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BS EN 16453:2014

BS EN 16453:2014

$102.76

Pulp, paper and paperboard. Determination of phthalates in extracts from paper and paperboard

Published By Publication Date Number of Pages
BSI 2014 16
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This European Standard specifies an analytical test method for the determination of phthalates in water, solvent and modified polyphenylene oxide (MPPO) extracts of paper and board materials and articles intended for food contact using gas chromat ography coupled to mass spectrometry (GC-MS).

This method is applicable to the determination of phthalates in concentration ranging from 0,025 mg/l to 0,5 mg/l for water and solvent extracts and 0,002 mg/dm2 to 0,040 mg/dm2 for MPPO migration depending on the individual substance, the specified volume used for analysis and the value of the blank.

PDF Catalog

PDF Pages PDF Title
4 Contents Page
5 Foreword
6 1 Scope
Table 1 — Phthlates determined by this method
2 Normative references
7 3 Principle
3.1 General
3.2 Interferences
4 Materials
4.1 General
8 4.2 Pasteur pipettes
4.3 Double mark glass pipette of 0,05 ml, 0,2 ml, 0,5 ml, 1 ml, 5 ml and 10 ml
4.4 Volumetric flasks of 5 ml, 10 ml, 50 ml and 100 ml
4.5 Screw-cap glass bottle PYREX0F ) of 250 ml with a Polytetrafluorethylene-septa cap
4.6 Graduated cylinder of 200 ml
4.7 Round flask of 50 ml and 250 ml
4.8 Glass funnel
4.9 Polytetrafluorethylene-screw-cap glass vial single use (capacity adapted to the volume of concentrate)
5 Apparatus
5.1 Balance: capable of accurately weighing 0,000 1 g
5.2 Round flask heater
5.3 Rotary vacuum evaporator
5.4 Gas chromatograph coupled to a mass spectrometer (GC-MS)
6 Reagents
6.1 General
6.2 Operating gases for gas chromatography/mass spectrometry, of high purity and in accordance with manufacturer’s specifications
6.3 Ethyl acetate, C4H8O2, CAS N 141-78-6
6.4 Isooctane, C8H18, CAS N 540-84-1
6.5 Internal standard stock solution: For example d4-ring-deuterated-dibutyl phthalate (D4-ring-DBP) at 10 g/l
6.5.1 General
9 6.5.2 Solution A of internal standard at 100 mg/l in ethyl acetate
6.5.3 Solution B of internal standard at 10 mg/l in ethyl acetate
6.5.4 Solution C of internal standard at 0,5 mg/l in ethyl acetate
6.6 Stock solutions of individual phthalate at 1 000 mg/l in ethyl acetate
6.6.1 General
6.6.2 Intermediate solution of phthalates at 50 mg/l in ethyl acetate
6.6.3 Calibration standard solutions of phthalates in isooctane
6.6.4 Individual solutions of phthalates in ethyl acetate à 1 mg/l for determination of GC retention times
7 Sampling
10 8 Preparation of the test sample of water extract
9 Preparation of the test sample of the organic solvent extract
10 Preparation of the test sample of the MPPO Extract
11 Procedure
11.1 GC conditions
11.1.1 Example of gas chromatographic conditions
11 11.1.2 MS conditions
11.2 Calibration
11.3 Analysis of test samples
12 12 Expression of results
12.1 For organic solvent extract: Expression of results
12.2 For MPPO extract: Expression of results
13 Test report
13 14 Precision data
Table 2 — Precision data
14 Annex A (informative) GC-MS total ion chromatogram of a standard calibration solution of 2 mg/l of phthalates
Figure A.1 — GC-MS Total Ion Chromatogram of a standard calibration solution at 2 mg/l of phthalates

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BS EN 16453:2014
$102.76