Chrysoula Kanakaki,1 Alfred Amon,2 Atanaska Trifonova,2 Erwin Rosenberg1
1 Vienna University of Technology, Institute of Chemical Technologies and Analytics, Getreidemarkt 9/164 AC, A-1060 Vienna, Austria
Rechargable Li-ion batteries have become an indispensable element of our daily life, as they power up laptops and mobile phones, consumer electronics, medical devices, and also electric and hybrid vehicles . For electrical transportation they are typically used in much larger aggregates. The larger scale of these batteries increases the hazard arising from malfunctioning or misuse significantly, and has thus prompted detailed studies regarding the safety of Li-ion batteries and particularly their electrolytes under extreme conditions. This electrolyte, consisting of a mixture of organic carbonates with the addition of a suitable lithium salt, degrades already under conditions of normal use, but even more under extreme conditions of temperature or overcharging/overdischarging, as well as under mechanical stress, thereby forming degradation products that represent both a fire or explosion hazard, and also may be toxicologically relevant.
We report here on the chromatographic characterization of the organic electrolyte and its volatile degradation products under conditions of normal use as well as after exposure to thermal and electrochemical stress. The great variety of reaction products formed under these conditions requires the application of different chromatographic techniques for their characterization . In particular, GC/MS and HPLC/MS are advantageously used for the characterization of the volatile degradation products and the electrolyte, respectively. Both an off-line and an on-line approach for the sampling of the volatile emissions from the headspace have been investigated, the latter also allowing the dynamic behavior of the emissions to be studied. Various experimental set-ups have been developed and applied to this end, and their performance and analytical potential will be presented and critically discussed [3,4].
Financial support of this work by the Austrian Research Promotion Agency (FFG) under Grant No. 835790 (SiLithium) is gratefully acknowledged.
J.B. Goodenough, K.-S. Park, J. Am. Chem. Soc.2013, 135, 1167-1176.
G. Gachot, P. Ribière, D. Mathiron, et al., Anal. Chem. 2011, 83, 478-485.
A. Amon, Master Thesis, Univ. of Vienna (2014).
C. Kanakaki, PhD Thesis, Vienna Univ. of Technology (in preparation, 2015)
1 National University of Science and Technology "MISIS", Leninskiy prospekt 4, 119049, Moscow, Russia
New family of heterochain N,S-containing sorbents has been synthesized by thiomethylation of polyamins. Applicability of the sorbents for extraction and concentration of noble metals (NM) and platinum group elements (PGE) was tested in the presence of macroscopic amounts of mineral and secondary raw materials for their further study by atomic-spectral methods. Quantitative information about PGE and NM was obtained by high resolution continuum source atomic absorption spectrometry (HRCS-AAS).The properties of the sorbents were studied depending on the composition and structure, the number of complex-forming groups, solvent composition, and concentration and nature of the secondary components. In order to achieve better understanding of the sorption mechanism EXAFS investigation at Pt LIII edge was performed using ANKA synchrotron source, Karlsruhe. Preliminary data suggest that Pt atoms are sulphur bonded. Kinetics of PGE, Au, Ag sorption was studied at static conditions at room temperature and on heating. Capacity of the sorbent was established. For example, for the sorbent (S - 29.40%, N - 11.89%, C - 44.28%, H - 7.36 %) the capacity is 3 g Ag per gram of the sorbent. The sorbents were developed and tested in the analytical laboratory practice “Separation and concentration in the chemical diagnosis of functional materials and objects of the environment” of NITU MISIS and the test analytical and certification center of Giredmet Institute.
The authors gratefully acknowledge the financial support of the Ministry of Education and SRF in the framework of Increase Competitiveness Program of NUST «MISiS»(№ К1-2014-026), financial support of RFBR (13-03-00440).
Mihail Simion Beldean-Galea,1 Radu Mihaiescu,1 Viorel Arghius,1 Adina Croitoru,2 Irina Ciotlaus,3 Virginia Coman3
1 Babes-Bolyai University, Faculty of Environmental Science and Engineering, 30 Fantanele Street, 400294 Cluj-Napoca, Romania
2 Babes-Bolyai University, Faculty of Geography, 5-7 Clinicilor Street, 400006 Cluj-Napoca, Romania
Priority substances are defined according to the Water Framework Directive (WFD) as the substances identified to present a significant risk to or via the aquatic environment. These substances include 45 organic compounds from different classes and heavy metals, their determination representing the base of the characterization of the chemical status of water body.
In the frame of NATO SfP 984440 Project the authors wish to develop a methodology able to identify the River Basin Specific Pollutants from Upper Tisza. For this purpose, the analysis of the priority substances in the water body is required as a starting point.
This paper contains the results of eight months monitoring of different classes of priority substances such as pesticides, halogenated compounds, polyaromatic hydrocarbons, phthalates and heavy metals performed on river water samples collected from the Upper Tisza and its Romanian Tributaries.
For the quantification of these compounds different analytical protocols based on solid phase extraction subsequent by gas and liquid chromatography were used.
The obtained results show that the priority substances found in the studied area are p,p’-DDT, chloroform, naphthalene, anthracene, fluoranthene and benzo(b)fluoranthene as organic compounds, and lead, cadmium and mercury as heavy metals. Except of p,p’-DDT and cadmium, the concentration of the other found priority substances do not exceed the Environmental Quality Standard (EQS) requirements. Other compounds not being included on this list such as acenaphthene, fluorene, phenanthrene and pyrene have also been found.
For a better estimation of the aquatic medium contamination with priority substances, analyses of sediment and biota were carried out. Specific methods for the extraction based on Soxhlet or ultrasound assisted methods followed by gas and liquid chromatography were developed. These analyses were focused on organochlorine pesticides, polyaromatic hydrocarbons and phthalates. The obtained results confirm the presence of these compounds in the analyzed samples.
Acknowledgements: This work is performed in the frame of NATO SfP 984440 Project, Science for Peace and Security Programme.
1 Waters, 9 Rue Jacques Monod, 78280 Guyancourt, France
2 Unilever R&D, Deltaweg 150, 3133 KM Vlaardingen, Netherlands
The performance and advantages of supercritical fluid chromatography (SFC) have been known already for decades. From a fundamental standpoint, SFC bridges the gap between liquid chromatography (LC) and gas chromatography (GC) combining various strengths of both technologies. UltraPerformance Convergence Chromatography (UPC²) was recently introduced and the availability of this kind of state-of-the-art SFC instrumentation opens perspectives for implementation in a variety of laboratories, in research environment as well as in laboratories carrying out routine analyses. An apparent advantage of SFC and UPC² is the increased speed that SFC allows in comparison to LC due to the higher diffusion coefficients in the supercritical mobile phase. SFC also allows fast transfer from reversed-phase applications to normal-phase chromatography. Furthermore, the selectivity can be easily altered by the modification of an important instrumental parameter in SFC, namely the pressure. Due to the properties of the mobile phase, the application of the technology can result in a broad compound coverage and hence increased flexibility covering both GC as well as LC methods. Next to these advantages, other key parameters in the development of analytical methods in the laboratories in an industrial environment are robustness, throughput and high flexibility. During this presention, the application and possibilities of the Waters UPC² instrument are presented for a wide variety of applications in the food area.