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Volume 11, Issue 8
Displaying 1-16 of 16 articles from this issue
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Motosuke FURUYA, Masatoshi TAJIRI1962 Volume 11 Issue 8 Pages 797-800
Published: August 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA simple and rapid method is proposed for sampling molten phosphor bronze in routine chemical analysis, where molten metal is dropped onto the exposed surface of a phosphor bronze block immersed in a basin filled with water. The resulting metal granules in the water are taken out, dried, sieved, and from 16 to 60 mesh grains are collected as analytical samples.
One gram contains ca. 800 granules, spherical and bright, without black oxide film on them. The proposed method is compared with the usual JIS method for the determination of Sn by the iodometric titration. The error due to segregation and mixing in the latter is eliminated in the proposed one. The time required for a sampling is 5 minutes.
The method has been applied also for copper, copper base alloys, white metal bearing alloys, and soft solders.View full abstractDownload PDF (688K) -
Shozo TODA, Yukio KOJIMA1962 Volume 11 Issue 8 Pages 801-806
Published: August 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSUltraviolet and visible absorption spectra of solids in KCl pellet prepared with an extremely vigorous grinding by hand and by a vibrator often showed a remarkable difference from those in the pellet prepared after a mere mixing by hand.
Compounds lacking polar groups in them did not give such a difference of the spectrum between both pellets, and the distortion of spectra in compounds with only weak hydrogen bondings was removed by heating the pellet. In compounds in which the types of the hydrogen bondings are complicated, however, the distortion of spectra could not be removed by heating.View full abstractDownload PDF (917K) -
Hiromu IMAI1962 Volume 11 Issue 8 Pages 806-811
Published: August 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSSpectrophotometric determination of antimony has been conventionally made by extracting Rhodamine B-Sb (V) complex with benzene, after the excess of Ce(IV) added for the oxidation of antimony was destoryed with hydroxylamine hydrochloride. In the cases, however, the absorbance was widely variable and dependent upon the time of standing for the reduction of excess Ce(IV), and also decreased remarkably with the time of standing of extracted benzene solution.
A new modified method has been presented by the author to overcome these difficulties, whereby much higher reproducibility and stability of absorbance were obtained by the addition of 3 drops of 0.61.5M sodium nitrite solution as oxidizing agent instead of Ce(IV), and 0.5 ml of 1 : 2 butyl cellosolve solution per 25 ml of the sample solution of more than 4N in hydrochloric acid.
In this method, the removal of excess sodium nitrite was unnecessary, and the determination of antimony was done with high sensitivity.View full abstractDownload PDF (1006K) -
Studies on extractive metallurgy of rare earths. IIIMasao SATO1962 Volume 11 Issue 8 Pages 811-813
Published: August 05, 1962
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSA flame photometric method for the determination of yttrium in yttrium group rare earths was presented. There were three characteristic peaks in flame emission spectrum of yttrium, and two of them (599 mμ, 615 mμ) were used to determine the amount of yttrium in 0.1N hydrochloric acid solution.
The relation between log. amount of yttrium and log. intensities of the flame spectra was shown in the straight line.
The amount of yttrium in the impure yttrium solution extracted from xenotime was determined. The effectiveness of the method was recognized by the satisfactory recovery of yttrium added to the impure yttrium solution. It is recommended for industrial analysis.View full abstractDownload PDF (457K) -
Shoichi KAWAMURA1962 Volume 11 Issue 8 Pages 814-818
Published: August 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA rapid separation of 137Cs, 90Sr, 144Ce and 95Zr by paper electrophoresis was studied. The filter strips (Toyo filter paper No. 3, 2 × 40 cm) were placed in a background electrolyte. After removal from the solution, they were blotted between sheets of dry paper.
The strips were sandwitched by plastics plate and cooling bath, and screwed tightly. They were allowed to equilibrate for 30 minutes
The sample solution (0.005 ml ) containing 137Cs, 90Sr, 144Ce and 95Zr was spotted at a point 10 cm apart from one end of the filter strip through a hole of plastics plate, and then the hole was covered with cellophane tape.
The most suitable conditions for the separation were investigated in detail, using tartaric acid, citric acid, acetic acid and formic acid.
Separation of trace 137Cs, 90Sr, 144Ce and 95Zr from each others was carried out only in 25 minutes using 0.05M ammonium citrate, pH 3.5, as the electrolyte at 1080 V, and the mixture of those with 0.05M carrier of each was separated in only 20 minutes at 1440 V.View full abstractDownload PDF (968K) -
Studies on the solvent extraction of dithizonates with benzene and its spectrophotometry. IMasao KAWAHATA, Heiichi MOCHIZUKI, Takeshi MISAKI1962 Volume 11 Issue 8 Pages 819-822
Published: August 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA fundamental study has been made for determination of gold, silver, copper, platinum, palladium, bismuth, cadmium, etc., by the extraction of them with dithizone-benzene solution followed by the spectrophotometric measurement.
Metals were extracted by shaking with 10 ml of 0.01% dithizone-benzene for 1 min. and the ranges of pH and concentration of sulfuric acid for 100% extraction have been determined.
The excess of dithizone was washed off by a dilute solution of alkali and absorption spectra and molecular extinction coefficients of complexes in benzene solution were obtained. Benzene showed a higher extractability of the complexes in comparison with chloroform or carbon tetrachloride. The whole operations including the extraction of complex and the removal of excess reagent were done simply in a separatory funnel.View full abstractDownload PDF (720K) -
Tadashi HAYAMI1962 Volume 11 Issue 8 Pages 822-826
Published: August 05, 1962
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSColorimetric determination of phosphorus in ultra micro amounts of serum by molybdenum blue method has been investigated.
An analytical procedure is as follows : 0.02 ml of serum sample is taken, proteins are precipitated with 2ml of about 10% perchloric acid and, after centrifuging, the supernatant liquid is poured into a 10ml test tube. 0.5ml of 5% ammonium molybdate solution and 2ml of n-butyl acetate are added to it and shaked vigorously for 30 seconds. After extracting complex phosphomolybdic acid with n-butyl acetate, 1 ml of extract is transfered into a 3ml measuring tube, 0.2 ml of stannous chloride solution is added and the whole is diluted exactly to the mark with ethyl alcohol. The absorbance is measured at 725 mμ. Recoveries of phosphorus in serum were 97102%.View full abstractDownload PDF (918K) -
Senjyo TOMIZAWA, Miyoshi KAWAHARA1962 Volume 11 Issue 8 Pages 826-831
Published: August 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA fundamental research on routine analysis by fluorescent X-ray method in the smelting of copper and nickel has been made. The sample used were ores, mattes and slags, while the elements determined were Cu, Ni, Co, Fe, Ca, S, Si, and Mg.
Several representative samples from each lot were chosen to give standard samples, and those were analyzed accurately by the standard chemical methods.
Calibration curves were made from the percentages of elements and their fluorescent X-ray intensities. Twenty nine combinations were obtained from the kinds of sample and the elements to be determined, and analytical conditions characteristic to each combination were given.
The analytical error in each case was given by the variation in the difference of values obtained by fluorescent X-ray analysis and those by the standard chemical method. The standard deviations were 13% for the prime grade elements and 310% for most of low grade ones. The errors were comparable with, or even less than, those usually met in the rapid chemical analysis.View full abstractDownload PDF (1128K) -
Tetsu KASHIMA1962 Volume 11 Issue 8 Pages 831-835
Published: August 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSHalogen ions are titrated in mixtures of an organic solvent and water in order to increase the sensitivity of the measurement. The effect of the organic solvent in the mixture has been examined by a direct differential potentiometric titration.
The conventional potentiometric titration in aqueous solution using a cell with a salt bridge would not be applied in the presence of any organic solvent, since the liquid junction potential between an aqueous solution of the salt bridge and an organic solution of the sample is very large and unstable, especially in the course of the titration.
In this paper the author has introduced a direct differential titration method using silver-silver retarded electrodes in order to avoid the fluctuation of the liquid junction potentials. Using a "squirt electrode" with a syringe and a three-way glass tube, or a nitrogen gas bomb and a three-way glass cock, the titration is carried out more conveniently and more accurately than the older method using a rubber squirt. The results of the experiments showed that the sensitivity and stability of the measurement were much increased.View full abstractDownload PDF (1094K) -
Differentiating titration by an abrupt change of the component of the sample solventTetsu KASHIMA1962 Volume 11 Issue 8 Pages 835-840
Published: August 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSGlass electrode serves as the reference electrode even in the presence of organic solvent, containing potassium hydrogen phthalate as an indifferent electrolyte.
The effect of various organic solvents and their concentrations on the argentimetric titration of halogens in solvent mixtures has been investigated by potentiometric titration with a silver indicator electrode and a glass reference electrode. By using isopropanol as the solvent of the standard, and aqueous acetone as that of the sample, the sensitivity of chloride determination has been increased four to ten times, comparing with that in the conventional aqueous titrations. The sensitivity for bromide is increased two to three times, but that for iodide only slightly.
Two halogens contained in a sample can be determined separately with high accuracies by a new method, in which the one in the sample is titrated as usual in the aqueous solution, and the other is then titrated in succession after adding plenty of acetone in the sample solution.View full abstractDownload PDF (1224K) -
Kyoichi HOSOHARA, Rokuro KURODA, Kazuaki KAWABUCHI1962 Volume 11 Issue 8 Pages 841-844
Published: August 05, 1962
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSHigh concentration of nitrite in solution can be determined conveniently by a differential spectrophotometric method by the use of an absorption peak at 355 mμ. The concentration of nitrite (C2) is obtained from the concentration of the reference (C1) and the absorbancy of sample solution Aγ by the following equation :
C2=C1+1/0.47×Aγ
As for the reference solution, the concentration C1=NO2- 6 mg/ml is recommended as an optimum, and with this method Beer's law holds to NO2-7.5 mg/ml. The method is rapid and needs no special reagent. As much as 10 times the weight of nitrate does not interfere.View full abstractDownload PDF (670K) -
Chemical analysis of chromium. IXAkira KAWASE1962 Volume 11 Issue 8 Pages 844-850
Published: August 05, 1962
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSMetallic chromium was dissolved in perchloric acid for its conversion to chromic acid and aluminum was coprecipitated with chromium hydroxide at pH 5.56.0 by using 20 mg chromium (III) as a carrier. A majority of chromium was removed as chromyl chloride and the residual chromium together with several disturbing elements were removed with DDTC extraction (Table IX and X).
The remaining trace of chromium was masked with citric acid (Table VII and VIII), and Ti, V, Nb, and Ta were inactivated with hydrogen peroxide (Table II). Aluminum was extracted with chloroform at pH 9 as its oxinate and was determined by measuring the absorbancy at 390 mμ.
Aluminum in high purity chromium and commercial products by the thermit process weredetermined (Table XII and XIV).
The conditions for coprecipitation and extraction of aluminum, and for removing of disturbing elements have been investigated in detail.View full abstractDownload PDF (1205K) -
Shozo OSHIMA, Akira KATSUMATA1962 Volume 11 Issue 8 Pages 850-854
Published: August 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA method for measuring mass spectra of highmass hydrocarbons has been presented. A special device is given for introducing samples in the instrument, where liquid hydrocarbon taken by a micropipet in a stainless steel bottle is heated and introduced by the evaporation into a sample vessel. Suitable conditions for evaporation of sample out of the bottle and absorption of it by the vessel are sought for to obtain high reproducibility of the mass spectra.
The mass spectra of C6C22 paraffins and the development of a method for analyzing normal-paraffin by molecular ion indicates a possibility of the analysis of normal-paraffins with high accuracy.View full abstractDownload PDF (908K) -
Shozo OSHIMA1962 Volume 11 Issue 8 Pages 854-860
Published: August 05, 1962
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSIn the earlier papers reporting the mass-spectrometric type-analysis of paraffines, the objects were confined in C6C11 normal-paraffines or iso-paraffines with only one branch.
The author presents in this paper the mass-spectra of C6C22 paraffines obtained by a mass-spectrometer of high resolving power with a high temperature sample introduction device.
The results indicate that the type analysis with the combining use of the total sum of peakheights of CnH2n ion of M/e>42 (relative values with M/e 57 of n-hexane as the base peak.) and the molecular ion is successfully applicable to C12C22 paraffines.View full abstractDownload PDF (984K) -
[in Japanese], [in Japanese]1962 Volume 11 Issue 8 Pages 861-863
Published: August 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDownload PDF (477K) -
[in Japanese]1962 Volume 11 Issue 8 Pages 864-871
Published: August 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESS
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