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
Current Stage
PPUB - Publication issued
Start Date
16-Aug-2024
Completion Date
13-Aug-2024
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Technical specification
IEC TS 62607-6-30:2024 - Nanomanufacturing - Key control characteristics - Part 6-30: Graphene-based material - Anion concentration: Ion chromatography method Released:13. 08. 2024 Isbn:9782832294963
English language
25 pages
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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
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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

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