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 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

Preparation and evaluation of sufficiently homogeneous and stable reference materials for priority hazardous substances in whole water

We have prepared and evaluated three whole water test materials containing eight polycyclic aromatic hydrocarbons (PAHs), six polybrominated diphenyl ethers (PBDEs) and tributyltin (TBT) with respect to homogeneity and short-term stability. The test materials were used as samples in two inter-laboratory comparisons. The materials were composed of natural mineral water and model suspended particulate matter (SPM) containing the target compounds at ng L-1 levels. The expanded uncertainty of the estimated mass concentrations in the final test materials was obtained by combining contributions from the homogeneity, the stability and the model-SPM characterization. The whole water materials were sufficiently homogeneous and stable at 4 °C for their intended use. Twelve out of fifteen investigated target parameters could be assessed to be present with a relative combined expanded uncertainty below 25 %. The outcome of the two inter-laboratory comparisons confirmed the good quality of the test materials and the level of uncertainties associated with the estimated mass concentrations. These findings are an important contribution towards the development of whole water matrix reference materials certified for PAH, PBDE and TBT in support of the Water Framework Directive of the European Union.JRC.D.2-Standards for Innovation and sustainable Developmen

Interaction of 15 priority substances for water monitoring at ng L-1 levels with glass-, aluminium- and fluorinated polyethylene bottles for the containment of water reference materials

Certified water reference materials (CRMs) are currently not available for most of the hydrophobic organic pollutants listed in the EU Water Framework Directive (WFD). To find the most suitable container type for subsequent reference material productions, feasibility studies for the preparation of waters with polycyclic aromatic hydrocarbons (PAHs), polybrominated diphenyl ethers (PBDEs) and tributyltin (TBT) close to Environmental Quality Standards (EQS) in water have been performed. Due to the hydrophobic nature of these compounds and their tendency to adsorb onto container-walls, an adequate selection of the most appropriate material for containment, storage and transport of water reference materials is crucial. Three different materials (aluminium, amber glass and fluorinated polyethylene, FPE) and three volume ranges (500/600 mL, 1000/1200 mL and 2000/3000 mL) were tested at ng L-1 level of the target compounds. FPE shows by far the highest loss of analytes due to adsorption onto the container walls for all compounds studied. Aluminium and glass are equally suited for PAHs and PBDEs, but aluminium is unsuitable as container material for TBT due to acid cleaning requirements. The volume of the containers had no dramatic effect on the adsorption behaviour of target compounds for the different volumes tested.JRC.D.2-Standards for Innovation and sustainable Developmen

Novel concepts for preparation of reference materials as whole water samples for priority substances at nanogram-per- liter level using model suspended particulate matter and humic acids

One of the unresolved issues of the European Water Framework Directive is the unavailability of realistic water reference materials for the organic priority pollutants at low ng L-1 concentrations. In the present study three different types of ready-to-use water test materials were developed for polycyclic aromatic hydrocarbons (PAHs), poly brominated diphenyl ethers (PBDEs) and tributyltin (TBT) at ng L-1 levels. The first type simulated the dissolved phase in the water and comprised of a solution of humic acids (HA) at 5 mg/L dissolved organic carbon (DOC) and a spike of the target compounds. The second type of water sample incorporated the particulate phase in water. To this end model suspended particulate matter (SPM) with a realistic particle size was produced by jet milling soil and sediments containing known amounts of PAHs, PBDEs and TBT and added as slurry to mineral water. The most complex test materials mimicked “whole water” consequently containing both phases, the model SPM and the HA solution with the target analytes strongly bound to the SPM. In this paper the development of concepts, processing of the starting materials, characterization of the HA and model SPMs as well as results for homogeneity and stability testing of the ready-to-use test materials are described in detail.JRC.D.2-Standards for Innovation and sustainable Developmen

An interlaboratory comparison on whole water samples

The European Water Framework Directive 2000/60/EC requires monitoring of organic priority pollutants in so called “whole water” samples, i.e. in aqueous non-filtered samples that contain natural colloidal and suspended particulate matter. Colloids and suspended particles in the liquid phase constitute a challenge for sample homogeneity and stability. Within the joint research project ENV08 “Traceable measurements for monitoring critical pollutants under the European Water Framework Directive 2000/60/EC” whole water test materials were developed by spiking defined amounts of aqueous slurries of ultra-finely milled contaminated soil or sediment and aqueous solutions of humic acid into a natural mineral water matrix. This paper presents the results of an European-wide interlaboratory comparison (ILC) using this type of test materials. Target analytes were tributyl tin, polybrominated diphenyl ethers and polycyclic aromatic hydrocarbons in the ng/L concentration range. Results of the ILC indicate that the produced materials are sufficiently homogeneous and stable to serve as samples for e.g. proficiency testing or method validation. To our knowledge, this is the first time that ready to use water materials with a defined amount of suspended particulate and colloidal matter have been applied as test samples in an interlaboratory exercise. These samples meet the requirements of the European Water Framework Directive. Previous proficiency testing schemes mainly employed filtered water samples fortified with a spike of the target analyte in a water-miscible organic solvent.JRC.D.2-Standards for Innovation and sustainable Developmen