The results of a research project (EU AIR Research Programme CT94-1025) aimed to introduce control of migration into good manufacturing practice and into enforcement work are reported. Representative polymer classes were defined on the basis of chemical structure, technological function, migration behaviour and market share. These classes were characterized by analytical methods. Analytical techniques were investigated for identification of potential migrants. High-temperature gas chromatography was shown to be a powerful method and 1H-magnetic resonance provided a convenient fingerprint of plastic materials. Volatile compounds were characterized by headspace techniques, where it was shown to be essential to differentiate volatile compounds desorbed from those generated during the thermal desorption itself. For metal trace analysis, microwave mineralization followed by atomic absorption was employed. These different techniques were introduced into a systematic testing scheme that is envisaged as being suitable both for industrial control and for enforcement laboratories. Guidelines will be proposed in the second part of this paper.
Samples of PVC cling films were taken at importers, wholesalers and retail shops, and their overall migration to the alternative food simulant iso-octane was measured, after establishment of a correlation between overall migration to olive oil at 40 degrees C in 10 days and to iso-octane in 2 h. Results of the migration testing were compared with the recommended and/or actual use of the PVC film and the labelling discussed in relation to the relevant EEC directives on food contact plastics. The correct labelling of plasticized PVC film intended for use in retail packaging is important to avoid the risk of significant consumer intakes of the plasticizer di-(2-ethylhexyl) adipate (DEHA) after the film has been used in contact with fatty foodstuffs. Sixty percent of the films declared for use in contact with fatty foods showed too high overall migration compared with the current interpretation of legislation at the time of sampling. In most instances DEHA made up about 80% of the total amount of plastic constituents migrating to iso-octane. Taking into consideration a specific migration limit of 3 mg DEHA/dm2, 77% of the films used for fatty foodstuff analysed were not acceptable. The migration of DEHA to non-fatty foods defined as the food simulant water was at or below 0.1 mg/dm2 in all PVC-films.
A reference material for the determination of overall migration from a plastic coextrudate into the fatty food simulant olive oil was produced and certified in an interlaboratory study. The analyses were carried out according to the ENV 1186 standard from the European Committee for Standardization (CEN) [ 1, 2, 3] with exposure of the coextrudate to olive oil for 10 days at 40 degrees C. After an initial preliminary interlaboratory study eight laboratories participated in the certification round, and two different methods were used to obtain single sided exposure of the plastic to the oil. The certified value was determined as the mean of laboratory mean values. No outliers were found. A reference value of 8.6 mg/dm2 +/- 1.4 mg/dm2 (+/- half width of the 95% confidence interval) was obtained which is within the range relevant for the regulatory limit (10 mg/ dm2), making this reference material suitable for laboratories measuring according to the EU overall migration limit [4]. The material has been found stable over 45 months.
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