EN ISO 4614:1999

Plastics - Melamine-formaldehyde mouldings - Determination of extractable formaldehyde (ISO 4614:1977)

Liquids simulating fodd and beverages are placed in contact with mouldings of the sample material, under defined conditions. The formaldehyde content of the liquid is then determined and the quantity of formaldehyde extracted per unit area of content is calculated. Two spectrophotometric methods for the determination of formaldehyde in the liquid, using chromotropic acid disodium salt or acetylacetone as reagents, are given.

Kunststoffe - Formteile aus Melamin-Formaldehyd-Harz - Bestimmung des extrahierbaren Formaldehyds (ISO 4614:1977)

Diese Internationale Norm legt ein Verfahren zur Bestimmung des extrahierbaren Formaldehyds in Formteilen aus Melamin-Formaldehyd-Harz fest, die zur Verwendung in Berührung mit Nahrungsmitteln und Getränken bestimmt sind.

Plastiques - Pièces moulées à base de résine mélamine-formaldéhyde - Détermination du formaldéhyde extractible (ISO 4614:1977)

La présente Norme internationale spécifie une méthode de détermination du formaidéhyde extractible dans les pièces moulées en matière à base de mélamine-formaldéhyde, destinées à l'usage au contact avec les denrées alimentaires et les boissons.

Polimerni materiali - Oblikovanci iz melamin-formaldehidnih smol - Določevanje formaldehida, izločenega z ekstrakcijo (ISO 4614:1977)

General Information

• Status: Published
• Publication Date: 18-May-1999
• Withdrawal Date: 29-Nov-1999
• ICS: 83.080.01 - Plastics in general
• Technical Committee: CEN/TC 249 - Plastics
• Drafting Committee: CEN/TC 249/SC 1/WG 13 - Thermosets
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 19-May-1999
• Completion Date: 19-May-1999
• Ref Project: SIST EN ISO 4614:2000 - Plastics - Melamine-formaldehyde mouldings - Determination of extractable formaldehyde (ISO 4614:1977)

Overview

EN ISO 4614:1999 is an international standard developed by CEN for the determination of extractable formaldehyde in melamine-formaldehyde plastics. This method is critical for ensuring the safety and compliance of melamine-formaldehyde mouldings, especially those intended for contact with food and beverages. The standard defines specific procedures to measure the formaldehyde released from plastic mouldings when exposed to liquids simulating food and beverages under controlled conditions.

Extractable formaldehyde content is an essential parameter in assessing the suitability of melamine-formaldehyde plastic products for the food industry. The standard provides two spectrophotometric methods using chromotropic acid disodium salt or acetylacetone as reagents for accurate quantification of formaldehyde in the extraction liquid.

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Key Topics

Scope and Purpose

• Applies to melamine-formaldehyde mouldings used in contact with food and beverages.
• Focuses on determining the formaldehyde extracted into food-simulating liquids under defined temperature and time conditions.
• Ensures that formaldehyde migration stays within safe limits for consumer health.

Extraction Procedure

• Samples (moulded containers like beakers or cups) are filled with extraction liquids such as distilled water, acetic acid solution, or ethanol solution.
• The liquids are heated to 80°C and then cooled, allowing formaldehyde to leach from the plastic sample.
• The amount of formaldehyde extracted is calculated relative to the surface area of the plastic in contact with the liquid.

Analytical Methods

The standard provides two validated methods for formaldehyde detection:

• Procedure A: Chromotropic Acid Method

  • Uses chromotropic acid disodium salt reagent.
  • Formaldehyde reacts with the reagent to form a colored complex, measured at 570 nm by a spectrophotometer.
  • Suitable for extracts with formaldehyde concentration from 1 to 10 µg/ml.

• Procedure B: Acetylacetone Method

  • Uses acetylacetone reagent in the presence of ammonium acetate and acetic acid.
  • Measures colored complex absorbance at 415 nm.
  • Suitable for formaldehyde concentrations from 0.5 to 8 µg/ml.

Calibration and Quality Control

• Both methods require preparing calibration curves from formaldehyde standards.
• All reagents used must be free of detectable formaldehyde contamination.
• Tests are normally carried out in duplicate for accuracy and reproducibility.
• Dilution steps are specified if formaldehyde concentrations exceed measurement ranges.

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Applications

• Food Contact Materials Testing: Ensures that melamine-formaldehyde mouldings used for food containers, utensils, and packaging comply with regulatory limits on formaldehyde migration.
• Quality Control in Manufacturing: Enables manufacturers to monitor and control the formaldehyde release from melamine resin products during production.
• Regulatory Compliance: Assists industries in meeting European and international regulations governing food safety related to plastics.
• Material Safety Assessment: Used by testing laboratories to evaluate the safety and chemical stability of melamine-formaldehyde plastics under simulated usage conditions.

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Related Standards

• ISO 2227: Specifies the determination of formaldehyde content in industrial formaldehyde solutions, used for calibration in EN ISO 4614.
• ISO 648: Defines the requirements for volumetric laboratory glassware used in preparation and analysis.
• ISO 1042: Specifies specifications for spectrophotometric glass cells, essential for absorbance measurements in formaldehyde determination.
• General Food Contact Materials Standards: Standards regulating testing methods for formaldehyde and other migrating substances from plastic materials.

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Keywords: EN ISO 4614, melamine-formaldehyde mouldings, formaldehyde determination, extractable formaldehyde, food contact plastics, spectrophotometric methods, chromotropic acid, acetylacetone, plastic safety testing, formaldehyde migration, CEN standards, food packaging compliance.

Standards Content (Sample)

SLOVENSKI STANDARD
01-maj-2000
3ROLPHUQLPDWHULDOL2EOLNRYDQFLL]PHODPLQIRUPDOGHKLGQLKVPRO'RORþHYDQMH
IRUPDOGHKLGDL]ORþHQHJD]HNVWUDNFLMR,62
Plastics - Melamine-formaldehyde mouldings - Determination of extractable
formaldehyde (ISO 4614:1977)
Kunststoffe - Formteile aus Melamin-Formaldehyd-Harz - Bestimmung des
extrahierbaren Formaldehyds (ISO 4614:1977)
Plastiques - Pieces moulées a base de résine mélamine-formaldéhyde - Détermination
du formaldéhyde extractible (ISO 4614:1977)
Ta slovenski standard je istoveten z: EN ISO 4614:1999
ICS:
83.080.01 Polimerni materiali na Plastics in general
splošno
83.080.10 Duromeri Thermosetting materials
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

INTERNATIONAL STANDARD
INTERNATIONAL ORGANIZATION FOR STANDARDIZATION l MEXjl(YHAPOLJHA5f OPI-AHM3AUHII no ~AHAAPTM3ALWi.ORGANISATION INTERNATIONALE DE NORMALISATION
Plastics - Melamine-formaldehyde mouldings -
Determination of extractable formaldehyde
Plastiques - Pikes moulkes ti base de rkine melamine-formalde’h yde - Determination
du formalddh yde extractible
First edition - 1977-07-01
-
LLI
-
UDC 678.652’737’21048 : 678.019
Ref. No. ISO 4614-1977 (E)
b
Descriptors : plastics, castings, melamine resins, food industry, food packaging, Chemical analysis, determination of content, formaldehyde,
extraction analysis.
Price based on 4 pages
FOREWORD
ISO (the International Orsanization for Standardization) is a worldwide federation
of national Standards institutes (ISO member bodies). The work of developing
International Standards is carried out through ISO technical committees. Every
member body interested in a subject for which a technical committee has been set
up has the right to be represented on that committee. International organizations,
governmental and non-governmental, in liaison with ISO, also take part in the work.
Draft International Standards adopted by the technical committees are circulated
to the member bodies for approval before their acceptance as International
Standards by the ISO Council.
International Standard ISO 4614 was developed by Technical Committee
ISO/TC 61, Plastics, and was circulated to the member bodies in December 1975.
lt has been approved by the member bodies of the following countries :
Australia Hungary Portugal
Austria India Romania
Belgium Iran Spain
Sweden
Brazil Ireland
Israel Switzerland
Canada
Turkey
Czechoslovakia Japan
Mexico United Kingdom
Finland
France Netherlands Yugoslavia
Poland
Germany
The member bodies of the following countries expressed disapproval of the
document on technical grounds :
U.S.A.
U.S.S.R.
0 International Organkation for Standardkation, 1977 l
Printed in Switzerland
INTERNATIONAL STANDARD ISO 46144977 (E)
Plastics - Melamine-formaldehyde mouldings -
Determination of extractable formaldehyde
6 EXTRACTION PROCEDURE
1 SCOPE AND FIELD OF APPLICATION
This International Standard specifies a method of deter- Rinse the test Container with warm distilled water and dry
mining the extractable formaldehyde in melamine-formal- thoroughly.
dehyde mouldings intended for use in contact with food
Place a suitable quantity (see 4.1) of the extraction liquid
and beverages.
(clause 5) at 80 “C into the test Container at room
temperature.
Cover the Container with a watch glass to
protect against evaporation and contamination, and allow
2 PRINCIPLE
to stand in air at room temperature for 30 min.
Certain liquids, simulating common food and beverage
constituents, are placed in contact with mouldings of the
Transfer the extract (without washing) to a 250 ml conical
Sample material, under defined conditions. The formal-
flask, stopper the flask and cool the Solution in a cold water
dehyde content of the liquid is then determined and the
bathto 20 + 0,5 “C.
quantity of formaldehyde extracted per unit area of
Immediately carry out the formaldehyde analysis by
contact with the moulding is calculated.
procedure A (7.3.2) or procedure B (8.3.2).
Two procedures for the determination of formaldehyde in
the liquid are given.
3 REFERENCE
7 DETERMINATION OF FORMALDEHYDE - PRO-
CEDURE A
ISO 2227, Formaldehyde solutions for industrial use -
Determination o f formaldeh yde con ten t.
7.1 Reagents
7.1.1 All reagents, including distilled water and extraction
4 TEST SPECIMENS
Iiquids, shall be free from formaldehyde in amounts
detectable by the method described.
4.1 Form
7.1.1.1 Water, distilled or de-ionized.
Moulded Containers, for example beakers or cups, having an
internal surface area of 150 to 250 cm2 and capacity 150
to 250 cm3 are suitable as test specimens. The quotient of
7.1 .1.2 Chromotropic acid disodium salt (disodium
the number expressing the surface wetted in Square
4,5-dihydroxy-2,7-naphthalene sulphonate) Solution.
centimetres by that expressing the volume of liquid in cubic
Dissolve 0,50 g of chromotropic acid disodium salt in 50 ml
centimetres must lie between 0,75 and 1.
of distilled water. Transfer the Solution to a 100 ml
volumetric flask and make up to volume. Prepare the
4.2 Number
Solution fresh each day.
Six specimens are required. The determination is carried
out in duplicate with each of the three extraction liquids
7.1 .1.3 Formaldehyde solutions.
(clause 5).
All solutions shall be made up at 20 ‘C.
5 EXTRACTION LIQUIDS
7.1 .1.3.1 Formaldehyde stock solutions.
Pipette 25,0 ml of industrial formalin (containing
5.1 Water, distilled or de-ionized.
approximately 400 g/l formaldehyde) into a 1 000 ml
volumetric flask and make up to volume with distilled
5.2 Acetic acid : 30 g/l solution of glacial acetic acid in
water. Determine the concentration of formaldehyde in the
distilled water.
stock Solution using the method described in ISO 2227.
This Solution shall not be kept longer than one week.
5.3 Ethanol : 100 g/l Solution of ethanol in distilled water.
ISO 4614-1977 (E)
7.1.1.3.2 Formaldehyde working Solution Ca. This will give the equivalent sf solutions containing from
approximately 10 to 1 pg/ml formaldehyde. lnto each of
Pipette IO,0 ml of formaldehyde stock Solution (7.1 .1.3.1)
the test tubes pipette 1,O ml of chromotropic acid disodium
into a 1 000 ml volumetric flask and make up to volume
salt Solution (7.1 .1.2) and add slowly, while shaking, 8,0 ml
with the extraction liquid (clause 5) to be used. Mix
of sulphuric acid (7.1 .1.4) from the 50 ml burette (725.3).
thoroughly.
Mix thoroughly by shaking and stopper the tubes. Place the
tubes in the water bath at 60 “C for 30 min. Remove the
7.1 -1.3.3 Formaldehyde working Solution B (approxi-
tubes from the water bath and allow them to stand at room
mately IO mg/l).
temperature for 45 to 60 min (solutions C).
Pipette IO,0 ml of Solution A (7.1 .1.3.2) into a 100 ml
Transfer a Portion of each Solution C, in turn, to a IO mm
volumetric flask and make up to the mark with the
glass cell and measure its absorbance at 570 nm against
extraction liquid (clause 5) to be used.
distilled watet-.
NOTE - The exact concentration of formaldehyde in Solution B
tan be calculated from the known formaldehyde content of the Carry out a blank determination on the reagents alone using
stock Solution (7.1 .1.3.1).
1,0 ml of the extraction liquid (clause 5) in place of the
formaldehyde Solution.
Solutions A and B shall be made up immediately Prior to
use.
Plot a graph of absorbance (IO mm cell) as Ordinate against
concentration of formaldehyde (pg/mI) as abscissa. This
7.1 .1.4 Sulphuric acid, concentrated, 81 % (mlm), of
shall be a straight line passing through
...