All issues
Volume 19, Issue 2
Displaying 1-26 of 26 articles from this issue
- |<
- <
- 1
- >
- >|
-
Fumio UEHARA, Akiyoshi FURUNO1970 Volume 19 Issue 2 Pages 183-187
Published: February 05, 1970
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSA selective spectrophotometric method has been proposed for the determination of molybdenum in tungsten-bearing steels, and the recommended procedure is as follows.
After adding tartaric acid and sodium hydroxide to a sample solution, it is made to contain 10% sulfuric acid.
To it are added 5 ml of 5% sodium thiocyanate and 5 ml of 35% stannous chloride solution, and the.colored molybdenum complex is extracted by shaking for 5 min. with 25 ml of butyl acetate.
The absorbance is measured at wavelength about 470 mμ (filter). Tungsten(VI) hundred times as much as molybdenum does not interfere. Also Cr(VI), V(V), Ni(II), Co(II) and Cu(II) are not influencing.
The Beer's law is obeyed over the range 3.2 μg Mo/ml, and apparent molar extinction coefficient is 18, 700.
The proposed method was applied to the determination of molybdenum in chromium steels and high speed steels.
The results agreed with standard values, the relative error being less than 3%.View full abstractDownload PDF (731K) -
Yutaka YAMAZAKI1970 Volume 19 Issue 2 Pages 187-190
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA rapid method is developed for the determination of sulfur in alumina by the reduction method with tin(II)-strong phosphoric acid {Sn(II)-SPA}. With 10 ml of Sn(II)-SPA, 0.5 g of alumina sample is decomposed in a simple glass tube at 280300°C in 2530 minutes. Alumina is resoluted completely and sulfur in alumina is reduced to hydrogen sulfide. The liberated hydrogen sulfide is introduced into zinc acetate solution in absorption bottles, then the solution is titrated with 0.01M iodine standard solution.
Experiments on various alumina samples show above 99% recoveries in each sulfur determination. Optimum condition of the reaction and influence of coexisting materials are examined.View full abstractDownload PDF (592K) -
Kouichiro UMEMOTO, Shingo HIROSE, Keiko SAKAMOTO, Takako KOURI, Keiich ...1970 Volume 19 Issue 2 Pages 191-195
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSAn accurate visual titration method for simultaneous microdetermination of calcium and magnesium has been introduced by using complexometry with GEDTA and CyDTA using MTB and BNP as indicators.
The investigation was carried out to obtain the optimum condition for simultaneous microdetermination of calcium and magnesium. As the result, a procedure was established in which calcium, in the first place, was determined by a back titration of excess standard GEDTA with standard calcium solution at pH 13 using BNP as an indicator in an aqueous acetone medium. Magnesium was successively determined by titration with standard CyDTA solution at pH 1011 using MTB as an indicator.
The method has been successfully applied to the flask combustion method for calcium and magnesium in organic compounds with sufficient accuracy, the standard deviation being less than 0.2%.View full abstractDownload PDF (738K) -
Takeichi SAKAGUCHI, Tomoko YOSHIDA, Sachiko HARA1970 Volume 19 Issue 2 Pages 196-200
Published: February 05, 1970
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSPrecipitated tetanus toxoides, precipitated pertussisdiphtheria combined vaccine and inactivated measles virus vaccine presently used usually contain 0.62.5 mg/ml or less of aluminum as an adjuvant.
Aluminum in these samples is now determined by aluminon method (the official method, Minimum Requirements of Biological Products, Ministry of Health and Welfare, Japanese Government), but this method is rather troublesome in procedure and gives poor recovery.
The authors tried to determine Al in vaccines with stilbazo by a method for Al in iron ores with a little modification and obtained good results by controlling the amount of reagents, pH and standing time and by selecting optimum wavelength. The recommended procedure is as follows.
To an aliquot of homogeneous suspension of sample (12 ml) after vigorous shaking is added 0.5 ml of 1.5N HCl. It is diluted to 50 ml with water after dissolution. After 10 times dilution five ml of this diluent is pipetted into a 25 ml measuring flask and 10 ml of acetate buffer (1M CH3COOH : 1M CH3COONa 1 : 9) and 5ml of 0.06% stilbazo solution are added. It is made up to 25 ml with distilled water. The pH of the final solution is 5.65.7.
After 530 min. the absorbancy at 520530 mμis measured against blank and the content of Al in sample is determined by referring to a calibration curve prepared beforehand. The proposed method is simple, highly sensitive and accurate, compared with other methods such as aluminon method and gravimetric oxine method.View full abstractDownload PDF (664K) -
Micro spectrophotometric determination of chloride ion with 4, 4'-bis(dimethylamino)thiobenzophenoneTakeichi SAKAGUCHI, Kiyomi TAGUCHI1970 Volume 19 Issue 2 Pages 200-204
Published: February 05, 1970
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESS4, 4'-Bis(dimethylamino)thiobenzophenone (TMK) produces an indigo-blue coloration having a maximum absorption at 640 mμ in an aqueous acetone solution with halogenide ions (Cl-, Br-, I-, CN- and CNS-) in the presence of cupric ion.
A new method was developed for a micro spectrophotometric determination of chloride ion by an application of this reaction.
The sensitivity was dependent on the ratio of water and acetone. The calibration line was linear for 220μg of Cl- in the recommended procedure. Determination of chloride ion in biological fluids such as urine and serum was carried out successfully by this method without deproteinization.View full abstractDownload PDF (726K) -
Mitsuyasu SUZUKI1970 Volume 19 Issue 2 Pages 204-207
Published: February 05, 1970
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSA high-frequency plasma torch spectrometry was applied to the determination of boron, and several experimental conditions were examined.
The most suitable conditions were as follows : magnetron anode current 180 mA, nitrogen gas flow rate as the carrier 8l/min, acid concentration of sample solution 3N HCl and analytical line BI 2497.73Å.
Iron, nickel, chromium and manganese as the coexisting elements did not influence on the intensity of analytical line, but sodium and potassium reduced the line intensity. The calibration curve had good linearity and coefficient of variation of the curve was about 3.7%.View full abstractDownload PDF (687K) -
Mitsuyasu SUZUKI1970 Volume 19 Issue 2 Pages 207-212
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSIn order to determine simultaneously tungsten and molybdenum by high-frequency plasma torch spectrometry, experimental conditions were examined.
The most suitable conditions were : magnetron anode current 140 mA, argon gas as the tangential gas 6l/min, argon gas as the carrier 2.5l/min, and analytical lines MoI 3864.11Å and WI 4008.75Å.
Iron, nickel, manganese, chromium etc. did not influence on the intensity of analytical lines, but the intensity was reduced by the sample solution containing sodium.
Tungsten and molybdenum in Fe-Mo alloys, Fe-W alloys, high-speed steels and tool steels could be determined rapidly with high precision, whereby the coefficient of variation of Mo (0.082%) and W (3.28%) in tool steel were, respectively, 4.0% and 6.8%.View full abstractDownload PDF (920K) -
Satoru EMURA, Susumu SUGIKAWA1970 Volume 19 Issue 2 Pages 212-216
Published: February 05, 1970
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSA remotely operating square-wave polarographic method was established for the determination of iron in dissolver and highly radioactive waste solutions (1AW) of irradiated fuel reprocessing.
By adding triethanolamine as complex agent, the iron wave caused a shift in E 1/2 to more negative potentials. Also, the interference from uranium was eliminated by the addition of ammonium carbonate.
The recommended procedure is as follows. In a polarographic cell are mixed 500 μl of sample solution and 5.0 ml of supporting electrolyte containing 13.2% triethanolamine, 0.22M ammonium carbonate and 1.1M ammonium hydroxide. After deareation with nitrogen for 15 minutes, the polarogram is recorded from 0-0.5V vs. mercury anode. Iron content is determined by referring to a calibration curve. The determinable limit of concentration of iron is 10 ppm.
The relative standard deviation was less than 5.0%, for iron in feed solution to 1A column (1AF) and highly radioactive waste solution of reprocessing plant.View full abstractDownload PDF (767K) -
Taitiro FUJINAGA, Masatada SATAKE, Tatsuo YONEKUBO1970 Volume 19 Issue 2 Pages 216-220
Published: February 05, 1970
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSA method of liquid-liquid extraction of zinc oxinate with melted naphthalene followed by a solid-liquid separation was successfully applied to the trace analysis of zinc.
In this experiment, the pH of the sample solution was adjusted to about 9.1 after the addition of 1 ml of 1% oxine solution. The solution was heated on a water bath, shaken vigorously after the addition of 1.5 g of naphthalene to extract zinc oxinate into the liquefied naphthalene layer and allowed to stand still at room temperature. The solidified naphthalene bead was washed with water, dissolved and diluted to 25 ml with ethyl alcohol. The absorbance was measured at 385 mμ against the reagent blank. Beer's law is obeyed for 33 to 360 μg of zinc in 25 ml of ethyl alcohol.
The interference from aluminum was removed by the addition of fluoride ion, and that from iron and copper by oxine-benzene extraction at pH 4.0.View full abstractDownload PDF (628K) -
Hiroshi NISHIDA1970 Volume 19 Issue 2 Pages 221-226
Published: February 05, 1970
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSChromazurol S (CAS; H4L) reacts with iron(III) to form the 2 : 1 (Fe2L2+) and 1 : 1 (FeHL) complexes at pH<2, and the 1 : 2 (FeL25-) and 1 : 3 (FeL39-) complexes at pH>4.
The coordination of iron(III) in the complexes occurred at the oxygen of phenolic-carboxylic site in CAS.
The 1 : 3 complex had an absorption maximum at 630 mμ and its absorbance was the highest and invariable in the presence of above 1.03×10-3M of CAS at pH 5.55.9. Beer's law held for 0.081.8 ppm of iron. The molar absorptivity was 5.5×104 and the sensitivity for 0.001 of the absorbance was 0.0009μg/cm2.View full abstractDownload PDF (688K) -
Koichi MUKAI1970 Volume 19 Issue 2 Pages 227-230
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA simultaneous polarographic procedure for the determination of bismuth and lead in 2011 aluminum alloy (Al-5.5%Cu-0.4%Bi-0.4%Pb) has been developed.
Two fifth gram of sample is decomposed with 8 ml of 20% sodium hydroxide solution, and it is diluted to 30 m/ with water. After adding 14 ml of (1+1) nitric acid, it is heated to complete dissolution and evaporated to 25 ml. To it are added successively with stirring 10 ml of 50% ammonium acetate solution, 1 ml of 10% ascorbic acid solution, 1 ml of 20% potassium thiocyanate solution and 2 ml of 0.2% carboxymethyl cellulose solution. It is diluted to 50 ml with water, and bismuth and lead are determined from a d. c. polarogram of the supernatant solution. The half wave potentials of Bi and Pb are -0.1 V and -0.4V vs. Hg pool, respectively. A caution should be taken to keep pH of the solution from 3.5 to 3.7. It takes 60 minutes for a determination, and the precision expected is approximately 3% as the coefficient of variation at 0.5% level of bismuth and lead.View full abstractDownload PDF (512K) -
Keisuke SUZUKI, Tsukasa KASHIWA1970 Volume 19 Issue 2 Pages 231-235
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA method was described for the spectrophotometric determination of captan in wettable powders and dusts. One milliliter of chloroform solution of the sample containing about 10 mg of captan was applied to a thin layer plate of silica gel with 0.5 mm thickness at a line 4cm from the bottom. The plate was developed ascendingly with chloroform until the solvent front arrived at 10cm line. The adsorbing band of captan was detected under the light of a short-wave UV lamp (250 mμ). The value of Rf for captan in this solvent was about 0.6. After air-drying for 30 minutes, the adsorbent of marked spot was scraped from the plate into a glass-filter and captan was eluted with acetone. After the removal of the solvent by evaporation, the residue was dissolved in 10 ml of a mixture of acetone-methanol (1 : 1) and decomposed by sodium-alcohol reduction. The liberated inorganic chloride was determined by mercuric thiocyanate method. The recovery tests gave reasonable results.View full abstractDownload PDF (722K) -
Noboru YAMAMOTO, Shigeo SOEJIMA, Masao HARADA1970 Volume 19 Issue 2 Pages 236-238
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA photometric method for the determination of a microamount of silicon in vanadium metal is proposed. The method involves the extraction of silicomolybdic acid into methyl isobutyl ketone (MIBK) and the formation of molybdenum blue in the extract. By the method, more than 20 ppm of silicon in vanadium can be determined. The procedure is as follows. The sample is dissolved in nitric acid, evaporated to dryness, fused with sodium carbonate and dissolved with hydrochloric acid. An aliquot (V<50 mg, Si<50 μg) of the solution is taken and made up to 50 ml while keeping the acidity at 0.4M in hydrochloric acid. The solution is then treated with ammonium molybdate and oxalic acid, and silicomolybdic acid is extracted with MIBK. The extract is washed with hydrochloric acid and treated with stannous chloride solution. The absorbance is measured at 750 mμ using the solvent as a reference. The calibration curve should be prepared in the presence of the same amount of vanadium as that in sample solution.View full abstractDownload PDF (401K) -
Hiroyuki YOSHIDA, Chushiro YONEZAWA1970 Volume 19 Issue 2 Pages 238-241
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA method is described for the determination of small amount of uranium in zirconium and zircaloy by neutron activation. The sample and standard solution containing known amount of uranium are irradiated. After cooling for one day, the sample is dissolved in hydrochloric acid and hydrofluoric acid. The solution is evaporated, and treated with sulfuric acid to remove excess fluoride ion. After dissolving the residue in 1N hydrochloric acid, 239Np is separated by 2-thenoyltrifluoroacetone extraction. Gamma-radioactivity of 239Np is measered using an NaI (Tl) scintillation counter. The proposed method has been successfully applied to several standard samples containing more than 2 ppm of uranium.View full abstractDownload PDF (560K) -
Masakazu DEGUCHI, Kouji SAKAI1970 Volume 19 Issue 2 Pages 241-243
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSMercury(II) formed a blue complex with Methylxylenol Blue (MXB) in an aqueous solution. The absorption maximum of the complex was at 615 mμ, and the absorbance was nearly constant over the pH range from 6.7 to 7.0. The calibration curve followed Beer's law over the range from 6 to 60 μg of mercury(II) in 25 ml solution. Variation coefficient for 50 μg of mercury(II) was 1.4%.
The recommended analytical procedure was as follows : fifteen milliters of the sample solution containing 6 to 60 μg mercury(II) was mixed with 1.0 ml of hexamethylenetetramine-HNO3 buffer and 1.0 ml of 0.1% MXB solution, and made up to 25ml with water (the final pH 6.8). After 5 minutes, the absorbance at 610 mμ was measured against the reagent blank. Many metal ions interfered. Good results were obtained for the analysis of tap water added with known amounts of mercury(II).View full abstractDownload PDF (386K) -
Yai SHIOBARA1970 Volume 19 Issue 2 Pages 243-245
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSSeparation of rhenium(VII), molybdenum(VI) and tungsten(VI) can be effected by thin-layer chromatography on an alumina-coated polyethylene terephthalate film (Eastman Chromagram Sheet 6062, 100 μ thick) in simple aqueous solutions of acids or salts. All the solvent systems tested which include the dilute aqueous solutions (<0.1N) of thiocyanic acid, ammonium thiocyanate, hydrochloric, acetic, oxalic, malonic, tartaric, citric acids and ammonia, are found to give the most favorable resolution of the three elements. Rf values are in the order Re (VII)>Mo(VI)>W(VI) irrespective of the developing solvents.View full abstractDownload PDF (515K) -
Potentiometric titration with potassium iodate. II.Nobuhiko IRITANI, Naomi SAWANISHI, Yoshio TAKINO1970 Volume 19 Issue 2 Pages 245-248
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSPotentiometric titration of potassium iodide with potassium iodate solution by the iodine-cyanide method was studied. The titration curve showed a distinct just corresponding to the reaction I--2e→I+.
The optimum conditions for the titration were as follows. Concentration of hydrochloric acid and potassium cyanide at the end point were respectively 11.5M and 0.3M. Temperature was 15°C. Titration rate was 0.2 ml per min. The reproducibilities were higher than 99.6% for 0.140.0028M potassium iodide solution.View full abstractDownload PDF (590K) -
Tsugio TAKEUCHI, Hideo HADA, Mituru YAMAZAKI1970 Volume 19 Issue 2 Pages 249-251
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA theoretical study of a constant-current series vacuum tube circuit was given. The improved circuit was more stable for the fluctuation of load, and possible ranges of current and load were 1200 mA and 00.3 kΩ, respectively.
The relative error in the determination of sodium thiosulfate by the use of this circuit was less than 0.8%.View full abstractDownload PDF (439K) -
Tomomi MIZUNO, Akihiko HARADA, Yutaka KUDO, Nobuhiro HASEGAWA1970 Volume 19 Issue 2 Pages 251-253
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA method is proposed for the determination of trace cadmium (0.11 ppm) in zirconium and its alloy. The sample is treated with H2SO4, HF-H3BO3 and HNO3 in a covered beaker to complete the dissolution. The solution is adjusted to pH 8 to 10 with aqueous NH3 in the presence of ammonium citrate. Cadmium is extracted into dithizone-chloroform from which it is re-extracted into 1 M HCl (5 ml). The extractant is atomized into the acetylene-air flame of an atomic absorption spectrophotometer ; measurement is made at 228.8 nm, with a hollow-cathode lamp as source. The scale expansion on measurement is taken 10 fold for the detection of less than 1 ppm of cadmium, but the method is applicable to higher concentration of cadmium by reducing the scale expansion. There is no interference from any other elements in zirconium and zircaloy.View full abstractDownload PDF (398K) -
Separation of cupric ion and nickel ion by fluorideMutsuaki SHINAGAWA, Kazuyoshi FURUSHIMA, Kumao UCHIDA, Takeo HARADA1970 Volume 19 Issue 2 Pages 253-255
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe focusing chromatographic separation for copper and nickel by a fluoride as a precipitation reagent was investigated. The experiments have been made by putting hydrochloric acid in the positive cell and a dilute aqueous solution of fiuoride in the negative cell. Fundamental factors as for selection of fluoride, pH values, concentration of fluoride solution, concentration of hydrochloric acid etc. were examined.
The above method gave good results for focusing and separating cupric ion and nickel ion.View full abstractDownload PDF (400K) -
[in Japanese]1970 Volume 19 Issue 2 Pages 256-261
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDownload PDF (3021K) -
[in Japanese], [in Japanese]1970 Volume 19 Issue 2 Pages 262-268
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDownload PDF (3792K) -
[in Japanese]1970 Volume 19 Issue 2 Pages 269-277
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESS -
[in Japanese], [in Japanese], [in Japanese], [in Japanese]1970 Volume 19 Issue 2 Pages 277-301
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDownload PDF (4661K) -
1970 Volume 19 Issue 2 Pages 302-304
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDownload PDF (275K) -
[in Japanese]1970 Volume 19 Issue 2 Pages 305-310
Published: February 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDownload PDF (7196K)
- |<
- <
- 1
- >
- >|