Use of aluminum containers in the determination of oxygen in organic substances by elemental microanalysis

The possibility of using cheap aluminum containers in oxygen elemental microanalysis of organic substances was studied. The absolute values of oxygen retention displayed by aluminum containers, as compared with silver ones, for CH(N)O(S)(Br) substances are shown. The magnitude of retention due an aluminum container is reproducible under given conditions. The precision and accuracy of the results of oxygen determination in CH(N)O compounds pyrolyzed in aluminum containers at 980 °C do not differ from the precision and accuracy of the results obtained with the use of silver containers.     

Matrix effects in (ultra)trace analysis of pesticide residues in food and biotic matrices

If one has to determine multiple residues of modern pesticides and/or other groups of (semi)polar and/or thermally unstable contaminants with a wide range of physico-chemical properties within a single analytical run, it can be complicated to obtain low limits of quantitation (LOQ), good precision as well as relevant trueness of results for all the target analytes. Matrix components, which are unavoidably present in analyzed samples (even after the thorough clean-up step), may be responsible for miscellaneous adverse affects impairing different stages of the GC and/or LC determinative step. In this review, the nature of various types of matrix effects are discussed together with suggestions for prevention, reduction and/or compensation of their occurrence when determining troublesome analytes in foods and other complex biotic matrices.     

Evaluation of two-dimensional gas chromatography-time-of-flight mass spectrometry for the determination of multiple pesticide residues in fruit

In recent years, comprehensive two-dimensional gas chromatography (GC x GC) has attained increasing attention for its outstanding separation potential and capability to solve demanding analytical tasks. Trace level analysis of pesticides residues in complex food matrices represents such a demanding task. For some commodities, such as baby food, the requirements on method detection limits are very strict and the unambiguous confirmation of the pesticide presence based on mass spectrometric detection is required. In this work, GC x GC coupled to time-of-flight mass spectrometry (TOF MS) has been evaluated for the determination of pesticides residues in fruit samples. Twenty modern pesticides with a broad range of physico-chemical properties were analysed in apple and peach samples. It has been demonstrated that the application of comprehensive two-dimensional gas chromatography brings distinct advantages such as enhanced separation of target pesticides from matrix co-extracts as well as their improved detectability. The limits of detection of the pesticides comprised in the study (determined at S/N = 5) ranged from 0.2 to 30 pg, injected with the exception of the last eluted deltamethrin, for which 100 pg could be detected. When compared to one-dimentional GC-TOF MS analysis under essentially the same conditions the detectability enhancement was 1.5-50-fold. Full mass spectral information by time-of-flight mass spectrometry and the deconvolution capability of the dedicated software allowed for reliable identification of most pesticides at levels below 0.01 mg/kg (< 10 pg injected) in fruit. Performance characteristics of the GC x GC-TOF MS method, such as linearity of calibration curves, repeatability of (summed) peak areas, as well as repeatability of first and second dimension retention times, were shown to fully satisfy the requirements for trace level analysis of the pesticide residues in food.     

Investigation of phenolic acids in yacon (Smallanthus sonchifolius) leaves and tubers

Thin-layer chromatographic (TLC) screening of crude extracts of dried leaves and tubers of yacon (Smallanthus sonchifolius, Asteraceae) and products of acid hydrolysis of tubers on the silica gel HPTLC plates using the developing solvents ethyl acetate-formic acid-water (85:10:15, v/v/v) and n-hexane-ethyl acetate-formic acid (20:19:1, v/v/v) proved the presence of chlorogenic, caffeic and ferulic acid. These phenolic acids were isolated from the crude extract of yacon leaves by preparative TLC, and identified after elution by HPLC/MS, as well as by direct injection of the crude extract into the HPLC/MS system. Acid hydrolysis of tubers released the increased amount of phenolic acids (e.g. caffeic acid and ferulic acid), flavonoid quercetin and an unidentified flavonoid, which was detected by TLC analysis. Ferulic acid, isomers of dicaffeoylquinic acid and still an unidentified derivative of chlorogenic acid (Mr = 562) as constituents of yacon leaves and ferulic acid as constituent of yacon tubers are reported here for the first time. These acids gave significant contribution to the radical scavenging activity detected directly on the TLC plate sprayed with 1,1-diphenyl-2-picrylhydrazyl (DPPH).     

Characterization of dextrans by size-exclusion chromatography on unmodified silica gel columns, with light-scattering detection, and capillary electrophoresis with laser-induced fluorescence detection

Unmodified silica gel size-exclusion columns were used in an on-line combination with light-scattering detection for a size characterization of dextrans. The influence of electrostatic interactions on analyte retention was briefly investigated. Size-exclusion chromatography was also used for evaluation of the fluorescence labeling procedure for dextrans with 8-aminonaphthalene-1,3,6-trisulfonic acid. The derivatives obtained through this procedure were used for electrophoretic measurements with laser-induced fluorescence detection. A comparison between the size-exclusion data and capillary electrophoresis indicates that the effectiveness of fluorescent labeling decreases with molecular mass of the dextran analytes.     

Solubility in the Systems MCl (M = Na, K)–1,4-Dioxane–Water at 25 ^C

Phase equilibria in the ternary systems, sodium chloride–dioxane–water and potassium chloride–dioxane–water, have been studied at 25 ^C and a section method for the determination of the immiscibility boundary has been tested. The phase diagrams exhibit the difference between the two systems. In the sodium chloride system an area of two liquid phases occurs, whereas with potassium chloride only a smooth solubility curve exists.Dedicated to Prof. Jaroslav Podlaha, an extraordinary chemist and great human being, on the occasion of his 70th birthday.     

Reactions of 2-Phosphonylethynylated 2-(Arylamino)malonates with Some Bases

Russian Journal of General Chemistry - The reaction of dialkyl 2-[(dialkoxyphosphoryl)ethynyl]-2-(arylamino)malonates with bases (CH3COOK, t-BuOK) can serve as a method for preparing original...     

Formation of microcracks upon the dynamic fracturing of rocks

The results from experimental studies on the parameters of microcracks formed after the dynamic fracture of rocks, performed by means of electron microscopy, are presented. Some physical aspects and mechanisms of the formation of microcracks in rocks are discussed. It is noted that an important characteristic of microcracks is the magnitude of their opening. According to experiments, the minimum value of the opening of microcracks is ~0.1 μm.     

Transformations of hydrated titanium dioxide in hydrothermal treatment

X-ray diffraction analysis, transmission electron microscopy, IR spectroscopy, mass spectrometry, chemical analysis, and thermogravimetry were used to study transformations in the course of a hydrothermal treatment (150–240°C of samples of hydrated titanium dioxide produced by thermal hydrolysis of sulfuric acid solutions of titanium(IV) compounds), in water. The dependences of the dispersion and chemical composition of the samples obtained on the thermal treatment temperature were determined.