EN 13130-4:2004
(Main)Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 4: Determination of 1,3-butadiene in plastics
Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 4: Determination of 1,3-butadiene in plastics
This part of this European Standard specifies a method for the determination of butadiene monomer in polymers.
The method is applicable to acrylonitrile-butadiene-styrene copolymer (ABS) and to high-impact polystyrene (HIPS) as well as to other 1,3-butadiene polymers and copolymers where these are soluble in N,N-dimethylacetamide or finely dispersed, swollen suspensions in N,N-dimethylacetamide. The level of 1,3-butadiene monomer determined is expressed as milligrams of 1,3-butadiene per kilogram of polymer. The method is appropriate for the quantitative determination of 1,3-butadiene at a level of 0,1 mg/kg in the polymer.
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen, die Beschränkungen unterliegen - Teil 4: Bestimmung von 1,3-Butadien in Kunststoffen
Matériaux et objets en contact avec les denrées alimentaires - Substances dans les matières plastiques soumises à des limitations - Partie 4 : Détermination du 1,3-butadiène dans les matières plastiques
La présente partie de cette Norme européenne spécifie une méthode de détermination du monomère de butadiène dans les polymères.
La méthode s'applique au copolymère d'acrylonitrile-butadiène-styrène (ABS) et au polystyrène à haute résistance au choc (HIPS) ainsi qu'aux autres polymères et copolymères de 1,3-butadiène lorsque ceux-ci sont solubles dans le N,N-diméthylacétamide ou finement dispersés et expansés en suspension, dans ce même N,N-diméthylacétamide. Le niveau du monomère de 1,3-butadiène déterminé est exprimé en milligrammes de 1,3-butadiène par kilogramme de polymère. La méthode convient au dosage quantitatif du 1,3-butadiène à un niveau de 0,1 mg/kg dans le polymère.
Materiali in predmeti v stiku z živili - Snovi v polimernih materialih, katerih koncentracija je omejena - 4. del: Določevanje 1,3-butadiena v polimernih materialih
General Information
- Status
- Published
- Publication Date
- 25-May-2004
- Withdrawal Date
- 29-Nov-2004
- Technical Committee
- CEN/TC 194 - Utensils in contact with food
- Drafting Committee
- CEN/TC 194/SC 1/WG 2 - Methods of test for monomers
- Current Stage
- 9092 - Decision on results of review/2YR ENQ - revise - Review Enquiry
- Start Date
- 10-Apr-2018
- Completion Date
- 14-Apr-2025
Relations
- Effective Date
- 22-Dec-2008
Overview
EN 13130-4:2004 - Materials and articles in contact with foodstuffs: Plastics substances subject to limitation - Part 4 specifies a validated analytical method for the determination of 1,3‑butadiene residual monomer in plastics intended to contact food. The procedure uses headspace gas chromatography (GC) with flame ionization detection (FID) after dissolving or swelling the polymer in N,N‑dimethylacetamide (DMAc). Results are reported as mg 1,3‑butadiene per kg polymer, with quantitative capability down to 0.1 mg/kg.
Key topics and technical requirements
- Scope: Applicable to ABS (acrylonitrile‑butadiene‑styrene), HIPS (high‑impact polystyrene) and other 1,3‑butadiene polymers/copolymers that dissolve or form swollen dispersions in DMAc.
- Analytical principle: Automated headspace GC‑FID of polymer in DMAc; n‑pentane used as an internal standard.
- Calibration: Standard addition to polymer samples is the primary quantification approach; external calibration (Annex A) is used if interferences affect n‑pentane.
- Confirmation: Positive results are confirmed by GC‑MS per the standard’s confirmation criteria.
- Alternative injection: If automated headspace sampling is not possible, manual injection is permitted (Annex B).
- Reagents and apparatus: High‑purity 1,3‑butadiene standard, DMAc free of interfering peaks, purified nitrogen, and GC columns suitable to separate DMAc, n‑pentane and 1,3‑butadiene.
- Sample prep and reference solutions: Procedures for preparing stock and working standards in DMAc are specified; stock solutions can be stored at −20 °C (up to 8 weeks) or 4 °C (up to 1 week) with light exclusion.
- Performance characteristics: The method was validated in a collaborative trial (ABS) and includes instructions on calculation, repeatability/reproducibility and detection limit assessment.
Practical applications
- Routine laboratory testing of food contact plastics to demonstrate compliance with regulatory limits for residual 1,3‑butadiene.
- Quality control during polymer manufacture or compounding to monitor monomer residues in ABS, HIPS and related copolymers.
- Supporting migration and safety assessments required by EU food contact legislation and conformity files.
- Use in testing programs for suppliers, brand owners, testing laboratories and regulatory bodies concerned with monomer residuals and consumer safety.
Who should use this standard
- Analytical chemists in food‑contact materials laboratories
- Polymer quality/control engineers and R&D teams
- Regulatory compliance officers and conformity assessors
- Third‑party testing and certification bodies
Related standards
- EN 13130‑1:2004 - Guide to test methods and selection of exposure conditions (referenced for preparatory procedures).
- Other EN 13130 parts cover related monomers and migration methods (e.g., Parts 3, 15) for comprehensive plastics testing and regulatory support.
Keywords: EN 13130-4:2004, 1,3-butadiene, headspace GC, food contact plastics, ABS, HIPS, DMAc, n‑pentane, GC‑MS, analytical method, residual monomer.
Frequently Asked Questions
EN 13130-4:2004 is a standard published by the European Committee for Standardization (CEN). Its full title is "Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 4: Determination of 1,3-butadiene in plastics". This standard covers: This part of this European Standard specifies a method for the determination of butadiene monomer in polymers. The method is applicable to acrylonitrile-butadiene-styrene copolymer (ABS) and to high-impact polystyrene (HIPS) as well as to other 1,3-butadiene polymers and copolymers where these are soluble in N,N-dimethylacetamide or finely dispersed, swollen suspensions in N,N-dimethylacetamide. The level of 1,3-butadiene monomer determined is expressed as milligrams of 1,3-butadiene per kilogram of polymer. The method is appropriate for the quantitative determination of 1,3-butadiene at a level of 0,1 mg/kg in the polymer.
This part of this European Standard specifies a method for the determination of butadiene monomer in polymers. The method is applicable to acrylonitrile-butadiene-styrene copolymer (ABS) and to high-impact polystyrene (HIPS) as well as to other 1,3-butadiene polymers and copolymers where these are soluble in N,N-dimethylacetamide or finely dispersed, swollen suspensions in N,N-dimethylacetamide. The level of 1,3-butadiene monomer determined is expressed as milligrams of 1,3-butadiene per kilogram of polymer. The method is appropriate for the quantitative determination of 1,3-butadiene at a level of 0,1 mg/kg in the polymer.
EN 13130-4:2004 is classified under the following ICS (International Classification for Standards) categories: 67.250 - Materials and articles in contact with foodstuffs. The ICS classification helps identify the subject area and facilitates finding related standards.
EN 13130-4:2004 has the following relationships with other standards: It is inter standard links to ENV 13130-4:1999. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
EN 13130-4:2004 is associated with the following European legislation: EU Directives/Regulations: 89/109/EEC; Standardization Mandates: M/052. When a standard is cited in the Official Journal of the European Union, products manufactured in conformity with it benefit from a presumption of conformity with the essential requirements of the corresponding EU directive or regulation.
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.OLPHUQLKPDWHULDOLKWerkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen, die Beschränkungen unterliegen - Teil 4: Bestimmung von 1,3-Butadien in KunststoffenMatériaux et objets en contact avec les denrées alimentaires - Substances dans les matieres plastiques soumises a des limitations - Partie 4 : Détermination du 1,3-butadiene dans les matieres plastiquesMaterials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 4: Determination of 1,3-butadiene in plastics67.250Materiali in predmeti v stiku z živiliMaterials and articles in contact with foodstuffsICS:Ta slovenski standard je istoveten z:EN 13130-4:2004SIST EN 13130-4:2004en,fr,de01-september-2004SIST EN 13130-4:2004SLOVENSKI
STANDARDSIST ENV 13130-4:20001DGRPHãþD
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13130-4May 2004ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 4: Determination of 1,3-butadiene in plasticsMatériaux et objets en contact avec les denréesalimentaires - Substances dans les matières plastiquessoumises à des limitations - Partie 4 : Détermination du1,3-butadiène dans les matières plastiquesWerkstoffe und Gegenstände in Kontakt mit Lebensmitteln- Substanzen in Kunststoffen, die Beschränkungenunterliegen - Teil 4: Bestimmung von 1,3-Butadien inKunststoffenThis European Standard was approved by CEN on 24 March 2004.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2004 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 13130-4:2004: ESIST EN 13130-4:2004
Calibration via external standardization.13 A.1 General.13 A.2 Construction of the calibration graph.13 A.3 Graphical determination.14 A.4 Calculation from the regression parameters.14 Annex B (normative)
Manual sample injection.16 Bibliography.17
EN 13130 are as follows. Part 1: Guide to test methods for the specific migration of substances from plastics to foods and food simulants and the determination of substances in plastics and the selection of conditions of exposure to food simulants Part 2: Determination of terephthalic acid in food simulants Part 3: Determination of acrylonitrile in food and food simulants Part 5: Determination of vinylidene chloride in food simulants Part 6: Determination of vinylidene chloride in plastics Part 7: Determination of monoethylene glycol and diethylene glycol in food simulants Part 8: Determination of isocyanates in plastics Part 9: Determination of acetic acid, vinyl ester in food simulants Part 10: Determination of acrylamide in food simulants
Part 11: Determination of 11-aminoundecanoic acid in food simulants
Part 12: Determination of 1,3-benzenedimethanamine in food simulants Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulants
Part 14: Determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indoline in food simulants SIST EN 13130-4:2004
Part 16: Determination of caprolactam and caprolactam salt in food simulants Part 17: Determination of carbonyl chloride in plastics
Part 18: Determination of 1,2-dihydroxybenzene, 1,3- dihydroxybenzene, 1,4- dihydroxybenzene, 4,4’-dihydroxybenzophenone and 4,4’dihydroxybiphenyl in food simulants Part 19: Determination of dimethylaminoethanol in food simulants Part 20:
Determination of epichlorohydrin in plastics Part 21:
Determination of ethylenediamine and hexamethylenediamine in food simulants Part 22:
Determination of ethylene oxide and propylene oxide in plastics Part 23:
Determination of formaldehyde and hexamethylenetetramine in food simulants Part 24:
Determination of maleic acid and maleic anhydride in food simulants Part 25: Determination of 4-methyl-pentene in food simulants Part 26: Determination of 1-octene and tetrahydrofuran in food simulants Part 27:
Determination of 2,4,6-triamino-1,3,5-triazine in food simulants Part 28:
Determination of 1,1,1-trimethylopropane in food simulants
Parts 1 to 8 are European Standards.
Parts 9 to 28 are Technical Specifications, prepared within the Standards, Measurement and Testing project, MAT1-CT92-0006, “Development of Methods of Analysis for Monomers”. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. SIST EN 13130-4:2004
During the manufacture of 1,3-butadiene copolymers, residual 1,3-butadiene monomer can remain in the polymer and can migrate into food coming into contact with the polymer.
The method described in this part of this standard is to be used in conjunction with part 1 of this standard, which describes the procedure required prior to determination of 1,3-butadiene.
The method has been validated by a collaborative trial using acrylonitrile-butadiene-styrene copolymer (ABS).
1 Scope This part of this European Standard specifies a method for the determination of butadiene monomer in polymers.
The method is applicable to acrylonitrile-butadiene-styrene copolymer (ABS) and to high-impact polystyrene (HIPS) as well as to other 1,3-butadiene polymers and copolymers where these are soluble in N,N-dimethylacetamide or finely dispersed, swollen suspensions in N,N-dimethylacetamide. The level of 1,3-butadiene monomer determined is expressed as milligrams of 1,3-butadiene per kilogram of polymer.
The method is appropriate for the quantitative determination of 1,3-butadiene at a level of 0,1 mg/kg in the polymer. 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text, and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies (including amendments).
EN 13130-1:2004; Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 1: Guide to test methods for the specific migration of substances from plastics to foods and food simulants and the determination of substances in plastics and the selection of conditions of exposure to food simulants 3 Principle The level of 1,3-butadiene in a polymer is determined by headspace gas chromatography of the polymer sample dissolved in N,N-dimethylacetamide, applying automated sample injection and using flame ionization detection (FID).
Quantification is achieved using n-pentane as an internal standard with calibration against polymer samples fortified with 1,3-butadiene according to the standard addition procedure.
If interferences are experienced with the internal standard, n-pentane, calibration is carried out by the external standardization as described in annex A.
If automated headspace sampling cannot be performed, manual injection as described in annex B shall be applied.
Confirmation of 1,3-butadiene levels is carried out by combined gas chromatography/mass spectrometry (GC/MS).
4 Reagents WARNING:
All chemicals are hazardous to health to a greater or lesser extent.
It is beyond the scope of this standard to give instructions for the safe handling of all chemicals, that meet, in full, the legal obligations in all countries in which this standard may be followed.
Therefore, specific warnings are not given and users of this standard shall ensure that they meet all the necessary safety requirements in their own country. 4.1 1,3-Butadiene, CH2=CH-CH=CH2, purity greater than 99,5 % (w/w). SIST EN 13130-4:2004
retention time as 1,3-butadiene. 4.3 N,N-Dimethylacetamide, CH3-CO-N(CH3)2, dT = 0,9600 - 0,00094 × T where T is the temperature in °C. The N,N-dimethylacetamide shall be free of any interferences (< 1 %) which elute at the same retention times as 1,3-butadiene and n-pentane peaks. 4.4 Prepare stock solutions of 1,3-butadiene in N,N-dimethylacetamide with defined concentrations in the range 5 mg/g to 10 mg/g as follows: a) Weigh a 50 ml sample vial (5.4) including septum and cap to an accuracy of 0,01 mg. Pipette 50 ml N,N-dimethylacetamide (4.3) into the vial (5.4), close and weigh again to 0,01 mg. Insert hollow needles for introducing 1,3-butadiene and venting air and weigh again to 0,01 mg. Introduce, under a fume hood, 0,3 g to 0,5 g 1,3-butadiene (4.1) by bubbling through the N,N-dimethylacetamide.
Re-weigh the vial plus needles to an accuracy of 0,01 mg and remove then the needles. Calculate the concentration in milligrams of 1,3-butadiene per gram of solution.
b) Repeat item a) to provide a second stock solution. NOTE The stock solutions can be stored at - 20 °C up to eight weeks protected from light in septum capped glass vials with minimum headspace; storage at 4 °C with the exclusion of light should not exceed
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