Report on the inter-laboratory comparison exercise organised by the European Union Reference Laboratory for Food Contact Materials: Determination of elements in acetic acid solutions and in migration from ceramic and glass tableware

This report presents the outcome of an inter-laboratory comparison exercise (ILC) on the determination of selected metals in acetic acid solutions and the determination of migration of elements from ceramic and glass tableware. The exercise was organised by the European Union Reference Laboratory for Food Contact Materials (EURL-FCM) to evaluate the enforceability of measures under discussion for the future revision(s) of ceramics Directive 84/500/EEC [1] and the implementation of provisions laid down in the Commission Regulation 10/2011 [2] for plastics. National Reference Laboratories (NRLs) requested the EURL-FCM to organise an ILC with the aim to check (i) the analytical abilities of participating laboratories to quantify Cu, Fe, Zn and Sb in a solution of acetic acid 3% and Ba, Co, Mn, Pb, Cd and Al in a solution of acetic acid 4%; (ii) to test the laboratories performance to carry out the migration test on ceramic and glass articles and (iii) to derive precision criteria, including repeatability and reproducibility for the release of elements from tableware. Participation in this ILC was mandatory for the nominated NRLs, and open to Official Control Laboratories (OCLs) and other invited laboratories. A total of 53 participants from 27 countries registered to the exercise. Twenty-nine NRLs from 27 countries participated in this ILC and all of them reported results. Laboratory results were rated using z-score in accordance with ISO 13528:2015 [3]. The target standard deviation for the ILC assessment (σ), for all measurands was calculated based on previous ILC03/04 2014 exercises [4] for spiked solutions and using the robust reproducibility standard deviation for the migration exercise on tableware. Repeatability and reproducibility standard deviations for the quantification of elements in acetic acid 3% and acetic acid 4% (spiked solutions and leachates) were calculated using robust approaches [3, 5]. The outcome of this exercise was satisfactory. The rate of success was almost always higher than 80% for all elements in all samples. No difference between the performance of NRLs and OCLs was observed. Since the exercise required the uncertainty estimation, an additional assessment was provided to each laboratory, indicating how reasonable their measurement uncertainty estimation was. lζ-scoresl were systematically higher than z-scores, that underlines the need of an improvement in estimation of the measurement uncertainties.JRC.F.5-Food and Feed Complianc

Suitability of new sources of olive oil intended to be used as simulant D in migration testing

Regulation EC/882/2004 on Feed and Food Controls establishes the JRC as Community Reference Laboratory for Food Contact Materials (CRL-FCM). The Regulation requires a supporting network of European National Reference Laboratories (NRLs). This Regulation supports the harmonised enforcement of food legislation including food contact materials and the creation of a reference laboratory system operated by the JRC to systematically exchange and assess information on emerging issues related to chemicals released from food contact materials. The Council Directive 85/572/EEC of 19 December 1985 lays down the list of simulants for overall and specific migration testing, to be used for testing migration of constituents of plastic materials and articles intended to come into contact with foodstuff. This Directive lists the appropriate simulants to be used in migration tests with a particular foodstuff or group of foodstuffs. Within simulants, simulant D is rectified olive oil that has to satisfy characteristics such as acidity, peroxide index, iodine index, refractive index. Until 2005 rectified olive oil with documented appropriate technical specifications was commercially available from the company Pira International (UK). However commercial production stopped, and other potential sources available (Korea Japan, Sigma) did not necessarily provide specifications documented specifically for use as ¿simulant D¿. Since the oil specifications set in the EU legislation are crucial, both for compliance testing but also in the frame of an ISO accreditation for migration in oil, NRLs suggested the CRL-FCM to investigate specifications potential sources of olive oil to develop a source of simulant D for their purposes. The purpose of this study was to: ¿ Find potential suppliers for rectified olive oil ¿ Evaluate characteristics of oil on batch samples ¿ Select one supplier to purchase a lot of adequate defined specifications ¿ Establish the adequacy and homogeneity of the oil of a 500L lot ¿ Confirm the evaluation by independent analyses and certification by a specialised accredited institution for those specifications. The results demonstrated the feasibility of at least one source of olive oil, which was then provided to the National Reference Laboratories as a deliverable of the workprogramme 2007.JRC.I.5-Physical and chemical exposure

Towards suitable tests for the migration of metals from ceramic and crystal tableware: Work in support of the revision of the Ceramic Directive 84/500/EEC

This JRC report summarises and distils a series of investigations on the technical feasibility to testing compliance of tableware to potential lower limits for the release of metals. It investigated different protocols for articles ranging from tableware ,bakeware to crystalware, and for testing the rim of decorated wares. It also evaluated the performance of analytical methods for the quantification of a range of metals. The work provides scientific evidence needed in support of future risk management initiatives to ensure the safety of ceramics and crystal in the EU while fostering the EU single market.JRC.F.7-Knowledge for Health and Consumer Safet

Consumer Perception Studies on the Safety of Food Packaging - Final Report of WP7 of the EU Project "Foodmigrosure" QLK1-CT2002-2390

Between March 2003 and September 2006 the FOODMIGROSURE project, contract number QLK-CT2002-2390, was carried out by 9 European project partners with the intention to develop an ¿into-food¿ migration model tool which should enable prediction of mass transfer of constituents from plastics food contact materials into foodstuffs in support of calculations/estimations of the exposure of consumers towards food packaging constituents. A further objective was to investigate the social acceptance of migration modelling versus chemical measurements, and its implications for exposure estimation. This was achieved by several approaches including focus group (as qualitative approach), and questionnaires with a large polling bas as quantitative approach from citizens. A test trial was run on consumer associations and the experiment was then conducted on citizens during a JRC Open Day. Questionnaires and comments were colleted for 700 units which represented about 1400 visitors to the food contact activities. In the last phase, a more specific technical questionnaire was directed to end-user of modelling, which was mailed to a variety of stakeholders such as National Reference Laboratories, commercial laboratories, industries, EFSA, CEN members etc. Globally, people in the overwhelming majority -both for the questionnaire approach and for the focus group approach- felt reassured regarding the safety of packaging simply from the fact that they did not previously know that such research and controls existed. Many citizens also clearly expressed the wish to have this type of research much more visible at the level of both consumer associations and consumers themselves. The responses were echoing quite interestingly between the different approaches directed at consumers/citizens. Although obtained by completely different methodologies, both focus groups and quantitative citizen polling questionnaires showed many similarities even in the specifics. There is a fundamental trust from the public in the scientists to distinguish and understand safety issues. The consumer wants sincerely to be approached and informed by scientists for this reason and is also ready to favour new approaches such as migration modelling if it can be an additional tool for better consumer protection. The benefits of packaging are recognised, and the presence of migrants is considered similarly to the presence of food additives in foods. Modelling is viewed as a additional helping tool to assist the scientist as first and foremost raison d¿être, and was found to have its strongest value as pointing the worst cases that could occur. The consumers or citizens made no mention of environmental or worker health effects benefits. However, the consumer especially in the context of the focus group remarked justly that one needs to be sure that at the root for use of these models are experimental data which demonstrate the applicability of the model.JRC.I.5-Nanobioscience

Report of the interlaboratory comparison organized by the Community Reference Laboratory Food Contact Material: Plasticisers in Gaskets and Oil

The Institute for Health and Consumer Protection (IHCP) of the European Commission¿s Directorate-General Joint Research Centre hosts the Community Reference Laboratory for Food Contact Materials (CRL-FCM). One of its core tasks is to organize interlaboratory comparisons (ILCs) among appointed National Reference Laboratories (NRLs). This report presents the results of the first ILC of the CRL-FCM which focused on the determination of Plasticisers content in PVC Gasket and in Oil matrix. The test materials used in this exercise were virgin gasket lids coming from industrial sources for the proficiency exercise part A. For the second part of the exercise an industrial source of sunflower oil was used and spiked with several plasticisers by the CRL-FCM. There were 41 participants to whom samples were dispatched 34 of which submitted results for at least 1 analyte-material. 21 laboratories reported results for more than 10 analyte-material combination out of 14 required. The homogeneity studies were performed by the CRL-FCM laboratory. The assigned value and its uncertainty for part A, virgin gaskets, were obtained after applying the robust statistics to the results obtained from the participants. The assigned values for part B, oil samples, were those obtained based on formulation, from the gravimetric measurements used to spike the material. The uncertainty of the assigned values for oil samples was calculated combining the uncertainty of the spiking procedure with a contribution for the between-bottle homogeneity. Participants were invited to report four replicates measurements. This was done by most of the participants. Laboratory results were rated with z and z¿ scores in accordance with ISO 13528 [1] Standard deviations for proficiency assessment (also called target standard deviations) were set based on Horwitz equation for substances in the two oil samples. For the plasticisers in the two gasket samples the target standard deviation was set by the organizers to 15% in order to fulfil the required criteria for sufficient homogeneity of the sample within the lots.JRC.I.2-Chemical assessment and testin

Report of the interlaboratory comparison organised by the European Reference Laboratory for Food Contact Material - ILC01 2011- Formaldehyde in food contact migration solution

The Institute for Health and Consumer Protection (IHCP) of the European Commission’s Directorate-General Joint Research Centre hosts the EU Reference Laboratory for Food Contact Materials (EURL-FCM). One of its core tasks is to organise interlaboratory comparisons (ILCs) among appointed National Reference Laboratories (NRLs). This report presents the results of the ILC of the EURL-FCM, which focused on the quantification of formaldehyde in migration solutions of 3% acetic acid from food contact materials. The test material used for preparation of the migration solutions were melamine kitchenware (spoons) containing formaldehyde. The EURL prepared and distributed three concentration levels of migration solution. The general aim of the exercise was to assess the proficiency of the official control laboratories and consequently the participants were free to use any analytical method of their choice. However, in view of the support to Regulation 284/2011, EURL suggested to limit the methods to the two procedures included in EN 13130-23 (i.e. standard for food contact). There were 62 participants to whom samples were dispatched (27 NRLs + 35 national control laboratories from Germany, Italy, United Kingdom, Poland, Spain, France, Portugal and Switzerland) and 61 of which submitted results. The homogeneity and stability studies were performed by the EURL-FCM laboratory. The assigned values were obtained after applying the robust statistics to the results of the participants. Participants were invited to report 4 results for each concentration level. Laboratory results were processed using several algorithms: ISO 13528 [1], Harmonized protocol [8], DIN 38402 A45 (Q-Hampel) [5] and ISO GUIDE 35:2006 [11]. Standard deviations for proficiency assessment (also called target standard deviations) were set based on Horwitz equation [2]. As a conclusion of the ILC exercise on the quantification of formaldehyde in the migration solution of kitchenware in 3% acetic acid, this ILC showed that: The participation in the ILC was satisfactory regarding the number of the participating laboratories. Sixty one participants laboratories submitted their results. Six of the participants submitted results obtained using two different sample preparation methods. From the EURL-NRL network all 27 laboratories reported results. For the network of NRL-FCM the outcome from the participation is regarded as satisfactory as there are all satisfactory results. For the network of national control laboratories only one laboratory does not send any results. More than 85% of all reported results were properly estimated. Comparing between the two sample preparation methods (EN 13130-23) used by the participants resulted in not significantly different mean values. Both methods were found interchangeable.JRC.I.1-Chemical Assessment and Testin

Precision criteria of methods for the quantification of metals migrated from Food Contact Materials: Pre-validation data derived from ILCs on elements representative for plastics and ceramics

Precision criteria for the quantification of metals in acetic acid 3% and acetic acid 4% migration solutions for different analytical techniques were calculated and are presented in this report. They were derived from two interlaboratory comparisons (ILC03/04 2014) data, including repeatability and reproducibility standard deviations. Three groups of analytical techniques were identified from the ILCs: Inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma Optical emission spectrometry (ICP-OES) and atomic absorption spectrometry (AAS). AAS included graphite furnace (GF-AAS) and flame (F-AAS). Precision criteria were calculated applying robust statistic methods with algorithms A and S (ISO 5725-5 and ISO 13528) and DIN 38402 A45 (Q-method/Hampel-estimator) The robust means calculated according to both algorithms were checked for significant difference (student's t-test) and equivalence test. Relative repeatability standard deviations were very low generally less than 2% and reached 4.4% only for Pb in acetic acid 4%. Relative reproducibility standard deviations for Pb were around 10% for ICP-MS and ICP-OES techniques and 16% for AAS. Relative reproducibility standard deviations for Cd were around 5%, 10% and 20% using respectively ICP-MS, AAS or ICP-OES techniques. For other elements the relative reproducibility standard deviations obtained were for most of the cases less than 10%. From the comparison study it was possible to establish with the exception of Fe, for all elements of the two ILCs in both solutions (corresponding to elements from ceramics and elements from plastics) the analytical techniques were generally equivalent and not significantly different at the concentrations investigated.JRC.I.1-Chemical Assessment and Testin

Report of an interlaboratory comparison organised by the European Reference Laboratory for Food Contact Materials : Formaldehyde in 3% acetic acid migration solution -follow up exercise

This report presents the results of the 2013 follow up of the EURL-FCM 2012 ILC formaldehyde and melamine in food contact migration solution. In the 2012, out of the 62 laboratories who submitted results, 23 laboratories (ca. 37%) had results that showed some discrepancies affecting the analysis of the highest concentration level sample. For the NRLs, for this test solutions, 10 laboratories out of 27 ( ca also 37%) had questionable or unsatisfactory scores. Therefore, as a follow up, the EURL sent prepared a new migration solution for underperforming laboratories to repeat this part of the ILC and improve their results. The test material used for preparation of the migration solution were melamine kitchenware (spoons) containing formaldehyde. The general aim of the exercise was to assess once again the performance of the official control laboratories which had some issues in the determination of formaldehyde in high concentrated solution where the dilution step was necessary. There were 23 participants to whom samples were dispatched and all laboratories submitted results (10 NRLs + 13 national control laboratories from European countries) and all of them submitted results. The homogeneity study was performed by the EURL-FCM laboratory. Participants were invited to report 4 results. Laboratory results were processed using DIN 38402 A45 (Q-Hampel) algorithm. The assigned values were obtained after applying the robust statistics to the results of the participants. Standard deviations for proficiency assessment (also called target standard deviations) were set based on Horwitz equation. The results of the quantification of in the migration solution of kitchenware in 3% acetic acid showed an improvement for the problematic high concentration from 63% satisfactory in 2012 to 92% satisfactory (for all laboratories indifferently of NRL or OCLs). For the NRLs, all results were satisfactory and the performance increased from 63% to 100%.JRC.I.1-Chemical Assessment and Testin

Effect of Calibration Standards on the Quantification of Hydroxy Products from Can Coatings

A liquid chromatographic (LC) method for Bisphenol A diglycidyl ether (BADGE), Bisphenol F diglycidyl ether (BFDGE) and their derivatives is currently being validated at the level of the European COmmittee for Standardisation (CEN). The method consists in hydrolysing the substances to their di-hydroxy forms with a quantification based on calibration using hydrolysed monomers (BADGE.2H2O or BFDGE.2H2O). Considering laboratories may use the standard of BADGE.2H2O or BFDGE.2H2O now commercially available, a comparison was made on the effect of using a calibration based on the commercial hydrolysis product versus hydrolysing the monomer on the quantification of the migration limit for enforcement purposes. In this work, the epoxy bis (diol) derivatives were quantified in three different food simulants.JRC.I.5-Physical and chemical exposure

Report of an Interlaboratory Comparison from the European Reference Laboratory for Food Contact Materials: ILC001-2013 – Proficiency Testing on Food Simulant E containing a cocktail of potential migrant substances

Food simulant E, also commercially named Tenax®, was established in Regulation (EU) No 10/2011 for testing specific migration into dry foodstuffs. This presents the results of an an Interlaboratory Comparison organised as Proficiency Testing on Food Simulant E containing a cocktail of potential migrant substances. The object of the ILC was to 1) expand the range of polarity and volatility of substance under the scope of the exercise; 2) test the ability of laboratories in the identification and quantification of substances with a free choice of any analytical method and 3) include the screening of unknown substances. The test material used in this exercise was a spiked food simulant E prepared by the EURL-FCM.The choice of the substances was based on the relevant scientific literature related to migration from food contact materials (plastic and paperboard) into simulant E.The participation of the laboratories on this PT on the identification and quantification of ACPH, BP, CAP, DEHA, DTBP, ETHX and OCT in the simulant E was satisfactory regarding the number of received results and thanks to the proactive involvement of the NRLs.JRC.I.1-Chemical Assessment and Testin