Volatile organo-halogen trace analysis in beverages by thin-layer headspace enrichment and electron-capture gas-chromatography

Applicability of thin-layer headspace (TLHS) procedure giving an aqueous concentrate and also classical purge and trap (PT) in off-line mode to isolate and enrich volatile organohalogen compounds in common beverages was tested. Both enrichment tech-niques were used in combination with gas chromatography – electron capture detection (GC-ECD). TLHS, combined with direct aqueous injection (DAI)-GC-ECD, proved applicable in the determination of volatile organohalogen compounds in all studied beverages, while the PT in a version with no preliminary sample pre-treatment was of limited applicability. Detection limits of the TLHS-based procedure were in the order of 1 ppt. Content of volatile organohalogen compounds in a number of beverages available on the Polish market including mineral waters, beers, juices, carbonated and non-carbonated soft drinks, etc. was determined by means of TLHS-DAI-GC-ECD.     

Analytical determination of intrinsic permeability of synthetic nonwoven filter fabrics

In this paper an analytical method for determining the permeability of nonwoven filter fabrics is presented. The derived formula shows that the intrinsic permeability, fully characterizing the porous medium, depends on fabric porosity, n, fibre diameter, d, and a shape factor determined experimentally.     

Thick film NO2 Sensor

 Thick film technology was used to manufacture a solid-state electrochemical nitrogen dioxide sensor. The prepared sensor has a linear dependence of electromotive force that is based in the NO₂ concentration level. This paper presents discussion on a thick-film sensor that has a much smaller dimension and shorter response time as compared to typical ceramic solid-state electrochemical devices. Received: 26 February 1996/Accepted: 27 June 1996     

Problems of nondestructive testing of wheel-pair components of rolling stock

Improving the effectiveness of nondestructive testing of railway rolling stock’s wheel-pair components during their manufacturing and repair is considered. The results of metallographic studies of PY-1 and PY-1III solid-rolled wheels and axles, analysis of the operating specifications, and experimental studies of the optimal methods of nondestructive testing are included.     

Strong Hydrogen Bonds in Acetylenedicarboxylic Acid Dihydrate

Acetylenedicarboxylic acid dihydrate (ADAD) represents a complex with strong hydrogen bonding between the carboxylic OH and the water molecule. An X-ray re-examination of the ADAD crystal structure confirms the O^…O distance of the short hydrogen bonds, and clearly shows different bond lengths between the two oxygen atoms with respect to the carbon atom in the carboxyl group, indicating a neutral structure for the complex. The neutral structure was also confirmed by vibrational spectroscopy, as no proton transfer was observed. The diffraction studies also revealed two polymorph modifications: room temperature (α) and low temperature (β), with a phase transition at approximately 4.9 °C. The calculated vibrational spectra are in satisfactory agreement with the experimental spectra. A comparison of the structure and the vibrational spectra between the ADAD and the oxalic acid dihydrate reveals some interesting details. The crystal structures of both crystal hydrates are almost identical; only the O^…O distances of the strongest hydrogen bonds differ by 0.08 Å. Although it was expected that a larger O^…O spacing in the ADAD crystal may significantly change the infrared and Raman spectra, especially for the frequency and the shape of the acidic OH stretching vibration, both the shape and frequency are almost identical, with all subpeaks topped on the broad OH stretching vibration. The O^…O distance dependent are only in- and out-of-plane OH deformations modes. The presence of polarons due to the ionized defects was not observed in the vibrational spectra of ADAD. Therefore, the origin of the broad OH band shape was explained in a similar way to the acid dimers. The anharmonicity of a potential enhances the coupling of the OH stretching with the low-frequency hydrogen bond stretching, which, in addition to the Fermi resonance, structures the band shape of the OH stretching. The fine structure found as a superposition of a broad OH stretching is attributed to Davydov coupling.     

The Synthesis and Properties of Diazaphenanthrene Aldehydes and their Simple Analogues

The synthesis of seven diazaphenanthrene aldehydes and their oximes via oxidation of corresponding methylderivatives is given and the n.m.r. spectra of the aldehydes are discussed. The synthesis of three new methyl diazaphenanthrenes by the Skraup method is presented.     

Synthesis of Azafluorenones

Syntheses of azafluorenones from monoazaphenanthrenes and phenanthrolines has ben investigated. 1- and 4-monoazaphenanthrenes have been oxidized by J₂O₅ in acetic acid to give quinones which were converted to 4- and 1-azafluoren-9-ones in alkaline media. Phenanthrolines can be oxidized directly by means of permanganate in alkaline medium to 1,5-, 1,6-, 1,8-, 2,5- and 3,5-diazafluoren-9-ones. From 1-, 4-azaphenanthrene- and 1,8-phenanthrolinequinones new benzopyrido- and dipyridophenazines have been synthesized.     

A generator of electrical discharges in water

A semiconductor high-voltage pulse generator for the electric-discharge water purification is described. It is based on a low-voltage capacitor storage, step-up pulse transformer, and high-voltage output circuit with a recuperation section returning inefficiently used energy to the power source of the capacitor storage.     

Prospects of further improvement of electric-discharge elastic-oscillation generators for treatment of melts in a ladle

On the basis of the functional analysis of the physicotechnical factors that have an effect on the load parameters of melts in a ladle under electrohydropulse treatment, recommendations on the further improvement of electric-discharge elastic-oscillation generators are given.