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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
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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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