IEC TS 62607-6-20:2022

Nanomanufacturing - Key control characteristics - Part 6-20: Graphene-based material - Metallic impurity content: Inductively coupled plasma mass spectrometry

IEC TS 62607-6-20:2022 (EN) IEC TS 62607 establishes a standardized method to determine the chemical key control characteristic
- metallic impurity content
for powders of graphene-based materials by
- inductively coupled plasma mass spectrometry (ICP-MS).
The metallic impurity content is derived by the signal intensity of measured elements through MS spectrum of ICP-MS.
- The method is applicable for powder of graphene and related materials, including bilayer graphene (2LG), trilayer graphene (3LG), few-layer graphene (FLG), reduced graphene oxide (rGO) and graphene oxide (GO).
– The typical application area is in the microelectronics industry, e.g. conductive pastes, displays, etc., for manufacturers to guide material design, and for downstream users to select suitable products.

General Information

• Status: Published
• Publication Date: 10-Oct-2022
• 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: 08-Nov-2022
• Completion Date: 11-Oct-2022

Standards Content (Sample)

IEC TS 62607-6-20 ®
Edition 1.0 2022-10
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –
Part 6-20: Graphene-based material – Metallic impurity content: Inductively
coupled plasma mass spectrometry
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IEC TS 62607-6-20 ®
Edition 1.0 2022-10
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –

Part 6-20: Graphene-based material – Metallic impurity content: Inductively

coupled plasma mass spectrometry

INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
ICS 07.120 ISBN 978-2-8322-5732-6

– 2 – IEC TS 62607-6-20:2022 © IEC 2022
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 in accordance with this document . 9
4 General . 9
4.1 Chemical reagents . 9
4.2 Description of measurement instrument and apparatus . 9
4.2.1 Measurement instrument . 9
4.2.2 Sample pre-treatment apparatus . 9
4.2.3 Other . 9
4.3 Calibration standards . 10
4.3.1 Standard stock solutions . 10
4.3.2 Internal standard (IS) solutions . 10
5 Sample preparation method . 10
5.1 General . 10
5.2 Sample pre-treatment procedure . 10
6 Measurement procedure . 12
6.1 Calibration of ICP-MS instrument . 12
6.2 Quantitative measurement procedure . 12
6.2.1 Whole element scanning . 12
6.2.2 Quantitative measurement of metal impurities. 12
6.2.3 Method recovery measurement . 12
6.2.4 Standard recovery measurement . 12
7 Data analysis . 13
7.1 Content of metal impurities in test samples . 13
7.2 Standard recovery. 13
8 Measurement uncertainty estimation. 13
9 Measurement report . 14
9.1 General . 14
9.2 Product or sample identification . 14
9.3 Measurement conditions . 14
9.4 Measurement specific information . 14
9.5 Measurement results . 14
Annex A (informative) Case study for FLG powder . 16
A.1 Test sample . 16
A.2 Sample pre-treatment . 16
A.3 Instrument information . 16
A.4 Standard calibration curve . 16
A.4.1 Standard stock solutions . 16
A.4.2 Standard calibration curve . 17
A.5 Measurement procedure . 17
A.6 Measurement results . 17
Annex B (informative) Case study for rGO powder . 19

B.1 Test sample . 19
B.2 Sample pre-treatment . 19
B.3 Measurement instrument . 19
B.4 Standard calibration curve . 19
B.5 Measurement results . 21
B.6 Standard recovery. 22
Annex C (informative) Comparison of different pre-treatment methods . 24
C.1 Test sample . 24
C.2 Comparison of different pre-treatment methods. 24
C.2.1 GO test sample preparation . 24
C.2.2 rGO test sample preparation . 25
C.3 Comparison of different digestion conditions . 25
Annex D (informative) Results comparison of ICP-MS and ICP-OES . 27
D.1 Test sample . 27
D.2 Measurement results comparison between ICP-MS and ICP-OES . 27
Bibliography . 28

Figure A.1 – Content distribution of metal impurities detected in FLG test sample . 18
Figure B.1 – Standard calibration curves of several metal elements contained in rGO

test sample . 20
Figure B.2 – Content distribution of metal impurities detected in rGO test sample . 22
Figure B.3 – Standard recovery of most species of metal impurities in rGO test sample . 23
Figure C.1 – Result comparison of three pre-treatment methods for industrial GO
powder . 25
Figure C.2 – Result comparison of different digestion methods for industrial rGO
powder . 25
Figure C.3 – Content of metal impurities detected in rGO test sample using microwave-

assisted digestion under different digestion conditions . 26

Table 1 – Potential interferences for several typical elements in industrial graphene
powder . 12
Table A.1 – Content of all metal impurities detected in FLG test sample . 17
Table B.1 – Content of all metal impurities detected in rGO test sample . 21
Table D.1 – Measurement results comparison between ICP-MS and ICP-OES . 27

– 4 – IEC TS 62607-6-20:2022 © IEC 2022
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
NANOMANUFACTURING – KEY CONTROL CHARACTERISTICS –

Part 6-20: Graphene-based material – Metallic impurity content:
Inductively coupled plasma mass spectrometry

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