Alfy Badie Sakla

Microdetermination of metals in organometallic compounds by the oxine method after oxygen flask combustion: I. Cadmium, magnesium, uranium, and zinc

Abstract A simple, accurate, and relatively rapid procedure for the estimation of cadmium, magnesium, uranium, and zinc in organometallic compounds is presented. The oxygen-filled flask is recommended for decomposition of the organic sample. Determination of the metal concerned is carried out by three methods using a single sample weight. Both the gravimetric and titrimetric finishes are applied. The method has the advantage of a favorable conversion factor for the gravimetric determination besides an 8- or 12-fold amplification reaction, depending on the valency of the metal, in case of the titrimetric finish.

Microdetermination of Mn, Fe, Co, Ni, Cu, Zn, Ag, Cd, Hg, Pb, Bi and U in inorganic and organometallic compounds with morpholinium morpholine-N-dithiocarboxylate

The chelates of morpholinium morpholine-N-dithiocarboxylate with manganese(II), iron(II), iron(III), cobalt(II), nickel, copper(II), zinc, silver, cadmium, mercury(II), lead, bismuth and uranium(VI) have been prepared and their compositions elucidated. Simple, accurate and relatively rapid procedures for the gravimetric and titrimetric microdetermination of these metals in inorganic and organometallic compounds are presented.

Individual microdetermination of chlorine, bromine and iodine in halogenated organic compounds by the oxygen-flask method.

A simple and accurate micro-method for the individual determination of Cl, Br and I in halogenated organic compounds by the oxygen-flask method is described. Addition of potassium bromate to oxidize bromide, and of hydrogen peroxide to oxidize iodide, followed by boiling, is used to eliminate these two halides in mixtures with chloride or each other.

Microdetermination of metals in organometallic compounds by the oxine method after oxygen flask combustion: II. Cobalt, manganese, and titanium

Abstract The microdetermination of metals in organometallic compounds by the oxine method after the oxygen flask combustion is used for cobalt, manganese, and titanium. The determinations are carried out gravimetrically (method I) and volumetrically (methods II, III) for the three metals, using a single sample weight. The method has the advantage of a favorable gravimetric factor, besides a sufficiently sharp end point with 8-fold amplification reaction in case of titrimetric finish.

Characterization of interfering effects in the determination of molybdenum by atomic absorption spectrometry

Abstract The effect of anions on molybdenum absorbance depends on the pH; low pH causes the formation of iso- or heteropoly anions which change the atomization process in the flame. Organic ligands also depress the release of molybdenum atoms but cyanide radicals in the flame scavenge, e.g., OH radicals from such ligands and prevent their depressive effect. Certain cations (La, Ce, Mg, Ca, Sr and Ba) appear to form spinels; boric acid minimizes this effect.

Characterization and elimination of the interfering effects of foreign species in the atomic-absorption determination of iron.

The inhibition-release titration method has been used to study interference effects in flame atomic-absorption determination of iron. Interferences from anions, cations and complexing agents with the atomic-absorption of iron when a stoichiometric air-acetylene flame is used, can be obviated by a preliminary treatment of the sample solution with sulphosalicylic acid to convert the iron into the same complex before aspiration, thus giving a constant environment for the iron in the flame processes.

Simultaneous microdetermination of carbon, hydrogen, mercury, chlorine, bromine and sulphur in organic compounds

Abstract A simple, reliable method for the simultaneous microdetermination of carbon, hydrogen, mercury, chlorine (or bromine) and sulphur in organic compounds is described. The intermediate storage technique is used. Sulphur and the halogens are absorbed on electrolytic silver and determined gravimetrically or titrimetrically. Mercury is absorbed on gold wire, and is weighed as the metal or desorbed and determined by a mercury-8-hydroxy-quinoline method.

Simultaneous microdetermination of carbon, hydrogen, chlorine, bromine, sulfur, and metals in organometallic compounds

Abstract A method for the simultaneous microdetermination of carbon, hydrogen, chlorine, bromine, sulfur, and metals which combines features of the known intermediate storage technique in organic microanalysis and formation of the metal-oxine complex, is described. Carbon and hydrogen are determined gravimetrically as usual. Sulfur and halogens are absorbed and stored on electrolytic silver. After completion of the combustion, the oxygen is replaced first by nitrogen and secondly by hydrogen which liberates the sulfur as sulfur dioxide and halogens as hydrogen halides and regenerates the silver layer. The liberated gases can be easily absorbed by dilute hydrogen peroxide and determined titrimetrically. The metal oxide, remaining in the platinum boat, is dissolved in a mixture of nitric-perchloric acids in a test tube and the metal content is determined gravimetrically and titrimetrically using 8-hydroxyquinoline.

Microdetermination of carbon in organic compounds by oxygen flask combustion with atomic absorption spectrophotometric, gravimetric, and titrimetric finishes

Abstract A simple and accurate method is presented for the determination of the carbon content of organic compounds by electric oxygen flask combustion. Five results are obtained for one experiment by atomic absorption spectrophotometric, gravimetric, and titrimetric finishes.

Coupling of diazonium salts with acetone

Diazonium salts or isodiazoates reacted with acetone in acid media to give the corresponding α-oxopropanal arylhydrazone in high yield. The kinetics of formation of α-oxopropanal p-nitrophenylhydrazone from sodium p-nitrobenzeneisodiazoate and acetone in presence of acids were studied in acetone solution at 25°. For a series of six acids of different acid strengths, pseudo-first-order rate constants were obtained, and the reaction was found to be of the second order, first order in the diazoate, and first order in acid. The mechanistic scheme proposed for hydrazone formation is supported by the present investigation.