CERTIFICATION REPORT: The certification of the mass fractions of PBDEs in Fish Tissue: ERM®-CE102

This report describes the production of ERM®-CE102, which is a fish tissue certified for the mass fraction of polybrominated diphenyl ethers (PBDEs) on a wet weight basis. This material was produced following ISO 17034:2016 and is certified in accordance with ISO Guide 35:2017. The Certified Reference Material is a fish tissue homogenate prepared from wild Wels catfish (Silurus glanis) originating from the Flix reservoir of the Ebro river (Spain) and aquaculture rainbow trout (Oncorhynchus mykiss) sourced in Belgium. The fish fillets were cut, shock-frozen in liquid nitrogen and cryogenically milled. After a pre-cooking step, a step-wise mixing and homogenisation were carried out. The resulting material was filled into jars, autoclaved for sterilisation and labelled as ERM-CE102. Between unit-homogeneity was quantified and stability during dispatch and storage were assessed in accordance with ISO Guide 35:2017 [2]. Within-unit homogeneity was quantified to determine the minimum sample intake. 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 in validation studies. ERM-CE102 is available in glass jars with twist-off lids containing at least 40 g of fish paste. The minimum amount of sample to be used is 8 g.JRC.F.6-Reference Material

CERTIFICATION REPORT: The certification of the absorbed energy (150 J nominal) of Charpy V-notch reference test pieces for tests at 20 °C: ERM®-FA415am

This certification report describes the processing and characterisation of ERM®-FA415am, a batch of Charpy V-notch certified reference test pieces certified for the absorbed energy (KV). Sets of five of these test pieces are used for the verification of pendulum impact test machines according to ISO 148-2 (Metallic materials - Charpy pendulum impact test – Part 2: Verification of testing machines). The absorbed energy (KV) is operationally defined and refers to the impact energy required to break a V-notched test piece of standardised dimensions, as defined in ISO 148-1. The certified value of ERM-FA415am is made traceable to the SI, via the SI-traceable certified value of the master batch ERM®-FA415s, by testing samples pieces of ERM-FA415am and ERM-FA415s under repeatability conditions on an impact pendulum verified and calibrated with SI-traceably calibrated tools. The certified value is valid only for strikers with a 2 mm tip radius. The certified value is valid at (20 ± 2) °C.JRC.F.6-Reference Material

CERTIFICATION REPORT The certification of the absorbed energy (low energy) of Charpy V-notch reference test pieces for tests at 20 °C: ERM®-FA013bz

This certification report describes the processing and characterisation of ERM®-FA013bz, a batch of Charpy V-notch certified reference test pieces certified for the absorbed energy (KV). Sets of five of these test pieces are used for the verification of pendulum impact test machines according to ISO 148-2 (Metallic materials - Charpy pendulum impact test – Part 2: Verification of testing machines). The absorbed energy (KV) is operationally defined and refers to the impact energy required to break a V-notched test piece of standardised dimensions, as defined in ISO 148-1. The certified value of ERM-FA013bz is made traceable to the SI, via the SI-traceable certified value of the master batch ERM®-FA013ba, by testing samples pieces of ERM-FA013bz and ERM-FA013ba under repeatability conditions on an impact pendulum verified and calibrated with SI-traceably calibrated tools. The certified value is valid only for strikers with a 2 mm tip radius. The certified value is valid at (20 ± 2) °C.JRC.F.6-Reference Material

CERTIFICATION REPORT The certification of the absorbed energy (150 J nominal) of Charpy V-notch reference test pieces for tests at 20 °C: ERM®-FA415ao

This certification report describes the processing and characterisation of ERM®-FA415ao, a batch of Charpy V-notch certified reference test pieces certified for the absorbed energy (KV). Sets of five of these test pieces are used for the verification of pendulum impact test machines according to ISO 148-2 (Metallic materials - Charpy pendulum impact test – Part 2: Verification of testing machines). The absorbed energy (KV) is operationally defined and refers to the impact energy required to break a V-notched test piece of standardised dimensions, as defined in ISO 148-1. The certified value of ERM-FA415ao is made traceable to the SI, via the SI-traceable certified value of the master batch ERM®-FA415s, by testing samples pieces of ERM-FA415ao and ERM-FA415s under repeatability conditions on an impact pendulum verified and calibrated with SI-traceably calibrated tools. The certified value is valid only for strikers with a 2 mm tip radius. The certified value is valid at (20 ± 2) °C.JRC.F.6-Reference Material

CERTIFICATION REPORT The certification of the absorbed energy (low energy) of Charpy V-notch reference test pieces for tests at 20 °C: ERM®-FA013by

This certification report describes the processing and characterisation of ERM®-FA013by, a batch of Charpy V-notch certified reference test pieces certified for the absorbed energy (KV). Sets of five of these test pieces are used for the verification of pendulum impact test machines according to ISO 148-2 (Metallic materials - Charpy pendulum impact test – Part 2: Verification of testing machines). The absorbed energy (KV) is operationally defined and refers to the impact energy required to break a V-notched test piece of standardised dimensions, as defined in ISO 148-1. The certified value of ERM-FA013by is made traceable to the SI, via the SI-traceable certified value of the master batch ERM®-FA013ba, by testing samples pieces of ERM-FA013by and ERM-FA013ba under repeatability conditions on an impact pendulum verified and calibrated with SI-traceably calibrated tools. The certified value is valid only for strikers with a 2 mm tip radius. The certified value is valid at (20 ± 2) °C.JRC.F.6-Reference Material

CERTIFICATION REPORT The certification of the absorbed energy (low energy) of Charpy V-notch reference test pieces for tests at 20 °C: ERM®-FA013bx

This certification report describes the processing and characterisation of ERM®-FA013bx, a batch of Charpy V-notch certified reference test pieces certified for the absorbed energy (KV). Sets of five of these test pieces are used for the verification of pendulum impact test machines according to ISO 148-2 (Metallic materials - Charpy pendulum impact test – Part 2: Verification of testing machines). The absorbed energy (KV) is operationally defined and refers to the impact energy required to break a V-notched test piece of standardised dimensions, as defined in ISO 148-1. The certified value of ERM-FA013bx is made traceable to the SI, via the SI-traceable certified value of the master batch ERM®-FA013ba, by testing samples pieces of ERM-FA013bx and ERM-FA013ba under repeatability conditions on an impact pendulum verified and calibrated with SI-traceably calibrated tools. The certified value is valid only for strikers with a 2 mm tip radius. The certified value is valid at (20 ± 2) °C.JRC.F.6-Reference Material

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 fipronil sulfone and the sum of fipronil and fipronil sulfone expressed as fipronil in egg powder ERM-BB125

This report describes the production of the ERM-BB125, which is an egg material certified for the mass fraction of fipronil sulfone and the sum of fipronil and fipronil sulfone expressed as fipronil. This material was produced following ISO 17034 and is certified in accordance with ISO Guide 35. Eggs from a farm embargoed by the Belgian food safety authorities were freeze-dried, cryo-milled and homogenised. Between-unit homogeneity was quantified and stability during dispatch and storage were assessed in accordance with ISO Guide 35. 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 during validation studies. The CRM is available in sealed glass vials containing at least 5 g of dried egg powder. The minimum amount of sample to be used is 1 g of the dry material.JRC.F.6-Reference Material

EURL-FA Control Proficiency test report: Determination of authorised coccidiostats in compound feed

The European Union Reference Laboratory for Feed Additives (EURL-FA), hosted by the Joint Research Centre (JRC), a Directorate General of the European Commission, has been mandated by the Directorate General for Health and Food Safety (DG SANTE) to organise a proficiency test (PT) among appointed National Reference Laboratories (NRLs) in the frame of its control activities (according to the Regulation (EC) No 882/2004 [1]). The aim of this PT was to assess the capacity of the NRLs to correctly determine selected authorised coccidiostats added to feed matrices at realistic authorised levels and at cross-contamination levels. Thirty-six European National and Official Control laboratories were invited and twenty-nine laboratories registered to the 2017 PT exercise. Twenty-five of the registered laboratories reported results for the analyses. The test items used in this exercise were produced by the JRC. Purchased commercial poultry compound feed, tested by the EURL-FA Control as being blank for the target analytes, was milled and ground and then spiked with the required coccidiostat standard solution or with the relevant authorised feed additive. The first item was spiked with a standard solution containing monensin, narasin and diclazuril, at cross-contamination level (MAT 1). The second test item (MAT 2) was spiked with an authorised feed additive Maxiban®, containing narasin (narasin AL) and nicarbazin, at additive level. MAT 1 and MAT 2 were subsequently homogenised and distributed in glass bottles. All bottles were labelled ensuring a random number encoding and dispatched to all registered participants on 27 June 2017. Laboratories were informed of the composition of the test material regarding the composition in coccidiostats for MAT 2 and had therefore only to quantify the content. For MAT 1 the laboratories had to screen for the presence of all 11 authorised coccidiostats and to quantify the detected ones. The assigned values (xpt) for the mass content of monensin, diclazuril and narasin in MAT 1 were calculated from the formulation as recommended by the IUPAC harmonized protocol [2]. The uncertainties for the assigned values (u(xpt)) were calculated according to the ISO Guide for the Expression of Uncertainty in Measurement (GUM) [3]. For narasin and nicarbazin in MAT 2, no assigned value was set since the criterion for sufficient homogeneity could not be met. Participants were invited to report their measurement uncertainties. This was done by twenty-three out of twenty-five reporting participants for monensin and narasin, seventeen for diclazuril, and twenty for narasin AL and nicarbazin. Laboratory results were rated using z and ζ (zeta) scores in accordance with ISO 13528:2015 [4]. The relative standard deviation for proficiency assessment (σpt) for each assigned value was calculated using the relevant Horwitz [5] or modified Horwitz equation [6]. The z scores obtained were considered satisfactory if their absolute values were equal to or below 2. The outcome of this PT exercise is mixed; the percentage of satisfactory results reported by the laboratories for MAT 1 is 88%, 80% and 57% for monensin, narasin and diclazuril respectively. For narasin AL and nicarbazin in MAT 2, no scoring was computed but the data reported by the laboratories were examined. In general, there was good agreement among the values of mass content of narasin and nicarbazin reported results. The laboratories also reported qualitative results as regards the presence of one or more of the other authorised coccidiostats. On the whole, the rate of false positive results was of 4% for robenidine, lasalocid, salinomycin and maduramicin; 5% for nicarbazin; 8% for decoquinate; and 0% for all the others. Two laboratories did not quantify diclazuril in MAT 1 while stating a limit of quantification of the method used lower than the assigned value, leading to a false negative rate of 9% for this analyte. One laboratory could not quantify diclazuril in MAT 1 due to the lack of sensitivity of the method used.JRC.F.5-Food and Feed Complianc

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