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BS EN 16453:2014 Pulp, paper and paperboard. Determination of phthalates in extracts from paper and paperboard, 2014
- Contents Page
- Foreword
- 1 Scope
- Table 1 — Phthlates determined by this method
- 2 Normative references
- 3 Principle [Go to Page]
- 3.1 General
- 3.2 Interferences
- 4 Materials [Go to Page]
- 4.1 General
- 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 [Go to Page]
- 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 [Go to Page]
- 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 [Go to Page]
- 6.5.1 General
- 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 [Go to Page]
- 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
- 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 [Go to Page]
- 11.1 GC conditions [Go to Page]
- 11.1.1 Example of gas chromatographic conditions
- 11.1.2 MS conditions
- 11.2 Calibration
- 11.3 Analysis of test samples
- 12 Expression of results [Go to Page]
- 12.1 For organic solvent extract: Expression of results
- 12.2 For MPPO extract: Expression of results
- 13 Test report
- 14 Precision data
- Table 2 — Precision data
- 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 [Go to Page]