In order to quantify organic impurities in gas produced from renewable sources, thermal desorption coupled with GC-MS or GC×GC-MS is very useful. However, the preparation of the standard tubes appears not to be trivial. For that, different strategies, based on commercial setups, have been developed. The goal of this study was to compare the classical manual deposit of a liquid standard solution with other commercial methods such as gas stream assisted deposit and vaporization followed by adsorption assisted by gas stream. A standard mixture of 48 compounds from different families was used for the comparison of the performances of the three strategies using the accuracy profile methodology. A global validation score was attributed to each strategy as well as a score according to family of compounds and boiling point range, in order to provide a detailed comparison of the techniques. On the set of studied molecules, commercial setups were found to be more efficient than the manual deposit.

Vehicle interior air quality is an issue of growing interest among car manufacturers and customers. GC-MS is the benchmark method for the analysis of indoor air or material emissions. It is suitable for the quantification of target pollutants and the most abundant compounds. It fails, however, to uncover the true molecular complexity of these samples. In the present study, we describe the development of a TD-GC × GC-TOFMS method designed to detect polar and potentially odorous molecules in car material emissions. Attention is paid to the hyphenation of the thermodesorber and the gas chromatograph, both at software and hardware levels, and the constraints due to pressure limitations on the thermodesorber (evaluated at 414 kPa/60 psi at the end of the temperature ramp and at 138 kPa/20 psi at rest). A compromise was made for the 2D column length and diameter to balance separation and pressure (50 × 0.18 × 0.18 cm × mm × µm + 60 cm transfer line selected). On various materials, we were able to observe several hundreds of polar molecules, among them were between 75 and 150 odorants per material. This work lays the foundation for the widespread screening of potential odorants in car material emissions.

Several chelating agents have been employed throughout decontamination processes in nuclear industry, EDTA (ethylenediaminetetraacetic acid) being the most abundantly used. The presence of these molecules in radioactive waste can affect the mobility of radionuclides and metals in environment during the long-term storage of the nuclear waste. This is why the quantification of certain chelating agents is required during nuclear waste management. The studied samples to be analysed present numerous challenges that require careful sample preparation before their measurement. In this paper, we describe how, based on a previous protocol for the quantification of EDTA, a novel unified method was developed for the simultaneous quantification of four aminopolycarboxylic acid (EDTA, NTA, DTPA and TTHA), and gluconic acid. Suspended solids present in the samples were eliminated by filtration, then the sample was basified to ensure precipitation of remaining metallic ions and their removal. Finally, an excess of Ni2+ was added to form complexes with the majority of the analytes. Speciation modelling studies predicted dominant anionic complexes with nickel for the aminopolycarboxylic acid family while gluconic acid remained under its free gluconate form. As experimentally demonstrated, the five anionic species were separated and detected simultaneously in less than 7 min through an ion-pair mechanism using an HPLC-ESI-HRMS system. Lastly, the limits of quantification were validated between 2.5 and 6.25 mg/L for all chelating agents in sludges.

Several chelating agents have been employed throughout decontamination processes in nuclear industry, EDTA (ethylenediaminetetraacetic acid) being the most abundantly used. The presence of these molecules in radioactive waste can affect the mobility of radionuclides and metals in environment during the long-term storage of the nuclear waste. This is why the quantification of certain chelating agents is required during nuclear waste management. The studied samples to be analysed present numerous challenges that require careful sample preparation before their measurement. In this paper, we describe how, based on a previous protocol for the quantification of EDTA, a novel unified method was developed for the simultaneous quantification of four aminopolycarboxylic acid (EDTA, NTA, DTPA and TTHA), and gluconic acid. Suspended solids present in the samples were eliminated by filtration, then the sample was basified to ensure precipitation of remaining metallic ions and their removal. Finally, an excess of Ni²⁺ was added to form complexes with the majority of the analytes. Speciation modelling studies predicted dominant anionic complexes with nickel for the aminopolycarboxylic acid family while gluconic acid remained under its free gluconate form. As experimentally demonstrated, the five anionic species were separated and detected simultaneously in less than 7min through an ion-pair mechanism using an HPLC-ESI-HRMS system. Lastly, the limits of quantification were validated between 2.5 and 6.25mg/L for all chelating agents in sludges.