SIST EN 16453:2014

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
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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

General Information

• Status: Published
• Public Enquiry End Date: 14-Oct-2012
• Publication Date: 13-Feb-2014
• ICS: 67.250 - Materials and articles in contact with foodstuffs
• ICS: 85.060 - Paper and board
• Technical Committee: VPK - Pulp, paper, board and products
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 30-Jan-2014
• Due Date: 06-Apr-2014
• Completion Date: 14-Feb-2014
• Ref Project: EN 16453:2014 - Pulp, paper and paperboard - Determination of phthalates in extracts from paper and paperboard

Overview

SIST EN 16453:2014 is a European Standard developed by CEN that specifies the method for determining phthalates in extracts from pulp, paper, and paperboard materials intended for food contact. This standard outlines the procedure for analyzing phthalates in water, organic solvent, and modified polyphenylene oxide (MPPO) extracts using gas chromatography coupled with mass spectrometry (GC-MS). The method targets phthalate concentrations ranging from 0.002 mg/L to 5 mg/L in water and solvent extracts, and from 0.0005 mg/dm² to 0.25 mg/dm² for MPPO migration, depending on the specific substance and blank values.

The standard ensures reliable quantification of phthalates-plasticizer compounds often subject to regulation due to health concerns-present in paper and board materials that come into direct contact with food.

Key Topics

• Scope and Application
  Applicable to paper, board, and pulp materials intended for food contact, SIST EN 16453:2014 details an analytical technique using GC-MS to detect and quantify phthalates such as diisobutyl-phthalate (DIBP), dibutyl-phthalate (DBP), and di-(2-ethylhexyl)-phthalate (DEHP).

• Sample Preparation
  The standard describes preparation methods for three types of extracts:

  • Water extract (cold or hot water, per EN 645 and EN 647)
  • Organic solvent extract (commonly isooctane, per EN 15519)
  • MPPO extract (simulant representing food contact conditions, per EN 14338)

• Analytical Procedure

  • Use of GC-MS for selective and sensitive phthalate determination.
  • Calibration with known standards including internal standards such as d4-ring-deuterated dibutyl phthalate.
  • Avoidance of phthalate contamination throughout laboratory handling, emphasizing glassware cleaning and exclusion of plastic materials.

• Quality and Precision
  Guidelines include duplicate analysis of extracts, blank controls to monitor contamination, and precision performance data to ensure result reliability.

• Materials and Apparatus
  Specifies the use of glassware (e.g., volumetric flasks, pipettes), rotary vacuum evaporators, precision balancing scales, and high-purity reagents and gases for chromatography.

Applications

• Food Safety Testing
  SIST EN 16453:2014 enables manufacturers and testing laboratories to monitor phthalate migration from paper and cardboard packaging materials, ensuring compliance with food safety regulations and minimizing health risks.

• Regulatory Compliance
  Supports compliance with EU directives and national regulations governing materials in contact with food, helping to verify that packaging does not exceed authorized phthalate limits.

• Quality Control in Manufacturing
  The method assists producers of paper and board materials to control and optimize production processes by monitoring phthalate content at various stages.

• Research and Development
  Facilitates development of new packaging materials by providing a standardized approach for phthalate quantification, useful in material safety assessments and migration studies.

Related Standards

• EN 645 & EN 647
  Methods for preparation of cold and hot water extracts from paper and board to simulate food contact conditions.

• EN 15519
  Specifies preparation of organic solvent extracts for testing substances migrating from paper and paperboard.

• EN 14338
  Outlines conditions for determining migration from paper and board using MPPO as a food simulant.

• EN ISO 18856
  Provides the protocol for determining selected phthalates in water using GC-MS, referenced for phthalate quantification.

• EN ISO 536 & EN ISO 638
  Standards for determining grammage and dry matter content in paper and board, supporting sample characterization.

Keywords

Phthalates determination, paper and paperboard, food contact materials, gas chromatography mass spectrometry, GC-MS, MPPO extract, organic solvent extract, water extract, migration testing, packaging safety, food packaging compliance, European standard, CEN EN 16453.

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By adhering to SIST EN 16453:2014, laboratories activate a robust and standardized method for the accurate measurement of phthalates in materials crucial for food safety, enhancing consumer protection and regulatory adherence in the food packaging industry.

Standards Content (Sample)

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
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

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

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
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