IMEP-112: Total and Inorganic Arsenic in Wheat, Vegetable Food and Algae. Report of the Twelfth Interlaboratory Comparison Organised by the European Reference Laboratory for Heavy Metals in Feed and Food.

The Institute for Reference Materials and Measurands (IRMM) of the Joint Research Centre (JRC), a Directorate-General of the European Commission, operates the European Union-Reference Laboratory for Heavy Metals in Feed and Food (EU-RL-HM). Two of its core tasks are to provide advice to the Directorate General for Health and Consumers (DG SANCO) on scientific matters and to organise interlaboratory comparisons (ILC) among appointed National Reference Laboratories (NRLs). This report presents the results of the twelfth ILC of the EU-RL-HM (former CRL-HM) which focused on the determination of total and inorganic As in wheat, vegetable food and algae. The test items used in this exercise are: wheat, spinach (SRM 1570a from NIST) and an algae candidate reference material. The test items were processed (in the case of wheat), bottled and labelled at IRMM and dispatched to the participants the second week of May 2011. Each participant received three bottles containing approximately 20 g of wheat, 15 g of spinach and 5 g of algae,respectively. Participation in this exercise was not limited to the NRLs but was open to laboratories from all around the world, to be able to judge the state-of-the-art of the determination of total and, more in particular, inorganic As in several food commodities. Seventy-four laboratories from 31 countries registered to the exercise, of which – 64 reported results in wheat, 49 in spinach and 51 in algae for total As, and – 43 reported results in wheat, and 40 in spinach in algae for inorganic arsenic. Thirty of the participants were NRLs of the EU-RL-HM network, out of which 13 reported values for inorganic As. The assigned values for IMEP-112 were provided by the certificates when available and otherwise by a group of seven laboratories expert in the field. The uncertainties of the respective assigned values (uref) were derived from the standard deviation of the means provided by the experts (uchar) and from the contribution for homogeneity (ubb) and stability (ust). Laboratory results were rated with z-and ζ-scores (zeta-scores) in accordance with ISO 13528. The standard deviations for proficiency assessment (also called target standard deviation) were fixed by the advisory board of this ILC on the basis of the outcome of previous ILCs organised by the EU-RL-HM and on the state-of-the-art in this field of analysis to: - 15 % for total and inorganic arsenic in wheat. - 22% for total arsenic and 25 % for inorganic arsenic in vegetable food, to account for the difficulty introduced by the relatively low concentration of both measurands in this test material. - 15 % for total arsenic and 22 % for inorganic arsenic in algae. Most of the participants performed satisfactorily for total arsenic and for inorganic arsenic in vegetable food (75 and 85 %); 60 % did for inorganic arsenic in wheat but only 20 % of the laboratories reported satisfactory results in the algae test material.JRC.D.6-Food Safety and Qualit

IMEP-34: Heavy Metals in Toys according to EN 71-3:1994

The Institute for Reference Materials and Measurements (IRMM) of the Joint Research Centre (JRC), a Directorate-General of the European Commission, operates the International Measurement Evaluation Programme (IMEP). It organises interlaboratory comparisons (ILC's) in support to EU policies. This report presents the results of an ILC which focussed on the determination of soluble antimony (Sb), arsenic (As), barium (Ba), cadmium (Cd), chromium (Cr), lead (Pb), mercury (Hg), and selenium (Se) according to European Standard EN 71-3:1994. The principle of the procedure in EN 71-3:1994 [1] consists in the extraction of soluble elements from toy material under the conditions simulating the material remaining in contact with stomach acid for a period of time after swallowing. Fifty eight participants from twenty six countries registered to the exercise, of which 54 reported results for As, Sb, Ba, Se and Hg and 58 for Cr, Pb, and Cd, respectively. The test item used was a certified reference material (CRM 623, comminuted paint flakes from alkyd resin paint), certified in 1998, which is not included anymore in the CRM catalogue. The validity of the certified values was assessed using some expert laboratories in the field. In most of the cases the results reported by the certifiers were not in agreement with the CRM reference values. The mean of the means reported by the expert laboratories was used as assigned value for the different measurands. The results reported by the expert laboratories for mercury were very scattered (RSD = 37.6 %). No assigned value could be attributed for mercury and therefore no scores were provided to the participants for this measurand. The associated uncertainties of the assigned values were obtained following the ISO GUM. Furthermore, participants were invited to report their measurement uncertainties. This was done by all laboratories having submitted results in this exercise. Laboratory results were rated with z- and zeta (ζ-) scores in accordance with ISO 13528. The standard deviations for proficiency assessment were based on the analytical correction laid down in EN 71-3:1994. The outcome of the exercise shows an improvement on the overall performance of the participants when compared to IMEP-24 (a proficiency test for heavy metals in toys run in 2009 in which, the same European standard was followed), particularly for cadmium, lead and to a lesser extent, for selenium and chromium. The share of satisfactory z-scores ranged from 65 to 79 %.JRC.D.5-Food Safety and Qualit

IMEP-35: Determination of Total Lead in Lipsticks (Interlaboratory Comparison Report)

The Institute for Reference Materials and Measurements (IRMM) of the Joint Research Centre (JRC), a Directorate-General of the European Commission, operates the International Measurement Evaluation Programme (IMEP). It organises interlaboratory comparisons (ILCs) in support to EU policies. This report presents the results of a proficiency test exercise (PT) focussed on the determination of total lead in lipsticks which was organised in support of the European Council Directive 79/768/EEC (1976).JRC.D.5-Standards for Food Bioscienc

IMEP-114: Determination of total Cd, Pb, As, Hg and Sn in feed premixes - Interlaboratory Comparison Report

This report presents the results of the proficiency test IMEP-114 of the EU-RL-HM which focused on the determination of total Cd, Pb, As, Hg and Sn in feed premixes in support to Directive 2002/32/EC of the European Parliament and of the Council on undesirable substances in animal feed. Thirty laboratories from 26 countries registered to the exercise of which 25 reported results for total As, 30 for total Cd, 29 for total Pb, 13 for total Hg and 9 for total Sn. Laboratories were asked to perform two or three independent measurements and to report the mean, the associated uncertainty, the coverage factor of the associated uncertainty and the technique used to perform the measurements. Laboratory results were rated using z- and ζ-scores (zeta-scores) in accordance with ISO 13528. The assigned values (Xref) for the measurands were determined as the mean of the values reported by two expert laboratories. The standard deviation for proficiency assessment (σˆ ), also called target standard deviation, was set to 15 % of the assigned value, for the analytes investigated. Between 60 and 90 % of the laboratories reported satisfactory results for total As and total Cd, and 50 % for total Pb. Only 3 participants reported satisfactory results for total Sn (out of 9 laboratories that reported values). Thirteen participants reported results for total Hg although, according to the expert laboratories the mass fraction for that measurand was below their limit of detection.JRC.D-Institute for Reference Materials and Measurements (Geel

IMEP-36: Determination of total Cd, Pb, As, Hg and Sn in feed premixes: Interlaboratory Comparison Report

This report presents the results of the proficiency test IMEP-36 which focused on the determination of total Cd, Pb, As, Hg and Sn in feed premixes according to Directive 2002/32/EC of the European Parliament and of the Council on undesirable substances in animal feed. Fifty laboratories from 22 countries registered to the exercise of which 45 reported results and answered the respective questionnaire. Laboratories were asked to perform two or three independent measurements and to report the mean, the associated uncertainty, the coverage factor of the associated uncertainty and the technique used to perform the measurements. Laboratory results were rated using z- and ζ-scores (zeta-scores) in accordance with ISO 13528. The assigned values (Xref) for the measurands were determined as the mean of the values reported by two expert laboratories both of them National Metrology Institutes (NMI). The results obtained by the participants were optimum in the case of total Cd and less satisfactory for total As and total Pb. For total Sn 16 participants reported results, from which one third scored satisfactorily. Twenty one participants reported results for total Hg although, the expert laboratories reported that the mass fraction for that measurand was below their limit of detection. Hence, no scoring was provided for total Hg.JRC.D.5-Standards for Food Bioscienc

IMEP-113: determination of total cadmium and lead in baby food - Interlaboratory Comparison Report - December 2011

This report presents the results of the thirteen proficiency test (PT) which focussed on the determination of total Cd and Pb in baby food according to Commission Regulation (EC) No 1881/2006 of 19 December 2006 setting maximum levels for certain contaminants in foodstuffs. The test material used in this exercise was baby food formula purchased in a local pharmacy and prepared by the Reference Material Unit of the IRMM for this exercise. Each participant received one bottle containing approximately 15 g of test material. Thirty five laboratories from 26 countries registered to the exercise and all of them reported results. Participants were asked to analyse the measurands in the powder and in the reconstituted form (powder diluted with water, 1:8 fold, to mimic the product as consumed). The assigned value for total Cd was determined by LGC Ltd (UK) and IRMM using direct isotope dilution inductively coupled plasma mass spectrometry. The assigned value for total Pb was determined at IRMM using the same technique as for Cd. The standard deviation for proficiency assessment was set at 22 % of the assigned value based on the modified Horwitz equation. Laboratories were rated with z- and ζ-scores (zeta-scores) in accordance with ISO 13528. The outcome of this exercise is clearly influenced by the very low level of Cd and Pb content in the test material which triggered: - a high number of "less than" values; - overestimated values especially for lead very likely due to contamination. Reported results were satisfactory for total cadmium in both forms, (powder and in the reconstituted formula).JRC.D.5-Food Safety and Qualit

IMEP-33: Total Cadmium and Lead in Baby Food - Interlaboratory Comparison Report, December 2011

The Institute for Reference Materials and Measurements (IRMM) of the Joint Research Centre (JRC), a Directorate-General of the European Commission, operates the International Measurement Evaluation Programme® (IMEP). It organises interlaboratory comparisons (ILC's) in support to EU policies. This report presents the results of an ILC which focussed on the determination of total Cd and Pb in baby food in support of Commission Regulation (EC) No 1881/2006 of 19 December 2006 setting maximum levels for certain contaminants in foodstuffs. The test material used in this exercise was baby food formula purchased in a local pharmacy and prepared by the Reference Material Unit of the IRMM for this exercise. Each participant received one bottle containing approximately 15 g of test material. Sixty-six laboratories from 23 countries registered to the exercise and 61 of them reported results. Participants were asked to analyse the measurands in the powder and in the reconstituted form. The assigned value for total Cd was determined by LGC Ltd (UK) and IRMM using direct isotope dilution inductively coupled plasma mass spectrometry. The assigned value for total Pb was determined at IRMM using the same technique as for Cd. The standard deviation for proficiency assessment ˆ was set at 22 % of the assigned value based on the modified Horwitz equation. Laboratories were rated with z- and ζ-scores (zeta-scores) in accordance with ISO 13528. Most of the participants reported uncertainties with their results. The outcome of this exercise is clearly characterised by the very low level of Cd and Pb content in the test material which triggered a high number of "less than" values, overestimation especially for lead very likely due to contamination, and a visible method influence in the case of lead. The results were also evaluated with regard to the reported limit of detection and some incoherencies were observed here as well.JRC.D.5-Food Safety and Qualit