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

This European Standard specifies a 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 chromatography coupled to mass spectrometry (GC-MS).
This method is applicable to the determination of phthalates in concentration ranging from 0,002 mg/L to 5 mg/L for water and solvent extracts and 0,0005 mg/dm² to 0,25 mg/dm² for MPPO migration depending on the individual substance and the value of the blank.

Zellstoff, Papier und Karton - Bestimmung von Phthalaten in Papier- und Kartonextrakten

Diese Europäische Norm beschreibt ein analytisches Prüfverfahren zur Bestimmung von Phthalaten aus Wasser-, Lösemittel- und modifizierten Polyphenylenoxid (MPPO)-Extrakten von Lebensmittel-kontaktmaterialien aus Papier und Pappe unter Verwendung von Gaschromatographie mit gekoppelter massenselektiver Detektion (GC-MS).
Dieses Verfahren dient der Bestimmung von Phthalaten in Konzentrationsbereichen von 0,025 mg/l bis 0,5 mg/l für Wasser- und Lösemittelextrakte und 0,002 mg/dm2 bis 0,040 mg/dm2 bei der Bestimmung der Migration auf MPPO. Die erreichbaren Bestimmungsgrenzen sind abhängig vom jeweils zu bestimmenden Analyten, dem für die Analyse festgelegten Volumen und vom Wert der Blindprobe.
Tabelle 1 - Phthalate, die mit diesem Verfahren bestimmt werden
[...]

Pâtes, papier et carton - Dosage des phtalates dans des extraits de papier et carton

La présente Norme européenne spécifie une méthode d'analyse permettant de déterminer la teneur en phtalates d'extraits aqueux, au solvant et à l'oxyde de polyphénylène modifié (MPPO) de papier, carton et articles destinés à être mis en contact avec des denrées alimentaires, par une méthode de chromatographie en phase gazeuse couplée à de la spectrométrie de masse (CG-SM).
Cette méthode est applicable au dosage des phtalates de concentration comprise entre 0,025 mg/l et 0,5 mg/l pour les extraits aqueux et les extraits au solvant, et entre 0,002 mg/dm² et 0,040 mg/dm² pour les MPPO, la migration étant fonction de la substance considérée, du volume utilisé pour l'analyse et de la valeur du blanc.

Vlaknine, papir, karton in lepenka - Ugotavljanje ftalatov v ekstraktih papirja, kartona in lepenke

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Status
Published
Publication Date
28-Jan-2014
Current Stage
9093 - Decision to confirm - Review Enquiry
Completion Date
17-Jan-2020

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Vlaknine, papir, karton in lepenka - Ugotavljanje ftalatov v ekstraktih papirja, kartona in lepenkeZellstoff, Papier und Karton - Bestimmung von Phthalaten in Papier- und KartonextraktenPâtes, papier et carton - Dosage des phtalates dans des extraits de papier et cartonPulp, paper and paperboard - Determination of phthalates in extracts from paper and paperboard85.060Papir, karton in lepenkaPaper and board67.250Materiali in predmeti v stiku z živiliMaterials and articles in contact with foodstuffsICS:Ta slovenski standard je istoveten z:EN 16453:2014SIST EN 16453:2014en,fr,de01-marec-2014SIST EN 16453:2014SLOVENSKI

STANDARD
SIST EN 16453:2014
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16453
January 2014 ICS 67.250; 85.060 English Version

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

Pâtes, papier et carton - Dosage des phtalates dans des extraits de papier et carton

Zellstoff, Papier und Karton - Bestimmung von Phthalaten in Papier- und Kartonextrakten This European Standard was approved by CEN on 9 November 2013.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,

B-1000 Brussels © 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16453:2014 ESIST EN 16453:2014

EN 16453:2014 (E) 2 Contents Page Foreword ..............................................................................................................................................................3 1 Scope ......................................................................................................................................................4 2 Normative references ............................................................................................................................4 3 Principle ..................................................................................................................................................5 3.1 General ....................................................................................................................................................5 3.2 Interferences ..........................................................................................................................................5 4 Materials .................................................................................................................................................5 4.1 General ....................................................................................................................................................5 4.2 Pasteur pipettes .....................................................................................................................................6 4.3 Double mark glass pipette of 0,05 ml, 0,2 ml, 0,5 ml, 1 ml, 5 ml and 10 ml .....................................6 4.4 Volumetric flasks of 5 ml, 10 ml, 50 ml and 100 ml ............................................................................6 4.5 Screw-cap glass bottle PYREX of 250 ml with a Polytetrafluorethylene-septa cap .......................6 4.6 Graduated cylinder of 200 ml ...............................................................................................................6 4.7 Round flask of 50 ml and 250 ml ..........................................................................................................6 4.8 Glass funnel ...........................................................................................................................................6 4.9 Polytetrafluorethylene-screw-cap glass vial single use (capacity adapted to the volume of concentrate) ...........................................................................................................................................6 5 Apparatus ...............................................................................................................................................6 5.1 Balance: capable of accurately weighing 0,000 1 g ...........................................................................6 5.2 Round flask heater.................................................................................................................................6 5.3 Rotary vacuum evaporator ...................................................................................................................6 5.4 Gas chromatograph coupled to a mass spectrometer (GC-MS) .......................................................6 6 Reagents .................................................................................................................................................6 6.1 General ....................................................................................................................................................6 6.2 Operating gases for gas chromatography/mass spectrometry, of high purity and in accordance with manufacturer's specifications.................................................................................6 6.3 Ethyl acetate, C4H8O2, CAS N° 141-78-6 ............................................................................................6 6.4 Isooctane, C8H18, CAS N° 540-84-1 .....................................................................................................6 6.5 Internal standard stock solution: For example d4-ring-deuterated-dibutyl phthalate (D4-ring-DBP) at 10 g/l ..................................................................................................................................6 6.6 Stock solutions of individual phthalate at 1 000 mg/l in ethyl acetate .............................................7 7 Sampling .................................................................................................................................................7 8 Preparation of the test sample of water extract .................................................................................8 9 Preparation of the test sample of the organic solvent extract ..........................................................8 10 Preparation of the test sample of the MPPO Extract .........................................................................8 11 Procedure ...............................................................................................................................................8 11.1 GC conditions ........................................................................................................................................8 11.2 Calibration ..............................................................................................................................................9 11.3 Analysis of test samples .......................................................................................................................9 12 Expression of results ......................................................................................................................... 10 12.1 For organic solvent extract: Expression of results......................................................................... 10 12.2 For MPPO extract: Expression of results ......................................................................................... 10 13 Test report ........................................................................................................................................... 10 14 Precision data ..................................................................................................................................... 11 Annex A (informative)

GC-MS total ion chromatogram of a standard calibration solution of 2 mg/l of phthalates ........................................................................................................................................ 12 SIST EN 16453:2014

EN 16453:2014 (E) 3 Foreword This document (EN 16453:2014) has been prepared by Technical Committee CEN/TC 172 “Pulp, paper and board”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by July 2014, and conflicting national standards shall be withdrawn at the latest by July 2014. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 16453:2014

EN 16453:2014 (E) 4 1 Scope 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 chromatography 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. Table 1 — Phthlates determined by this method Name Abbreviation Formula CAS N° Structure Diisobutyl-phthalate DIBP C16H22O4 84–69–5

Dibutyl-phthalate DBP C16H22O4 84–74–2
Di-(-ethylhexyl)-phthalate DEHP C24H38O4 117–81–7

2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 645, Paper and board intended to come into contact with foodstuffs - Preparation of a cold water extract EN 647, Paper and board intended to come into contact with foodstuffs - Preparation of a hot water extract EN 14338, Paper and board intended to come into contact with foodstuffs - Conditions for determination of migration from paper and board using modified polyphenylene oxide (MPPO) as a simulant EN 15519, Paper and board intended to come into contact with foodstuffs - Preparation of an organic solvent extract EN 27213, Pulps - Sampling for testing (ISO 7213) EN ISO 186, Paper and board - Sampling to determine average quality (ISO 186) EN ISO 536, Paper and board - Determination of grammage (ISO 536) EN ISO 638, Paper, board and pulps - Determination of dry matter content - Oven-drying method (ISO 638) SIST EN 16453:2014

EN 16453:2014 (E) 5 EN ISO 18856, Water quality - Determination of selected phthalates using gas chromatography/mass spectrometry (ISO 18856) 3 Principle 3.1 General Phthalates in the test extract from paper and board materials are determined by gas chromatography / mass spectrometry. The test extract is prepared from water, organic solvent and/or MPPO simulant according to respectively: EN 645, EN 647, EN 15519, EN 14338. Other phthalates, as listed in Table 1, may also be analysed by this procedure but it is necessary to determine its applicability in each case. 3.2 Interferences Due to their use as plasticizer agents, phthalates are ubiquitous. Therefore, pay special attention to avoi

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