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BS EN 16377:2013

BS EN 16377:2013

$142.49

Characterization of waste. Determination of brominated flame retardants (BFR) in solid waste

Published By Publication Date Number of Pages
BSI 2013 32
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This European Standard specifies a method for the determination of selected polybrominated flame retardants (BFR), chemically known as polybrominated diphenylethers (BDE), in waste materials using gas chromatography/mass spectrometry (GC-MS) in the electron impact (EI) ionisation mode (GC-EI-MS).

When applying GC-EI-MS, the method is applicable to samples containing 100 µg/kg to 5 000 µg/kg of tetra-to octabromodiphenylether congeners and 100 µg/kg to 10 000 µg/kg of decabromo diphenylether (see Table 1). It is also possible to analyse other brominated flame retardants applying the method described in this European Standard, provided the method’s applicability has been proven.

Table 1 — Brominated flame retardants determined by this method

a Numbering for the BDE according to IUPAC nomenclature for PCB.

PDF Catalog

PDF Pages PDF Title
5 Foreword
6 Introduction
7 1 Scope
Table 1 — Brominated flame retardants determined by this method
2 Normative references
3 Principle
8 4 Interference
5 Reagents and standards
Table 2 — Examples of internal standards for GC-EI-MS analysis
9 6 Equipment
10 7 Sample pretreatment
11 8 Procedure
8.1 Blank determination
8.2 Extraction
8.2.1 General
8.2.2 Soxhlet extraction
12 8.2.3 Sonication
8.2.4 Pressurised fluid extraction
8.3 Clean-up
8.4 Measurement
13 8.5 Identification
Table 3 — Ions for electron impact ionisation detection
9 Calibration
9.1 General
14 9.2 Procedure steps
9.2.1 Evaluation of the range of the linear relationship
9.2.2 Two point calibration over the total linear range
9.2.3 Estimation of the accuracy of the calibration for the concentration of interest
9.2.4 Accuracy improvement
15 Table 4 — Example concentrations in solutions for evaluating the linear range
9.3 Calibration with internal standards
16 9.4 Quantification with the internal standard
17 9.5 Determination of recoveries of the internal standards
9.6 Results and reporting
10 Test report
18 Annex A (normative) Clean-up procedures
A.1 Multi-layer column chromatography I (Al2O3), column size: 22 mm × 190 mm
A.1.1 Reagents
A.1.2 Preparation of clean-up column
A.1.3 Procedure
A.2 Multi-layer column chromatography II (Silica), column size: 22 mm × 190 mm
A.2.1 Reagents
19 A.2.2 Preparation of clean-up multi-layer column
A.2.3 Procedure
20 A.3 Gel permeation chromatography (GPC)
A.3.1 General
A.3.2 GPC apparatus
A.3.3 Evaporation apparatus
A.3.4 Glassware
A.3.5 Reagents
21 A.3.6 Automatic GPC clean-up procedure
A.3.6.1 General
A.3.6.2 Automatic GPC clean-up conditions
A.3.7 Manual GPC clean-up
22 Annex B (informative) Examples of separation conditions in gas chromatography and mass spectrometry
24 Annex C (informative) Typical ions and time windows for electron impact ionisation detection
Table C.1 — Typical ions and time windows for electron impact ionisation detection
25 Annex D (informative) Examples of chromatograms
Figure D.1 — GC-MS-Chromatogram of an electronic waste sample after clean-up (both columns and GPC), showing the BDE congeners and DBDPE [decabromodiphenylethane]
26 Figure D.2 — GC-MS-Chromatogram of a shredder light fraction sample after clean-up (both columns and GPC), showing the BDE congeners and DBDPE [decabromodiphenylethane]
27 Annex E (informative) Precision data
Table E.1 — Validation data
29 Annex F (informative) Summary of general requirements and recommendations
Table F.1 — General requirements and recommendations
30 Bibliography

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BS EN 16377:2013
$142.49