Fluorescent X-ray analysis has found its narrower applications in the field of glass industry compared with other silicate industries as the cement manufacture, because the accurate determination of lighter elements as Na andMg by the X-ray method was rather difficult. The possibility of the fluorescent X-ray analysis as the practical method was examined by using an X-ray tube with a chromium anti-cathode recently practized. The comparisons of the Cr anti-cathode with Au anticathode are shown in Figs.17, and those of chemical analysis with X-ray analysis in TableVI. Fig. 8 gives a calibration line for the sodium oxide in sheet glass. The fluorescent X-ray analysis seems to prove to be a practical method for the rapid determinations in the glass industries.

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The film thickness of various platings on iron plate is determined by the measurement of fluorescent X-ray intensity of FeKα from the substrate iron. The results on Zn platings are shown in Figs. 2 and 3, and those on Cd and Sn platings are, respectively, in Figs. 4 and 5. The examinations of the slopes of full lines in those figures indicate that the absorption of primary X-rays by plating films, namely, μ₁ in the equation(2), is almost negligible, not equal to one corresponding to the absorption edge wavelengths of the substrate metals. Therefore, provided that the mass absorption coefficient of FeKα by plating films, the radiation angle (θ₂) of fluorescent X-rays and the density of the plating metals are known or measurable, the thickness of plating film is calculated from the equation(4) by the comparison of FeKα intensities on pure and electroplated iron plates. However, to obtain much higher accuracy, considerations on absorption and enhancement effects of primary X-rays are necessary.

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An attachment for commercially available spectrophotometer is described which is capable of observing absorption spectra of fused salt at temperature up to 1000°C.
The light source is displaced so that the attachment can be inserted between the light source and the monochromator. The attachment consists of a light-tight and air-tight stainless-steel box containing an insulating block which carries the furnace block. The insulating block rides on a ball bearing track and is provided with click stops to permit alternate placement of the two cells in the light beam.
Absorption spectra of copper (II) and (I) chlorides in fused KCl-LiCl (eutectic)mixture have been measured at 500°C using this attachment.

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An yellow selenium-Bismuthiol II complex formed in hydrochloric acid solution was extracted quantitatively with chloroform. The coloration in the organic phase was applied for the determination of small amounts of selenium. The procedure is as follows: Add 0.1% Bismuthiol II solution to a sample solution containing up to 20μg of selenium. Extract the complex with chloroform and wash the chloroform extract with a buffer solution (pH 7.5) to remove the excess reagent from the organic phase. Measure the absorbance of the chloroform at a wavelength of 330 mμ (maximum absorption). In the concentration range of 0.520μg of selenium in 10ml of chloroform the calibration curve obeys the Beer's law. The sensitivity of this method is 0.0025μg of selenium per cm² at 330mμ. Effect of the several diverse ions has been studied. The mole ratio of selenium to Bismuthiol II by means of continuous variation method was 1 : 4.

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A simple method for determining traces of fluorine in uranium oxides using pyrolytic separation technique and alizarin complexone (ALC) photometric method has been established.
Up to 10 grams of uranium oxide sample, containing 3 to 30μg of fluorine, is mixed with 3 grams of powdered tungstic oxide by grinding, and the mixture is packed into a platinum boat. Pyrolysis is then carried out for 15 minutes under a stream of moist oxygen (1.6l/min.) in a fused silica reactor tube (850°C). The volatilized fluorine is absorbed in 15ml of a dilute alkaline solution without increasing the volume of the solution. The solution is then transferred into a 25 ml volumetric flask and treated with 8ml of a La-ALC composite reagent solution. Fluorine is determined by measuring the absorbance of the La-ALC-F complex at 620 mμ using a reagent blank (La-ALC chelate).
The pyrolytic separation method is rapid and simple, and does not need the dissolution of the sample. In addition, excessive dilution of the released fluoride by condensate, which occurs if pyrohydrolytic or distillation techniques are used, is avoided.

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Major components of clay, SiO₂, Al₂O₃, Fe₂O₃ and MgO, were determined by X-ray spectrochemical analysis. The portion whose grain size was less than 5μ was divided from clayey soils of different localities and various clay minerals contained. The specimens for measurement were prepared by pressing. The relation between the intensity of spectra and the matrix change was investigated on oxide mixtures, SiO₂ Al₂O₃, Fe₂O₃ and MgO: FeKα and SiKα obey Beattie's equation for absorption. The enhancement effect of Si to AlKα appears to be constant with SiO₂ of more than 60%. The effect of P, when ADP crystal used, to MgKα was ascertained. SiO₂(3070%), Al₂O₃ (1037%), Fe₂O₃ (0.516%), and MgO(0.521%) in clay samples were determined with the standard deviation to chemical analysis of 1.12%, 0.64%, 0.46% and 0.53%, respectively.

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A method is presented for the determination of trace amounts of copper (II) in water for high pressure boilers etc. Cadmium diethyldithiocarbamate in chloroform is used as the reagent for extraction of copper (II) from water. The recommended procedure is as follows.
Ten ml of buffer solution containing sodium acetate and hydrochloric acid, and 10 ml of 1M citric acid solution are added to 400 ml of sample solution in a 500 ml separatory funnel. Adding 20 ml of cadmium diethyldithiocarbamate chloroform solution, 1 ml of which is equivalent to about 17 μg of copper, the mixture is shaken vigorously for 3 min. After being set aside for 2 min., chloroform phase is separated. The extract is transferred into a 25 ml volumetric flask containing 2 ml of ethanol, and is diluted to the mark with pure chloroform.
The absorbance is measured at 435 mμ in a 50 mm cell, using pure chloroform as a reference blank solvent.
The interference due to iron (II) is avoided by the addition of citric acid. One ppb of copper can be determined, whereby 95% confidence interval extends from 0.71 ppb to 1.29 ppb at 1 ppb copper (II) concentration.
The regression line is given by X=44.420Y+0.045, where Y is the absorbance at copper concentration X.

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2-Pyridinaldazine has been known to react with iron(II) to form two complexes. The authors have found that hydroxylamine contributes favorably to this reaction to give a stable orange-red complex with much higher sensitivity, and studied the analytical conditions for the application of this reaction to the determination of iron(II). As little as 0.1-2 ppm of iron(II) can be determined by the measurement of the absorbance at 480 mμ of the complex obtained at pH 4.2 in the presence of hydroxylamine.

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For the determination of microamounts of chromium in pure iron, as the spectrophotometric method by using diphenylcarbazide lacks in sensitivity, the organic solvent extraction method was studied as follows.
One tenth gram of sample is dissolved in hydrochloric acid and nitric acid, and the iron is removed by extraction with the mixture of two parts of methyl-iso-butylketone and one part of amyl acetate. The lower layer is evaporated to almost dryness after nitric acid is added.
It is dissolved with 10 ml of sulfuric acid (1.4 v/v %), 1 ml of potassium permanganate solution (0.1 % ) is added and boiled for 3 minutes. After cooling, 10 ml of urea solution (20%) is added and sodium nitrite solution (10%) is added dropwise until the pink color is extinguished. The solution is put in a separating funnel, diluted to 25 ml with water, 3 ml of diphenyl carbazide (0.2%) alcohol solution is added and stood for one minute.
Eight ml of sulfuric acid (1+1), 5 g of anhydrous sodium sulfate and 10.0 ml of iso-amylalcohol are added to the solution and shaken vigorously for one minute. After the upper layer is separated, the absorbancy at 543 mμ is measured againstiso-amylalcohol as a blank. Ten folds of Al, As, B, Ca, Ce, Co, Cu, Mg, Mn, Mo, Nb, Ni, P, Pb, Sn, Ta, Ti, V, W, and Zn do not interfere. From 0.1 to 50 ppm of chromium was determined within about one hour.

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At the present time Arsenazo III appears to be the most sensitive colorimetric reagent for uranium. Unfortunately, thorium and zirconium interfere seriously with the determination of uranium. Therefore, a method has been developed for the determination of uranium in the presence of the interfering elements.
The scheme of the analytical method is shown in Fig. 1. Uranium(VI) is extracted with 5 wt/vol % tri-iso-octylamine in xylene from 5 M hydrochloric acid solution. Uranium is back-extracted with 0.5 M hydrochloric acid. The extraction and back-extraction of uranium are repeated. The second back extract containing uranium is evaporated to dryness, and the residue is treated with nitric and perchloric acids. The residue is dissolved in hydrochloric acid and uranium is reduced to the quadrivalent state with zinc. Oxalic acid is added to mask a small amount of zironium, and Arsenazo III is added. The solution is made up to 25 mland its absorbance is measured in a 1 cm cell at 665 mμ.
By this method 20 μg of uranium can be determinedin the presence of 10 mg of thorium or 10 mg of zirconium. The effect of diverse ions has been studied.

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Separations and identifications of Te, Se, and Cr of different valencies were studied with two kinds of silica gel plates, using MIBK, ethylacetate, n-butylacetate, n-butanol staturated with 2N HCl, or acetone, as a developping solvent.
The use of MIBK, ethylacetate, and n-butylacetate resulted in good separations of Te(IV) from Te(VI), Se(IV) from Se(VI), and Cr(VI) from Cr(III) (Fig. 1 and 2), and Te(IV) was separated from Se(IV) by n-butanol (Fig. 1, d).
The chromatogram of Te(IV) in 6N HCl solution or in the MIBK extractfrom the 6N HCl solution appeared in two or three separated parts when it was developed by MIBK or acetone, and this fact suggests that two or more species of Te(IV) may exist in 6N HCl solution and in the MIBK extract from the 6N HCl solution.

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A method for determining manganese in beryllium has been established. The method involves the extraction of manganese into benzene as its diethyldithiocarbamate(DDTC) and the formation of manganese 2-methyl-oxinate in the organic extract. By measuring the absorbance of the organic phase, down to 2ppm of manganese in beryllium can be determined.
Not more than 1 gram of beryllium metal sample is dissolved in hydrochloric acid. To remove interfering metals such as iron and copper, the solution is treated with ammonium citrate and oxine, the pH of the solution is adjusted to 5.05.5, and the metal oxinates are extracted by shaking with chloroform. The pH of aqueous solution is adjusted to 7.59.5, it is treated with 10 ml of 8% DDTC solution, and the manganese DDTC complex is then extracted with exactly 10 ml of benzene. The manganese DDTC complex is converted into 2-methyl-oxinate in the benzene solution by adding 0.3 gram of solid 2-methly-oxine and shaking with 15 mll of 0.1N sodium hydroxide solution. The absorbance of the organic solution is measured at 400 mμ against a reference blank.

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