Evaluation of a carbon-rod atomizer for routine determination of trace metals by atomic-absorption spectroscopy applications to analysis of lubricating oil and crude oil

A carbon-rod atomizer (CRA) fitted with a 'mini-Massmann' carbon rod was evaluated for routine analysis of petroleum and petroleum products for trace metal content by atomic-absorption spectroscopy. Aspects investigated included sensitivity, detection limit, effect of solvent type, and interferences. The results of analysis of oil samples with this technique were compared with those obtained by other techniques. Metals studied were silver, copper, iron, nickel, and lead. Sensitivity and detection limit values obtained with the CRA were similar to those obtained with the carbon-filament atomizer. Strong 'solvent effects' were observed as well as interference by cations. On the basis of this study, design changes for the CRA are suggested, with the object of minimizing 'solvent effects' and interferences, increasing the atomization efficiency, and increasing the residence time of the atomic vapour in the optical path of the instrumental system.     

Reaction of β-amino-α,β-unsaturated esters and amides with aryl diazonium salts : Synthesis of cinnoline derivatives

Conjugated esters and amides react with aryldiazonium salts at room temperature (MeCN) to form the corresponding iminium hydrazone derivatives, which can be thermally cyclized to cinnoline-3-esters and cinnoline-3-amides. In general the intermediate iminium salts derived from the enamine amides cyclize faster than those from the enamine esters. Furthermore, the ease of cyclization depends upon the structure of the base-component of the enamine ester or the amide and the substituent in the aryl moiety of the diazonium salt. The configurational structure of the iminium hydrazones, studied by NMR spectroscopy, has been shown to involve H-bonding of the hydrazonyl N-H with the ester or the amide CO group.     

Determination of nanogram amounts of boron in some antimony compounds

Summary A method has been developed for determining boron in antimony compounds in the range 10^–7–10^–6%. The method comprises the isolation of the boron by distillation as methyl borate and its determination fluorimetrically with dibenzoylmethane. For the three materials analysed, SbCl₃, Sb₂O₃, and SbCl₅, individual procedures of dissolution as well as distillation were developed. The results obtained are reproducible, the mean deviation being about 12% at boron concentrations of 10^–7–10^–6%.

---

Zusammenfassung Ein Verfahren zur Bestimmung von 10^–7 bis 10^–6% Bor in Antimon-verbindungen wurde ausgearbeitet. Es umfaßt die Abtrennung des Bors durch Destillation als Methylborat und dessen fluorimetrische Messung mit Dibenzoylmethan. Für SbCl₃, Sb₂O₃ und SbCl₅ wurden jeweils eigene Arbeitsweisen der Auflösung und Destillation angegeben. Die Analysenergebnisse sind reproduzierbar; die mittlere Abweichung beträgt etwa 12% für Borkonzentrationen von 10^–7 bis 10^–6%.

     

Integral intensities of the absorption bands of the skeletal vibrations of substituted furocoumarins

Conclusions The IR spectra of 5- and 8-hydroxyfurocoumarins and their esters, 5,8-disubstituted furocoumarins containing hydroxyl, methoxyl, and alkoxyl groups, and 4,5-dihydrofurocoumarins differ with respect to the intensity and number of the bands in the 1630–1500 cm^–1 region of the spectrum. The integral intensities of the absorption bands in this frequency region differ markedly in the derivatives mentioned.Khimiya Prirodnykh Soedinenii, Vol. 5, No. 5, pp. 355–359, 1969     

Rotation about the exocyclic carbon-carbon double bond of amino dienes of the indolo[2,3-a]-and benzo[a]quinolizidine series

Quinolizidines containing an exocyclic double bond at C-2 (1,2) give on mild oxidation the amino dienes (3,4), as mixtures of geometric isomers with respect to the exocyclic double bond. The free enthalpy of activation for the rotation about the double bond has been estimated by NMR.     

Photosensitive decomposition of organic solvents at 77 degrees K by an aromatic amine, diphenylparaphenylenediamine

Abstract— –By e.s.r. we have studied the photoexcitation of an aromatic amine to its triplet state at 77°K, its photoionization to a radical cation and the simultaneous formation of solvent radicals proceeding from the photosensitization of the organic glassy matrix. In the case of methanol and ethanol matrix we observe approximately one solvent radical per solute radical cation. In the case of isopropanol and methyltetrahydrofuran we find respectively three and two solvent radicals per solute radical cation. The results suggest two possible processes of photosensitization. By successive absorption of two photons, the amine reaches an excited triplet state which is able either to dissociate giving one electron and one cation radical or to transfer its energy to the solvent, this last being decomposed. It is assumed that in the case of methanol and ethanol, the radicals from the solvent are only formed by reaction on the matrix by the released electron, whereas in the case of isopropanol and methyltetrahydrofuran, the second process is prevalent or exclusive.     

Characterization of nickel loaded mordenite catalysts by temperature programmed reduction

Temperature programmed reduction (TPR) has been used to study the redox behavior of Ni(II) ions in nickel sodium mordenite (NiNaM) and decationated nickel mordenite (NiHM). The TPR profiles suggest that Ni(II) ions occupy nonequivalent sites with different cooridination states in the mordenite. The reducibility of Ni(II) depends strongly on the zeolite acidity.

---

() Ni^II NiNaM NiHM. . .

     

Na+ transport across the beta alumina-propylene carbonate interface

Interfacial Na⁺ ion transport between polycrystalline beta alumina and propylene carbonate has been studied using a galvanostatic transient technique which separates interfacial overpotential from bulk resistivity effects. No interfacial polarization is detected during ion entry into beta alumina and exit from beta alumina across a dry interface from 30–1000 μA cm^?2. Transport across an interface contaminated with adsorbed water follows Tafel-type i/E behavior with a transition coefficient (α) of 0.24 and exchange current (i₀) of 3.0×10^?6 A cm^?2 at 23°C. Interfacial transport appears to take place through an intermediate state in which the mobile ion is adsorbed on the interface. Large increases in interfacial polarization occur at both dry and hydrated interfaces for ionic currents exceeding the rate of adsorption or desorption.     

The Spectrophotometric Determination of Gallium (III) with Glycine Thymol Blue

The reaction between gallium (III) and glycine thymol blue has been studied spectrophoptometrically in order to establish the optimum conditions for determining traces of gallium. The gallium (III) glycine thymol blue complex has an absorption maximum at 560 nm against a reagent blank and is stable between pH 4.0 and 5.5. The complex has a composition 1 : 2 and a formation constant of 6.4×10⁷ under the conditions studied. Beer's law is obeyed upto 126 μg of gallium. The net molar absorptivity has been found to be 11,000. The present method is very sensitive and rapid. Anions such as citrate and tartrate inhibit the colour development of the complex.