IEC TS 62607-6-13:2020

Nanomanufacturing - Key control characteristics - Part 6-13: Graphene-based material - Oxygen functional group content: Boehm titration method

IEC TS 62607-6-13:2020 establishes a standardized method to determine the chemical key control characteristic
• oxygen functional group content on graphite oxide, graphene oxide, reduced graphene oxide and other types of functionalized graphene by
• Boehm titration method.
In this document, the measured functional groups are carboxyl groups (also in the form of their cyclic anhydrides), lactone groups, hydroxyl groups and reactive carbonyl groups. Oxygen functional groups that exhibit no reactivity such as epoxides cannot be measured
The contents of the corrigendum 1 of October 2020 have been included in this copy.

General Information

• Status: Published
• Publication Date: 27-Jul-2020
• ICS: 01 - GENERALITIES. TERMINOLOGY. STANDARDIZATION. DOCUMENTATION
• ICS: 07.120 - Nanotechnologies
• Technical Committee: TC 113 - Nanotechnology for electrotechnical products and systems
• Drafting Committee: PT 62607-6-13 - TC 113/PT 62607-6-13
• Current Stage: PPUB - Publication issued
• Start Date: 28-Aug-2020
• Completion Date: 28-Jul-2020

Relations

• Corrected By: IEC TS 62607-6-13:2020/COR1:2020 - Corrigendum 1 - Nanomanufacturing - Key control characteristics - Part 6-13: Graphene-based material - Oxygen functional group content: Boehm titration method
• Effective Date: 05-Sep-2023

Standards Content (Sample)

IEC TS 62607-6-13 ®
Edition 1.0 2020-07
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –
Part 6-13: Graphene powder – Oxygen functional group content: Boehm titration
method
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IEC TS 62607-6-13 ®
Edition 1.0 2020-07
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –

Part 6-13: Graphene powder – Oxygen functional group content: Boehm titration

method
INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
ICS 07.120 ISBN 978-2-8322-8726-2

– 2 – IEC TS 62607-6-13:2020  IEC 2020
CONTENTS
FOREWORD . 4
INTRODUCTION . 6
1 Scope . 7
2 Normative references . 7
3 Terms, definitions, symbols and abbreviated terms . 7
3.1 Terms and definitions . 8
3.1.1 General terms . 8
3.1.2 Key control characteristics measured according to this document . 9
oxygen functional group . 9
3.1.3 Terms related to the measurement method . 9
3.2 Symbols and abbreviated terms . 9
4 General . 9
4.1 Measurement principle . 9
4.2 Sample preparation method . 10
4.3 Description of measurement equipment / apparatus . 11
4.3.1 Analytical balance, readability is 0,1 mg. . 11
4.3.2 Electric thermostatic drying oven . 11
4.3.3 Numerical control magnetic agitator/oscillator . 11
4.3.4 Automatic potentiometer, with pH electrode and accurate to 0,1 mV. . 11
4.3.5 HDPE bottles, the volume are 1 000 mL and 100 mL, with stopper. . 11
4.4 Supporting materials . 11
4.5 Ambient conditions during measurement . 11
5 Measurement procedure . 11
5.1 Detailed protocol of the measurement procedure . 11
5.1.1 Preparation of solutions . 11
5.1.2 Reactions between graphene and bases . 13
5.1.3 Instrument preparation . 13
5.1.4 Titration of the filtrate . 13
5.2 Measurement uncertainty . 14
5.3 Operation procedure, key control steps and case study . 14
6 Data analysis / interpretation of results . 14
6.1 Normalized base consumption . 14
6.2 Oxygen functional group content . 15
7 Results to be reported . 15
7.1 General . 15
7.2 Product/sample identification . 15
7.3 Test results . 15
Annex A (informative) Operation procedure and key control steps . 16
A.1 Operation procedure . 16
A.2 Key control steps . 17
Annex B (informative) Influence of CO . 18
B.1 Effect of CO on titration of base concentration . 18
B.2 Effect of CO on base consumption . 19
Annex C (informative) Lower limit of determination . 20
C.1 Experiment of lower mass of reacted sample A . 20

C.2 Determination of detection limits . 20
Annex D (informative) Test report . 23
D.1 Example of a test record . 23
D.2 Format of the test report . 23
Annex E (informative) Case study . 25
E.1 Preparation of solution . 25
E.2 Sample preparation . 25
E.3 Reactions between graphene and bases . 25
E.4 Titration of the filtrate . 26
E.5 Calculation . 28
E.6 Test report . 30
Bibliography . 31

Figure 1 – Test principle of Boehm titration . 10
Figure A.1 – Operation procedure . 16
Figure A.2 – Key control steps . 17
Figure B.1 – Titration curves of NaOH solution . 18
Figure C.1 – The normalized base consumption of different amounts of sample A . 20
Figure E 1 – Titration curves of A0 filtrate (upper left), B0 filtrate (upper right),
C0 filtrate (lower left), and D0 filtrate (lower right) . 27

Table 1 – Four types of oxygen functional group and their structures . 10
Table 2 – Reagents used in this document . 11
Table B.1 – Titration results of back titration and direct titration of NaOH solution . 19
Table B.2 – Results of base consumption of NaOH with and without bubbling N . 19
Table C.1 – Base consumption result of sample A . 21
Table C.2 – Oxygen functional group content result . 22
Table C.3 – Detection limits for different sample amounts . 22
Table D.1 – Data for calibration of titrant acid . 23
Table D.2 – Data for Boehm titration . 23
Table D.3 – Product identification (according to IEC 62565-3-1) . 24
Table D.4 – General material description (according to IEC 62565-3-1) . 24
Table D.5 – Measurement results . 24
Table E.1 – Measurement data . 27
Table E.2 – Normalized base consumption of sample 1 . 29
Table E.3 – Product identification of sample 1 . 30
Table E.4 – General material description of sample 1 . 30
Table E.5 – Measurement results of sample 1 . 30

– 4 – IEC TS 62607-6-13:2020  IEC 2020
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
NANOMANUFACTURING – KEY CONTROL CHARACTERISTICS –

Part 6-13: Graphene powder – Oxygen functional group content:
Boehm titration method
FOREWORD
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