All issues
Volume 15, Issue 11
Displaying 1-18 of 18 articles from this issue
- |<
- <
- 1
- >
- >|
-
Yoshiaki WATANABE, Katsutoshi ISOMURA1966 Volume 15 Issue 11 Pages 1215-1219
Published: November 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA gas chromatographic method for determining traces of methanol in hydrocarbons by using calcium carbide has been developed. The sample injected as a pulse is passed through a tube of calcium carbide heated to 300°C, where the methanol is converted completely to acetylene dimethyl ether. Their mole ratio in this case is 65 : 35.
The dimethyl ether is separated from hydrocarbons using an oxydipropionitrile column and is detected with a hydrogen flame ionization detector.
The method is comparable to the colorimetric method.View full abstractDownload PDF (742K) -
Ohiko KAMMORI, Hirahisa KAWASE, Isamu INAMOTO1966 Volume 15 Issue 11 Pages 1219-1223
Published: November 05, 1966
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSquare-wave polarographic determination of microamounts of tin (0.256 μg) was studied and for the first time applied to the analysis of pure iron as follows.
One tenth g of sample is decomposed with the mixed acid (HCl and HNO3) and then each 10 ml of beryllium solution (1 mg Be/ml) and EDTA solution (10%) are added. Then tin is precipitated with beryllium hydroxide as a collector by adding 5 ml of ammonium hydroxide after neutralization. The precipitate is separated by centrifuge and dissolved in 3 ml of hydrochloric acid. After the dilution with water to exact 10 ml, the solution is applied to spuare-wave polarography under the voltage between-0.3 and-0.6 V against mercury pool and the amount of tin is determined from the wave height of about-0.45 V.
This determination was carried out with an absolute error of less than 2.5 ppm for 2.560 ppm of tin. The time required for an analysis was about 100 min. Fifty μg each of Ag, Al, As, B, Bi, Ca, Cd, Ce, Co, Cr, Cu, K, Mg, Mn, Mo, Na, Ni, P, Pb, Sb, Si, Ta, Ti, Tl, U, V, W, Y, Zn and Zr do not interfere but 20 μg of Nb does with the determination of 4 μg of Sn.View full abstractDownload PDF (672K) -
Ohiko KAMMORI, Isamu TAGUCHI1966 Volume 15 Issue 11 Pages 1223-1227
Published: November 05, 1966
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method of direct dissolution of metal with organic reagent was applied to the spectrophotometric determination of 2100% of metallic iron in iron ores. Acetylacetone, 2-thenoyltrifluoroacetone and a mixture of the two as the solvent were compared. The mixture was found most suitable since it dissolved metallic iron rapidly but was practically inert to iron oxides time required for an analysis was about 2 hours. The results were about 3% higher than those by HgCl2 method.
The recommended procedure is as follows: Take 0.8mg of sample in a 100ml-conical beaker equipped with a glass tube (inside diameter: 3mm, length: 250mm). Add 10ml of acetylacetone and 3.0g of 2-thenoyltrifluoroacetone and shake the whole for 90 min. at 70°C. Cool in water for 5min. and dilute to 50ml with carbon tetrachloride. Measure the absorbance at 470mμ against carbon tetrachloride.View full abstractDownload PDF (909K) -
Shinkichi IMAYOSHI, Keiichi FURUYA, Iichi OGAHARA, Hitoshi KAMADA1966 Volume 15 Issue 11 Pages 1227-1233
Published: November 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSOxygen in silver, palladium, and their alloy was determined by vacuum fusion method (A), isotope dilution method using 18O labelled carbon monoxide (B), and fast neutron activation method (C). Oxygen from silver sample was extracted at the furnace temperature of 1400°C. when metal bath technique was not used. Trace oxygen was extracted in the case of palladium not using metal bath at the temperature of 2100°C. The results of oxygen in silver gave the same value of 125ppm under these conditions: (A) gas extraction temperature of 1750°C with the platinum-tin bath, (B) no metal bath and the same gas extraction temperature, and (C) noise level between 6 MeV and 9MeV. The results of oxygen in palladium gave the same value of 63ppm by three methods. The analytical conditions are as follows: (A) 1750°C with the platinum and the platinum-tin bath techniques, (B) 1850°C without metal bath. The results of oxygen in palladiumsilver alloy by three methods were not coincident. Carbon monoxide was allowed to circulate in a furnace and gas adsorption curves by sample metals were measured at the different furnace conditions according to the operation presented in Bunseki Kagaku, 14, 708 (1965). Comparisons of determinations by these methods at various experimental conditions can easily give an accurate procedure, and the effects of gas adsorption and incomplete gas extraction from the furnace can be estimated.View full abstractDownload PDF (1227K) -
Takayoshi YOSHIMORI, Yoshihisa HINO, Tsugio TAKEUCHI1966 Volume 15 Issue 11 Pages 1234-1238
Published: November 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe purity of potassium dichromate was estimated by the coulometric titration using ferric sulfate as generating electrolyte and commercially available apparatus. The end point of titration was detected by the sensitive amperometric or potentiometric method. The coefficients of variation of these results were 0.016% and 0.068%, respectively. Potassium dichromate and potassium permanganate standard solutions were standardized by the same method in which the end point was detected by the sensitive amperometric method. The coefficients of variation of these results were 0.038% and 0.061%, respectively. Sodium arsenite standard solution was also standardized by the dead stop end point method using potassium iodide as generating electrolyte. The coefficient of variation of the results was 0.048%. Sources of the errors have been also discussed.View full abstractDownload PDF (985K) -
Isao FUJII, Koichi TAKADA, Haruo MUTO1966 Volume 15 Issue 11 Pages 1239-1245
Published: November 05, 1966
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA fast neutron activation method was applied to the determination of oxygen in aluminum metal and aluminum alloy. In this paper, a pre-treatment method of sample surface before analysis, optimum conditions on the measurement of gamma-rays from nitrogen-16, and a correction method for the absorption of neutrons, beta-rays, and gamma-rays in the sample were discussed.
The samples including oxygen of the order of 10% 0.0008% were analyzed by the proposed method. Relative standard deviations of the method in the oxygen levels of 0.1%, 0.01%, and 0.001% were 3%, 5%, and 30%, respectively. The sensitivity obtained was 2000 counts/mg of oxygen.View full abstractDownload PDF (1234K) -
Yoshitaka KOBAYASHI, Hiroshi TAKENO, Tetsuzo KITAGAWA, Saburo KANNO, T ...1966 Volume 15 Issue 11 Pages 1245-1251
Published: November 05, 1966
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple method for the determination of cyanide in water by a detector tube was studied.
The cyanide ion detector tube consisted of two layers of packed silica gel particles in a small-diameter glass tube. One of the layers was added with ο-tolidine dihydrochloride and the other added with copper sulfate. A Conway's diffuser was used for the elimination of the coexisting interfering substances. The sample water was acidified to give off hydrogen cyanide which would then be absorbed in the alkali solution in the diffuser. The alkali solution obtained was then sent into the detector tube. The concentration of cyanide ion in sample water was determined from the length of the blue-colored zone in the detector tube. Analytical range of the proposed method is CN-: 120 ppm.View full abstractDownload PDF (1207K) -
Hitoshi KOHARA, Kuniki UENO, Nobuhiko ISHIBASHI1966 Volume 15 Issue 11 Pages 1252-1257
Published: November 05, 1966
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSBrownish-black iron(III)-morin complex was extracted with aliphatic alcohols. The complex showed absorption maxima at 500 mμ and 600 mμ with constant absorbances at pH 3.55.0, and they were applied to the determination of small amounts of iron(III).
The procedure was as follows: 1.0 ml of 0.05M morin solution in dimethylformamide, and 5.0 ml of buffer solution (pH 4.0) containing sodium acetate and acetic acid were added to a sample solution. After adding 10 ml of iso-amyl alcohol, the mixture was shaken vigorously for 10 min. The absorbance was measured at 500 mμ or 600 mμ. In the concentration range of 1.07.0 μg of iron(III) in 10 ml of organic phase, the calibration curve obeyed the Beer's law. Mn(II), Ni(II), Co(II), Zn(II), Al(III), Mo(VI), W(VI), V(V), Ti(IV), Th(IV) etc. scarcely interfered. with the determination of iron(III).View full abstractDownload PDF (799K) -
Ohiko KAMMORI, Hirahisa KAWASE, Yasuo HIYAMA1966 Volume 15 Issue 11 Pages 1258-1260
Published: November 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe photometric method for the determination of microamounts of calcium (580ppm) with glyoxalbis-(2-hydroxy-anil) (GHA) was studied and for the first time applied to the analysis of pure iron as follows.
One tenth g of sample is decomposed with 20ml of hydrochloric acid (1+1) and 5ml of hydrogen peroxide (15%), then the ferric and other interfering ions are removed with the MIBK extraction or the mercury cathode electrolysis. After adjusting the pH (12.5) by sodium hydroxide solution (20%), the complex of calcium and GHA is extracted in 10ml of n-butyl alcohol. Calcium is determined by measuring the absorbance of the organic layer against n-butyl alcohol at 517mμ.
Fifty μg each of Al, As B, Ce, Co, Cr, Cu, Mg, Mn, Mo, Nb, Ni, P, Pb, Si, Sn, Ta, Ti, V, W, and Zn do not interfere, but Cd does. Its interference is removed by a pre-extraction of the complex of cadmium and GHA with mixed chloroform and pyridine.View full abstractDownload PDF (583K) -
Ohiko KAMMORI, Akihiro ONO, Satoshi OKUBO1966 Volume 15 Issue 11 Pages 1260-1264
Published: November 05, 1966
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSFor the determination of microarnounts of silicon (01.5μg) in pure iron after the separation of iron by mercury cathode electolysis, a spectrophotometric method by chloroform extraction of the complex of molybdenum blue and polyoxyethylenelaurylamine was studied as follows.
One tenth gram of sample is dissolved in exactly 10ml of sulfuric acid (3:160) and 2ml of hydrogen peroxide (15%) and the iron is removed by mercury cathode electrolysis. The solution is diluted to exact 100ml with distilled water. A 25ml aliquot is placed in a polyethylene beaker and diluted to about 100ml with water. After 2ml of ammonium molybdate solution (5%) is added and the mixture is stood for 15 min.5ml of oxalic acid solution (5%) is added with stirring and the mixture is stood for 5 min. After 5ml of sulfuric acid (1:3) and 5ml of the reducing reagent (stannous oxalate 2.2g, oxalic acid 4.2g, sodium formate 4.0g, formic acid 2.4ml, and water 240ml) were added, the mixture is stood for 10min, and placed in a polyethylene separatory funnel.
Two ml of polyoxyethylenelaurylamine solution (5%, in sulfuric acid 1:3) and 5.00ml of chloroform were added and the mixture is shaken by a shaker for 3min. Silicon is determined by measuring absorbance of the organic layer at 800 or 655mμ against the blank solution.
Twenty micrograms of each of Al, As, B, Ca, Ce, Co, Cr, Cu, Mg, Mn, Mo, Nb, Ni, P, Pb, Sn, Ta, Ti, V, W, and Zn do not interfere.View full abstractDownload PDF (760K) -
Takanobu HAMAGUCHI, Kazuya HORIUCHI, Nariaki TANAKA1966 Volume 15 Issue 11 Pages 1264-1268
Published: November 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSSpectrographic determination of manganese quantity in blood, urine and feces of normal male has been studied, in order to examine the occupational manganese poisoning, because of its trace amonut of contents, restriction of the sampling quantity and also of easy operation of the sample. Sample blood was dried, and sample urine and feces were dried to ashes, and they are discharged between graphite powder electrode, either copper or lithium carbonate being used as an internal standard material and crater graphite electrode with alternating current are of 220V, at 68A and the calibration was made according to the Seidel density method.
The results show that it is determined in the range of 0.01ppm with 24 ml of sample bIood and 0.001ppm with feces, with 1020% precision.View full abstractDownload PDF (774K) -
Hitoshi YOSHIDA, Mitsuhiko TAGA, Seiichiro HIKIME1966 Volume 15 Issue 11 Pages 1268-1270
Published: November 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAs one of the simultaneous continuous recording method of multi-components in flowing sample solutions, a method to record automatically only peak current values continuously in the square wave polarogram has been studied. In a part of the applied voltage of the square wave polarograph, an optional constant potential was added to the electrolytic cell successively for the improvement. These set-up potential was adjusted in advance to the peak current of the subjected component and the change was made by the synchronizer equipped with 6-points recorder. After the periodic changes of current signal, produced by the dropping mercury electrode, was inhibited by using synchronized circuit, only the peak current value was recorded.
The applicability of this method was examined with a mixture of copper, lead and cadmium in hydrochloric acid as a supporting electrolyte, and the results obtained by this method was found to be available to the analysis of multi-components in continuous measurements.View full abstractDownload PDF (532K) -
Keisuke SUZUKI, Sinko GOTO, Fuzio ITO1966 Volume 15 Issue 11 Pages 1271-1273
Published: November 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method was proposed for the gas-liquid chromatographic determination of diphenamide in wettablepowder.
Diphenamide was extracted with acetone from the sample and it was analyzed with added benzylbenzoate as an internal standard with a Shimadzu Gas Chromatograph, GC-2B by a thermal conductivity detector, using helium as a carrier gas, maintaining the flow rate to be 50 ml per minute.
The column (4 mm × 1 m, stainless steel) used contains 20 weight per cent Silicone Gum SE-30 and 1 weight per cent Emulsogen WS-32 as a stationary phase on the support of Celite 545 and the column temperature was adjusted at 185°C.
A calibration curve in the 0.52.0 weight ratio (Diphenamide/benzylbenzoate) was found to be almost linear.
The results of the recovery test were tabulated in Table II.View full abstractDownload PDF (523K) -
Keisuke SUZUKI, Sinko GOTO, Fuzio ITO1966 Volume 15 Issue 11 Pages 1273-1275
Published: November 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method was proposed for the gas-liquid chromatographic determination of CMMP in emulsifiable concentrates.
CMMP was dissolved in acetone and it was analyzed with adding benzylbenzoate as an internal standard with a Shimadzu Gas Chromatograph GC-2B by a thermal conductivity detector, using helium as a carrier gas, maintaining the flow rate to be 50 ml per minute. The column (4 mm × 1 m, stainless steel) used contains 20 weight per cent Silicone Gum SE-30 and 1 weight per cent Emulsogen WS-32 as a stationary phase on the support of Celite 545 and the column temperature was adjusted at 185°C.
A calibration curve in the 1.02.5 weight ratio (CMMP/benzylbenzoate) was found to be almost linear. The results of the recovery test were tabulated in Table II.View full abstractDownload PDF (488K) -
Minoru FUKUDA1966 Volume 15 Issue 11 Pages 1275-1276
Published: November 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIt was ascertained that the platinum contact used as a catalyst for burning the alkyl iodides formed in the microdetermination of alkoxyl groups can be successfully replaced with cupric oxide. The alkyl iodides formed by hydrolysis of a sample with hydriodic acid are carried by air over cupric oxide heated about 750°C, and burned into iodine and carbon dioxide. The iodine is absorbed with silver, and the carbon dioxide with soda asbestos, and they are weighed. From the amount of the iodine and the molecular ratio between the carbon dioxide and the iodine, the alkoxyl groups are determined separately. Analytical conditions are also discussed.View full abstractDownload PDF (330K) -
[in Japanese], [in Japanese], [in Japanese], [in Japanese]1966 Volume 15 Issue 11 Pages 1277-1290
Published: November 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (2666K) -
[in Japanese]1966 Volume 15 Issue 11 Pages 1291-1297
Published: November 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (1275K) -
[in Japanese]1966 Volume 15 Issue 11 Pages 1298-1303
Published: November 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (1116K)
- |<
- <
- 1
- >
- >|