BS EN 62697-1:2012:2013 Edition
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Test methods for quantitative determination of corrosive sulphur compounds in unused and used insulating liquids – Test method for quantitative determination of dibenzyldisulfide (DBDS)
| Published By | Publication Date | Number of Pages |
| BSI | 2013 | 36 |
IEC 62697-1:2012 specifies a test method for the quantitative determination of corrosive sulfur compounds-dibenzyl disulfide (DBDS) in used and unused insulating liquids over a 5 to 600 mg kg-1 concentration range.
PDF Catalog
| PDF Pages | PDF Title |
|---|---|
| 6 | English CONTENTS |
| 9 | INTRODUCTION |
| 11 | 1 Scope 2 Normative references 3 Terms, definitions and abbreviations 3.1 Terms and definitions |
| 15 | 3.2 Abbreviations 4 Sampling 5 Procedure 5.1 Principle 5.2 Significance and use |
| 16 | 5.3 Interferences 5.3.1 Co-eluting compounds 5.3.2 Electron capture detector (ECD) 5.3.3 Atomic emission detector (AED) 5.3.4 Mass spectrometer (MS) 5.3.5 MS/MS 5.3.6 Interference from the matrix |
| 17 | 5.4 Apparatus 5.4.1 Balance 5.4.2 Gas chromatography system |
| 18 | 5.4.3 Data system 5.5 Reagents and materials 5.5.1 Purity of reagents 5.5.2 Gases 5.5.3 Solvents 5.6 Standard materials 5.6.1 Dibenzyl disulfide (DBDS) 5.6.2 Diphenyl disulfide (DPDS) 5.6.3 Blank oil |
| 19 | 5.7 Standard solutions 5.7.1 Stock solution 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 |
| 20 | 6.1.5 ECD detection 6.1.6 AED detection 6.1.7 MS detection 6.1.8 MS/MS detection Tables Table 1 – Column oven temperature programming parameters Table 2 – Mass spectrometer parameters |
| 21 | 6.2 Calibration 6.2.1 General 6.2.2 Calibration procedure 6.2.3 Response factor determination (ECD and AED) 6.2.4 Response factor determination (MS) |
| 22 | 6.2.5 Response factor determination (MS/MS) 6.3 Analysis 6.3.1 Sample pre-treatment 6.3.2 Sample injection 6.3.3 Chromatographic run 6.3.4 Peak integration |
| 23 | 6.4 Calculations 6.4.1 ECD and AED 6.4.2 Mass spectrometer (MS) 6.4.3 MS/MS 6.5 Results 7 Precision data 7.1 Detection limit |
| 24 | 7.2 Repeatability 7.3 Reproducibility 8 Report Table 3 – Repeatability limit Table 4 – Reproducibility limit |
| 25 | Annex A (informative) Figures with typical chromatograms and results Figures Figure A.1 – GC-ECD chromatogram of 2 mg kg–1 DBDS and DPDS (IS) in white mineral oil |
| 26 | Figure A.2 – GC-ECD chromatogram of 200 mg kg–1 DBDS and DPDS (IS) in white mineral oil Figure A.3 – GC-ECD chromatogram of commercial mineral insulating oil with a known DBDS contamination |
| 27 | Figure A.4 – GC-ECD chromatogram of commercial mineral insulating oil with no known DBDS contamination Figure A.5 – GC-ECD chromatogram of commercial mineral insulating oil with known DBDS contamination fortified with acommercial polychlorinated biphenyls (PCBs) formulation |
| 28 | Figure A.6 – Carbon and sulfur (C-S) oil finger prints of a commercial mineral insulating oil with known DBDS contamination obtained with GC-AED Figure A.7 – C-S oil fingerprints of a commercial mineral insulating oil with no known DBDS contamination obtained with GC-AED |
| 29 | Figure A.8 – C-S oil fingerprints of a commercial mineral insulating oil with known DBDS contamination obtained with GC-AED Figure A.9 – Extracted ion chromatograms of DPDS (IS) molecular ion m/z 218 and DBDS molecular ion m/z 246 in white mineral fortified with DBDS, concentration 4 mg kg–1 |
| 30 | Figure A.10 – Extracted ion chromatograms DPDS (IS) molecular ion m/z 218 and DBDS molecular ion m/z 246 in commercial mineral insulating oil with known DBDS contamination Figure A.11 – Extracted ion chromatograms m/z 109 derived from CID of DPDS (IS) molecular ion m/z 218 and m/z 91 derived from CID of DBDS molecular ion m/z 246 in white mineral fortified with DBDS (4 mg/kg) |
| 31 | Figure A.12 – Extracted ion chromatograms m/z 109 derived from CID of DPDS (IS) molecular ion m/z 218 and m/z 91 derived from CID of DBDS molecular ion m/z 246 in a commercial mineral oil with known DBDS contamination |
| 32 | Annex B (informative) Operating parameters for other suitable detectors |
| 33 | Bibliography |
