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Volume 16, Issue 9
Displaying 1-22 of 22 articles from this issue
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Liquid amalgam method in nonaqueous media. IChozo YOSHIMURA, Hiroshi HARA, Toshiko HARA1967 Volume 16 Issue 9 Pages 883-887
Published: September 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSLiquid zinc amalgam method for the determination of Fe(III), Sn(IV), Ti(IV) with visual titration by antimony pentachloride as standard oxidant in methyl cellosolve was studied.
Congo Red for Fe(II), Methyl Orange for Sn(II) and Safranine T for Ti(III) were used as indicators.
The results of titration indicated that their reduced valencies were similar to those in acidic aqueous solution regardless of the unlike coloration.
Carbon tetrachloride used as a replacement liquid did not interfere with the titration. The application of a preliminary extraction with ether to the proposed method gave satisfactory results on macro amount of elements.View full abstractDownload PDF (752K) -
Tsugio TAKEUCHI, Shigenori SAKURAI1967 Volume 16 Issue 9 Pages 888-894
Published: September 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe authors used a plasma jet generator proposed by M. Yamamoto. It consists of a nozzle-shaped copper anode and a tungsten rod cathode containing 2% thoria, and uses argon as discharging gas. Fundamental studies were done on the determination of nickel, manganese and chromium in aqueous solution. Current 280A, flow rate of argon 15l/min., feeding rate of sample solution 1ml/min. and time of exposure about 10 seconds were most favorable. Comparison of the results with those by alternating arc discharge indicated that (1) the plasma jetmethod gave much higher linearity of calibration line, and (2) it was less affected by co-existing elements. In the case of aqueous solution, however, the background values due to water itself is so large that the sensitivity of detection of minute components by plasma jet excitation was not always higher than that by alternating arc excitation.View full abstractDownload PDF (975K) -
Hiroo SASUGA1967 Volume 16 Issue 9 Pages 894-899
Published: September 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSFor the purpose of estimating metallic iron in reduced iron powder by an X-ray diffractometer, an investigation was made on the selection of standard iron metal, preparation of standard mixture and measurements of diffraction intensity.
Taking electrolytic iron as the standard substance, the standard mixtures were prepared by using iron oxide as the diluent. By using Co-Kα line of X-rays and by measuring the intensity of 2.03Å diffraction line of iron by the counting method, metallic iron was determined by the direct procedure.
The amounts of metallic iron in various samples of reduced iron powder were determined. The comparison of the results with those by chemical analysis showed that the X-ray analysis would be more accurate. The reproducibility of the proposed method was 122%.View full abstractDownload PDF (927K) -
Teruo IMAI1967 Volume 16 Issue 9 Pages 900-908
Published: September 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSVarious conditons for the determination of zinc by atomic absorption spectrometry, including fuel gas. pressure, height of burner, influences of acids and diverse elements, etc., were examined. Calcium chloride was effective as a suppressor of interference, but could not remove that from a large amount of copper. In the presence of copper, therefore, the determination was carried out by adding a large amount of copper salt, by which the variation of results with the amount of copper was remarkably diminished.
A method was given for the determination of zinc in high-purity indium metal and in ores. Results or practical samples were satisfactory.View full abstractDownload PDF (1290K) -
Study on analytical methods of steel-making materials. VRokuro KAJIYAMA, Katsumasa YAMAGUCHI1967 Volume 16 Issue 9 Pages 908-912
Published: September 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSFrom 0.02 to 0.60% of titanium as an impurity in ferro-niobium was determined with diantipyryl methane as a colorimetric reagent. Titanium and niobium are similar in their analytico-chemical properties, and often interfere each other with their spectrophotometric determination. With this reagent, diantipyrylmethane, however, niobium several hundred times as much as titanium did not interfere, provided that niobium had been previously converted to its oxalate.
A sample was fused with potassium pyrosulfate, and digested into a sulfuric acid solution containing ammonium oxalate. An appropriate aliquot (corresponding to 10100 μg Ti) was taken out, and iron was reduced by adding ascorbic acid. Eight milli liters of hydrochloric acid (1+1) and 20 ml of the 1% reagent solution were added, and the whole volume was made up to 50 ml with water. The amount of titanium was obtained by the measurement of absorbance at 385 mμ after 45 minutes.View full abstractDownload PDF (698K) -
A study of quantitative analysis using exchange reaction of metal chelates. INorio FUKUSHI1967 Volume 16 Issue 9 Pages 913-917
Published: September 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA theoretical study on the mechanism of exchange reaction of trien (triethylenetetramine) and EDTA(ethylenediaminetetraacetate) between their nickel(II) and copper (II) complexes has been previously performed. It is initiated by a trace of either of these multidentate ligands, and then the following reaction takes place : Ni-trien+Cu-EDTA→Ni-EDTA+Cu-trien. A method using this exchange reaction can be used for trace analysis of metal ions, as its first-order rate constant depends on the concentration of free ligand. In this paper, an investigation is given on some analytical conditions, i. e., pH, temperature, ionic strength, ratio of Cu-EDTA to Ni-trien, etc.
Experiments were done spectrophotometrically by measuring absorbance at 550 mμ for Cu-trien formed. The optimum pH range giving convenient length of time for measurement was from 8 to 9. The effect of temperature could be minimized by means of serial measurements carried through in parallel.
Reagent ratio of Cu-EDTA to Ni-trien was not important so far as either concentration of reagents was 10-410-3M. The method was applied to the analysis of steels and other metals with preliminary separation of the metal ion to be estimated from matrix elements.View full abstractDownload PDF (777K) -
Teruji ISHII, Michiko KENMOKU, Koji ISHII, Mioko YOSHIKAWA1967 Volume 16 Issue 9 Pages 917-921
Published: September 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe conventional thermal analysis is mostly based upon the thaw-melt method (Rheinboldt method) using capillaries or Kofler's hot stage.
The authors have applied the melt-melt method thermal analysis with the automatic thermoanalyzer developed by them to several two-component systems, including phenacetin-acetanilide, caffeine-theophylline, etc., and the results were compared with the phase diagrams obtained by the conventional methods.
Since this instrument records directly the temperature change of the sample itself by the aid of a thermistor, the melting and eutectic points were readily determined from the temperature-time diagram of melting curves. This gives an advantage in removing ambiguity in visual measurements involving personal errors on melting or wetting point.View full abstractDownload PDF (689K) -
Yukio KITANO, Wataru ISHIBASHI, Shoji SATO1967 Volume 16 Issue 9 Pages 922-926
Published: September 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSFor the determination of microamounts of niobium in pure tantalum, a spectrophotometric method by using MIBK-phenylfluorone and Amberlite LA-2-benzene extraction was established as follows. Sample is dissolved with hydrofluoric acid (1+1) and 68 drops of nitric acid. The solution is evaporated nearly to dryness on a water bath, and 0.5 ml of hydrofluoric acid (1+1) is added to the residue. It is dissolved in 0.15 M HF- 8 M HCl, and tantalum is removed by extraction into 10% Amberlite LA-2-benzene solution.
The aqueous layer is evaporated nearly to dryness with nitric acid. The residue is dissolved in the mixture of 10% sulfuric and 10% tartaric acids, to which is then added hydrochloric acid. Niobium is then extracted into MIBK. The extracted niobium reacts with an alcoholic solution of phenylfluorone in the MIBK phase, and the absorbancy at 502 mμ is measured.
Less than 100 μg each of Zr, V, or W, <500 μg each of Ti, Fe, Sn, Ni, or Pt, <1000 μg of Ta and <2000 μg each of Bi, Sb, or Cu do not interfere, but >100 μg of Mo or HF does. The interference from the latters is removed by a pre-extraction and evaporation.
Beer's law is obeyed over the range 0.28.0 μg/ml. Molecular extinction coefficient at 502 mμ is 2.81 × 104.View full abstractDownload PDF (839K) -
Takayoshi YOSHIMORI, Ikuko HIKAWA1967 Volume 16 Issue 9 Pages 927-930
Published: September 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSPurities of some standard reagents for volumetric analysis were determined directly by the coulometric titration method. The apparatus used was nearly the same as that in the previous paper {Yoshimori et al.: This Journal, 15, 1234 (1966)}, but the end points were located by a pH meter with glass electrode.
A little lower results were obtained for standard potassium biphthalate reagents, with coefficient of variation about 0.034%. Results obtained for the standard samples of sulfamic acid and sodium carbonate were satisfactorily coincided with their certificated values. Coefficients of variation for them were about 0.017% and 0.044%, respectively.
It seems that these differences in coefficients of variation depend largely on the magnitude of change in pH through the end points.View full abstractDownload PDF (784K) -
Yuroku YAMAMOTO, Sumiyoshi KIKUCHI, Yasuhisa HAYASHI, Takahiro KUMAMAR ...1967 Volume 16 Issue 9 Pages 931-936
Published: September 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA spectrophotometric method for the determination of mercury(II), based on a solvent extraction of the associated ion pairs formed between 2, 2'-bipyridyliron(II) chelate cations and bromo-mercury(II) complex anions, is described.
The best extractant is 1, 2-dichloroethane, whereas other organic solvents are useless in this system. The absorbance maximum of 2, 2'-bipyridyl-iron (II) chelate in the organic phase is at 526 mμ.
The recommended procedure for the calibration curve is as follows.
Five milliliters of potassium bromide (1 M ), varying amounts of standard mercury(II) solution (25 μg Hg2+ /ml, 010 ml), 1 ml of acetate buffer solution (1 M, pH 4.5) and 5 ml of 2, 2'-bipyridyl-iron(II) solution (5 × 10-3 M) are mixed. This solution is diluted to 25 ml with distilled water, and shaken for 3 min. with 10.0 ml of 1, 2-dichloroethane. The absorbance of the organic phase is measured at 526 mμ against the solvent.
The percentage of the extraction is determined to be 82% (19°C) by radiochemical technique using Hg197. Beer's law is obeyed over the range of 110 μg/ml of mercury(II).
Several features of the proposed method are as follows: A good extraction is obtained in the wide range of pH (210), the reagent employed is readily available in pure form, and the solution remains stable over a long period of storage. The method is convenient, accurate and highly selective for the determination of a small amount of mercury(II).View full abstractDownload PDF (1011K) -
Yuroku YAMAMOTO, Takahiro KUMAMARU, Masahiro TSUBOUCHI, Ichizo OKIMURA1967 Volume 16 Issue 9 Pages 937-941
Published: September 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA spectrophotometric method for the determination of salicylic acid, based on solvent extraction of the ionpair formed between tris(bathophenanthroline)iron(II) and the anion of salicylic acid into n-butyl acetate, is proposed.
The absorbance maximum of tris(bathophenanthroline)iron(II) chelate in the organic phase is at 536mμ. The chemical formula of the extracted species is deduced by continuous variation method to be [Fe (bathophen)3] ·[C6H4(OH) COO]2. Good extraction is obtained in the range of pH 610.
The recommended procedure for the calibration curve is as follows. The mixture (pH 2.54.5) of 1 ml of hydroxylamine sulfate (0.25 M) and 5ml of iron(II) solution (3×10-3 M) is shaken for 1 min. with 10.0 ml of n-butyl acetate containing bathophenanthroline (4.5×10-3 M). To this mixture are added 5 ml of phosphate-borate buffer (pH 8.5) and varying amounts of standard salicylic acid solution (1.0×10-4M, 010 ml). After the aqueous phase is diluted to 25ml with water, it is shaken again for 1 min. The absorbance of the organic phase, which is separated from the aqueous phase and then filtrated through filter paper, is measured at 536 mμ against the reagent blank.
Beer's law is followed in the range of 8×10-64×10-5 M of salicylic acid in aqueous solution, using 10 mm glass cells.View full abstractDownload PDF (767K) -
Yoshiaki WATANABE, Katsutoshi ISOMURA, Yasuo TOMARI1967 Volume 16 Issue 9 Pages 942-945
Published: September 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSGas chromatographic analysis of carbonyl sulfide in high-concentration propylene gas has been achieved using Porapak, silica gel or their combination for the separation column.
On the silica gel column, carbonyl sulfide cannot be separated from propane. On the Porapak column, carbonyl sulfide is eluted between C2 and C3 hydrocarbons, and is separated completely from other compounds, although propane and propylene are eluted only with overlap.
By use of the Porapak-silica gel column, however, not only carbonyl sulfide is separated completely from other compounds in propylene, but also propane can be separated from propylene. The combined column can be used also for the detection of carbonyl sulfide in propylene containing water without interference.View full abstractDownload PDF (585K) -
Giichi MUTO, Haruo MIYASHITA, Yoshinori TAKATA1967 Volume 16 Issue 9 Pages 946-951
Published: September 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA new type of colorimeter was presented. The instrument, of a rod type of 12 mm in diameter and 150 mm in length, was operated by only inserting one end of it into a sample solution. After stirring the solution with the instrument itself, the absorbance or the transmittance of the solution at a certain wavelength was read out. The light sources were a miniature tungsten lamp for the visible region and a Pen-Ray lamp (a miniature quarts tube mercury discharge lamp) for the ultraviolet. The detectors of light were a photoconductive cell (CdS) for visible light and a cell with a filter cutting off visible light or with a fluorescent screen for ultraviolet. It could be used as an ordinary colorimeter and was especially useful as a detector in photometric titrations.View full abstractDownload PDF (887K) -
Hitoshi KAMADA, Takuji UI, Shizuo KIMOTO, Masayuki SATO1967 Volume 16 Issue 9 Pages 952-957
Published: September 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA primary X-ray analyzer with a flat crystal vacuum X-ray spectroscope, for generating characteristic X-rays on the surface of specimen by electron beam of 28mmφ and for analyzing mean concentration of the desired element, has been developed. Details of this instrument and some of its applications to qualitative and quantitative analysis of solid materials are presented. The measurements of spectra such as B-Kα, C-Kα, N-Kα, O-Kα etc. prove that the electron excitation is effective in the region of soft X-rays or light element analysis, and optimum excitation voltage for light elements is so low as 10 kV for O-Kα. The analytical curve of silicon low alloy steels has a good linearity, and shows that the minimum detectable limit of silicon will be 0.003% for one minute counting time, or it is able to determine the concentration of silicon with the precision of 0.001 per cent or less as standard deviation. The qualitative analysis of glass and low alloy steels are carried out.View full abstractDownload PDF (875K) -
Shinji TAKAGI, Kazuma KUMAI1967 Volume 16 Issue 9 Pages 958-959
Published: September 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA bathophenanthroline method was examined to determine microamounts of iron in water. Investigations were made with artificial standards of ferrous diammonium sulfate solution. Analytical procedure was similar to the Wilson's method [found in Analyst, 89, 389 (1964)] but pH adjustment was made with a glass-electrode pH-meter. Ferrous-bathophenanthroline complex was stable in isoamyl alcohol for more than twenty hours. Determinations could be available within the errors 0.4 μg/l (95% confidence limits). This value is smaller than that of authorized in JIS B 8224(1961).View full abstractDownload PDF (272K) -
Shingo MIYAKE, Isao SAKAMOTO1967 Volume 16 Issue 9 Pages 960-962
Published: September 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe chelatometric titration of Ca2+ in the presence of Mg2+ is mostly accompanied with a negative error. The authors observed that such error was avoidable by the addition of a proper amount of Al3+, though the reason is still remained uncleared. An optimum amount of Al3+ to be added was found to be about 2.5 mg for each 10 mg of Mg2+. Aluminum ion must be added and mixed well with the sample solution prior to the pH adjustment. After the pH being adjusted to 13, the titration was carried out in the presence of Dotite NN, as an indicator, and of both KCN and trimethanolamine as masking reagents. It is desirable to detect the end point spectrophotometrically measured at 650 mμ, because the visible change of the color at the end point is not observed so clear. The addition of more than 10 mg of Al3+ to 100 ml each of the titrated solution makes the end point obscur.View full abstractDownload PDF (496K) -
Isamu TSUBAKI1967 Volume 16 Issue 9 Pages 962-963
Published: September 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAlthough H2S2O8 shows weak oxidizing property at room temperature, it works as a strong oxidizing agent at higher temperature via H2SO5 to H2O2 finally and therefore it had been used only as an oxidizing agent. However, H2O2 oxidizes compounds of lower valency, while it reduces that of higher valency, namely it reduces oxidizing compounds and so H2S2O8, which converted to H2O2 at higher temperature is considered. to react as a reducing agent towards oxidizing com pounds. While H2SO4 was added to heat with KMnO4, MnO2, Ce(SO4)2, CeO2, K2Cr2O7, CrO3, NH4VO3 and V2O5, and then (NH4)2S2O8 was added, they were recognized to be reduced. Therefore, if (NH4)2S2O8 is used as an oxidizing agent, it should be heated after it is added at room temperature, however, in order to use it as a reducing agent, it should be added after it is heated.View full abstractDownload PDF (391K) -
Shigenari WASHIZUKA1967 Volume 16 Issue 9 Pages 963-966
Published: September 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA precise method for the chelatometric titration of thioacetamide(TAA) with mercury(II)-ethylenedi-aminetetraacetate has been described. Hg(II)-EDTA solution was added in excess to a sample solution of TAA buffered to pH 10 with ammonia and ammonium nitrate. The concentration of the buffer in the sample solution ([NH3]+[NH4NO3]) was at about 0.3 M, and stirring was continued for 20 minutes. The reaction was found to occur quantitatively at pH above 8.0, according to the following equation:
TAA+Hg(II)-EDTA→HgS+EDTA
The titrimetric determination of TAA was based on the filtration of mercuric sulfide, and on the subsequent titration of the EDTA liberated with a standard solu tion of 0.01 or 0.0025 Mzinc perchlorate. Eriochrome Black T was used as an indicator. For 0.2 m mol TAA in the sample, a standard deviation of the determination was found to be±0.25%, and for 0.004 m mol TAA, ±3%.
In the presence of Zn, Ni, Co, Mn, Cd, Pb, or Cu, these metals were titrated with EDTA, and TAA was then determined by the method described above.View full abstractDownload PDF (815K) -
Hiroshi TSUKIYAMA, Isamu IWAMOTO1967 Volume 16 Issue 9 Pages 967-968
Published: September 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSW, Pt and Cr target X-ray tube have usually been used for X-ray fluorescence analysis, and Mo and Cu. target tube have also been sometimes employed. However, these tubes have following defects. First, it is very hard to determine W by W target tube, Pt by Pt target tube, Cr by Cr target tube, Mo by Mo target tube, and Cu by Cu target tube. But these elements. must be analyzed quite often.
Second, a fluorescence yield of heavy elements by W and Pt target tube is very high, while that of light elements is very low. Therefore the analytical precision of the light elements is very poor.
As to the character of Cr target tube, it is opposed to the above tubes, that is, the yield of heavy elements isvery low.
Being attempted to investigate a new tube without the above defects, Rh target X-ray tube was developed. The fluorescence yield of heavy and light elements by this tube is about 2 times and about 11.2 times as much as the yield by Cr tube, respectively. And Cr, W, Mo and Cu in specimen can be determined with very good precision, too.View full abstractDownload PDF (283K) -
1967 Volume 16 Issue 9 Pages 969-979
Published: September 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (2202K) -
[in Japanese]1967 Volume 16 Issue 9 Pages 980-990
Published: September 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (1729K) -
[in Japanese]1967 Volume 16 Issue 9 Pages 991-1008
Published: September 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (11663K)
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