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Volume 11, Issue 11
Displaying 1-22 of 22 articles from this issue
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X-ray fluorescence analysis of tantalite and allied substances. IKoichi NISHIMURA, Yutaka KAWASAKI1962 Volume 11 Issue 11 Pages 1107-1111
Published: November 05, 1962
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSOne half g of tantalite is mixed with 0.35g of an internal standard consisting of HfO2: 300, MoO3: 50 and Co: 50, and fused with 8.5 g of KHSO4 in a porcelain crucible. This procedure for preparation of sample has an advantage of reducing matrix effect and gives a better result comparing with the case of the direct X-ray fluorescence analysis without a preliminary treatment.
Concentration of Ta2O5, Nb2O5 and MnO in tantalite are in the range of 6075, 515 and 1020% respectively. Intensities for fused samples (TaLα and HfLα, NbKα and MoKα, MnKα and CoKα) are measured comparing with those for four standard samples as references, containing 5080% Ta2O5, Nb2O5 and 1230% MnO.
Standard deviations of analytical values are 0.33% for Ta2O5 and 0.03% for Nb2O5 and MnO. Determination of three elements on ten samples are done in 1012 hours.View full abstractDownload PDF (769K) -
X-ray fluorescence analysis of tantalite and allied substances. IIKoichi NISHIMURA, Yutaka KAWASAKI1962 Volume 11 Issue 11 Pages 1111-1115
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSIn order to see the matrix effects in the X-ray fluorescence analysis of tantalite and its leaching residue, analyses were carried out for synthetic samples as Ta2O5 (20, 50 and 80%) added with TiO2 as a light component or SnO2 as a heavy component and MnO (20, 50 and 80%) added with TiO2 or Ta2O5.
No enhancement or absorbance effect was seen in the experiment, and good calibration curves with the standard sample (Table II) were obtained for the widely varying concentrations of each components as Ta2O5 (275%), Nb2O5 MnO (1088%), Fe2O3 (430%) and TiO2 (230%), (Fig. 59).
The Procedure and measuring conditions employed were quite similar to those in the preceding report.View full abstractDownload PDF (709K) -
Tsutomu MATSUDA, Hideo YATSUGI1962 Volume 11 Issue 11 Pages 1116-1122
Published: November 05, 1962
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSThe following two-component stationary phase composed of polar and nonpolar stationary liquids : silicon oil DC 703-P. E. G. 1500, Squalane-P. E. G. 1500 and D. N.-β, β'-iminodipropionitrile, were prepared by two procedures using Shimalite B (a kind of fire-brick for gaschromatographic use) or Celite 545 as the solid support ; one (method A) by coating the solid with mixtures of two stationary liquids and the other (method B) by mixing two stationary phases prepared independently.
The effects of the composition of stationary liquids upon retention times were compared with these two-component stationary phases for the mixtures of cyclohexane, benzene, tetrahydro-furan, acetone and methanol at 35°C and cyclooctane, p-xylene, mesityl oxide and n-butanol at 90°C, respectively.
The results indicated that the mixed phases by both method A and B had nearly same characteristics and the polarity of the mixed phaseschanged in parallel with the composition of stationary liquids. The addition of a small amount of the polar stationary liquids (2.5%) to 20% nonpolar phases caused an effective depression of tailing of oxygen-containing materials in either method A or B.View full abstractDownload PDF (1081K) -
Studies on the polarographic analysis. XXXXIITaitiro FUJINAGA, Mitihiro ISIBASI, Kazuo YAMASITA1962 Volume 11 Issue 11 Pages 1122-1127
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe extraction of copper (II) -diethyldithiocarba-mate (DDTC) into chloroform was examined in the presence of masking agents such as EDTA or potassium cyanide and of buffering agents such as sodium citrate, sodium phosphate and glycine ; the chloroform extract was evaporated with small amounts of aqueous mineral acid and the resulting solution was examined polarogra-phically after the addition of suitable supporting electrolyte.
It was found that copper could be extracted quantitatively from the solution of pH ranging from 1 to 13 even in the presence of EDTA, however it was not extracted by the method in the presence of potassium cyanide. The reextraction of copper from chloroform layer into aqueous solution with mercuric ion was also studied and the reextraction was found quite qualitative when the amount of mercuric ion exceeded that of copper. As the results, it was found that 1× 10-5 mole/l copper could be conveniently separated, concentrated and determined polarographically ; the excess mercuric ion could be removed by the reduction with hydrazine sulfate if necessary.
Bismuth did not disturb the determination of copper by the use of sodium citrate-EDTA mixture as the supporting electrolyte.
The method was successfully applied for the micro determination of copper in a large amount of mercury ; 0.005% (w/w) copper in mercury was determined within an error ±4%.View full abstractDownload PDF (997K) -
Ion exchangepolarographic methodShizo HIRANO, Atsushi MIZUIKE, Yoshio IIDA1962 Volume 11 Issue 11 Pages 1127-1131
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSAn ion exchange separation has been applied to the polarographic determination of trace amounts of cadmium in reactor-grade high-purity thorium compounds. A hydrochloric acid solution of the sample is introduced into an anion exchanger column (Amberlite IRA-400, Cl-form, 50100 mesh, 1.8cm φ × 4 cm).
Cadmium, as its negatively charged chloride complex, is retained strongly in the column, whereas thorium passes through completely. The cadmium is then desorbed with 1N nitric acid, and determined finally by means of a D. C. or A. C. polarograph. A hundredth to 5 ppm of cadmium in thorium can be determined by this method with an accuracy of about 10% at 0.1 ppm. The time required for a determination is approximately 3 to 4 hrs. A modified procedure has also been proposed by the use of liquid ion exchanger (Amberlite LA-2, as 10% xylene solution) instead of the ion exchange resin. This procedure saves time without a serious loss of accuracy comparing with the original one.View full abstractDownload PDF (832K) -
Study on analytical methods of steel making materials. IIMasao KAWAHATA, Heiichi MOCHIZUKI, Rokuro KAJIYAMA, Masao ISHII1962 Volume 11 Issue 11 Pages 1132-1136
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA method was presented for the determination of total rare earths, cerium, silicon, iron and calcium in calcium-silicon containing a large amount of rare earths.
Total rare earths together with iron were separated from calcium by precipitation with ammonium hydroxide. The precipitate was dissolved in hydrochloric acid, adjusted to pH 2, oxalic acid was added for precipitation of total rare earths and they were weighed after ignition. Cerium in the precipitate was dissolved in sulfuric acid, the solution was oxidized with ammonium persulfate in the presence of silver nitrate and titrated with ferrous ammonium sulfate and potassium permanganate.
Calium, iron and silicon were determined by conventional methods. Fundamental experiments have been carried out in detail, and good results were obtained for the analysis of a sample containing 0.05% carbon, 15% calcium, 25% rare earth metals and 5% iron, respectively.View full abstractDownload PDF (793K) -
Kyuya OIDA, Kozo FUZITA, Isamu TAKAHASHI1962 Volume 11 Issue 11 Pages 1136-1142
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSFor the production and quality controls in the manufacturing of high-purity aluminum, a spectrochemical method using a quantorecorder was developed for the determination of trace impurities.
Si, Fe and Cu present in 0.00050.01% concentrations in high-purity aluminum were determined successfully by the direct point-to-plane method by the excitation with overdamped discharge (L=360 μH, C=50 μf, R=20 Ω, sample negative) by the low voltage. Need for the special care to avoid outside contamination at the sample preparation and cutting of the graphite counter electrode was emphasized.
Precision of the method was 1015% by coefficient of variation. The values obtained were in agreement with those by chemical analysis with errors of less than 1030% for each element.View full abstractDownload PDF (962K) -
Yuko OKAZAKI1962 Volume 11 Issue 11 Pages 1142-1146
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe electrode reaction of four sulfanilamide derivatives with pyrimidine nucleus, N1-(2-pyrimidyl)-sulfanilamide (I), N1-(4-methyl-2-pyrimidyl)-sulfanilamide (II), N1-(2, 4-dimethyl-6-pyrimidinyl)-sulfanilamide (III) and N1-(2, 4-dimethoxy pyrimidinyl)-sulfanilamide (IV), was investigated, and the mechanism of reduction of these sulfanilamides was ascribed to the reduction of pyrimidine nucleus as in the case of 2-aminopyrimidine.
The polarographic properties of those sulfanilamide derivatives were investigated, and the relation between the concentration and the wave height of sulfanilamides under the most suitable condition for their determination was persued. Available concentration ranges for the determination were, respectively, 0.11.0mM for (I) and (II) in a buffered solution of pH 3.0 or 9.0, 0.11.0mM for (III) in a buffer pH 3.0, and 0.21.0mM for (IV) in an unbuffered solution containing tetramethylammonium bromide as a supporting electrolyte. Recommended procedure for each is given.View full abstractDownload PDF (774K) -
Yuko OKAZAKI1962 Volume 11 Issue 11 Pages 1147-1151
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSN1-(6-methoxy-3-pyridazinyl)-sulfanilamide (sulfamethoxypyridazine) gives a reducing wave due to the reduction of pyridazine nucleus in the same way as in other pyridazine derivatives, while N1-(5-methyl-1, 3, 4-thiadiazol-2-yl)-sulfanilamide (sulfamethylthiadiazole) gives a hydrogen wave due to the reduction of hydrogen in N1-position in the same way as in sulfaisoxazole of group I.
Polarographic determination of these has been carried out for 0.11.0mM of the former in a buffer of pH 5 and for 0.21.0mM of the latter in a nonbuffered solution containing tetramethylammonium bromide as a supporting electrolyte. A recommended procedure for each is given.View full abstractDownload PDF (855K) -
Shigeo WAKAMATSU1962 Volume 11 Issue 11 Pages 1151-1155
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSSteel sample was decomposed in nitric-perchloric acid mixure and heated to white fuming for precipitation of silicon, tungsten, etc. The precipitate was filtered off and the filtrate was treated with sufficient EDTA and beryllium sulfate solution for masking of iron and others. Ammonium hydroxide was added to pH 89, and the solution was boiled for min. for precipitation of tin and beryllium as their hydroxides and for separation from iron and others.
The precipitate was filtered, washed with NH4OH (2+ 100) containing EDTA and taken up in H2SO4 (1+ 5). It was heated with KClO3 to white fuming to destroy any contaminating EDTA and excess KClO3. The residue was taken up in water. A trace of iron was reduced by an addition of ascorbic acid. A definite amount of standard EDTA solution was added in a slight excess against Sn, ammonium acetate added to pH and Sn was estimated by the back titration of EDTA with standard thorium solution using Xylenol Orange as an idicator.View full abstractDownload PDF (1018K) -
Chemical analysis of chromium. XAkira KAWASE, Haruno OGAWA1962 Volume 11 Issue 11 Pages 1155-1162
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSAn a. c. polarographic determination of tin in high-purity chromium has been investigated and a procedure was recomended as follows.
The chromium metal was dissolved in hydrochloric acid. After cooling, chromous and stannous ions were oxidized to chromic and to stannic by passing air and hydrochloric acid saturated with bromine was added to complete the oxidation. In order to remove interfering elements such as lead and chromium, the solution was adjusted to 8M with hydrochloric acid and passed through an anion exchange resin column (10 mmφ × 60 mm, Dowex 1-X8, 100200 mesh). After the column was washed with 50 ml of 8M hydrochloric acid, tin was eluted with 1M nitric acid. The effluent was heated with 3 ml of sulfuric acid (1+ 10) and evaporated to fume of sulfuric acid. The residue was dissolved with 4 ml of 3.75M hydrochloric acid and 1 ml 50% ethanol solution of 2.5 × 10-3M tetraphenylarsonium chloride, and then tin was determined polarographically.
An analysis of electrolytic high-purity chromium and commercial electrolytic chromium of 99.99% purity found 2.8 and 1.2 ppm of tin respectively. The result of recovery tests was practically satisfiable.View full abstractDownload PDF (1202K) -
Chemical analysis of tellurium. IIAkira KAWASE1962 Volume 11 Issue 11 Pages 1162-1168
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDetermination of above 0.1 ppm of lead in high purity tellurium has been carried out. The sample was dissolved in nitric acid-hydrochloric acid. Ammonium citrate was added and the pH was adjusted to about 10. The lead was extracted with dithizone-benzene and was taken up into nitric acid. The determination of lead was achieved by the square wave polarography with sodium hydroxide-sodium chloride-sodium sulfite as supporting electrolyte or by the dithizone spectrophotometry.
In case of the content of lead was extremely small, a majority of tellurium was removed as tellurous oxide before the extraction (Table X).
Determinations of lead in commercial tellurium of 99.97% and 99.999% purity by the proposed. method gave values 17 ppm and 0.2 ppm, respectively (Table I).View full abstractDownload PDF (1237K) -
Masakatsu SUGIMOTO1962 Volume 11 Issue 11 Pages 1168-1176
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe equation developed by Beattie et al. for the relation between fluorescent X-ray intensity and the composition of matrix {II = KII0WI/∑(μiJ + μfIJ) WJ} is extensively criticized, and is proved to be a fine approximation which highly satisfies the diverse physical requirements.
The standard deviations after the correction are ± 0.13% for 734% Cr, ±0.05% for 820% Ni and ± 0.5% for 5580% Fe, respectively.
There is also good correlation between the correction coefficient obtained by statistical methods and the mass absorption coefficient, the matrix effect in fluorescent X-ray intensity being ascribed mainly to the absorption of fluorescent X-ray by the matrix components.
The results indicate that a correction formula for fluorescent X-ray analyses can be derived from the Beattie's equation, offering a simple and accurate correction method in routine analyses.View full abstractDownload PDF (1369K) -
Yohe TSUCHIYA1962 Volume 11 Issue 11 Pages 1176-1180
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSEDTA titrations of zirconium and hafnium can be performed in boiling solutions containing 0.9 ± 0.3N free hydrochloric acid using xylenol orange as an indicator. The color change is from red to yellow, which should persist on boiling for one minute. Interferences are not caused by 1 g of uranium (VI), iron (II), aluminum, zinc, tin, or magnesium, 0.1 g of titanium or sulfate, and 1 mg of phosphate ions. Iron (III) must be reduced with tin (II) chloride.
Interference from 0.1 g of thorium can be overcome by addition of about 5 mg of sulfate ion. When hafnium is present with zirconium, the former can be calculated by combining the the gravimetric method with mandelic acid.
The method has been successfully applied for the rapid determination of zirconium and hafnium in zircon sands, special porcelains, and a magnesium alloy.View full abstractDownload PDF (834K) -
Takashi TANAKA, Kazuo HIIRO1962 Volume 11 Issue 11 Pages 1180-1184
Published: November 05, 1962
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSA new method for the spectrophotometric determination of arsenic with quercetin as a color reagent is proposed. Quercetin reacts with arsenic (V) and develops yellow color, the maximum absorption wavelength of which is 398 mμ. For the determination of arsenic (V), evaporate the sample solution to dryness in presence of quercetin, and dissolve the dried residue with ethyl alcohol and then measure the absorbancy of the colored solution at 398 mμ.
The effects of several variables are studied and optimum operating conditions are decided. Beer's law is obeyed over a range of 0.02.0 ppm of arsenic (V). The molar absorbancy index is 25, 000. The error in this method is 6.2% and the standard deviation is 0.01024 in absorbancy for ten reproducible measurments for each 1.0 ppm arsenic (V). Certain amounts of phosphate and arsenic(III) do not interfere.View full abstractDownload PDF (717K) -
Eiji NIKI, Kazuo MASATO, Takero KYOYA1962 Volume 11 Issue 11 Pages 1185-1191
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSMetallic phase in titanium carbide-nickel cerment has been extracted rapidly by constant current electrolysis, and the content of titanium in the nickel phase has been determined.
The coulomb of electrolytic current and the potential of the specimen as anode have been measured during electrolysis in 1N hydrochloric acid solution. The endpoint of extraction of nickel phase is able to be decided at the time that the potential of the specimen jumps up steeply during electrolysis.
The Ti/Ni ratio in the nickel phase of 70 titanium carbide-30 nickel cermet, heat treated in vacuum for 1 hr at 1300°C followed by water quenching, was 2.4%, and in that heat treated in the same manner for hr. 2 at 600°C, was 0.3%.
It is considered that the difference of the ratio shows corresponding change of the solubility of TiC in the nickel phase.View full abstractDownload PDF (4786K) -
[in Japanese], [in Japanese]1962 Volume 11 Issue 11 Pages 1192-1194
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESS -
[in Japanese], [in Japanese], [in Japanese]1962 Volume 11 Issue 11 Pages 1194-1196
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
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[in Japanese]1962 Volume 11 Issue 11 Pages 1197-1199
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
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[in Japanese]1962 Volume 11 Issue 11 Pages 1200-1202
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
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[in Japanese]1962 Volume 11 Issue 11 Pages 1203-1210
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDownload PDF (1186K) -
[in Japanese], [in Japanese]1962 Volume 11 Issue 11 Pages 1211-1222
Published: November 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDownload PDF (1825K)
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