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Volume 5, Issue 1
Displaying 1-14 of 14 articles from this issue
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KAZUO OTA1956 Volume 5 Issue 1 Pages 3-7
Published: January 05, 1956
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSFundamental studies of ο-phenanthroline method for the estimation of Fe and its applications to white metals and solders are made. The maximum absorption of orange-red complex of ο-phenanthrolme and Fe (II) is shown at 508515mμ, and also the time required for completion of the developmentof color varies depending on the order of addition of reagents, pH and temperature of solutions. Interfering elements present in such alloys are Sn, Sb, As, Pb, Cu (>15ppm) and Zn (>30ppm). Sn, Sb and As in sample solution with H2SO4 are volatilized off by heating at 200220°with HBr by Hoffman-Lundell method, the solution is evaporated to 5 cc, neutralized with NH4OH, clarified with the addition of 2cc H2SO4(1:1), and then CH3COONa-CH3COOH buffer, NH2OH. HCl and ο-phenanthrolire are added in order named, let stand for 20 minutes above 20° and Fe is determined photometrically. When the sample contains Pb, Cu or Zn as the constituents, Pb is separated as PbSO4, Cu and Zn are removed to permissible extent by catching Fe in Al(OH)3 as a carrier, the precipitate is dissolved in dil. H2SO4 and treated as above.View full abstractDownload PDF (1297K) -
SHIZO HIRANO, HITOKO MURAYAMA, MITSUKO KITAHARA1956 Volume 5 Issue 1 Pages 7-11
Published: January 05, 1956
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIt is well known that the presence of even a small amount of vanadium in the electrolysis of brine by mercury method causes a marked lowering of current efficiency. The authors have been investigated a rapid method of estimation of a trace of vanadium in brine and commercial salt. To a sample solution acidified with hydrochloric acid, ferric salt (about 50mg Fe), hydrogen peroxide water and aqueous ammonia are added to precipitate ferric hydroxide, to which all the vanadium is absorbed and the precipitate is filtered, taken up in 20ml sulfuric aid (1:3), treated with 20ml sulfuric acid (1:1), 15ml phosphoric acid, 1ml approximately 0.1N ferrous ammonium sulfate and 5ml 20% urea solution, the vanadium is oxidized by adding dropwise 3% potassium permanganate, the excess permangate is decomposed by adding dropwise 3% sodium nitrite solution, also, the excess of nitrous acid is decomposed with urea previously added, the solution., is treated with 5ml 0.01% sodium diphenylaminesulfonate, made up to 100ml with water, the red purple colored solution is taken up in a cell and the light absorbency is estimated, using 570mμ, filter. The cell is then treated with a drop of approximately 0.1N ferrous ammonium sulfate for decolorization of red purple color due to vanadium and the vanadium is estimated from the differences in absorbency in these two estimations. The error in this method was ±2?3γ vanadium and the time required for the estimation was about 40 minutes. The vanadium in brine electrolyte was about30γ/l and that in salt was 0.00001?0.00004%, also the vanadium content in sludge obtained from refining of brine was 0.00017%.View full abstractDownload PDF (1222K) -
TOMOYUKI MUKOYAMA1956 Volume 5 Issue 1 Pages 12-16
Published: January 05, 1956
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe titrations of alkali cyanide with standard nickel sulfate solution in the presence of murexide were studied in comparison with the Liebig-Denigès method. To a sample solution containing 0.3g alkali cyanide in a 300ml conical beaker, 8ml 6N ammonium hydroxide is added, diluted to 100ml with water, 0.03-0.05g murexide powder (0.4g ammonium purpurate+100g sodium chloride) added as an indicator, and titrated immediately with a standard 0.1N nickel sulfate until all the cyanide has complexed with the nickel and the color of the solution changed from violet-pink to clear yellow. Although the standardization of 0.1N nickel sulfate could be carried out gravimetrically in the usual dimethylglyoxime method (I), and volumetrically against the standard EDTA solution (II) or against the standard 0.1N silver nitrate solution (III) by comparing the volume of 0.1N nickel sulfate solution required in the titration of the same volume of a potassium cyanide solution by the present method, with that of the standard silver solution by Liebig-Denigès method, the latter method gave better result when a nickel salt, with which the standard solutions were prepared, was contaminated with considerable amounts of cobalt, copper etc. The present method proved excellent reproducibility and showed a sharp end point unless too much murexide powder was added. The results obtained were closely consistent with that of Liebig-Denigès method. An addition of 2-30ml 6N ammonium hydroxide gave the constant result. No difficulty was found in the procedure in the presence of considerable amounts of halide, carbonate, acetate, thiocyanate, nitrate, sulfate, phosphate, oxalate, ferrocyanide and chromate, with the exception of ferricyanide, nickel, cobalt, silver, copper and calcium. The disturbance by the presence of calcium was removed by adding an excess amount of sodium oxalate before the titration. In the end, the present method is recommended especially for the technical routine analysis instead of the usual argentometry on accoun t of a lower cost of nickelsalts and their applicability for turbid sample solutions.View full abstractDownload PDF (986K) -
HIROSHI NISHIDA1956 Volume 5 Issue 1 Pages 17-20
Published: January 05, 1956
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSQuantitative determination of about 10ppm Ge in sulfite ore by acid decomposition method gives very low value. In order to find the cause of this result, Ge4+ in HNO3 or H2SO4 is heated on a water bath or sand bath with the addition of Na2SiO3, SiO2 prepared from Na2SiO3 and -250 mesh quartzite and the Ge is distilled in HCl acidity. In this case, 20γ of Ge added to 0.1g. of the SiO2 was found to be absorbed to the extent of 20γ, 17.5γ and 1.513γ, respectively. The absorption of Ge was greater with an increase of the temperature of digestion or by increasing the amount or finess of the SiO2. The effect of SiO2 was examined on sulfite ore with Ge and the decomposition of the SiO2 with HF gave good result; also, an experimental result of separation of Ge from Fe3+ by use of SiO2 as a carrier is shown. Quantitative determination is made on 50cc sample solution containing 5cc of 0.04%-phenylfluorone and 9cc of HCl. After the solution is allowed to stand from 4hours to over night to develop the color and the intencity of the color is measured by use of S 50 light filter plate. The method followed Beer's Law very well within the limit of 140γ.View full abstractDownload PDF (999K) -
Polarographic Behaviors of Tetraphenylphosphonium Chloride for Bismuth IonMUTSUAKI SHINAGAWA, HIROSHI MATSUO, HIROYUKI NEZU1956 Volume 5 Issue 1 Pages 20-23
Published: January 05, 1956
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn this experiment, tetraphenylphosphonium chloride, (C6H5)4PCl, is synthesized and its polarographic behaviors have been investigated. The reagent shows one-step reducing wave having a maximum wave at about -1.85V (vs. S. C. E.) which is difficult to be suppressed. The reagent, with the use of suitable complex ion-forming agents, showed to give precipitation reaction with the following metal ions; Hg2+, Cu2+, Cd2+, Bi3+, Sn2+, Sn4+, Sb3+, Co2+, Mn2+, Fe3+, Ni2+, Zn2+ etc., and anions such as I3-, SCN-, ClO4-, IO4-, BE4-, MnO4-, S2O82-, WO42-, MoO42-, Cr2O72-, VO43-, Fe(CN)63-, Fe(CN)64-, and Fe(C2O4)33-, also it reacts to form precipitates with various heteropoly acids. The reaction with Bis+ among above metal ions is especially sensitive and gives a complete precipitation polarographically. A successful result is obtained for amperometric titration of Bi3+ by use of the reagent and the determination is carried out within the error of ±1%.View full abstractDownload PDF (861K) -
MASAFUMI MAKI1956 Volume 5 Issue 1 Pages 23-29
Published: January 05, 1956
Released on J-STAGE: February 16, 2010
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Spectrophotometric Determination of Cobalt as Tetraphenylphosphonium CobaltothiocyanateMUTSUAKI SHINAGAWA, HIROSHI MATSUO, RIKUSEI KOHARA1956 Volume 5 Issue 1 Pages 29-32
Published: January 05, 1956
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThis investigation deals with the application of tetraphenylphosphonium chloride as a quantitative reagent for cobalt by polarographic and spectrophotometric methods. The reagent gives clearblue colored precipitate by the reaction with cobaltothiocyanate complex salt, the precipitate is extracted completely by use of chloroform. The extract showeda maximum absorption at 620mμ and the lightabsorbancy showed no change after standing for 1 week and the determinationis carried out within the errors of 3?5% when the concentration of Co2+ is 72.6 γ/ml. (or Co2+ 3.62γ/ml. CHCl3) to 652. 6γ/ml. (or Co2+ 32. 63γ/ml. CHCl3). The effect of pH on the light absorbancy is not very important. The presence of metal ions, such as Zn2+, Cd2+, Hg2+, Sn2+, Sb3+, Pb2+ and Mn2+ up to an equal weight of 167γ of Co2+ in a solution is not interfering, but interfered by the presence of several γ of Fe3+, Cu2+ and Bi3+.View full abstractDownload PDF (817K) -
ROKURO KURODA, Tsuneo SHIMIZU, TOSHI KAWASHIMA1956 Volume 5 Issue 1 Pages 33-37
Published: January 05, 1956
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSVarious factors in the separation and determination of copper by use of mercaptoacetic acid, CH2 (SH) COOH, have been investigated. Mercaptoacetic acid reacts quantitatively with copper and forms a light yellow precipitate in solution acidified with sulfuric acid, that slightly acidified with nitric acid or that acidified with acetic acid. In order to determine the conditions for quantitative determination, kind and concentration of acids, condition for aging of the precipitate, required amount of reagent, composition of the precipitate, disturbing elements, accuracy and precision of the method have been investigated. Silver, mercury and lead form light yellow precipitates in the same way as in copper but the formation of precipitates from mercury and lead is prevented by adding ammonium nitrate in large excess in a slightly acidified solution with nitric acid or in acetic acid solution, and the separation and quantitative estimation of copper is Possible. However, the disturbance by the silver cannot be prevented even by this method. In general, the presence of Cl- in this method should be avoided with the exception of a minute amount.View full abstractDownload PDF (1220K) -
Behavior of Traces of Cesium Revealed by a Tracer Method with Cs137NOBORU YAMAGATA, TOSHIKO YAMAGATA1956 Volume 5 Issue 1 Pages 37-40
Published: January 05, 1956
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe loss of cesiun in the process of separation and concentration from sea water was examined. When the quantity of cesium is very small (K/Cs>2000 by atomic ratio), cesium does not always behave as potassiun in the separation of NaCl and KCl. Cesium is precipitated almost perfectly with potassium by chloroplatinate method and remains perfectly in solution by alcoholic-HCl method. On the other hand, about 80% of cesium moves into the NaClO4 fraction by perchlorate method, and 30-40 % is lost by cobaltinitrite method. The whole process of separation and concentration of cesium by the removal of alkaline earth elements with oxin, precipitation of sulfate ion with barium chloride and elimination of the excess barium carbonate adopted by E, Minami. et al, who gave 0.1 to 1γ Cs/l of sea water in 1947 was proved to be satisfactory. Also, G. Jander's concentration process of removing of KCl from carnallite with HCl and precipitation of cesium silicomolybdate was proved to be satifsctory.View full abstractDownload PDF (1019K) -
[in Japanese]1956 Volume 5 Issue 1 Pages 41-42
Published: January 05, 1956
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1956 Volume 5 Issue 1 Pages 42
Published: January 05, 1956
Released on J-STAGE: June 30, 2009
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[in Japanese]1956 Volume 5 Issue 1 Pages 43-47
Published: January 05, 1956
Released on J-STAGE: June 30, 2009
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[in Japanese]1956 Volume 5 Issue 1 Pages 47-53
Published: January 05, 1956
Released on J-STAGE: February 16, 2010
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[in Japanese]1956 Volume 5 Issue 1 Pages 54-57
Published: January 05, 1956
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (950K)
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