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.<\/p>\n
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| 6<\/td>\n | English CONTENTS <\/td>\n<\/tr>\n | ||||||
| 9<\/td>\n | INTRODUCTION <\/td>\n<\/tr>\n | ||||||
| 11<\/td>\n | 1 Scope 2 Normative references 3 Terms, definitions and abbreviations 3.1 Terms and definitions <\/td>\n<\/tr>\n | ||||||
| 15<\/td>\n | 3.2 Abbreviations 4 Sampling 5 Procedure 5.1 Principle 5.2 Significance and use <\/td>\n<\/tr>\n | ||||||
| 16<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
| 17<\/td>\n | 5.4 Apparatus 5.4.1 Balance 5.4.2 Gas chromatography system <\/td>\n<\/tr>\n | ||||||
| 18<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
| 19<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
| 20<\/td>\n | 6.1.5 ECD detection 6.1.6 AED detection 6.1.7 MS detection 6.1.8 MS\/MS detection Tables Table 1 \u2013 Column oven temperature programming parameters Table 2 \u2013 Mass spectrometer parameters <\/td>\n<\/tr>\n | ||||||
| 21<\/td>\n | 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) <\/td>\n<\/tr>\n | ||||||
| 22<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
| 23<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
| 24<\/td>\n | 7.2 Repeatability 7.3 Reproducibility 8 Report Table 3 \u2013 Repeatability limit Table 4 \u2013 Reproducibility limit <\/td>\n<\/tr>\n | ||||||
| 25<\/td>\n | Annex A (informative) Figures with typical chromatograms and results Figures Figure A.1 \u2013 GC-ECD chromatogram of 2 mg kg\u20131 DBDS and DPDS (IS) in white mineral oil <\/td>\n<\/tr>\n | ||||||
| 26<\/td>\n | Figure A.2 \u2013 GC-ECD chromatogram of 200 mg kg\u20131 DBDS and DPDS (IS) in white mineral oil Figure A.3 \u2013 GC-ECD chromatogram of commercial mineral insulating oil with a known DBDS contamination <\/td>\n<\/tr>\n | ||||||
| 27<\/td>\n | Figure A.4 \u2013 GC-ECD chromatogram of commercial mineral insulating oil with no known DBDS contamination Figure A.5 \u2013 GC-ECD chromatogram of commercial mineral insulating oil with known DBDS contamination fortified with acommercial polychlorinated biphenyls (PCBs) formulation <\/td>\n<\/tr>\n | ||||||
| 28<\/td>\n | Figure A.6 \u2013 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 \u2013 C-S oil fingerprints of a commercial mineral insulating oil with no known DBDS contamination obtained with GC-AED <\/td>\n<\/tr>\n | ||||||
| 29<\/td>\n | Figure A.8 \u2013 C-S oil fingerprints of a commercial mineral insulating oil with known DBDS contamination obtained with GC-AED Figure A.9 \u2013 Extracted ion chromatograms of DPDS (IS) molecular ion m\/z\u00a0218 and DBDS molecular ion m\/z\u00a0246 in white mineral fortified with DBDS, concentration 4\u00a0mg\u00a0kg\u20131 <\/td>\n<\/tr>\n | ||||||
| 30<\/td>\n | Figure A.10 \u2013 Extracted ion chromatograms DPDS (IS) molecular ion m\/z\u00a0218 and DBDS molecular ion m\/z\u00a0246 in commercial mineral insulating oil with known DBDS contamination Figure A.11 \u2013 Extracted ion chromatograms m\/z\u00a0109 derived from CID of DPDS (IS) molecular ion m\/z\u00a0218 and m\/z\u00a091 derived from CID of DBDS molecular ion m\/z\u00a0246 in white mineral fortified with DBDS (4\u00a0mg\/kg) <\/td>\n<\/tr>\n | ||||||
| 31<\/td>\n | Figure A.12 \u2013 Extracted ion chromatograms m\/z 109 derived from CID of DPDS (IS) molecular ion m\/z\u00a0218 and m\/z\u00a091 derived from CID of DBDS molecular ion m\/z\u00a0246 in a commercial mineral oil with known DBDS contamination <\/td>\n<\/tr>\n | ||||||
| 32<\/td>\n | Annex B (informative) Operating parameters for other suitable detectors <\/td>\n<\/tr>\n | ||||||
| 33<\/td>\n | Bibliography <\/td>\n<\/tr>\n<\/table>\n","protected":false},"excerpt":{"rendered":" Test methods for quantitative determination of corrosive sulphur compounds in unused and used insulating liquids – Test method for quantitative determination of dibenzyldisulfide (DBDS)<\/b><\/p>\n |