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PD IEC TS 62607-6-13:2020 Nanomanufacturing. Key control characteristics - Graphene-based material. Oxygen functional group content: Boehm titration method, 2020
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- CONTENTS
- FOREWORD
- INTRODUCTION
- 1 Scope
- 2 Normative references
- 3 Terms, definitions, symbols and abbreviated terms [Go to Page]
- 3.1 Terms and definitions [Go to Page]
- 3.1.1 General terms
- 3.1.2 Key control characteristics measured according to this document
- oxygen functional group
- 3.1.3 Terms related to the measurement method
- 3.2 Symbols and abbreviated terms
- 4 General [Go to Page]
- 4.1 Measurement principle
- 4.2 Sample preparation method
- Figures [Go to Page]
- Figure 1 – Test principle of Boehm titration
- Tables [Go to Page]
- Table 1 – Four types of oxygen functional group and their structures
- 4.3 Description of measurement equipment / apparatus [Go to Page]
- 4.3.1 Analytical balance, readability is 0,1 mg.
- 4.3.2 Electric thermostatic drying oven
- 4.3.3 Numerical control magnetic agitator/oscillator
- 4.3.4 Automatic potentiometer, with pH electrode and accurate to 0,1 mV.
- 4.3.5 HDPE bottles, the volume are 1 000 mL and 100 mL, with stopper.
- 4.4 Supporting materials
- 4.5 Ambient conditions during measurement
- 5 Measurement procedure [Go to Page]
- 5.1 Detailed protocol of the measurement procedure [Go to Page]
- 5.1.1 Preparation of solutions
- Table 2 – Reagents used in this document [Go to Page]
- 5.1.2 Reactions between graphene and bases
- 5.1.3 Instrument preparation
- 5.1.4 Titration of the filtrate
- 5.2 Measurement uncertainty
- 5.3 Operation procedure, key control steps and case study
- 6 Data analysis / interpretation of results [Go to Page]
- 6.1 Normalized base consumption
- 6.2 Oxygen functional group content
- 7 Results to be reported [Go to Page]
- 7.1 General
- 7.2 Product/sample identification
- 7.3 Test results
- Annexes [Go to Page]
- Annex A (informative) Operation procedure and key control steps [Go to Page]
- A.1 Operation procedure
- Figure A.1 – Operation procedure [Go to Page]
- A.2 Key control steps
- Figure A.2 – Key control steps
- Annex B (informative) Influence of CO2 [Go to Page]
- B.1 Effect of CO2 on titration of base concentration
- Figure B.1 – Titration curves of NaOH solution [Go to Page]
- B.2 Effect of CO2 on base consumption
- Table B.1 – Titration results of back titration and direct titration of NaOH solution
- Table B.2 – Results of base consumption of NaOH with and without bubbling N2
- Annex C (informative) Lower limit of determination [Go to Page]
- C.1 Experiment of lower mass of reacted sample A
- C.2 Determination of detection limits
- Figure C.1 – The normalized base consumption of different amounts of sample A
- Table C.1 – Base consumption result of sample A
- Table C.2 – Oxygen functional group content result
- Table C.3 – Detection limits for different sample amounts
- Annex D (informative) Test report [Go to Page]
- D.1 Example of a test record
- D.2 Format of the test report
- Table D.1 – Data for calibration of titrant acid
- Table D.2 – Data for Boehm titration
- Table D.3 – Product identification (according to IEC 62565-3-1)
- Table D.4 – General material description (according to IEC 62565-3-1)
- Table D.5 – Measurement results
- Annex E (informative) Case study [Go to Page]
- E.1 Preparation of solution
- E.2 Sample preparation
- E.3 Reactions between graphene and bases
- E.4 Titration of the filtrate
- Figure E 1 – Titration curves of A0 filtrate (upper left), B0 filtrate (upper right), C0 filtrate (lower left), and D0 filtrate (lower right)
- Table E.1 – Measurement data [Go to Page]
- E.5 Calculation
- Table E.2 – Normalized base consumption of sample 1 [Go to Page]
- E.6 Test report
- Table E.3 – Product identification of sample 1
- Table E.4 – General material description of sample 1
- Table E.5 – Measurement results of sample 1
- Bibliography [Go to Page]