1、 IEC 62697-1 Edition 1.0 2012-08 INTERNATIONAL STANDARD NORME INTERNATIONALE Test methods for quantitative determination of corrosive sulfur compounds in unused and used insulating liquids Part 1: Test method for quantitative determination of dibenzyldisulfide (DBDS) Mthodes dessai pour la dterminat
2、ion quantitative des composs de soufre corrosif dans les liquides isolants usags et neufs Partie 1: Mthode dessai pour la dtermination quantitative du disulfure de dibenzyle (DBDS) IEC62697-1:2012 colourinsideTHIS PUBLICATION IS COPYRIGHT PROTECTED Copyright 2012 IEC, Geneva, Switzerland All rights
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16、Clients - webstore.iec.ch/csc Si vous dsirez nous donner des commentaires sur cette publication ou si vous avez des questions contactez-nous: csciec.ch. IEC 62697-1 Edition 1.0 2012-08 INTERNATIONAL STANDARD NORME INTERNATIONALE Test methods for quantitative determination of corrosive sulfur compoun
17、ds in unused and used insulating liquids Part 1: Test method for quantitative determination of dibenzyldisulfide (DBDS) Mthodes dessai pour la dtermination quantitative des composs de soufre corrosif dans les liquides isolants usags et neufs Partie 1: Mthode dessai pour la dtermination quantitative
18、du disulfure de dibenzyle (DBDS) INTERNATIONAL ELECTROTECHNICAL COMMISSION COMMISSION ELECTROTECHNIQUE INTERNATIONALE V ICS 29.040 PRICE CODE CODE PRIX ISBN 978-2-83220-305-7 Registered trademark of the International Electrotechnical Commission Marque dpose de la Commission Electrotechnique Internat
19、ionale Warning! Make sure that you obtained this publication from an authorized distributor. Attention! Veuillez vous assurer que vous avez obtenu cette publication via un distributeur agr. colourinside 2 62697-1 IEC:2012 CONTENTS FOREWORD . 5 INTRODUCTION . 7 1 Scope . 9 2 Normative references . 9
20、3 Terms, definitions and abbreviations 9 3.1 Terms and definitions 9 3.2 Abbreviations 13 4 Sampling 13 5 Procedure 13 5.1 Principle 13 5.2 Significance and use . 13 5.3 Interferences . 14 5.3.1 Co-eluting compounds . 14 5.3.2 Electron capture detector (ECD) 14 5.3.3 Atomic emission detector (AED) 1
21、4 5.3.4 Mass spectrometer (MS) 14 5.3.5 MS/MS 14 5.3.6 Interference from the matrix . 14 5.4 Apparatus 15 5.4.1 Balance . 15 5.4.2 Gas chromatography system . 15 5.4.3 Data system 16 5.5 Reagents and materials . 16 5.5.1 Purity of reagents 16 5.5.2 Gases 16 5.5.3 Solvents 16 5.6 Standard materials 1
22、6 5.6.1 Dibenzyl disulfide (DBDS) . 16 5.6.2 Diphenyl disulfide (DPDS) . 16 5.6.3 Blank oil 16 5.7 Standard solutions 17 5.7.1 Stock solution 17 5.7.2 Internal standard (IS) solution 17 6 Instrument set-up . 17 6.1 Gas chromatograph . 17 6.1.1 General . 17 6.1.2 Carrier gas 17 6.1.3 Injector 17 6.1.
23、4 Separation parameters 17 6.1.5 ECD detection . 18 6.1.6 AED detection . 18 6.1.7 MS detection . 18 6.1.8 MS/MS detection . 18 6.2 Calibration . 19 6.2.1 General . 19 6.2.2 Calibration procedure 19 62697-1 IEC:2012 3 6.2.3 Response factor determination (ECD and AED) . 19 6.2.4 Response factor deter
24、mination (MS) 19 6.2.5 Response factor determination (MS/MS) 20 6.3 Analysis 20 6.3.1 Sample pre-treatment 20 6.3.2 Sample injection 20 6.3.3 Chromatographic run . 20 6.3.4 Peak integration 20 6.4 Calculations 21 6.4.1 ECD and AED 21 6.4.2 Mass spectrometer (MS) 21 6.4.3 MS/MS 21 6.5 Results 21 7 Pr
25、ecision data 21 7.1 Detection limit . 21 7.2 Repeatability . 22 7.3 Reproducibility 22 8 Report 22 Annex A (informative) Figures with typical chromatograms and results 23 Annex B (informative) Operating parameters for other suitable detectors . 30 Bibliography 31 Figure A.1 GC-ECD chromatogram of 2
26、mg kg1DBDS and DPDS (IS) in white mineral oil . 23 Figure A.2 GC-ECD chromatogram of 200 mg kg1DBDS and DPDS (IS) in white mineral oil . 24 Figure A.3 GC-ECD chromatogram of commercial mineral insulating oil with a known DBDS contamination . 24 Figure A.4 GC-ECD chromatogram of commercial mineral in
27、sulating oil with no known DBDS contamination 25 Figure A.5 GC-ECD chromatogram of commercial mineral insulating oil with known DBDS contamination fortified with acommercial polychlorinated biphenyls (PCBs) formulation 25 Figure A.6 Carbon and sulfur (C-S) oil finger prints of a commercial mineral i
28、nsulating oil with known DBDS contamination obtained with GC-AED 26 Figure A.7 C-S oil fingerprints of a commercial mineral insulating oil with no known DBDS contamination obtained with GC-AED . 26 Figure A.8 C-S oil fingerprints of a commercial mineral insulating oil with known DBDS contamination o
29、btained with GC-AED . 27 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 kg1. 27 Figure A.10 Extracted ion chromatograms DPDS (IS) molecular ion m/z 218 and DBDS molecular ion m/z 246 in
30、 commercial mineral insulating oil with known DBDS contamination . 28 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) 28 4 62697-1 IEC:2012 Fig
31、ure 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 29 Table 1 Column oven temperature programming parameters . 18 Table 2 Mass spectromete
32、r parameters . 18 Table 3 Repeatability limit 22 Table 4 Reproducibility limit . 22 62697-1 IEC:2012 5 INTERNATIONAL ELECTROTECHNICAL COMMISSION _ TEST METHODS FOR QUANTITATIVE DETERMINATION OF CORROSIVE SULFUR COMPOUNDS IN UNUSED AND USED INSULATING LIQUIDS Part 1: Test method for quantitative dete
33、rmination of dibenzyldisulfide (DBDS) FOREWORD 1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising all national electrotechnical committees (IEC National Committees). The object of IEC is to promote international co-operation on all quest
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43、 9) Attention is drawn to the possibility that some of the elements of this IEC Publication may be the subject of patent rights. IEC shall not be held responsible for identifying any or all such patent rights. International Standard IEC 62697-1 has been prepared by IEC technical committee 10: Fluids
44、 for electrotechnical applications. The text of this standard is based on the following documents: FDIS Report on voting 10/887/FDIS 10/891/RVD Full information on the voting for the approval of this standard can be found in the report on voting indicated in the above table. This publication has bee
45、n drafted in accordance with the ISO/IEC Directives, Part 2. 6 62697-1 IEC:2012 The committee has decided that the contents of this publication will remain unchanged until the stability date indicated on the IEC web site under “http:/webstore.iec.ch“ in the data related to the specific publication.
46、At this date, the publication will be reconfirmed, withdrawn, replaced by a revised edition, or amended. IMPORTANT The colour inside logo on the cover page of this publication indicates that it contains colours which are considered to be useful for the correct understanding of its contents. Users sh
47、ould therefore print this document using a colour printer. 62697-1 IEC:2012 7 INTRODUCTION Sulfur can be present in insulating liquids in various forms, including elemental sulfur, inorganic sulfur compounds and organic sulfur compounds. The number of diverse sulfur species comprised of different is
48、omers and homologous can run into hundreds. The total sulfur(TS) concentration in insulating liquids depends on the origin of the liquid, refining processes and the degree of refining and formulation including addition of additives to the base oils. Base oils include mineral based paraffinic and nap
49、hthenic oils, synthetic iso- paraffins obtained through gas to liquid conversion process (GTL-Fischer-Tropsch), esters, poly alpha olefins, poly alkylene glycols, etc. Additives can be comprised of electrostatic discharge depressants, metal deactivators, metal passivators, phenolic and sulfur containing antioxidants such as the polysulfides, disulfides, dibenzyl disulfide (DBDS), etc. Certain sulfur co
