Syntheses of azo dyes containing 4,5-diphenylimidazole and their evaluation as analytical reagents

Eight azo dyes containing the 4,5-diphenylimidazole group have been synthesized, and their potential for determinations of metals has been studied spectrophotometrically. Of these reagents, the pyridylazo and quinolylazo derivatives are suitable as chromogenic reagents, the best being 2-(quinolylazo)-4,5-diphenylimidazole (QAI), which reacts with several metal ions. The copper and mercury complexes of QAI show molar absorptivities of the order of 80 000 l mol^?1 cm^?1.     

Determination of nitrate in natural waters by flow-injection analysis

Summary Nitrate was determined in natural water samples by flow-injection spectrophotometry. It was reduced to nitrite with copperized cadmium and the nitrite thus produced reacted with p-aminoacetophenone and m-phenylenediamine. The limit of detection was about 1.5 g l^–1 for sample injections of 650 l. The sampling rate was about 40 samples h^–1 and the relative standard deviation was above 1% for 0.1–0.3 mg l^–1 nitratenitrogen. Nitrite present in the sample was determined separately and subtracted.

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Nitratbestimmung in natürlichen Wässern mit Hilfe der Fließinjektions-Analyse

Zusammenfassung Nitrat wird bei dieser Methode mit Hilfe einer Cu/Cd-Reduktionssäule zu Nitrit reduziert, das mit p-Aminoacetophenon und m-Phenylendiamin zur Reaktion gebracht wird. Die gebildete Verbindung wird spektral-photometrisch gemessen. Die Nachweisgrenze beträgt etwa 1,5 g/l bei injizierten Probevolumina von 650 l. Der Probendurchsatz beträgt 40/h. Die relative Standardabweichung liegt über 1% bei 0,1–0,3 mg/l Nitrat-Stickstoff. Vorhandenes Nitrit wird gesondert bestimmt und abgezogen.

     

Light scattering study of ferroelastics Hg2Br2

Brillouin and Raman scattering spectra of the soft modes in Hg₂Br₂ have been measured using triple pass Fabry-Perot interferometers. The temperature dependence of the coupled soft optical and acoustic modes are analyzed by use of the thermodynamic potential and the equations of motion for the coupled oscillators. These two methods have given the same result for explaining the elastic anomaly of Hg₂Br₂ crystals below the transition temperature.     

Electrothermal atomic absorption spectrometric determination of ng g-1 levels of cadmium in bone after dithizone extractions

After removal of lipid and acid digestion of bone samples, cadmium is separated from the matrix by two extractions with dithizone in carbon tetrachloride. The first extraction at pH 3–3.5 removes cadmium from the matrix; the second extraction, at pH 8.5 in the presence of 2-hydroxyethylethylenediaminetriacetic acid, is needed to prevent suppression of the cadmium signal by zinc. Cadmium is finally measured in the back-extract into 0.24 M hydrochloric acid. Less than 10 ng g^-1 cadmium in fresh bone can be determined within a relative standard deviation of 10%.     

Determination of sulphate in natural water by flow-injection analysis

Summary Sulphate was determined in natural water samples by flow-injection analysis using dimethylsulphonazo-III as reagent. The interference by Ca was eliminated by a cation-exchanger column inserted directly after the sample injection valve. In order to ensure high sensitivity and reproducibility it was necessary to saturate the carrier solution with barium sulphate and to fill the reaction coil with ethanol-water (11) when not in use. Standard deviations were 0.94–1.2% for 6–10mg/l sulphate. The limit of detection was about 0.2mg/l. The calibration graph was linear up to 14mg/l Mg²⁺, NH ₄ ⁺ , Na⁺, K⁺, Cl^–, NO ₃ ^– , PO ₄ ^3– , HCO ₃ ^– and SiO ₃ ^2– did not interfere in the normally occurring concentrations.

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Sulfatbestimmung in natürlichem Wasser durch Flow-Injection-Analyse

Zusammenfassung Als Reagens dient Dimethylsulfonazo-III. Die Störung durch Calcium bei dieser Bestimmung wird durch eine Kationenaustauschersäule eliminiert, die direkt nach dem Probeinjektions-Ventil angeordnet ist. Zur Erhöhung der Empfindlichkeit und Reproduzierbarkeit ist es notwendig, die Trägerlösung mit Bariumsulfat zu sättigen sowie bei Nichtbenutzung des Systems den Reaktionsteil mit Ethanol-Wasser (11) zu füllen. Mit dem so modifizierten Verfahren ergaben sich Standardabweichungen von 0,94–1,2% für 6–10 mg/l Sulfat, die Nachweisgrenze liegt bei 0,2 mg/l. Die Eichkurve ist bis 14 mg/l linear. Mg²⁺, NH ₄ ⁺ , Na⁺, K⁺, Cl^–, NO ₃ ^– , PO ₄ ^3– , HCO ₃ ^– und SiO ₃ ^2– stören in den normalerweise vorkommenden Konzentrationen nicht.

     

Temperature dependence of Raman linewidth and shift in CuI

The temperature dependence of the optical phonon linewidth and frequency shift in CuI has been measured in the temperature range of 4.2 ～ 300 K. Utilizing phonon dispersion curves obtained from neutron scattering measurements, the linewidths and frequency shifts are calculated in terms of three-phonon interactions proposed by Pine and Tannenwald. The experimental results for the change in linewidth and frequency with temperature are in good agreement with this theory.     

Electron-phonon interaction in Raman scattering of Li-doped ZnTe

Raman scattering has been measured at low temperatures on Li doped ZnTe, using Kr and dye lasers. Besides the usual phonon spectrum, electronic transitions between acceptor bound states 1S→2S (A band), 1S→3S, 1S→4S, are observed. A peak located between the TO and LO bands is interpreted in terms of a bound LO-phonon mode related to the p acceptor states. The sidebands of the A band, at one and two LO-phonons are observed as well, whose energies are found to be respectively 12 and 26 cm^?1 smaller than the expected values. A simple self-energy model is invoked to explain the energy shift due to electron-phonon interaction.