Determination of Polycyclic Aromatic Hydrocarbons in Soils and Bottom Sediments by Gas Chromatography–Mass Spectrometry with QuEChERS Sample Preparation

Journal of Analytical Chemistry - The work is dedicated to the determination of polyaromatic hydrocarbons (PAHs) in soils and bottom sediments by gas chromatography–mass spectrometry using...     

气相色谱法探究聚醚醚酮的热降解及热氧化降解（英文）

Poly(ether ether ketone)(PEEK)was synthesized via polycondensation of hydroquinone with 4,4′-difluorobenzophenone at 320℃for 5 h.Thermal and thermo-oxidative degradation of PEEK was studied over a wide range of temperatures.In an inert medium,decomposition of the polymer occurred in one stage,with the formation of a coke residue accounting for approximately 50%of the original polymer mass.In air,the mass loss curve exhibited two distinct stages.The first stage involved breakdown of the main polymer chain,the speed of which indicated a radical chain failure mechanism.In the second stage,the rate of mass loss clearly decreased,indicating a transition from the radical chain failure mechanism to simple combustion reactions(wherein the polymer combusted completely).To further investigate the nature of the processes occurring during the pyrolysis of PEEK,the investigations were carried out using gas chromatograph under isothermal conditions.It was concluded that during thermal degradation,the decomposition of the polymer starts with the rupture of ketone and ether bonds and proceeds to destruction of the benzene ring at higher temperatures,which is accompanied by the formation of H2O and CH4.Above 500℃,the polymer degradation further involved thermohydrolysis.The thermo-oxidation of PEEK,which was accompanied mainly by the formation ofH2,was noticeable beginning at 325℃.The total yield of the latter indicated oxidation of fragments of the benzene ring.     

Fluorine-functionalized nanoporous graphene as an effective membrane for water desalination

Most water in the world is as saline water in seas and oceans. Desalination technology is a promising method to solve the global water crisis. Recently, many attentions have been paid to the graphene-based membranes in water desalination due to their low production cost and high efficiency. In this paper, molecular dynamics simulations are employed to investigate the effect of functionalized graphene nanosheet (GNS) membranes on the performance of salt separation from seawater in terms of water permeability and salt rejection. For this purpose, the hydrogenated (–H) and fluorinated (–F) pores were created on the GNS membrane. Then, the functionalized graphene membrane was placed in the middle of the simulation box in an aqueous ionic solution containing Na⁺ and Cl^? ions. The applied pressure (in the range of 10–100 MPa) was used as the driving force for transport of water molecules across the reverse osmosis (RO) graphene-based membrane in order to obtain the water permeability and salt rejection. Also, radial distribution functions (RDFs) of ion–water and water–water as well as the water density map around the membrane were obtained. The results indicated that the hydrophilic chemical functions such as fluorine (–F) can improve the water permeability at low pressures.

     

Preparation and properties of silica gel with immobilized formazan group

A new sorption material, silica gel with covalently immobilized formazan group, was suggested and characterized. The material was prepared by coupling the immobilized aryldiazonium salt with benzaldehyde phenylhydrazone. The equilibrium and kinetic characteristics of the sorption of Cu(II), Co(II), Ni(II), and Cd(II) from solutions onto the modified silica gel were determined. The material proved to efficiently concentrate Cu(II) from multicomponent solutions. The coordination surrounding of Cu(II) in the complex on the sorbent surface was determined by ESR.     

Indirect voltammetric determination of total surfactants in waters

The effect of anionic, cationic, and nonionic surfactants on anodic peaks of metals in their voltammetric determination was studied. It was shown that the total of synthetic surfactants in waters can be determined. Neonol was chosen as a reference substance for the determination of synthetic surfactants in solution; zinc and cadmium were chosen as reference elements     

Simultaneous Dispersive Liquid–Liquid Microextraction and Determination of Different Polycyclic Aromatic Hydrocarbons in Surface Water

Polycyclic aromatic hydrocarbons (PAHs) are a class of persistent organic pollutants of water, and their determination at trace levels in the aquatic ecosystems is essential. In this work, an ultrasound-assisted dispersive liquid–liquid microextraction (DLLME) procedure was suggested utilizing a binary dispersive agent for recovery of different molecular weight polycyclic aromatic hydrocarbons (PAHs) from waters. The detection was carried out by gas chromatography–mass spectrometry (GC-MS) as well as high-performance liquid chromatography with fluorescence and diode-array detection (HPLC-FD/PDA). The method was optimized for the extraction of analytes with respect to the mixture composition, ratios of components, ultrasonication time and centrifugation parameters. The analytical schemes for PAHs extraction from water samples using different ratios of extraction and dispersive solvents are reported. The mixture consisting of chloroform and methanol was applied for the extraction of PAHs containing two or three fused aromatic rings; the mixture of chloroform and acetonitrile is suitable for PAHs containing more than four aromatic rings. The mixture of chloroform:acetone + acetonitrile was applied in the universal scheme and allowed for the simultaneous extraction of 20 PAHs with different structures. The developed sample preparation schemes were combined with GC-MS and HPLC-FD/PDA, which allowed us to determine the analytes at low concentrations (from 0.0002 µg/L) with the recoveries exceeding 80% and relative standard deviations of about 8%. The developed methods for the determination of 20 PAHs were applied to the analysis of water samples from the Karasun Lake (Krasnodar), Azov Sea (Temryuk) and Black Sea (Sochi).     

Supplemental Educational Programs as a Tool for Expanding the Professional Skills of Analytical Chemists

The requirements for the minimum content and level of training to give the supplemental Expert in Environmental Safety qualification to graduates of classical universities specializing in chemistry (specialty no. 011000) were developed. An educational program is proposed. The program can be used as an efficient supplement of the professional training of students specializing in analytical chemistry; it allows the level of stating analytical problems and interpreting analytical results (for environmental samples) to be improved. The program has been approved by the Ministry of Education of the Russian Federation. It has already been launched at the Chemical Faculty of the Kuban' State University.     

LC–MS/MS Determination of Catecholamines in Urine Using FMOC-Cl Derivatization on Solid-Phase Extraction Cartridge

A method for the determination of catecholamine derivatives in human urine is proposed that includes the derivatization of target compounds on a solid-phase extraction cartridge and determination of the analytes by a UHPLC method with tandem mass-spectrometric detection. 9-Fluorenyl-methoxycarbonyl chloride was used as the derivatization agent. The limits of detection for the analytes were 2.5 ng mL^?1 for 9-fluorenyl-methoxycarbonyl-adrenaline, 5 ng mL^?1 for 9-fluorenyl-methoxycarbonyl-octopamine, and 25 ng mL^?1 for 9-fluorenyl-methoxycarbonyl-dopamine. The proposed procedure was tested on real samples obtained from volunteers.