration. This document can be used as the reference for other carbonaceous materials,
such as single-walled and multi-walled carbon nanotubes.

NANOMANUFACTURING – KEY CONTROL CHARACTERISTICS –

Part 6-22: Graphene-based material – Ash content: incineration

1 Scope
This part of IEC TS 62607 establishes a standardized method to determine the key control
characteristic
• ash content
of powder and dispersion of graphene-based material by
• incineration.
The ash content is derived by residue obtained after incineration under the operating
conditions specified in this document, being divided by the mass of the dried test portion.
• The method is applicable for graphene, graphene oxide and reduced graphene oxide in
forms of both dry powder and dispersion. This document can be used as reference for
graphite oxide and other modified graphene.
• Typical application areas of this method are research, manufacturer and downstream user
to guide material processing and quality control.
2 Normative references
There are no normative references in this document.
3 Terms, definitions, symbols and abbreviated terms
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
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]

– 8 – IEC TS 62607-6-22:2022  IEC 2022
3.1.2
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.
3.1.3
reduced graphene oxide
rGO
reduced oxygen content form of graphene oxide
[SOURCE: ISO/TS 80004-13:2017 [1], 3.1.2.14]
3.1.4
graphene oxide
GO
chemically modified graphene prepared by oxidation and exfoliation of graphite, causing
extensive oxidative modification of the basal plane
[SOURCE: ISO/TS 80004-13:2017. 3.1.2.13]
3.1.5
graphite oxide
chemically modified graphite prepared by extensive oxidative modification of the basal planes
Note 1 to entry: The structure and properties of graphite oxide depend on the degree of oxidation and the
particular synthesis method.
[SOURCE: ISO/TS 80004-13:2017, 3.1.2.12]
3.2 Key control characteristics measured in accordance with this document
3.2.1
key control characteristic
KCC
key performance indicator
material property or intermediate product characteristic which can affect safety or compliance
with regulations, fit, function, performance, quality, reliability or subsequent processing of the
final product
Note 1 to entry: The measurement of a key control characteristic is described in a standardized measurement
procedure with known accuracy and precision.
Note 2 to entry: It is possible to define more than one measurement method for a key control characteristic if the
correlation of the results is well-defined and known.
3.2.2
ash
residue obtained after incineration at a temperature of 650 °C under the operating conditions
specified in this document, divided by the mass of the test portion
Note 1 to entry: The content of ash is usually expressed as a percentage.

3.2.3
thermal gravimetry
TG
method in which the change in mass of a sample is measured as a function of temperature
while the sample is subjected to a controlled temperature programme
[SOURCE: ISO 80004-13:2017, 3.3.2.5]
3.2.4
differential scanning calorimetry
DSC
method in which the difference in energy inputs into a substance and a reference material is
measured as a function of temperature while the substance and reference material are
subjected to a controlled temperature programme
[SOURCE: ISO/TS 80004-6:2021, 6.2.1]
3.2.5
TG-DSC
combined technology of TG and DSC in which TG and DSC data of tested sample are
obtained simultaneously
4 General
4.1 Measurement principle
4.1.1 Incineration principle
A test portion is pre-treated, dried and then incinerated at a controlled and programmed
temperature in air, until complete disappearance of the carbon in the residue. After cooling to
room temperature, the mass of the residue is determined.
4.1.2 Operation principle of this method
4.1.2.1 GO and graphite oxide
a) GO and graphite oxide have high content of oxygen functional groups. These oxygen
functional groups can be decomposed at 130 °C to 200 °C to produce gas and heat, as
shown in TG-DSC of graphite oxide (Figure 1a). Decomposition will happen at both outer
surface and interior of sample at the same time.
1) On one hand, the produced gas increases the pressure between graphene sheets
inside the sample. When this pressure is larger than the total of Van der Waals force
...