Isopoly-molybdic acids

From the measurements of conductivity, diffusion coefficient etc., Jander indicated the presence of several isopoly-anions of molybdenum under different pH conditions. He and subsequent workers in the field dealt with solutions only. In the present work one free molybdic acid, and one ammonium acid molybdate were isolated in solid condition at pH 4.6 and 2. On analysis, their compositions were found to be H₄Mo₃O₁₁ and NH₄H₅Mo₆O₂₁ (or (NH₄)₂H₄Mo₇O₂₄) respectively.     

Spectrophotometric determination of nicoumalone, acebutolol hydrochloride and procainamide hydrochloride

A sensitive spectrophotometric method is described for the determination of nicoumalone (NIC), acebutolol hydrochloride (ACBH) or procainamide hydrochloride (PAH) either in pure form or in pharmaceutical formulations. The method is based on the oxidative coupling reaction through the involvement of an aromatic primary amino group (released through reduction in NIC or hydrolysis in ACBH or existing free in PAH) in the drug with 3-methyl-2-benzothiazolinone hydrazone hydrochloride (MBTH) in the presence of ferric chloride [Fe(III)]. The resulting chromophores are measured at 620 nm for NIC and ACBH and 580 nm for PAH. The concentration measurements are reproducible within a relative standard deviation of 1%.     

Pressure induced phase transitions in hydroquinone

High pressure behavior of alpha-hydroquinone (1,4-dihydroxybenzene) has been studied using Raman spectroscopy up to pressures of 19 GPa. Evolution of Raman spectra suggests two transitions around 3.3 and 12.0 GPa. The first transition appears to be associated with the lowering of crystal symmetry. Above 12.0 GPa, Raman bands in the internal modes region exhibit continuous broadening suggesting that the system is progressively evolving into a disordered state. This disorder is understood as arising due to distortion of the hydrogen-bonded cage across the second transition around 12 GPa.     

Electron-capture gas chromatographic analysis of beta-phenylethylamine in tissues and body fluids using pentafluorobenzenesulfonyl chloride for derivatization

A gas chromatographic procedure is described for the analysis of beta-phenylethylamine (PEA) in tissues and body fluids. The method involves the use of pentafluorobenzenesulfonyl chloride for extraction and derivatization of PEA. This is followed by separation and analysis of the derivatized amine on a gas chromatograph equipped with a fused-silica capillary column and an electron-capture detector. The procedure is rapid, provides a stable and sensitive derivative, and has been applied to analysis of PEA in brain, heart, kidney, liver, lung, spleen and blood from the rat and urine from human subjects.     

Determination of gas-oil miscibility conditions by interfacial tension measurements

Processes that inject gases such as carbon dioxide and natural gas have long been and still continue to be used for recovering crude oil from petroleum reservoirs. It is well known that the interfacial tension between the injected gas and the crude oil has a major influence on the efficiency of displacement of oil by gas. When the injected gas becomes miscible with the crude oil, which means that there is no interface between the injected and displaced phases or the interfacial tension between them is zero, the oil is displaced with maximum efficiency, resulting in high recoveries. This paper presents experimental measurements of interfacial tension between crude oil and natural gases (using a computerized drop shape analysis technique) as a function of pressure and gas composition at the temperature of the reservoir from which the crude oil was obtained. The point of zero interfacial tension was then identified from these measurements by extrapolation of data to determine minimum miscibility pressure (MMP) and minimum miscibility composition (MMC). The gas-oil miscibility conditions thus obtained from interfacial tension measurements have been compared with the more conventional techniques using slim-tube tests and rising-bubble apparatus as well as predictive correlations and visual observations. The miscibility pressures obtained from the new VIT technique were 3-5% higher than those from visual observations and agreed well with the slim-tube results as well as with the correlations at enrichment levels greater than 30 mol% C2+ in the injected gas stream. The rising bubble apparatus yielded significantly higher MMPs. This study demonstrates that the VIT technique is rapid, reproducible, and quantitative, in addition to providing visual evidence of gas-oil miscibility.     

Inter-ring rotational potential of biphenyl and its effect on poly(p-phenylene)

Detailed ab initio studies have been done on the inter-ring torsional states of the biphenyl molecule using self-consistent field molecular orbital method. The potential goes through a minimum at an angle of 38°. The height of the potential barrier for the coplanar state is 2.01 kcal/mol. When the phenyl rings are perpendicular to each other, this height increases to 2.37 kcal/mol. The role of correlation and polarization is found to be important. The shape of the potential suggests that polyparaphenylene may possibly exist as a super helix.     

Extraction spectrophotometric determination of cobalt and nickel using ethylthioxanthate

A spectrophotometric method for the determination of cobalt and nickel using a new reagent sodium ethylthioxanthate has been described. The yellow-colored cobalt complex and red-colored nickel complex have been extracted quantitatively using carbon tetrachloride in the pH ranges 4.0–11 and 4.0–6.7, respectively. The colors of these complexes are stable and absorbances have been measured at 389 nm for cobalt and 495 nm for the nickel complexes. Few ions interfere but the method has been applied successfully for the determination of these metal ions in various complex materials.     

Oxidation of formate by alkaline ferricyanide

Summary A catalytic oxidation of formate by alkaline ferricyanide has been studied. To the formate solution an excess of ferricyanide and osmium tetroxide as catalyst were added and the excess ferricyanide was back titrated with arsenious oxide using the amperometric dead stop end point method. The method is superior to the oxidative determination of formate by alkaline permanganate.

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Zusammenfassung Formiat kann durch katalytische Oxydation mit alkalischer Hexacyanoferrat(III)-lösung bestimmt werden, indem man die Probelösung mit einem Überschuß des Reagenses sowie Osmiumtetroxid als Katalysator versetzt und den Überschuß mit Arsen(III)-lösung zurücktitriert.Der Endpunkt wird nach der Dead stop-Methode bestimmt. Das Verfahren ist der Oxydation mit alkalischer Permanganatlösung überlegen.

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Sincere thanks of the authors are due to Prof. G. B. Singh for providing the necessary facilities. The award of a U.G.C. Scholarship to one of them (A.L.J.R.) is also acknowledged.     

The Pharmaceutical Use of Captisol®: Some Surprising Observations

The purpose of this paper is to share some recent observations on the pharmaceuticaluses and properties of Captisol^® or SBE_7M--CD in controlled porosity osmotic pump tablets (CP-OPT) and the underlying mechanism/sthat lead to apparent zero-order drug release pattern. It would have been simple toattribute the apparent zero-order release mechanism/s of poorly water-soluble drugsfrom CP-OPTs and pellets utilizing Captisol^®as both a solubilizing andosmotic agent, to purely osmotic and diffusional components. However, the mechanismmay be more related to a counterbalancing of physical properties as the concentration of Captisol^®changes within the matrix. Specifically, the initial concentration of Captisol^®within a core is 0.3–0.4M. When this drops to lower values an osmotic pressure drop occurs across the membrane. Therefore, drug release should not follow apparent zero-order kinetics if all the drug is solubilized. However, as the viscosity within the tablet also drops, the apparent diffusion coefficient of both Captisol^® and drug increases. Therefore, it appears that there is an initial resistance (hydraulic pressure) to fluid flow from the tablet through the rate-limiting microporous membrane. This resistance decreases so that even as osmotic pressure and concentration differences drop with time, counterbalancing faster release occurs. Osmotic driving force appears to be the most important initial driving force but a diffusional component becomes more significant with time.     

Far infrared spectra of solid molecular nitrogen

This paper reports the observation of the far infrared absorption spectrum of a single crystal of N₂, measured over absorption paths of 4 cm (lengthwise) and 2 cm (across the crystal). The crystal chamber, with quartz windows, was immersed in a flow of cold helium gas. The spectrum from 20 to 120 cm^–1 was recorded in the liquid phase, the-phase, and over the full temperature range of the-phase (35.6–2.0 K) with a Fourier transform spectrometer. The spectral resolution, which was not instrument-limited, and the large path allowed the observation of more detailed multiphonon-transition structure in the spectrum of the-phase than has previously been observed.