IEC TS 62607-6-30:2024

Nanomanufacturing - Key control characteristics - Part 6-30: Graphene-based material - Anion concentration: Ion chromatography method

IEC TS 62607-6-30:2024 establishes a standardized method to determine the chemical key control characteristic
- anion concentration
for powder of graphene-based material by
- ion chromatography.
In this document, the measured anions are fluoride, chloride, nitrite, bromide, nitrate, sulphate, and phosphate. These anions, present in the extraction solution of graphene-based materials, are separated into distinct elution bands on the ion chromatographic separation column and subsequently measured using a conductivity detector. Quantification of these anions is accomplished by establishing a proportional relationship between the measured signal (peak area or peak height) and the concentration of each anion. This is achieved by calibrating the system using a series of standards containing known amounts of each anion. Subsequently, unknown samples are analysed under the same conditions as the standards to determine their anion concentrations.
- Powder of graphene-based material addressed by this document includes graphene oxide, reduced graphene oxide and functionalized graphene, graphene, bilayer graphene, trilayer graphene and few-layer graphene.
Note: This document can also be used for other carbonaceous material such as graphite and graphite oxide.
- This document targets graphene-based material manufacturers and downstream users to guide their material design, production and quality control.

General Information

• Status: Published
• Publication Date: 12-Aug-2024
• ICS: 07.120 - Nanotechnologies
• Technical Committee: TC 113 - Nanotechnology for electrotechnical products and systems
• Drafting Committee: WG 8 - TC 113/WG 8
• Current Stage: PPUB - Publication issued
• Start Date: 13-Aug-2024
• Completion Date: 16-Aug-2024

Overview

IEC TS 62607-6-30:2024 defines a standardized ion chromatography (IC) method to determine the key chemical control characteristic - anion concentration - in powders of graphene-based material. The Technical Specification covers sample extraction, IC system setup (separation column + conductivity detector), calibration with multi-anion standards, and quantitative data treatment based on peak area or peak height. Measured anions include fluoride, chloride, nitrite, bromide, nitrate, sulphate, and phosphate. The method applies to graphene oxide, reduced graphene oxide, functionalized graphene, graphene (mono‑ to few‑layer) and can also be used for related carbonaceous materials such as graphite and graphite oxide.

Key Topics and Requirements

• Measurement principle: separation of target anions on an ion chromatographic column and detection by conductivity; quantification via calibration curves linking signal to concentration.
• Analytes: fluoride, chloride, nitrite, bromide, nitrate, sulphate, phosphate.
• Sample preparation: procedures to produce an extraction solution from low‑density, often hydrophobic graphene powders; sample handling steps are specified to ensure representative extraction prior to IC analysis.
• Instrumentation: recommended IC system components (eluent options, separation column, conductivity detector) and typical operating conditions are provided.
• Calibration and quality control: preparation of calibration solutions with known anion concentrations, blank tests, and regular calibration to ensure linearity and accuracy.
• Data analysis & reporting: instructions for calculating concentrations, expressing limits of detection/quantification, measurement uncertainty, and required test report elements.
• Validation information: informative annexes include example chromatograms, interlaboratory study results, case studies, and example test report formats.

Applications and Users

• Who should use it: graphene‑based material manufacturers, downstream users (battery, capacitor, coating, thermal management sectors), analytical testing laboratories, and quality control teams.
• Practical value:
  • Ensures consistent quality control and specification of anionic impurities that impact electrochemical performance (e.g., batteries, capacitors).
  • Guides material design and production process optimization by identifying residual anions from reagents or processing.
  • Provides a reproducible method for regulatory, procurement, and acceptance testing across the supply chain.

Related Standards

• Part of the IEC TS 62607 series (“Nanomanufacturing – Key control characteristics”) developed by IEC TC 113 (Nanotechnology). Users should consult other parts of IEC TS 62607 for complementary test methods and nanomanufacturing control characteristics.

Keywords: IEC TS 62607-6-30:2024, ion chromatography, anion concentration, graphene-based material, graphene oxide, quality control, nanomanufacturing.

Standards Content (Sample)

IEC TS 62607-6-30 ®
Edition 1.0 2024-08
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –
Part 6-30: Graphene-based material – Anion concentration: Ion chromatography
method
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IEC TS 62607-6-30 ®
Edition 1.0 2024-08
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –

Part 6-30: Graphene-based material – Anion concentration: Ion chromatography

method
INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
ICS 07.120  ISBN 978-2-8322-9496-3

– 2 – IEC TS 62607-6-30:2024  IEC 2024
CONTENTS
FOREWORD . 4
INTRODUCTION . 6
1 Scope . 7
2 Normative references . 7
3 Terms and definitions . 7
3.1 General terms . 8
3.2 Key control characteristics measured in accordance with this document . 8
3.3 Terms related to the measurement method . 9
4 General . 9
4.1 Measurement principle . 9
4.2 Description of measurement apparatus . 9
4.3 Reagents . 10
4.4 Calibration solutions . 11
4.5 Sample preparation . 11
4.6 Ambient conditions during measurement . 12
5 Measurement procedure . 12
5.1 Instrument set-up . 12
5.2 Calibration . 13
5.3 Detailed protocol of the measurement procedure . 14
5.3.1 Preparation of sample solutions . 14
5.3.2 Blank test . 14
5.3.3 Measurement of sample extraction solution . 15
6 Data analysis and interpretation of results . 15
7 Measurement accuracy . 15
8 Test report . 16
8.1 Cover sheet . 16
8.2 Sample identification . 16
8.3 Measurement specific information . 16
8.4 Test results . 16
Annex A (informative) Reference graphs . 17
Annex B (informative) Results of interlaboratory validation study . 18
Annex C (informative) Example format of the test report . 19
Annex D (informative) Case study . 21
D.1 Sample preparation . 21
D.2 Preparation of calibration solution . 21
D.3 IC condition . 22
D.4 Data analysis / interpretation of results . 22
D.4.1 Results of sample test of IC chromatogram . 22
D.4.2 Data recorded and calculation . 22
D.5 Measurement report . 23
Bibliography . 25

Figure 1 – Schematic diagram of ion chromatographic system . 10
Figure 2 – Change of wettability by ball milling . 12
Figure 3 – Change of dispersibility after shaking the sample vial sufficiently . 14

Figure A.1 – Chromatogram of the calibration solution using potassium hydroxide
eluent . 17
Figure A.2 – Chromatogram of the calibration solution using sodium carbonate and

sodium hydrogen carbonate eluent . 17
Figure D.1 – Photos and typical transmission electron microscope (TEM) images of the
samples before and after ball milling . 21
Figure D.2 – Chromatogram of the sample solution by IC . 22

Table 1 – Typical operation conditions I for potassium hydroxide eluent . 13
Table 2 – Typical operation conditions II for sodium carbonate and sodium hydrogen
carbonate eluent . 13
Table 3 – Concentration of calibration solutions . 14
Table 4 – Limit of detection of two different eluents . 16
Table B.1 – Statistical anion concentration results of two materials . 18
Table C.1 – Product identification (in accordance with the relevant blank detail

specification) . 19
Table C.2 – Measurement conditions . 19
Table C.3 – Calibration results . 20
Table C.4 – Measurement results . 20
Table D.1 – Data of calibration curve . 22
Table D.2 – Data of sample solution test . 23
Table D.3 – Product identification of sample #1A . 23
Table D.4 – Measurement conditions of sample #1A . 24
Table D.5 – Measurement results of sample #1A . 24

– 4 – IEC TS 62607-6-30:2024  IEC 2024
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
NANOMANUFACTURING –
KEY CONTROL CHARACTERISTICS –
Part 6-30: Graphene-based material –
Anion concentration: Ion chromatography method

FOREWORD
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8) Attention is drawn to the Normative references cited in this publication. Use of the referenced publications is
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shall not be held responsible for identifying any or all such patent rights.
IEC TS 62607-6-30 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
113/824/DTS 113/846/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, or
• revised.
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 62607-6-30:2024  IEC 2024
INTRODUCTION
In recent years, graphene-based materials have drawn increasing attention from academia and
industry due to their unique physical and chemical properties. Powders consisting of
graphene-based material are now mass produced and widely used in fields such as battery,
capacitor, coating, heat conducting, etc.
Anions are common and significant non-metallic impurities in graphene-based materials,
originating from raw materials or chemicals used during the production process. These anions
play a crucial role in influencing the applications of graphene-based materials. For instance,
anions can lead to changes in reversible capacity and coulombic efficiency when
graphene-based materials are employed in batteries and capacitors. Therefore, anion
concentration stands as a key characteristic of graphene-based materials. Fluoride, chloride,
nitrite, bromide, nitrate, sulphate, and phosphate are among the prevalent anions detected in
numerous graphene-based materials gathered from the market.
Various methods have been utilized for determination of anions. The most common techniques
for quantifying anions include titration, colorimetric determination, and ion chromatography (IC).
IC offers several advantages – such as unique selectivity, fast analysis speed, high sensitivity,
good accuracy, and easy operation – over alternative techniques in the analysis of anions.
Moreover, one of its significant advantages is the capability to simultaneously determine
multiple types of anions.
Sample preparation is a critical step in the analytical process, particularly when dealing with
powders characterized by very low density and strong hydrophobic properties. It is essential to
obtain a sample extraction solution to effectively isolate the analytes from the matrix before
conducting IC instrumental determinations. Consequently, the accuracy, precision, and
quantification limits of the analysis are significantly influenced by the sample preparation
process. This document furnishes specific sample preparation details tailored for powders
composed of graphene-based materials. Importantly, the described method is not confined
solely to graphene-based materials but is also applicable to other carbonaceous materials such
as graphite and graphite oxide.
The purpose of this document is to describe a test method to determine contents of anions in
graphene-based material. A case study illustrating the application of this document can be
found in Annex D.
NANOMANUFACTURING –
KEY CONTROL CHARACTERISTICS –
Part 6-30: Graphene-based material –
Anion concentration: Ion chromatography method

1 Scope
This part of IEC TS 62607 establishes a standardized method to determine the chemical key
control characteristic
• anion concentration
for powder of graphene-based material by
• ion chromatography.
In this document, the measured anions are fluoride, chloride, nitrite, bromide, nitrate, sulphate,
and phosphate. These anions, present in the extraction solution of graphene-based materials,
are separated into distinct elution bands on the ion chromatographic separation column and
subsequently measured using a conductivity detector. Quantification of these anions is
accomplished by establishing a proportional relationship between the measured signal (peak
area or peak height) and the concentration of each anion. This is achieved by calibrating the
system using a series of standards containing known amounts of each anion. Subsequently,
unknown samples are analysed under the same conditions as the standards to determine their
anion concentrations.
– Powder of graphene-based material addressed by this document includes graphene oxide,
reduced graphene oxide and functionalized graphene, graphene, bilayer graphene, trilayer
graphene and few-layer graphene.
NOTE This document can also be used for other carbonaceous material such as graphite and graphite oxide.
– This document targets graphene-based material manufacturers and downstream users to
guide their material design, production and quality control.
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 terminology databases for use in standardization at the following
addresses:
• IEC Electropedia: available at https://www.electropedia.org/
• ISO Online browsing platform: available at https://www.iso.org/obp

– 8 – IEC TS 62607-6-30:2024  IEC 2024
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 layer, 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.
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.
[SOURCE: IEC TS 62607-6-3:2020, 3.2.4]
3.2 Key control characteristics measured in accordance with this document
3.2.1
anion concentration
amount of negatively charged ions divided by the mass of graphene-based material
Note 1 to entry: The term is presumed to mean mass concentration. The unit "milligram per kilogram" is
recommended.
Note 2 to entry: Anions (fluoride, chloride, nitrite, bromide, nitrate, sulphate and phosphate) present in
graphene-based material can be non-intentionally added substances that come from raw materials or chemicals used
during production process or intentionally added substances to improve the performance.

3.3 Terms related to the measurement method
...