BSI PD IEC/TR 62697-3:2018
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Test methods for quantitative determination of corrosive sulfur compounds in unused and used insulating liquids – Test method for quantitative determination of elemental sulfur
| Published By | Publication Date | Number of Pages |
| BSI | 2018 | 28 |
This part of IEC 62697 specifies a test method for the quantitative determination of elemental sulfur in used and unused insulating liquids over a 2 mg kg–1 to 400 mg kg–1 concentration range.
PDF Catalog
| PDF Pages | PDF Title |
|---|---|
| 2 | undefined |
| 4 | CONTENTS |
| 6 | FOREWORD |
| 8 | INTRODUCTION |
| 10 | 1 Scope 2 Normative references 3 Terms and definitions |
| 11 | 4 Sampling 5 Procedure 5.1 Principle 5.1.1 Determination with gas chromatography 5.1.2 Determination with differential pulse voltammetry 5.2 Significance and use |
| 12 | 5.3 Interferences 5.3.1 Co-eluting compounds 5.3.2 Electron capture detector (ECD) 5.3.3 Flame photometric detector (FPD) 5.3.4 Mass spectrometer (MS) 5.3.5 Interference from the matrix 5.4 Apparatus 5.4.1 Balance |
| 13 | 5.4.2 Gas chromatography system 5.4.3 Differential pulsed voltammetry 5.5 Reagents and materials 5.5.1 Purity of reagents 5.5.2 Gases |
| 14 | 5.5.3 Solvents 5.6 Standard materials 5.6.1 Elemental sulfur 5.6.2 Diphenyl disulfide (DPDS) 5.6.3 Blank oil 5.7 Standard solutions 5.7.1 Stock solutions |
| 15 | 5.7.2 Internal standard (IS) solution 6 Instrument set-up 6.1 Gas chromatograph 6.1.1 General 6.1.2 Carrier gas 6.1.3 Injector 6.1.4 Separation parameters |
| 16 | 6.1.5 ECD detection 6.1.6 FPD detection 6.1.7 MS detection 6.2 Calibration 6.2.1 General 6.2.2 Calibration procedure Tables Table 1 – Column oven temperature programming parameters Table 2 – Mass spectrometer parameters |
| 17 | 6.2.3 Response factor determination (ECD and FPD) 6.2.4 Response factor determination (MS) 6.3 Analysis 6.3.1 Sample pre-treatment |
| 18 | 6.3.2 Sample injection 6.3.3 Chromatographic run 6.3.4 Peak integration 6.4 Calculations 6.4.1 ECD and FPD 6.4.2 Mass spectrometer (MS) |
| 19 | 6.4.3 Differential pulse voltammetry measurements 6.5 Results Figures Figure 1 – Typical peak form and concentration calculation |
| 20 | 7 Precision data 7.1 Detection limit 7.2 Repeatability 7.3 Reproducibility 8 Report Table 3 – Repeatability limit Table 4 – Reproducibility limit |
| 21 | Annex A (informative)Figures with typical chromatograms and results Figure A.1 – GC-ECD chromatogram of 5 mg kg–1 elemental sulfurand (IS) in white mineral oil |
| 22 | Figure A.2 – GC-ECD chromatogram of 100 mg kg–1 elemental sulfurand (IS) in white mineral oil |
| 23 | Annex B (informative)RRT results Statistical evaluation of elemental sulfur dataGC-ECD/FPD Table B.1 – Reproducibility with same chemical analysis approach Table B.2 – Reproducibility with different chemical analysis approach |
| 24 | Table B.3 – Repeatability |
| 25 | Bibliography |
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BSI PD IEC/TR 62697-3:2018
Test methods for quantitative determination of corrosive sulfur compounds in unused and used insulating liquids…
