SIST EN 13130-3:2004
(Main)Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 3: Determination of acrylonitrile in food and food simulants
Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 3: Determination of acrylonitrile in food and food simulants
This part of this European Standard specifies a method for the determination of acrylonitrile monomer in foods and food simulants. The method is applicable to aqueous food simulants, to the fatty food simulant olive oil and other fatty food simulants, simulants D, e.g. a mixture of synthetic triglycerides or sunflower oil or corn oil, as well as to liquid and solid foodstuffs such as beverages and soft margarine. The level of acrylonitrile monomer determined is expressed as milligrammes of acrylonitrile per kilogram of food or food simulant.
The method is appropriate for the quantitative determination of acrylonitrile monomer at minimum levels of down to 0,01 mg/kg to 0,005 mg/kg, or lower, in food simulant, depending on the applied test conditions (see NOTE in 8.2.3). With regard to the performance in the mentioned foodstuffs, in general, a direct detection limit of 0,02 mg/kg is achievable.
NOTE This method was developed for the determination of acrylonitrile in 15 % v/v aqueous ethanol, as required by the regulations in force at the time the development work was carried out. However, this method, developed for 15 (v/v) aqueous ethanol, should be applicable to the determination in 10 (v/v) aqueous ethanol.
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen, die Beschränkungen unterliegen - Teil 3: Bestimmung von Acrylnitril in Lebensmitteln und Prüflebensmitteln
Matériaux et objets en contact avec des denrées alimentaires - Substances dans les matieres plastiques soumises a des limitations - Partie 3 : Détermination de l'acrylonitrile dans les aliments et les simulants d'aliments
Cette partie de la présente norme spécifie une méthode de détermination du monomere d'acrylonitrile dans les denrées alimentaires et les simulants d'aliments. La méthode s'applique aux simulants d'aliments aqueux, a l'huile d'olive et a d'autres simulants d'aliments gras, aux simulants D, par exemple un mélange de triglycérides synthétiques ou de l'huile de tournesol ou de mais, ainsi qu'aux denrées alimentaires liquides et solides telles que les boissons et les margarines molles. La quantité de monomere d'acrylonitrile déterminée est exprimée en milligrammes d'acrylonitrile par kilogramme de denrée ou de simulant d'aliments.
La méthode convient a la détermination quantitative dans les simulants d'aliments du monomere d'acrylonitrile a des quantités minimales comprises entre 0,01 mg/kg et 0,05 mg/kg, ou inférieures, selon les conditions dans lesquelles s'est déroulé l'essai (voir la note en 8.2.3). Pour ce qui est des performances des denrées alimentaires mentionnées, une limite de détection directe de 0,02 mg/kg est en général acceptable.
NOTE Cette méthode a été élaborée pour déterminer la quantité d'acrylonitrile dans de l'éthanol aqueux a 15 % v/v, comme exigé par les réglementations en vigueur au moment ou le travail de mise au point a été effectué. Cependant, cette méthode, élaborée pour de l'éthanol aqueux a 15 % (v/v), devrait pouvoir s'appliquer a la détermination dans de l'éthanol aqueux a 10 % (v/v).
Materiali in predmeti v stiku z živili - Snovi v polimernih materialih, katerih koncentracija je omejena - 3. del: Določevanje akrilonitrila v živilih in modelnih raztopinah za živila
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen, die Beschränkungen unterliegen - Teil 3: Bestimmung von Acrylnitril in Lebensmitteln und PrüflebensmittelnMatériaux et objets en contact avec des denrées alimentaires - Substances dans les matieres plastiques soumises a des limitations - Partie 3 : Détermination de l'acrylonitrile dans les aliments et les simulants d'alimentsMaterials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 3: Determination of acrylonitrile in food and food simulants67.250Materiali in predmeti v stiku z živiliMaterials and articles in contact with foodstuffsICS:Ta slovenski standard je istoveten z:EN 13130-3:2004SIST EN 13130-3:2004en,fr,de01-september-2004SIST EN 13130-3:2004SLOVENSKI
STANDARDSIST ENV 13130-3:20001DGRPHãþD
SIST EN 13130-3:2004
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13130-3May 2004ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 3: Determination ofacrylonitrile in food and food simulantsMatériaux et objets en contact avec des denréesalimentaires - Substances dans les matières plastiquessoumises à des limitations - Partie 3 : Détermination del'acrylonitrile dans les aliments et les simulants d'alimentsWerkstoffe und Gegenstände in Kontakt mit Lebensmitteln- Substanzen in Kunststoffen, die Beschränkungenunterliegen - Teil 3: Bestimmung von Acrylnitril inLebensmitteln und PrüflebensmittelnThis 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 13130-3:2004: ESIST EN 13130-3:2004
EN 13130-3:2004 (E) 2 Contents
page Foreword.3 1 Scope.6 2 Normative references.6 3 Principle.6 4 Reagents.6 5 Apparatus.7 6 Samples.8 6.1 Laboratory samples.8 6.2 Test sample preparation.8 7 Procedure.9 7.1 GC preparation.9 7.2 Performance of GC measurements.10 8 Expression of results.10 8.1 General.10 8.2 Method of calculation.10 8.3 Precision data and detection limit.12 9 Confirmation.12 9.1 Requirement for confirmation.12 9.2 Confirmation by combined gas chromatography-mass spectrometry.12 9.3 Confirmation by re-analysis on a GC column of different polarity.13 10 Test report.13 Annex A (normative)
Method of standard addition.14 Annex B (normative)
Calibration via external standardization.16 Annex C (normative)
Manual sample injection.17 Bibliography.18
SIST EN 13130-3:2004
EN 13130-3:2004 (E) 3 Foreword This document (EN 13130-3:2004) has been prepared by Technical Committee CEN/TC 194 “Utensils in contact with food”, the secretariat of which is held by BSI. This document was prepared by Subcommittee SC1 of TC 194 as one of a series of analytical test methods for plastics materials and articles in contact with foodstuffs. 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 November 2004, and conflicting national standards shall be withdrawn at the latest by November 2004. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association.
This standard is intended to support Directives 2002/72/EC [1], 89/109/EEC [2], 82/711/EEC [3] and its amendments 93/8/EEC [4] and 97/48/EC [5], and 85/572/EEC [6]. At the time of preparation and publication of this part of EN 13130 the European Union legislation relating to plastics materials and articles intended to come into contact with foodstuffs is incomplete. Further Directives and amendments to existing Directives are expected which could change the legislative requirements which this standard supports. It is therefore strongly recommended that users of this standard refer to the latest relevant published Directive(s) before commencement of a test or tests described in this standard.
EN 13130-3 should be read in conjunction with EN 13130-1 Further parts of EN 13130, under the general title Materials and articles in contact with foodstuffs - Plastics substances subject to limitation, have been prepared, and others are in preparation, concerned with the determination of specific migration from plastics materials into foodstuffs and food simulants and the determination of specific monomers and additives in plastics. The other parts of
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 4: Determination of 1,3-butadiene in plastics
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 13130-3:2004
EN 13130-3:2004 (E) 4
Part 15: Determination of 1,3-butadiene in food simulants
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 13130-3:2004
EN 13130-3:2004 (E) 5 Introduction Acrylonitrile, CH2=CH-CN, is a monomer used in the manufacture of certain plastics materials and articles intended to come into contact with foodstuffs.
During the manufacture of acrylonitrile copolymers, residual acrylonitrile monomer can remain in the polymer and can migrate into food coming into contact with the polymer. The method described in this part of the standard should be used in conjunction with part 1 of this standard which describes the procedures required prior to the determination of acrylonitrile. The method has been validated by collaborative trial using fruit juice, wine and sunflower oil. SIST EN 13130-3:2004
EN 13130-3:2004 (E) 6
1 Scope This part of this European Standard specifies a method for the determination of acrylonitrile monomer in foods and food simulants. The method is applicable to aqueous food simulants, to the fatty food simulant olive oil and other fatty food simulants, simulants D, e.g. a mixture of synthetic triglycerides or sunflower oil or corn oil, as well as to liquid and solid foodstuffs such as beverages and soft margarine.
The level of acrylonitrile monomer determined is expressed as milligrammes of acrylonitrile per kilogram of food or food simulant. The method is appropriate for the quantitative determination of acrylonitrile monomer at minimum levels of down to 0,01 mg/kg to 0,005 mg/kg, or lower, in food simulant, depending on the applied test conditions (see NOTE in 8.2.3).
With regard to the performance in the mentioned foodstuffs, in general, a direct detection limit of 0,02 mg/kg is achievable. NOTE This method was developed for the determination of acrylonitrile in 15 % v/v aqueous ethanol, as required by the regulations in force at the time the development work was carried out.
However, this method, developed for 15 (v/v) aqueous ethanol, should be applicable to the determination in 10 (v/v) aqueous ethanol. 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 acrylonitrile (AN) in a food, or a food simulant, is determined by headspace gas chromatography with automated sample injection, using nitrogen specific detection.
Quantification is achieved using propionitrile (PN) as an internal standard with calibration against blank samples fortified with acrylonitrile.
If blank samples cannot be obtained then the method of standard addition described in annex A is employed.
If interferences are experienced with the internal standard then calibration is carried out by external standardization as described in annex B. If automated headspace sampling cannot be performed, manual injection as described in annex C shall be applied.
Confirmation of acrylonitrile levels is carried out either by combined gas chromatography/mass spectrometry (GC/MS) or by re-analysis on a second GC column of different polarity. 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 SIST EN 13130-3:2004
EN 13130-3:2004 (E) 7 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 Acrylonitrile, CH2=CH-CN, purity greater than 99% (w/w). 4.2 Propionitrile, CH3-CH2-CN, containing no impurity at > 1 % by area which will elute at the same GC retention time as acrylonitrile.
4.3 Propylene carbonate, CH3-CH-OCOO-CH2, boiling point 240 °C to 243 °C at normal pressure, free of any interferences (< 1 % area) with the acrylonitrile and propionitrile peaks. 4.4 Nitrogen, purified to 99,9999 %. 4.5 Standard solutions of acrylonitrile in propylene carbonate with defined concentrations in the range 25 µg/ml to 25 µg/ml, prepared as described in 4.5.1 and 4.5.2. 4.5.1 Prepare concentrated standard acrylonitrile solutions at approximately 12,5 mg/ml as follows: a) Fill a 100 ml volumetric flask with 50 ml propylene carbonate (4.3), close and weigh to an accuracy of 0,2 mg.
Add to the propylene carbonate a quantity of approximately 1,5 ml (1,25 g) acrylonitrile (4.1) and shake the closed flask.
Determine the exact mass of acrylonitrile added by re-weighing to an accuracy of 0,2 mg.
Fill the flask to the 100 ml mark.
b) Repeat item a) to provide a second concentrated standard solution. 4.5.2 Prepare dilute standard acrylonitrile solutions as follows: a) With an accuracy of 0,1 ml throughout, dilute one of the solutions prepared in 4.5.1 by a factor of 100 in two steps, taking for each step 10 ml acrylonitrile solution and 90 ml propylene carbonate, to give an intermediate standard solution of approximately 125 µg acrylonitrile per millilitre.
Place 48 ml or 45 ml or 40 ml of propylene carbonate into three 55 ml glass vials and add 2 ml or 5 ml or 10 ml of the intermediate standard solution, respectively.
Close the vials with a polytetrafluoroethylene (PTFE) seal and cap and shake thoroughly.
b) Repeat item a) using the second solution prepared in 4.5.1 to provide a second set of three dilute standard acrylonitrile solutions. NOTE The standard solutions with known acrylonitrile concentrations of approximately 5 µg/ml, 12,5 µg/ml and 25 µg/ml, respectively, can be stored at 4 °C for up to four weeks. 4.6 Dilute standard propionitrile solution in propylene carbonate, with a known concentration of approximately 25 µg/ml of propionitrile (4.2) prepared by following an analogous procedure to that described in 4.5. 5 Apparatus NOTE An instrument or item of apparatus is listed only where it is special, or made to a particular specification, usual laboratory equipment being assumed to be available. 5.1 Gas-chromatograph, equipped with a nitrogen specific detector and fitted with an automatic headspace sampler. 5.2 Gas-chromatographic column, capable of the separation of propylene carbonate from acrylonitrile and propionitrile such that the peaks of acrylonitrile and propionitrile do not overlap by more than 1 % peak area with other compounds. NOTE The following are examples of GC columns known to be suitable for acrylonitrile analysis: SIST EN 13130-3:2004
EN 13130-3:2004 (E) 8 a) 2 m x 3 mm internal diameter stainless steel column packed with 15 % polyethylene glycol 1500 on 60 mesh to 100 mesh diatomite support; b) 1,8 m x 2 mm internal diameter stainless steel column packed with 0,2 % polyethyleneglycol 1500 on 80 mesh to 100 mesh graphitized carbon black USP (S7) solid support; c) 3 m x 2 mm internal diameter glass column packed with 20 % polyethylene glycol 20 on 60 mesh to 80 mesh flux-calcined diatomite support; d) 25 m x 0,32 mm internal diameter, fused silica capillary column with 1,2 µm film thickness of 100 % dimethylpolysiloxane; e) 12 m x 0,20 mm internal diameter, fused silica capillary column with 0,33 µm film thickness of free fatty acid phase (modified polyethylene glycol). 5.3 Sample vials, 25 ml, or of another size suitable for the particular autosampler employed, with butyl rubber septa and crimp-closures. NOTE The butyl rubber septa should not give rise to acrylonitrile or interference peaks and in some circumstances PTFE-faced septa are preferred. 5.4 Microsyringes, of 50 µl capacity and syringes, of 5 ml capacity. 6 Samples 6.1 Laboratory samples The laboratory samples of food, or food simulant, to be analysed are obtained as described in EN 13130-1.
Acrylonitrile-free samples of the same type as those to be analysed are also required for use for calibration purposes.
Keep the samples refrigerated at 4 °C in closed containers with the exclusion of light. NOTE Acrylonitrile losses are unlikely during sampling, losses during transport and short-term storage for up to 4 weeks are unlikely. 6.2 Test sample preparation 6.2.1 General NOTE Since the determination of acrylonitrile in food or food simulant is performed close to the detection limit of the method, extreme care should be taken with respect to possible adventitious contamination during preparation of the test samples. The following precautions are advisable: a)
purge the empty sample vials (5.3) with purified nitrogen before filling with food or food simulant; b)
to avoid cross-contami
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