CERTIFICATION REPORT: The certification of the mass fractions of cadmium copper, manganese and nickel in dark chocolate: ERM BD512

This report describes the production of ERM-BD512, which is a matrix material certified for the mass fraction of cadmium, copper, manganese and nickel. This material was produced following ISO Guide 34:2009 and is certified in accordance with ISO Guide 35:2006. The CRM was produced from commercially available dark chocolate produced in Peru. About 15 kg of chocolate bars were melted, the melt was homogenised and cast into moulds to produce pellets of about 0.5 g. Between unit-homogeneity was quantified and stability during dispatch and storage were assessed in accordance with ISO Guide 35:2006 [ ]. Within-unit homogeneity was quantified to determine the minimum sample intake. The certified mass fraction of Cd was obtained by measurement, using the technique of isotope dilution ICP MS. The mass fractions of Cu, Mn and Ni were obtained by an interlaboratory comparison of laboratories of demonstrated competence and adhering to ISO/IEC 17025:2005. Technically invalid results were removed but no outliers were eliminated on statistical grounds only. Uncertainties of the certified values were calculated in accordance with the Guide to the Expression of Uncertainty in Measurement (GUM) and include uncertainties related to possible inhomogeneity, instability and characterisation. The material is intended for quality control and assessment of method performance. As with any reference material, it can be used for establishing control charts or validation studies. The CRM is available in packages of 6 glass vials, each containing a single pellet of about 0.5 g, which were sealed under an atmosphere of argon. The minimum amount of sample to be used is 250 mg. The CRM was accepted as European Reference Material (ERM®) after peer evaluation by the partners of the European Reference Materials consortium.JRC.F.6-Reference Material

The certification of different mass fractions of MON-Ø4Ø32-6 in soya bean powder Certified Reference Materials ERM®-BF410ap, ERM®-BF410bp, ERM®-BF410cp, ERM®-BF410dp and ERM®-BF410ep

This report describes the production of a set of Certified Reference Materials (CRMs), ERM BF410ap, bp, cp, dp and ep, which are certified for their GTS 40-3-2 soya bean (unique identifier MON-Ø4Ø32-6) event mass fractions. These materials were produced following ISO Guide 34:2009 and are certified in accordance with ISO Guide 35:2006. The materials are intended for the calibration or quality control of real-time PCR measurements to identify GTS 40-3-2 soya bean and quantify its mass fraction. As with any reference material, they can also be used for establishing control charts or for carrying out validation studies. The CRMs were accepted as European Reference Material (ERM®) after peer evaluation by the partners of the European Reference Materials panel.JRC.F.6-Reference Material

CERTIFICATION REPORT The certification of the mass fractions of elements in bovine liver: ERM-BB185

This report describes the production of ERM-BB185, which is a bovine liver material certified for the mass fraction of As, Cd, Cu, Mn, Pb, Se and Zn. This material was produced following ISO Guide 34:2009 and is certified in accordance with ISO Guide 35:2006. This CRM is produced and certified to replace the CRM BCR-185R. The CRM was produced from raw livers from cattle slaughtered in Belgium. The raw livers were cut into cubes and freeze dried. The freeze dried cubes were milled and sieved to obtain a fine powder. The powder was homogenised and afterwards checked for water content and particle size distribution. The homogenised powder was put in vials and packed in aluminised pouches. Between unit-homogeneity was quantified and stability during dispatch and storage were assessed in accordance with ISO Guide 35:2006. The material was characterised by an interlaboratory comparison of laboratories of demonstrated competence and adhering to ISO/IEC 17025. Technically invalid results were removed but no outlier was eliminated on statistical grounds only. Uncertainties of the certified values were calculated in accordance with the Guide to the Expression of Uncertainty in Measurement (GUM) and include uncertainties related to possible inhomogeneity, instability and characterisation. The material is intended for the quality control and assessment of method performance. As with any reference material, it can be used for establishing control charts or validation studies. The CRM is available in amber glass vials containing at least 10 g of dried powder which were sealed under an atmosphere of argon and packed in aluminised pouches. The minimum amount of sample to be used is 400 mg.JRC.F.6-Reference Material

CERTIFICATION REPORT The certification of different mass fractions of VCO-Ø1981-5 in maize seed powder Certified Reference Materials ERM®-BF438a, ERM®-BF438b, ERM®-BF438c, ERM®-BF438d and ERM®-BF438e

This report describes the production of a set of Certified Reference Materials (CRMs) ERM BF438a, b, c, d and e, which are certified for their VCO-Ø1981-5 mass fractions. These materials were produced following ISO Guide 34:2009 and are certified in accordance with ISO Guide 35:2006. Genetically modified (GM) seeds of the maize event VCO-Ø1981-5 and seeds from a non-GM maize variety were milled to obtain GM and non-GM seed powders with a similar particle size distribution. Mixtures of non-GM and GM maize powder were prepared gravimetrically. The certified value was obtained from the gravimetric preparations, taking into account the genetic purity with respect to the event VCO-Ø1981-5 of the two powder materials and their water mass fractions. The certified values were confirmed by event-specific real-time PCR as an independent verification method (measurements were within the scope of accreditation to ISO/IEC 17025:2005). The uncertainties of the certified values were estimated in accordance with the Guide to the Expression of Uncertainty in Measurement (GUM) [4] and include uncertainties relating to possible inhomogeneity (Section 4), instability (Section 5) and characterisation (Section 6). The materials are intended for the calibration or quality control of real-time PCR measurements to identify VCO-Ø1981-5 maize and/or quantify its mass fraction. As with any reference material, they can also be used for establishing control charts or for carrying out validation studies. The CRMs are available in glass bottles containing at least 1 g of dried maize seed powder, which were sealed under atmosphere of argon. The minimum amount of sample of the mixtures to be used and recommend for the blank and pure VCO-Ø1981-5 materials is 200 mg. The CRMs were accepted as European Reference Material (ERM®) after peer evaluation by the partners of the European Reference Materials consortium.JRC.D.2-Standards for Innovation and sustainable Developmen

CERTIFICATION REPORT: The certification of different mass fractions of Bt11 in maize powder: Certified Reference Materials: ERM®-BF412ak, ERM®-BF412bk, ERM®-BF412ck, ERM®-BF412dk and ERM®-BF412ek

This report describes the production of a set of Certified Reference Materials (CRMs), ERM-BF412ak, bk, ck, dk and ek, which are certified for their Bt11 maize (unique identifier SYN-BTØ11-1) event mass fractions. These materials were produced following ISO Guide 34:2009 and are certified in accordance with ISO Guide 35:2006. Genetically modified (GM) maize seeds of the Bt11 event and seeds from a non GM maize variety were milled to obtain GM and non-GM seed powders with a similar particle size distribution. Mixtures of non-GM and GM maize seed powder were prepared gravimetrically. The certified values were obtained from the gravimetric preparations, taking into account the water mass fractions of the two powder materials and the genetic purity with respect to the Bt11 maize. The certified values were confirmed by event-specific real-time PCR as an independent verification method (measurements were within the scope of accreditation to ISO/IEC 17025:2005). The uncertainties of the certified values were estimated in accordance with the Guide to the Expression of Uncertainty in Measurement (GUM) and include uncertainties relating to possible inhomogeneity (Section 4), instability (Section 5) and characterisation (Section 6). The materials are intended for the calibration or quality control of real-time PCR measurements to identify Bt11 maize and quantify its mass fraction. As with any reference material, they can also be used for establishing control charts or for carrying out validation studies. The CRMs are available in glass bottles containing at least 1 g of dried maize seed powder, sealed under an atmosphere of argon. The minimum amount of sample to be used for extraction of the DNA is 200 mg.JRC.F.6-Reference Material

IMEP-38: Determination of total As, Cd, Pb, and Hg in compound feed - Interlaboratory Comparison Report

The Institute for Reference Materials and Measurements (IRMM) of the Joint Research Centre, a Directorate General of the European Commission, operates the International Measurement Evaluation Programme (IMEP). IMEP organizes interlaboratory comparisons (ILCs) in support to EU policies. This report presents the results of the proficiency test (PT) which focused on the determination of total As, Cd, Pb and Hg in compound feed according to Directive 2002/32/EC of the European Parliament and of the Council on undesirable substances in animal feed. The IMEP-38 exercise was organized aiming to assess the performance of food and feed control laboratories and official control laboratories. The test material used in this exercise was commercially available compound feed for cats which after the appropriate processing was spiked, bottled, labelled, numbered accordingly and dispatched to the participants on the 27th of June 2013. Forty-seven laboratories from 24 countries registered to the exercise of which 44 reported results and answered the respective questionnaire. The percentage of satisfactory z-scores ranged from 58 % (total arsenic) to 74 % (total cadmium) and the ζ-scores obtained were lower by 10 to 21%.JRC.D.5-Standards for Food Bioscienc

Determination of total As, Cd, Pb and Hg in vegetable feed: IMEP-119 Proficiency Test Report

This report presents the results of a PT (IMEP-119) of the EURL-HM focussing on the determination of total As, Cd, Pb and Hg in vegetable feed in support to Directive 2002/32/EC of the European Parliament and of the Council on undesirable substances in animal feed. IMEP-119 was also opened to all laboratories who wish to take part in the exercise as a way to benchmark their performance against NRLs and other laboratories. One hundred and two participants from 45 countries registered to the exercise. Only eight participants did not report their results. Laboratory results were rated using z- and zeta (ζ-) scores in accordance with ISO 13528. The relative standard deviation for proficiency assessment was set to 15 % for the total As, Cd and Pb mass fractions, and to 22 % for the total Hg mass fraction, respectively. An overall adequate performance for NRLs and feed control laboratories is shown by the percentage of satisfactory performance (expressed as z-scores). These percentages were ranging from 93 to 74 % for NRLs and from 92 to 69 %, for feed control laboratories, respectively.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

EURL-HM-22 Proficiency test report: Determination of total As, Cd, Pb, Hg, MeHg and inorganic As in fish

The European Union Reference Laboratory for Heavy Metals in Feed and Food (EURL-HM) organised a proficiency test (EURL-HM-22) for the determination of total As, Cd, Pb, Hg and inorganic As (iAs) in fish to support the Commission Regulation (EC) 1881/2006 setting maximum levels for certain contaminants in foodstuffs. This PT was open only to National Reference Laboratories (NRLs). The reference material "IAEA-436" (Tuna fish flesh homogenate) was used as test item. The finely ground dry powder material was rebottled, relabelled and dispatched to the participants. The reference values of interest were provided by the IAEA, together with an informative value for total Pb. The University of Graz (Austria) was requested to analyse the mass fraction of iAs in the material and reported a truncated value ("less than" 0.005 mg kg-1). Forty two participants from 30 countries registered to the exercise (all EU Member States plus Iceland and Norway). Only one participant could not report results due to technical instrumental problems. Laboratory results were rated using z- (z'- for MeHg) and zeta scores in accordance with ISO 13528:2015. The following relative standard deviations for proficiency assessment (σpt) were set according to the modified Horwitz equation: 13% for total Hg and MeHg; 15% for total As; and 22% for total Cd. No scoring was provided for total Pb and iAs. More than 92% of the participating NRLs reported satisfactory results (according to the z-score) for total As, Cd, Hg and MeHg, thus confirming their ability in monitoring the maximum levels set by the European Regulation (EC) No 1881/2006 for fish commodities. However, only 9 (out of 41) participants reported results for MeHg. Most of the laboratories provided realistic estimates of their measurement uncertainties.JRC.F.5-Food and Feed Complianc