Evaluation of the performance of the short-listed candidate markers regarding the technical requirements: Call for expression of interest to present products suitable for use as a marker in gas oils and kerosene

The European Commission adopted the Euromarker (SY124) in 2001 as a common pan-European fiscal marker to label gas oil and kerosene. In parallel, several other marking systems based on other dyes and markers were already in use in different member states. Generally the use of a marker makes it possible to sell fuel with a lower tax for use in dedicated sectors like agriculture, marine use and for domestic heating. In contrast, non-marked fuels are normally fully taxed and intended for road transport. Unfortunately SY124 is easy to remove or destroy which has made wide-spread fraud possible. This has resulted in substantial losses of tax revenue and a number of member states have repeatedly notified the European Commission of this problem. Some member states currently invest considerable amounts of resources and effort in tracking illegal use of laundered fuel by performing >10,000 measurements per year of SY124 in gasoil and diesel. Other member states have recently adopted a new national marker to prevent this kind of fraud. To improve the situation on a European level DG TAXUD published an open call in order to find a new marker that could potentially replace SY124 as Euromarker. To support DG TAXUDs policies to find a better fiscal marker, JRC has performed different kinds of tests resulting in more than 1200 samples for checking resilience of four candidate markers alongside with SY124. Generally the tests involved laundering over different adsorbents, chemical break-down and different physical treatments. All new candidate markers are colourless but road-side detection of the candidate markers is possible and based on dedicated instrumentation. Based on these experiments one candidate marker outperforms the others and is resilient to most treatments. This candidate marker could potentially be used to replace SY124.JRC.F.6-Reference Material

CERTIFICATION REPORT: The certification of the cold filter plugging point (CFPP) and cloud point (CP) in automotive diesel fuel containing a volume fraction of 7 % biodiesel: ERM®-EF004

This report describes the production of ERM®-EF004, which is an automotive diesel fuel material containing a volume fraction of 7 % fatty acid methyl ester (biodiesel) certified for the cold filter plugging point and the cloud point. This material was produced following ISO Guide 34:2009 and is certified in accordance with ISO Guide 35:2006. The material is an automotive diesel fuel containing a volume fraction of approximately 7 % biodiesel that is based on rapeseed oil fatty acid methyl ester with the addition of 1 g/kg antioxidant (butylhydroxytoluene). It was provided by a producer in Germany. The material was filled in amber glass ampoules. Between unit-homogeneity was quantified and stability during dispatch and storage were assessed in accordance with ISO Guide 35:2006 [ ]. Within-unit homogeneity was not quantified as the minimum sample intake is defined by the required sample volume stipulated in the respective documentary standard and comprises almost the whole volume of the two ampoules of every unit. The material was characterised by an interlaboratory comparison of laboratories of demonstrated competence and adhering to ISO/IEC 17025:2005). 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 quality control and assessment of method performance. As with any reference material, it can be used for establishing control charts or validation studies. The certified reference material (CRM) is available in sets of two amber glass ampoules, each containing 27 mL of automotive diesel fuel material with a volume fraction of 7 % biodiesel closed under argon atmosphere.JRC.F.6-Reference Material

Evaluation of EC Measurement Comparison for 137Cs, 40K and 90Sr in Milk Powder

This report describes the full life cycle of the measurement comparison of 137Cs, 40K and 90Sr in milk powder among 60 European laboratories monitoring radioactivity in food and the environment. An available IAEA reference material was re-processed at IRMM into suitable intercomparison samples and the homogeneity of the distributed samples together with other quality parameters was determined. Reference values of the three radionuclides under study in this intercomparison were determined at IRMM using tracer techniques and standardised radionuclide solutions and are thus traceable to the SI units. The sample preparation and measurement processes applied in the participating laboratories are described and the results of the intercomparison are presented and discussed in detail. Whereas, in general, the measurement results for 137Cs and 40K show good agreement with the reference value, the results of this comparison point at problems of 90Sr determination in about one third of the laboratories. The corresponding participants should investigate and revise their analytical methods, next to many laboratories needing to improve their estimation of measurement uncertainty.JRC.D.4-Isotope measurement

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

Precision of test methods to assess the release of organic substances from construction products

The precision of the methods developed by the European Committee for Standardization (CEN) to assess the release of dangerous organic substances from construction products was evaluated as part of the validation of the methods aiming to convert them in EU standards. This evaluation of precision was done by an interlaboratory comparison organised by the Joint Research Centre (JRC) of the European Commission, in support of the Regulation 305/2011/EU (Construction Products Regulation). The present study focused on organic substances since inorganic substances were studied in previous work. The objective of this work was to evaluate for organic substances the precision (repeatability and reproducibility) of the methods developed by CEN Technical Committee 351 on dynamic surface leaching and up-flow percolation procedures from construction products, analysis of leachates/eluates and content analysis. This was done by comparing the results obtained by different laboratories when they analysed samples obtained from the same materials using the CEN methods under validation. The materials and analytes were proposed by CEN Technical Committee 351 to cover a reasonable range of products and substances at measurable levels. Validation plans were drawn up by the JRC in agreement with CEN/TC351. The tested substances were biocides, phthalates, mineral oil, polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs); and the selected construction products were render, sealant, asphalt aggregate and recycled aggregate. The methods assessed were horizontal dynamic surface leaching test CEN/TS 16637-2; horizontal up-flow percolation test CEN/TS 16637-3; content of organic substances – methods for extraction and analysis CEN/TS 17331; and analysis of organic substances in eluates CEN/TS 17332. Specific methods were used for the determination of biocides (WI 351035) and PAHs (WI 351034). Raw materials were obtained from industrial providers and processed to obtain laboratory samples at the JRC premises in Geel, Belgium. This interlaboratory test was open to expert laboratories from all Member States. Despite all efforts to recruit a higher number of participants, eventually 12 laboratories registered to the study and reported results; between 5 and 7 laboratories analysed each of the product following the CEN methods mentioned above. Precision of the reported results was evaluated according to ISO 5725-2. The obtained values for repeatability and reproducibility are shown in the annexes of this JRC report, together with the content levels, for each construction product and analyte within this study. For the dynamic surface leaching test CEN/TS 16637-2, relative repeatability standard deviation (RSDr) was 6 % and relative reproducibility standard deviations (RSDR) was 54 % (median values). Because of limited stability of biocides in water, it is recommended to assess their release at leaching times shorter than 64 days and to store the leachates in dark glass bottles at 4ºC. For the up-flow percolation test CEN/TS 16637-3, RSDr of 20 % and RSDR of 70 % were obtained as median values. For the analysis of eluates, RSDr were 2-32 % and RSDR were 23-51 %. And for content analysis, the values for RSDr are 6-9 % and for RSDR 27-63%. Due to the limited number of participants, any conclusion or recommendation must be made with the utmost care. However, despite the limited number of participants which might affect the robustness of this study, the results obtained for organic substances are consistent with the ones obtained for inorganic substances. Therefore it seems reasonable to incorporate the RSD values for organic substances to the standard methods.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

CERTIFICATION REPORT The certification of the mass concentration of As, Cd, Co, Cu, Mn, Mo, Ni and Pb, and density in seawater: ERM®-CA403

Summary This report describes the production of ERM®-CA403, a seawater material certified for the density and the mass concentrations of As, Cd, Co, Cu, Mn, Mo, Ni, and Pb. The material was produced following ISO Guide 34:2009. The starting material was 1500 L of seawater collected at Southern Bight just inside of Belgian territorial waters. The sample was filtered, acidified and spiked before filling into 500 mL high density polyethylene (HDPE) bottles which were placed into an aluminised PET/M (metallized polyethylene terephthalate) sachets. The material was sterilised by gamma irradiation. Between unit-homogeneity was quantified and stability during dispatch and storage were assessed in accordance with ISO Guide 35:2006 . Due to the inherent homogeneity of filtered water samples, determination of minimum sample intake (within-unit heterogeneity) was not required. The material was characterised by an inter-comparison among laboratories of demonstrated competence and adhering to ISO/IEC 17025:2005. Technically invalid results were removed but no outlier was eliminated on statistical grounds only. Uncertainties of the certified values were calculated in compliance with the Guide to the Expression of Uncertainty in Measurement (GUM) and include uncertainties related to possible inhomogeneity, and instability and to characterisation. The material is intended for the quality control and assessment of method performance. As any reference material, it can also be used for control charts or validation studies. The certified reference material (CRM) is available in bottles containing 500 mL of seawater. 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

CERTIFICATION REPORT: The certification of the mass fraction of Solvent Yellow 124 in gas oil: ERM®-EF318k

This report describes the production of ERM®-EF318k, which is a matrix material certified for the mass fraction of Solvent Yellow 124, SY124. It is a remake of ERM-EF318, which is out of stock since 2016. This material was produced following ISO Guide 34:2009 and is certified in accordance with ISO Guide 35:2006. The starting materials were commercially available B0 gas oil (B0: without biodiesel) and SY124 produced as a CRM (ERM-AC316a). The material was prepared gravimetrically using calibrated balances and the mass fraction was confirmed by independent measurements. The solution of SY124 in gas oil was ampouled under argon atmosphere and stored at 18 °C in the dark. Between-unit homogeneity was quantified and stability during dispatch and storage were assessed in accordance with ISO Guide 35:2006 [2]. The minimum sample intake was established based on the data available in the certification report of ERM-EF318. The certified value was obtained from the gravimetric preparations, taking into account the purity of the base materials. The certified value was confirmed by HPLC-UV, i.e. Community Reference Method to analyse SY124, as an independent verification method (measurements were within the scope of accreditation to ISO/IEC 17025:2005). The uncertainty of the certified value was calculated in accordance with the Guide to the Expression of Uncertainty in Measurement (GUM) [6] and includes uncertainties related to possible inhomogeneity, instability and characterisation. The material is intended for the quality control / 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 ampoules containing at least 4.2 mL of gas oil which were sealed under an atmosphere of argon. The minimum amount of sample to be used is 20 µL.JRC.F.6-Reference Material

The certification of the mass fraction of the total content of As, Cd, Cu, Hg, Pb, Se and Zn in Bladderwrack (Fucus vesiculosus): ERM®-CD200

This report describes the production of ERM®-CD200, a powdered bladderwrack material (Fucus vesiculosus) certified for the mass fraction of the total content of As, Cd, Cu, Hg, Pb, Se and Zn. The material was produced following ISO Guide 34:2009. Approximately 60 kg of brown algae seaweed (bladderwrack, Fucus vesiculosus) was collected in Galway (Ireland) and processed at IRMM (Belgium) to produce a certified reference material (CRM) of seaweed powder. The produced vials containing the processed seaweed were carefully capped, sealed and stored for further certification studies. Between-unit homogeneity was quantified as well as stability during dispatch and storage in accordance with ISO Guide 35:2006. Within-unit homogeneity was also quantified to determine the minimum sample intake. The material was characterised by an inter-laboratory comparison among 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 compliance with the Guide to the Expression of Uncertainty in Measurement (GUM) including uncertainty contribution related to possible heterogeneity and instability of the material as well as to the characterisation. The material is intended for the quality control and assessment of method performance. As any reference material, it can also be used for control charts or validation studies. The CRM is available in amber glass vials containing approximately 5 g of dried powder, placed in aluminized polythene sachet closed under a nitrogen atmosphere. The minimum amount of sample to be used is 200 mg. The CRM was 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 OF THE MASS FRACTION OF PERFLUORALKYL SUBSTANCES (PFASs) IN FISH TISSUE (PIKE-PERCH): IRMM-427

This report describes the production of IRMM-427, a fish material certified for the mass fraction of perfluoroalkyl substances (PFASs). The material was produced following ISO Guide 34:2009. The starting material for the CRM is naturally contaminated pike-perch fillets originating from the rivers Nieuwe Merwede and Amer in the Netherlands. After converting the tissue into a paste, the material was sterilized by autoclavation at 120 °C and the jars stored at 18 °C. 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 material was characterised by an intercomparison among laboratories of demonstrated competence and in most cases adhering to ISO/IEC 17025:2005. Technically invalid results were removed but no outlier was eliminated on statistical grounds only. Uncertainties of the certified values were estimated in compliance 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 any reference material, it can also be used for control charts or validation studies. The CRM is available in glass jars containing approximately 35 g of fish paste. The minimum amount of sample to be used is 1 g.JRC.D.5-Standards for Food Bioscienc