Determination of the specific heat using laser flash apparatus

Journal of Thermal Analysis and Calorimetry - The main aim of this article was to describe the methodology for the measurement of specific heat using the laser flash apparatus. The obtained values...     

Determination of acid volatile sulphur in river sediments by ICP-OES coupled with purge and trap method

The developed and tested method is based on the acid volatile sulphur (AVS) releasing from a sample of sediment by acidification with hydrochloric acid and sequential absorption of released hydrogen sulphide into the absorption solution of sodium hydroxide. Total sulphur absorbed in the absorption solution is subsequently determined by inductively coupled plasma optical emission spectrometry (ICP-OES) technique. The method was tested using both model and real samples of the river sediment. Obtained results were compared with the results of iodometric determination as the method routinely used for the AVS determination. In case of using ICP-OES with purge and trap, there is no spectral interference of calcium; therefore for the determination of sulphur, it is possible to use atomic emission line of sulphur S I 180.7 nm. The tested method provides the results comparable with the iodometric method within the range of tested concentrations. The detection limit (LOD) of this method is 0.09 mg· S^2? ? L^?1 in the absorption solution which corresponds to 0.23 mg S^2?·kg^?1 in a sediment. Value of LOD is comparable with the iodometric determination.     

In-line coupling of microextractions across polymer inclusion membranes to capillary zone electrophoresis for rapid determination of formate in blood samples

Polymer inclusion membranes (PIMs) have several important features, i.e., PIMs are dry and non-porous membranes, which can be prepared ahead of use and stored without noticeable deterioration in extraction performance. In this contribution, in-line coupling of microextractions across PIMs to a separation method for clinical purposes was demonstrated for the first time. Formate (the major metabolite in methanol poisoning) was determined in undiluted human serum and whole blood by capillary zone electrophoresis (CZE) with simultaneous capacitively coupled contactless conductivity detection (C⁴D) and UV–Vis detection. A purpose-made microextraction device with PIM was coupled to a commercial CZE instrument in order to ensure complete automation of the entire analytical procedure, i.e., of formate extraction, injection, CZE separation and quantification. PIMs for formate extractions consisted of 60% (w/w) cellulose triacetate as base polymer and 40% (w/w) Aliquat™ 336 as anion carrier. The method was characterized by good repeatability of peak areas (≤7.0%) and migration times (≤0.8%) and by good linearity of calibration curves (r² = 0.993–0.999). Limits of detection in various matrices ranged from 15 to 54 μM for C⁴D and from 200 to 635 μM for UV–Vis detection and were sufficiently low to clearly distinguish between endogenous and toxic levels of formate in healthy and methanol intoxicated individuals. In addition, PIMs proved that they may act as phase interfaces with excellent long-term stability since once prepared, they retained their extractions properties for, at least, two months of storage.     

Utilization of GDOES for the study of friction layers formed on the surface of brake discs during the friction process

The paper deals with the chemical characterization of friction layer, generated on the surface of friction materials during the friction test using the glow discharge optical emission spectrometry (GDOES). Friction layer is formed during the friction process and its character depends on several factors. One of the most important factors is the material composition of brake pads and brake disc. When the brake pressure is released at the end of the braking event, the specific friction layer remains on the surface of both pairs (brake pads and brake disc). Using the GDOES profile analysis, the thicknesses of friction layers were estimated and these results were compared with results obtained by scanning electron microscopy together with X-ray microanalysis.     

Untersuchung der verdickung von latex-dispersionen durch ethylacrylat-methacrylsäure-copolymere

Zusammenfassung Es wurden dynamische and stationdre Scherversuche durchgeführt, um den Verdickungseinfluß von Copolymeren aus Ethylacrylat and 15, 40 bzw. 65 Gew. % Methacrylsdure auf Latex-Dispersionen aus Ethylacrylat mit 0 bzw. 1 Gew. % Acrylsaure zu untersuchen. Nach Überschreiten eines Schwellwertes der Verdickungsmittelkonzentration, welche mit dem Sauregehalt im Verdickungsmittel und im Latex abnahm, wurde ein starker Anstieg des Speicher-und Verlust-Moduls (G and G) sowie der Fließgrenze und der Thixotropie beobachtet. Gleichzeitig wurde ein Überwiegen der viskosen Eigenschaften sowie eine zunehmende Flockulationsfähigkeit des Verdickungsmittels festgestellt. Bei größerem Säuregehalt im Latex überwogen die elastischen Eigenschaften, gleichzeitig erhöhte sich die Bestandigkeit gegen Flockulation. Die Verdickungswirkung der unterschiedlich zusammengesetzen Systeme wird durch die Ausbildung einer Raumnetzstruktur erklärt. Das Flockulationsverhalten wird auf Änderungen der Ladung und des freien Volumens zurückgeführt.

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The thickening effect of latices of ethylacrylate-methacrylic acid copolymers (15, 40, and 65 wt. % of the acid) on latices of ethylacrylate-acrylic acid copolymers (0 and 1 wt. % of the acid) was studied by using dynamic and steady shear flow measurement. It was found that beyond a certain concentration of the thickener the storage modulus G, the loss modulus G, the yield stress values, and thixotropic behavior rapidly increased. At the same time, viscous properties and the flocculation ability of the thickeners prevailed. On the contrary, an increase in acid content in the latex made the elastic properties and flocculation resistance of the system more pronounced. The thickening effect is explained by the formation of an ordered structure. The flocculation behavior is explained by changes of the electrical charge and the free volume.

Teilweise vorgetragen an der Jahrestagung der Deutschen Rheologischen Gesellschaft, 13.–15. Mai 1991, Berlin.     

Distribution of Platinum and Palladium between Dissolved,Nanoparticulate, and Microparticulate Fractions of Road Dust

Ageing processes of vehicle catalytic converters inevitably lead to the release of Pt and Pd into the environment, road dust being the main sink. Though Pt and Pd are contained in catalytic converters in nanoparticulate metallic form, under environmental conditions, they can be transformed into toxic dissolved species. In the present work, the distribution of Pt and Pd between dissolved, nanoparticulate, and microparticulate fractions of Moscow road dust is assessed. The total concentrations of Pt and Pd in dust vary in the ranges 9–142 ng (mean 35) and 155–456 (mean 235) ng g⁻¹, respectively. The nanoparticulate and dissolved species of Pt and Pd in dust were studied using single particle inductively coupled plasma mass spectrometry. The median sizes of nanoparticulate Pt and Pd were 7 and 13 nm, respectively. The nanoparticulate fraction of Pt and Pd in Moscow dust is only about 1.6–1.8%. The average contents of dissolved fraction of Pt and Pd are 10.4% and 4.1%, respectively. The major fractions of Pt and Pd (88–94%) in road dust are associated with microparticles. Although the microparticulate fractions of Pt and Pd are relatively stable, they may become dissolved under changing environmental conditions and, hence, transformed into toxic species.     

Effects of Hydrogen Peroxide on In Vitro Cultures of Tea (Camellia sinensis L.) Grown in the Dark and in the Light: Morphology,Content of Malondialdehyde,and Accumulation of Various Polyphenols

Tea plants (Camellia sinensis L.) are phenol-accumulating crops that are widely used for public health. The healing effect of tea leaf products is due to the biosynthesis of such phenolic compounds (PCs) as flavans, which have P-vitamin capillary-strengthening activity. Due to their limited habitat and the value of their specialized metabolites of a phenolic nature, a promising approach is to establish in vitro cultures from them that retain the ability to form PCs, which is characteristic of ex vivo tea plants. The aim of this study was to investigate the effect of exogenic H₂O₂ (0.01 mM; 0.1 mM; 1 mM) on the growth, morphology, degree of stress response, and accumulation of various phenolic compounds in tea plant callus cultures of different ages (24 or 36 days) grown under different cultivation conditions (darkness or light). According to the results obtained, the H₂O₂ effect on tea callus cultures of different ages did not cause changes in their morphophysiological characteristics, both after 2 h of exposure (rapid response of callus culture, RRCC) and after 48 h (delayed response of callus culture, DRCC). The determination of the malondialdehyde (MDA) content, which serves as an indicator of changes in the level of lipid peroxidation (LPO) and the presence of stress responses in plant cells, indicated either its maintenance at the control level, a decrease, or an increase. All these effects depended on the growth conditions of the tea callus cultures (darkness or light), their age, the duration of exposure (rapid or delayed response), and the H₂O₂ concentration. Similar trends were noted for the total content of PCs as well as the amount of flavans, proanthocyanidins (soluble and insoluble forms), and lignin. The plant cell responses reflected changes in its adaptation programs, when specialized metabolites act as a target for the action of H₂O₂, thereby contributing to an increase in their resistance.     

Synthesis,Leishmanicidal, Trypanocidal,Antiproliferative Assay and Apoptotic Induction of (2-Phenoxypyridin-3-yl)naphthalene-1(2H)-one Derivatives

The coexistence of leishmaniasis, Chagas disease, and neoplasia in endemic areas has been extensively documented. The use of common drugs in the treatment of these pathologies invites us to search for new molecules with these characteristics. In this research, we report 16 synthetic chalcone derivatives that were investigated for leishmanicidal and trypanocidal activities as well as for antiproliferative potential on eight human cancers and two nontumor cell lines. The final compounds 8–23 were obtained using the classical base-catalyzed Claisen–Schmidt condensation. The most potent compounds as parasiticidal were found to be 22 and 23, while compounds 18 and 22 showed the best antiproliferative activity and therapeutic index against CCRF-CEM, K562, A549, and U2OS cancer cell lines and non-toxic VERO, BMDM, MRC-5, and BJ cells. In the case of K562 and the corresponding drug-resistant K562-TAX cell lines, the antiproliferative activity has shown a more significant difference for compound 19 having 10.3 times higher activity against the K562-TAX than K562 cell line. Flow cytometry analysis using K562 and A549 cell lines cultured with compounds 18 and 22 confirmed the induction of apoptosis in treated cells after 24 h. Based on the structural analysis, these chalcones represent new compounds potentially useful for Leishmania, Trypanosoma cruzi, and some cancer treatments.