Polarographic behaviour and determination of azintamide

Azintamide was found to be reduced at the dropping mercury electrode over the pH range 1.8–9.4 in Britton Robinson buffers containing 20% methanol. At pH 7.42 a well defined diffusion-controlled cathodic wave was produced. The limiting current versus concentration plot was linear over the range 0.025–1.0 mM and 0.005–1.0 mM in the DC_t and DPP modes, respectively, with a lower detection limit of 1 × 10^–7 M by the latter technique. A mechanism for the electrode reaction has been proposed. The method has been applied to the determination of azintamide in tablets, and the results obtained were in agreement with those obtained by a reference method.AvH Scholar 1989–1991.     

Quality assurance and statistical control

In scientific research laboratories it is rarely possible to use quality assurance schemes, developed for large-scale analysis. Instead methods have been developed to control the quality of modest numbers of analytical results by relying on statistical control: Analysis of precision serves to detect analytical errors by comparing thea priori precision of the analytical results with the actual variability observed among replicates or duplicates. The method relies on the chi-square distribution to detect excess variability and is quite sensitive even for 5–10 results. Interference control serves to detect analytical bias by comparing results obtained by two different analytical methods, each relying on a different detection principle and therefore exhibiting different influence from matrix elements; only 5–10 sets of results are required to establish whether a regression line passes through the origo. Calibration control is an essential link in the traceability of results. Only one or two samples of pure solid or aqueous standards with accurately known content need to be analyzed. Verification is carried out by analyzing certified reference materials from BCR, NIST, or others; their limited accuracy of 5–10% make them less suitable for calibration purposes.     

Synthesis and structure of neutral π-arene complex (η6-C6H5Me)U(AlCl4)3

A new neutral -arene complex of trivalent uranium, (⁶-C₆H₅Me)U(AlCl₄)₃ (1), was obtained by the reductive Freidel-Crafts reaction. The crystal structure of 1 was determined by single crystal X-ray diffraction analysis. The U atom in 1 is bound to the C₆H₅Me group by the ⁶ mechanism and is linked to the three AICl₄ groups through two g-CI bridges. The coordination of the U atom is a distorted pentagonal bipyramid in which the center of the arene ring is in one apical position, and the bridging Cl atoms occupy the other vertices.Translated from Izvestiva Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 469–472, February, 1996.     

Spectrophotometric flow-injection determination of zinc in plant digests based on a spot test

A spot test was implemented in a flow-injection system for the spectrophotometric determination of zinc in digests of plant materials. It is based on the influence of Zn²⁺ on the oxidation rate of 1-naphthylethylenediamine (NED) by hexacyanoferrate(III) under acidic conditions. In order to control the precipitate formation and to maintain the resulting suspension, a micellar medium was established by adding Triton X-100. The proposed system handles about 65 samples per hour, meaning 72 μg NED and 9.0 mg K₃[Fe(CN)₆] per determination. Baseline drift is usually <0.01 absorbance per hour and the analytical signals for 0.5-2.5 mg l⁻¹ Zn range within ca. 0.07-0.45 absorbance. Linearity of the analytical curve is fair (r>0.999, n=6) and detection limit was estimated as 0.2 mg l⁻¹ Zn. Results are precise (R.S.D.<1%, n=10) and in agreement with flame atomic absorption spectrometry and with certified values of standard reference materials.     

A way of establishing quality of measurements in gas analysis—national and international aspects

Standardising quality of measurements at both the national and international level results in a unity in measurement that may be regarded a synonym of traceability. In gas analysis, the key issue in achieving this aim is production of gaseous reference materials. Establishing a network of secondary measurement standards at gaseous CRM producers’ sites in Ukraine might be interesting for those involved in gas analysis activities. Inevitably, problems concerning the recognition of measuring capabilities of both national metrological institutes and local CRM producers are now an international issue. Thus, the problems of national adoption of international standards, as well as harmonisation between different international documents are currently relevant, and Ukrainian experience may be useful to others in this field. Presented at the 3rd International Conference on Metrology, November 2006, Tel Aviv, Israel.     

Applications of thermal analysis in some solid-state reactions

TG-DTG-DTA has been used to characterize various isomers of CoCl₂·2(CH₃C₆H₄NH₂). Thermal analysis is further used to analyse the binary mixtures of these isomers. DTA recorded after different elapsed times follows the progress of reaction between cobalt chloride and benzocaine where progressively small endotherms are associated with starting materials. The application of thermal analysis to following the solid-solid reactions between metal acetates and 8-hydroxyquinoline was highlighted. The stoichiometry of such reactions was confirmed from the decrease in intensity of an endotherm as one increases the stoichiometry.Thanks are due to Drs. Keshav Chander, K. Kaur, Rajinder Singh and G. S. Chopra for helpful discussions and experimental work.     

Measuring trihalomethane concentrations in water using supported capillary membrane sampling-gas chromatography

The objective of this study was to develop and evaluate a supported capillary membrane sampling-gas chromatography method for the analysis of trihalomethanes (THMs) in drinking water. The effects of experimental parameters, such as flow rate of carrier gas, water temperature, ionic strengths of solutions and transfer line temperature on the system performance were investigated. The results of method detection limit and accuracy and precision studies are reported.     

Modern Analysis

The important advances being made in modern analytical methods are indicative of the fundamental changes that are occuring in the theory and practice of “analytical chemistry”. “Information optimization” demands a new approach in teaching and research, and calls for the intergration of chemistry with other scientific and technical disciplines.     

Modification of polysulfone membranes 4. Ammonia plasma treatment

The effect of NH₃ and NH₃/Ar plasma on ultrafiltration polysulfone membranes have been studied. Results of contact angle, FTIR-ATR and X-ray photoelectron spectroscopy experiments clearly showed that both plasmas introduced hydrophilic, nitrogen- and oxygen-containing moieties on the polymer surface and that NH₃/Ar plasma was more efficient. That plasma was also more aggressive--signs of strong etching could be seen on the SEM pictures. Redeposition of etched material seemed to take place inside the pores. On the contrary, ammonia plasma was soft and caused cleaning the surface and pores enlargement. Performance of ammonia plasma modified membranes was greatly improved and independent on solution pH. The last observation proved amphoteric character of the surface. NH₃/Ar plasma treatment gave membranes of acidic surface and filtration indices not so good as for ammonia plasma.     

简易型离子选择电极-流动注射分析仪的研制及卤水中氯、溴和碘的连续测定

本文设计研制了简单实用的流通池,组装了简易型离子选择电极—流动注射分析仪,对体系的分析特点和影响因素进行了考察。此装置性能可靠,能满足简单流注分析的需要,并建立了卤水中Cl~-、Br~-和I~-的连续测定方法。