A new method for the titrimetric determination of perchlorate

A new method for the titrimetric determination of perchlorate has been developed, based on its reduction to chloride by iron(II) in a strong sulphuric acid medium at high temperature. The effect of variables, such as the sulphuric acid concentration, the temperature and the period of heating, on the extent of reduction has been studied and the optimal conditions for analytical determination of perehlorate derived.

Determination of sulphur monochloride by oxidation with chloramine-T

A rapid method is described for the determination of sulphur monochloride by adding excess of chloramine-T and determining the excess iodometrically.

Spectrophotometric and potentiometric investigations of copper (II)-ethanolamine complexes - Part II. Monoethanolamine (Analysis of mixed hydroxy complexes with polarographic evidence)

Potentiometric, spectrophotometric and polarographic evidence has been presented for the formation of mixed hydroxy complexes in coppermonoethanolamine system. A method has been developed for the analysis of Bjerrum formation curves taken in presence of 0·1, 0·2, 0·5 and 1·0 M monoethanolammonium ion with respect to hydroxy complexes. The formation of CuAOH+, CuA2OH+ and CuA3OH+ is shown and the corresponding stability constants are calculated at different concentrations of MEA ion. Curves showing the distribution of pure and hydroxy complexes at various pA values in solutions containing different concentrations of MEA ion have also been given.

A colorimetric method for determination of pyrocatechol and related substances

A colorimetric assay for the quantitative determination of catecholic compounds was developed. The method was based on the observation that a red color was formed when nitrite was added to a solution containing pyrocatechol and sodium tungstate. Aromatic amines interfere with the reaction but this could be overcome by the addition of formaldehyde. When interfering substances are present along with pyrocatechol, it can be readily separated by paper chromatography and estimated after elution from the filter paper.

Spectrophotometric and potentiometric investigations of copper (II)-ethanolamine complexes - Part I. Monoethanolamine

Spectrophotometric and potentiometric investigations have been carried out on copper-monoethanolamine complexes. Job plots at 920, 760 and 620 mµ have indicated the formation of CuA++, CuA2/++ and CuA3 ++. The$$\bar n - pA$$ curves have been obtained by a slight modification of the method of corresponding solutions and by pH measurements. The$$\bar n$$ vs. pA curves obtained at different metal concentrations coincide indicating the formation of mononuclear complexes. Experiments conducted with 0·1. 0·2, 0·5 and 1·0 M monoethanolammonium ion indicate the formation of mononuclear hydroxy complexes above pH 6. The nature of E m vs pA curves is closely analogous to that of$$\bar n$$ vs. pA curves. Absorption spectra taken at pH 9·8 with different amounts of monoethanolamine has given evidence for the formation of (CuA3OH·A)+.$$\bar n - pA$$ curves have been analyzed and the values ofβ 1, 1,β 1, 2 andβ 1, 3 have been obtained. Curves showing the distribution of complexes and the absorption curves of the individual complexes (CuA++, CuA2/++, and CuA3/++) have been calculated.

New benzidine procedure for determination of manganese in biological samples

A simple and accurate method for the determination of 0.25 to 1.0 μg. of manganese (in samples containing 1 to 4 μg. of manganese) has been developed by modifying the conditions for the reaction between permanganate and benzidine. Manganese is oxidized with potassium periodate in orthophosphoric acid and selectively estimated in the presence of excess oxidant with benzidine in formic acid. The procedure is applicable for estimation of manganese in biological samples, with recoveries in the range 97.5 to 106.1%.

Potentiometric and spectrophotometric investigation of nickel-monoethanol-amine complexes

A detailed study of nickel-monoethanolamine complexes has been made employing potentiometric and spectrophotometric methods. The conditions for the formation of mono as well as polynuclear complexes have been investigated by potentiometric method. Evidence is presented for the formation of the following complexes and their stability constants are determined: NiA2+, Ni22+, Ni32+, NiA42+, NiA52+, NiA22+, Ni2A24+ and Ni3A36+. Combining potentiometric data with the spectrophotometric data, absorption spectra of the pure mononuclear complexes NiA2+ to NiA42+ and NiA2+6 have been computed. The absorption spectrum of NiA2+6 has been discussed on the basis of ligand field and molecular orbital theories. The absorption spectra of intermediate complexes have been interpreted on the basis of average ligand field theory. There has been good agreement between the experimental (10,400 cm-1) value of 10 Dq of NiA2+6 and the calculated value of 10 Dq (11,400 cm-1) on the basis of M.O. theory.

Colorimetric determination of 2,4-dinitrophenylamino groups by sodium borohydride reduction

When sodium borohydride is added to aqueous solutions of 2,4-dinitrophenylamino acids and related derivatives, an intense red color is formed. Measurement of the red color, with a 420 filter, permits the determination of such compounds in concentrations of 0.01 to 0.06 μmole per ml. with a precision to 2%. The reaction is highly specific-while 2,4-dinitroaniline will react to the test, o-, m-, and p-nitroanilines, 2,4-dinitrophenyl aryl or alkyl ethers, and 2,4-dinitrophenyl-imidazole and pyrrolidine derivatives will not. Heretofore aromatic nitro groups have been considered resistant to attack by sodium borohydride. The method, as developed, is applicable to the evaluation of the degree of substitution of protein amino groups by fluorodinitrobenzene.

A method for the determination of dixanthogens

One mole of diethyl dixanthogen reacts with 26 moles of chloramine-T, and this reaction can be used for the determination of the dixanthogen. Higher alkyl dixanthogens react in a more complicated fashion, but may still be estimated using an empirical correction.

Spectrophotometric determination of copper with piperidinium piperidyl dithioformate

The reagent piperidinium piperidyl dithioformate forms with copper in aqueous solution a yellowish brown complex which can be extracted with carbon tetrachloride. The copper-PPDF complex in carbon tetrachloride solution has maximum absorption at 434 nm. A spectrophotometric method for determining copper has been developed as the reagent has been shown to form a definite complex.

Potentiometric titrations in nonaqueous cerimetry

Potassium iodide and hydroquinone can be estimated potentiometrically in nonaqueous medium using ammonium nitrato cerate as oxidant. A platinum indicator electrode coupled with either a glass electrode or an antimony electrode as reference electrode, can be used in nonaqueous medium satisfactorily, for following the potentiometric titration. Direct potentiometric titration of xanthate with ammonium nitrato cerate in nonaqueous medium yields slightly lower values than the actual values in presence of platinum indicator electrode.

Determination of carbon disulphide by chloramine-T

Carbon disulphide, on treatment with alcoholic potash, can readily be oxidised quantitatively by chloramine-T, converting all the sulphur to sulphuric acid. Fourteen equivalents of the oxidant are consumed for every mole of carbon disulphide. Since excess of chloramine-T may be determined iodimetrically, this reaction may be used for the determination of carbon disulphide. It may also be applied to the determination of xanthates.

Spectrophotometric and potentiometric investigations of copper (II)-Ethanolamine complexes - Part III. diethanolamine (Gaussian analysis of electronic spectra in mono and diethanolamine systems)

Spectrophotometric and potentiometric investigations have been carried out on copper-diethanolamine system. Job plots at 900, 900 and 580 mμ have indicated the formation of CuD++, CuD2++ and CuD3++. The n- pA curves obtained indicate the formation of CuD++, CuD2++, CuD3++, CuDOH+, CuD2OH+ and CuD3OH+. The n- pA curves have been analyzed to obtain the stability constants of these complexes. Absorption curves of pure complexes have been computed by a graphical method. Gaussian analysis of the absorption curves of pure and hydroxy complexes show the presence of a second band, indicating that the structure is that of a distorted octahedron.