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eLibrary > BS EN IEC 62321-3-3:2021 Determination of certain substances in electrotechnical products - Screening. Polybrominated biphenyls, polybrominated diphenyl ethers and phthalates in polymers by gas chromatography-mass spectrometry using a pyrolyser/thermal de >

BS EN IEC 62321-3-3:2021 Determination of certain substances in electrotechnical products - Screening. Polybrominated biphenyls, polybrominated diphenyl ethers and phthalates in polymers by gas chromatography-mass spectrometry using a pyrolyser/thermal de, 2021

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BS EN IEC 62321-3-3:2021 Determination of certain substances in electrotechnical products - Screening. Polybrominated biphenyls, polybrominated diphenyl ethers and phthalates in polymers by gas chromatography-mass spectrometry using a pyrolyser/thermal de, 2021

undefined [Go to Page]
European foreword
Endorsement notice
English [Go to Page]
CONTENTS
FOREWORD
INTRODUCTION
1 Scope
2 Normative references
3 Terms, definitions and abbreviated terms [Go to Page]
3.1 Terms and definitions
3.2 Abbreviated terms
4 Principle [Go to Page]
4.1 Overview
4.2 Principle of test
5 Reagents and materials
6 Apparatus
7 Sampling
8 Procedure [Go to Page]
8.1 General instructions for the analysis
8.2 Sample preparation [Go to Page]
8.2.1 General
8.2.2 Polymer sample
8.2.3 Stock solution or polymer reference material
8.3 Instrumental parameters
Tables [Go to Page]
Table 1 – Measurement conditions of Py/TD-GC-MS
8.4 Calibration [Go to Page]
8.4.1 General
8.4.2 Determination of RRFs
9 Calculation of PBBs, PBDEs and phthalates concentration [Go to Page]
9.1 General
9.2 Determination of RF of DEHP
9.3 Calculation [Go to Page]
9.3.1 Calculation of RF
9.3.2 Calculation of concentration
10 Precision [Go to Page]
10.1 Screening judgement
Table 2 – IIS3-3 Screening and threshold judgement
10.2 Repeatability and reproducibility
Table 3 – IIS3-3 Repeatability and reproducibility (phthalate)
Table 4 – IIS3-3 Repeatability and reproducibility (PBB)
Table 5 – IIS3-3 Repeatability and reproducibility (PBDE)
11 Quality assurance and control [Go to Page]
11.1 General
11.2 Quality control [Go to Page]
11.2.1 Sensitivity test
11.2.2 Blank test
11.2.3 System stability test
11.2.4 Degradation test
11.2.5 RRF test
11.3 Method detection limit (MDL) and limit of quantification (LOQ)
12 Test report
Annex A (informative)Flow chart of screening and verification test method
Figures [Go to Page]
Figure A.1 – Flow chart for screening step and verificationtest step for PBDEs, PBBs and phthalates
Table A.1 – Screening methods for phthalate esters,PBBs and PBDEs in the IEC 62321 series
Annex B (informative)Principle of Py/TD-GC-MS instruments [Go to Page]
Figure B.1 – Example of Py/TD-GC-MS instrument
Annex C (informative)Other test methods [Go to Page]
Table C.1 – Other test methods
Annex D (informative)Commercially available reference solutions and materials [Go to Page]
D.1 Reference solution
Table D.1 – Example list of commercially availablereference solutions of PBBs and PBDEs
D.2 Polymer reference materials
Table D.2 – Example list of commercially available reference solutions of phthalates
Table D.3 – Example list of commercially available reference materials of PBBs, PBDEs and PS considered suitable for Py/TD-GC-MS
Figure D.1 – Sample preparation of reference materials
Table D.4 – Example list of commercially available reference materialsof phthalates considered suitable for Py/TD-GC-MS
Annex E (informative)Sampling procedure [Go to Page]
E.1 Sample preparation using cutting tools
E.2 Sample preparation using cryogenic grinding mill
E.3 Accurate weighing of sample
E.4 Method of sample injection
Table E.1 – Example of variation of weighting samples
Annex F (informative)Verification of the EGA thermal desorption zone [Go to Page]
Figure F.1 – Example of EGA thermogram of a PVC sample containing phthalates
Figure F.2 – Example of EGA thermogram of a polystyrene sample containing PBDEs
Annex G (informative)Example of chromatograms [Go to Page]
Figure G.1 – Total ion current chromatogram of 0,1 µg of PBBs, PBDEsand phthalates mixture by Py/TD-GC-MS
Annex H (informative)Examples of RRFs [Go to Page]
Table H.1 – RRFs of analytes
Annex I (informative)Sample analysis sequence [Go to Page]
Table I.1 – Sample analysis sequence for Py/TD-GC-MS analysis
Annex J (informative)Results of international inter-laboratory study 3-3 [Go to Page]
Table J.1 – Statistical data for phthalates
Table J.2 – Statistical data for polybrominated biphenyls
Table J.3 – Statistical data for polybrominated diphenyl ethers
Bibliography
Français [Go to Page]
SOMMAIRE
AVANT-PROPOS
INTRODUCTION
1 Domaine d'application
2 Références normatives
3 Termes, définitions et termes abrégés [Go to Page]
3.1 Termes et définitions
3.2 Termes abrégés
4 Principe [Go to Page]
4.1 Présentation
4.2 Principe de l’essai
5 Réactifs et matériaux
6 Appareils
7 Échantillonnage
8 Procédure [Go to Page]
8.1 Instructions générales pour l’analyse
8.2 Préparation des échantillons [Go to Page]
8.2.1 Généralités
8.2.2 Échantillon de polymère
8.2.3 Solution mère ou matériau polymère de référence
8.3 Paramètres instrumentaux
Tableaux [Go to Page]
Tableau 1 – Conditions de mesure par Py/TD-GC-MS
8.4 Étalonnage [Go to Page]
8.4.1 Généralités
8.4.2 Détermination des RRF
9 Calcul de la concentration des PBB, des PBDE et des phtalates [Go to Page]
9.1 Généralités
9.2 Détermination du RF de DEHP
9.3 Calcul [Go to Page]
9.3.1 Calcul du RF
9.3.2 Calcul de la concentration
10 Fidélité [Go to Page]
10.1 Estimation de la détection
Tableau 2 – Estimation de la détection et du seuil IIS3-3
10.2 Répétabilité et reproductibilité
Tableau 3 – Répétabilité et reproductibilité IIS3-3 (phtalate)
Tableau 4 – Répétabilité et reproductibilité IIS3-3 (PBB)
Tableau 5 – Répétabilité et reproductibilité IIS3-3 (PBDE)
11 Assurance qualité et contrôle de la qualité [Go to Page]
11.1 Généralités
11.2 Contrôle de la qualité [Go to Page]
11.2.1 Essai de sensibilité
11.2.2 Essai témoin
11.2.3 Essai de stabilité du système
11.2.4 Essai de dégradation
11.2.5 Essai de RRF
11.3 Limite de détection de la méthode (MDL) et limite de quantification (LOQ)
12 Rapport d'essai
Annexe A (informative)Organigramme de la méthode d’essai de détection et de vérification
Figures [Go to Page]
Figure A.1 – Organigramme de l’étape d’essai de détection et de l’étape d’essai de vérification des PBDE, PBB et phtalates
Tableau A.1 – Méthodes de détection des esters de phtalates, des PBB et des PBDE de la série IEC 62321
Annexe B (informative)Principe des instruments Py/TD-GC-MS [Go to Page]
Figure B.1 – Exemple d’instrument Py/TD-GC-MS
Annexe C (informative)Autres méthodes d’essai [Go to Page]
Tableau C.1 – Autres méthodes d’essai
Annexe D (informative)Solutions et matériaux de référence disponibles dans le commerce [Go to Page]
D.1 Solution de référence
Tableau D.1 – Exemple de liste de solutions de référence de PBB et de PBDE disponibles dans le commerce
D.2 Matériaux polymères de référence
Tableau D.2 – Exemple de liste de solutions de référence de phtalates disponibles dans le commerce
Tableau D.3 – Exemple de liste de matériaux de référence de PBB, PBDE et de PS du commerce considérés comme appropriés pour l’analyse Py/TD-GC-MS
Figure D.1 – Préparation d'échantillon de matériaux de référence
Tableau D.4 – Exemple de liste de matériaux de référence de phtalate du commerce considérés comme appropriés pour l’analyse Py/TD-GC-MS
Annexe E (informative)Procédure d’échantillonnage [Go to Page]
E.1 Préparation des échantillons à l’aide d’outils de coupe
E.2 Préparation des échantillons à l’aide d’un broyeur cryogénique
E.3 Exactitude de pesée de l’échantillon
E.4 Méthode d’injection de l’échantillon
Tableau E.1 – Exemple de variation du poids des échantillons de pesée
Annexe F (informative)Vérification de la zone de thermodésorption par AGE [Go to Page]
Figure F.1 – Exemple de thermogramme d’AGE d’un échantillon de PVC contenant des phtalates
Figure F.2 – Exemple de thermogramme d’AGE d’un échantillon de polystyrène contenant des PBDE
Annexe G (informative)Exemple de chromatogrammes [Go to Page]
Figure G.1 – Chromatogramme du courant ionique total de 0,1 µg de mélange PBB/PBDE et phtalates par analyse Py/TD-GC-MS
Annexe H (informative)Exemple de résultats de RRF obtenus [Go to Page]
Tableau H .1 – RRF des analytes
Annexe I (informative)Séquence d’analyse d’échantillon [Go to Page]
Tableau I.1 – Séquence d’analyse d’échantillon pour l’analyse Py/TD-GC-MS
Annexe J (informative)Résultats de l'étude internationale interlaboratoires 3-3 [Go to Page]
Tableau J.1 – Données statistiques pour les phtalates
Tableau J.2 – Données statistiques pour les diphényles polybromés
Tableau J.3 – Données statistiques pour les diphényléthers polybromés
Bibliographie [Go to Page]

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