Studies on Flame Photometry by Organic Solvent Extraction Method. III : Determination of Manganese and Copper by Oxine-Organic Solvent Extraction Method

In connection with the micro-determination of metals by flame photometric studies are being made of the use of extraction with organic solvents in order to separate and remove interfering elements and to raise the sensitivity. In the present series of work, micro-determination of copper and manganese was carried out by extraction of oxine complex salts with organic solvent. The oxine complex salts of copper and manganese were extracted with methyl isobutyl ketone or other organic solvents, and the extract solution was directly sprayed and excited with an oxyhydrogen flame. The emission intensity of spectral lines was measured at 324.8 mμ for copper and at 403.5 mμ for manganese. In this case, sensitivity was increased by 6～8 folds for copper and by 20～30 folds for manganese compared with the intensities in aqueous solution. Interference of co-existing elements was practically eliminated by controlling the pH of the aqueous layer for the extraction. Conditions for flame photometry of the extract solution differed with different solvents, and these points were also examined

A New Method for the Determination of Very Small Amount of Antimony in Various Kinds of Metals

The determinations of very small amount of antimony in various kinds of metals were carried out by applying the method reported previously by the present authors, in which precipitates of antimony with methylviolet in hydrochloric acid solutions were extracted by amylacetate and then determined by the photometric method. Antimony in copper, lead, zinc, cadmium, bismuth, nickel and iron was separated out by one or double treatment, by which it was co-precipitated with permanganic acid in acidic solutions. Antimony in tin was liberated first by the reduction with iron, and then separated from iron by the above method

Microdeterminations of Arsenic and Antimony in Metallic Germanium and Germanium Dioxide

The method for the determination of minute amounts of impurities in high-purity germanium was studied and a simple method for the determination of arsenic and antimony was successfully completed, by using only a small amount of sample. For the determination of arsenic, germanium was removed as germanium tetrachloride by distillation, or by dissolving the sample and, omitting the distillation and the isolation processes, reducing quinquevalent arsenic to trivalent arsenic and extracting with carbon tetrachloride after the addition of sodium diethyldithiocarbamate, arsenic was determined as molybdenum blue. Antimony was determined after removing germanium tetrachloride by distillation or separating antimony by coprecipitation with manganese dioxide, determined by the methyl violet method, a sensitive method of determination was developed by the present study. In this way, the determination of up to 0.1 p.p.m. of arsenic and 0.01 p.p.m. of antimony in metallic germanium was possible

Determination of Component in Binary Alloy by Backscattering of Beta Particles

The saturation backscattering of β particles changes by the atomic number of a target material and the maximum range of backscattered β particles from the same source also changes by the target material. These properties were applied to the quantitative analyses of the component elements in binary alloys. After investigating the backscattering of the particles emitted from Sr-90 (Y-90) and P-32 by various target elements with or without aluminium absorbers, the optimum conditions for the determination of copper in aluminium and tungsten in tungsten-iron alloy were found. Copper could be determined by counting the backscattering of β emission from Sr-90 (Y-90) through 345 mg/cm^2 absorber and tungsten could be determined with 490 mg/cm^2 absorber

Rapid Photometric Determination of Vanadium in Iron and Steel

The complex compound formed when the chloroform solution of benzoylphenylhydroxyl-amine is added to solutions of quinquevalent vanadium in strong hydrochloric acid is extracted to chloroform layer and then vanadium is determined, photometrically. The reaction is extremely selective, and commonly associated metals do not interfere. The method may be applicable to the rapid determination of vanadium in iron and steel

Determination of Microamounts of Calcium, Magnesium and Aluminium in Titanium Metal

As the complete separation of calcium, magnesium and aluminium from titanium metal is difficult, it was examined by extracting titanous thiocyanate with ether, and satisfactory results were obtained. Photometric determination was carried out after separation by using chlorophenol azodihydroxynaphthalenesulfonate for calcium, titan yellow for magnesium and extraction of the oxinate for aluminium

Analysis of Alloys by Fluorescent X-Ray Spectroscopy Non-Destructive-Addition Method

In order to determine metal samples rapidly and with a few standard samples, a new method, non-destructive-addition method was proposed. As theoretical equations for this method, the following equations were introduced : x=a(I_M/I_a-1)/I_M/I_x・(1-a)+I_M/I_aa-1 where x is the weight fraction of the element to be analyzed in the unknown smaple and I_x is X-ray intensity of it, a is the weight fraction of the element to be analyzed in the standard sample and I_a is the X-ray intensity of it. I_M is the X-ray intensity of the pure metals of the element to be analyzed ; and I_M/I_M\u27・W_m\u27/W_m-1/W_m\u27-W_m=I_M/I_M\u27・W_m\u27\u27/W_m-1/W\u27\u27_m-W_m where W_m and W_m\u27 are weight fraction of the element to be analyzed in the standards and I_M, I_M\u27 are the X-ray intensity of them, W_M" is the weight fraction of the element to be analyzed in the unknown sample and I_m" is the X-ray intensity of it. After preliminary experiments on some powdered samples, these equations were applied to the determination of some metals, for example nickel, chromium or manganese in steels. Satisfactory results were obtained

A New Microdetermination of Bismuth and Mercury by the Extraction of Their Iodides with Organic Solvent

Microdetermination of bismuth and mercury in the range of a few gammas was found to be possible by extraction of the respective iodide complex salts from acid solution with an organic solvent (isoamyl alcohol or mixture of this alcohol and ethyl acetate) and measuring the absorbance of the solvent extract in the ultraviolet region. The absorption maximum of bismuth iodide complex salt was found in the region of 330 mμ, and that of mercury compound in the region of 303 mμ. Optimal conditions for these analytical procedures and effects of coexistent elements were also studied

Catalytic Analysis. XVII : Microdetermination of Iron by the Reaction between p-Phenylendiamine and Hydrogen Peroxide

Applying the catalytic action of iron to the reaction between p-phenylendiamine and hydrogen peroxide, the relation between the time required for the development of the brown color and the amount of iron added was studied with Duboseq\u27s colorimeter, which rendered it possible to determine 0.5～5γ of iron by the time measurement under the same condition. The condition of the solution and influences of some diverse ions on the determination were studied