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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
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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
BSI PD IEC/TR 62697-3:2018
$142.49