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eLibrary > BS EN 62697-1:2012 Test methods for quantitative determination of corrosive sulphur compounds in unused and used insulating liquids - Test method for quantitative determination of dibenzyldisulfide (DBDS) >

BS EN 62697-1:2012 Test methods for quantitative determination of corrosive sulphur compounds in unused and used insulating liquids - Test method for quantitative determination of dibenzyldisulfide (DBDS), 2013

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BS EN 62697-1:2012 Test methods for quantitative determination of corrosive sulphur compounds in unused and used insulating liquids - Test method for quantitative determination of dibenzyldisulfide (DBDS), 2013

iec62697-1{ed1.0}b.pdf [Go to Page]
English [Go to Page]
CONTENTS
FOREWORD
INTRODUCTION
1 Scope
2 Normative references
3 Terms, definitions and abbreviations [Go to Page]
3.1 Terms and definitions
3.2 Abbreviations
4 Sampling
5 Procedure [Go to Page]
5.1 Principle
5.2 Significance and use
5.3 Interferences [Go to Page]
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
5.4 Apparatus [Go to Page]
5.4.1 Balance
5.4.2 Gas chromatography system
5.4.3 Data system
5.5 Reagents and materials [Go to Page]
5.5.1 Purity of reagents
5.5.2 Gases
5.5.3 Solvents
5.6 Standard materials [Go to Page]
5.6.1 Dibenzyl disulfide (DBDS)
5.6.2 Diphenyl disulfide (DPDS)
5.6.3 Blank oil
5.7 Standard solutions [Go to Page]
5.7.1 Stock solution
5.7.2 Internal standard (IS) solution
6 Instrument set-up [Go to Page]
6.1 Gas chromatograph [Go to Page]
6.1.1 General
6.1.2 Carrier gas
6.1.3 Injector
6.1.4 Separation parameters
6.1.5 ECD detection
6.1.6 AED detection
6.1.7 MS detection
6.1.8 MS/MS detection
6.2 Calibration [Go to Page]
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)
6.2.5 Response factor determination (MS/MS)
6.3 Analysis [Go to Page]
6.3.1 Sample pre-treatment
6.3.2 Sample injection
6.3.3 Chromatographic run
6.3.4 Peak integration
6.4 Calculations [Go to Page]
6.4.1 ECD and AED
6.4.2 Mass spectrometer (MS)
6.4.3 MS/MS
6.5 Results
7 Precision data [Go to Page]
7.1 Detection limit
7.2 Repeatability
7.3 Reproducibility
8 Report
Annex A (informative) Figures with typical chromatograms and results
Annex B (informative) Operating parameters for other suitable detectors
Bibliography
Figures [Go to Page]
Figure A.1 – GC-ECD chromatogram of 2 mg kg–1 DBDS and DPDS (IS) in white mineral oil
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
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
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
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
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)
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
Tables [Go to Page]
Table 1 – Column oven temperature programming parameters
Table 2 – Mass spectrometer parameters
Table 3 – Repeatability limit
Table 4 – Reproducibility limit
Français [Go to Page]
SOMMAIRE
AVANT-PROPOS
INTRODUCTION
1 Domaine d’application
2 Références normatives
3 Termes, définitions et abréviations [Go to Page]
3.1 Termes et définitions
3.2 Abréviations
4 Echantillonnage
5 Procédure [Go to Page]
5.1 Principe
5.2 Signification et utilisation
5.3 Interférences [Go to Page]
5.3.1 Composés coéluants
5.3.2 Détecteur à capture d’électrons (DCE)
5.3.3 Détecteur à émission atomique (AED)
5.3.4 Spectromètre de masse (SM)
5.3.5 MS/MS
5.3.6 Interférence provenant de la matrice
5.4 Appareil [Go to Page]
5.4.1 Balance
5.4.2 Système de chromatographie en phase gazeuse
5.5 Réactifs et matériaux [Go to Page]
5.5.1 Pureté des réactifs
5.5.2 Gaz
5.5.3 Solvants
5.6 Matériaux normalisés [Go to Page]
5.6.1 Disulfure de dibenzyle (DBDS)
5.6.2 Disulfure de diphényle (DPDS)
5.6.3 Huile vierge
5.7 Solutions étalons [Go to Page]
5.7.1 Solutions mères
5.7.2 Solution étalon interne (IS)
6 Configuration des instruments [Go to Page]
6.1 Chromatographe en phase gazeuse [Go to Page]
6.1.1 Généralités
6.1.2 Gaz vecteur
6.1.3 Injecteur
6.1.4 Paramètres de séparation
6.1.5 Détection du CDE
6.1.6 Détection AED
6.1.7 Détection SM
6.1.8 Détection MS/MS
6.2 Étalonnage [Go to Page]
6.2.1 Généralités
6.2.2 Procédure d’étalonnage
6.2.3 Détermination du facteur de réponse (DCE et AED)
6.2.4 Détermination du facteur de réponse (MS)
6.2.5 Détermination du facteur de réponse (MS/MS)
6.3 Analyse [Go to Page]
6.3.1 Traitement préalable de l’échantillon
6.3.2 Injection de l’échantillon
6.3.3 Exécution chromatographique
6.3.4 Intégration du pic
6.4 Calculs [Go to Page]
6.4.1 DCE et AED
6.4.2 Spectromètre de masse (MS)
6.4.3 MS/MS
6.5 Résultats
7 Données de précision [Go to Page]
7.1 Limite de détection
7.2 Répétabilité
7.3 Reproductibilité
8 Rapport
Annexe A (informative) Schémas avec des chromatogrammes et des résultats typiques
Annexe B (informative) Paramètres de fonctionnement pour les autres détecteurs utilisables
Bibliographie
Figures [Go to Page]
Figure A.1 – Chromatogramme GC-ECD de 2 mg kg–1 DBDS et DPDS (IS) dans l’huile de paraffine
Figure A.2 – Chromatogramme GC-ECD de 200 mg kg–1 DBDS et DPDS (IS) dans l’huile de paraffine
Figure A.3 – Chromatogramme GC-ECD de l’huile minérale isolante disponible dans le commerce à contamination DBDS connue
Figure A.4 – Chromatogramme GC-ECD de l’huile minérale isolante disponibledans le commerce à contamination DBDS inconnue
Figure A.5 – Chromatogramme GC-ECD de l’huile minérale isolante disponible dansle commerce à contamination DBDS connue enrichie d’une formulation depolychlorobiphényle (PCB) disponible dans le commerce
Figure A.6 – Empreintes de carbone et de soufre (C-S) d’une huile minérale isolante disponible dans le commerce à contamination DBDS connue obtenue avec la GC-AED
Figure A.7 – Empreintes d’huile C-S d’une huile minérale isolante disponibledans le commerce à contamination DBDS inconnue obtenue avec la GC-AED
Figure A.8 – Empreintes d’huile C-S d’une huile minérale isolante disponibledans le commerce à contamination DBDS connue obtenue avec la GC-AED
Figure A.9 – Chromatogrammes d’ion extrait d’ion moléculaire DPDS (IS) m/z 218 et d’ion moléculaire DBDS m/z 246 dans l’huile de paraffine enrichie en DBDS, concentration de 4 mg kg–1
Figure A.10 – Chromatogrammes d’ion extrait d’ion moléculaire DPDS (IS) m/z 218 et d’ion moléculaire DBDS m/z 246 dans l’huile minérale isolante disponible dans le commerce à contamination DBDS connue
Figure A.11 – Chromatogrammes d’ion extrait m/z 109 dérivé de la dissociation induite par collision d’ion moléculaire DPDS (IS) m/z 218 et m/z 91 dérivé de la dissociation induite par collision d’ion moléculaire DBDS m/z 246 dans l’huile de paraffine enrichie en DBDS (4 mg/kg)
Figure A.12 – Chromatogrammes d’ion extrait m/z 109 dérivé de la dissociation induite par collision d’ion moléculaire DPDS (IS) m/z 218 et m/z 91 dérivé de la dissociation induite par collision d’ion moléculaire DBDS m/z 246 dans l’huile minérale disponible dans le commerce à contamination DBDS connue
Tableaux [Go to Page]
Tableau 1 – Paramètres de programmation de la température du four à colonne
Tableau 2 – Paramètres du spectromètre de masse
Tableau 3 – Limite de répétabilité
Tableau 4 – Limite de reproductibilité [Go to Page]

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BS EN 62697-1:2012 Test methods for quantitative determination of corrosive sulphur compounds in unused and used insulating liquids - Test method for quantitative determination of dibenzyldisulfide (DBDS), 2013

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please select your company type below: