BUNSEKI KAGAKU
Print ISSN : 0525-1931
Volume 10, Issue 2
Displaying 1-35 of 35 articles from this issue
  • Kenji MOTOJIMA, Hiroshi HASHITANI, Hideyo YOSHIDA
    1961 Volume 10 Issue 2 Pages 79-82
    Published: February 05, 1961
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A new spectrophotometric method for copper in uranium, based on the extraction with chloroform as the 8-quinolinate has been developed. Submilligram quantities of uranium and all other metals which are apt to accompany with copper, can readily be eliminated by washing the extract with a sodium hydroxide washing solution (15%). A minor disadvantage is the rather narrow range of pH (3.13.3) that had to be maintained at the first extraction.
    It is an accurate and rapid method for copperdetermination in uranium down to 0.5 ppm.
    Download PDF (659K)
  • Yutaka NISHINO
    1961 Volume 10 Issue 2 Pages 83-86
    Published: February 05, 1961
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Respective determination of acetaldehyde and acetone is often necessary in vinyl acetate industry. When acetaldehyde in vinyl acetate is determined by hydroxylamine HCl method without modification, it is thought that acetone in the sample also reacts on hydroxylamine partially or fully. The author has found that the obtained value of acetaldehyde includes total acetone, indicating that it reacts on hydroxylamine completely. From this reason, measurements of ultraviolet spectra through a 10 mm layer of vinyl acetate were proposed by the author. By the estimation of light absorbancy at 290 mμ and 300 mμ, less than 0.05% of acetaldehyde and acetone can be determined simultaneously and respectively with an accuracy of ±0.002%, the limit of detection being 0.002% for both. As compared with the other methods of instrumental analysis, the proposed one is thought to be the most useful for the routine works.
    Download PDF (649K)
  • Yutaka NISHINO
    1961 Volume 10 Issue 2 Pages 86-89
    Published: February 05, 1961
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    It is needed on the process control of the vinyl acetate production that small amounts of benzene and toluene in vinyl acetate are determined. The author has compared a number of instrumental analyses with eath other, and concluded that the ultraviolet spectrometry is the most fitted for the purpose.
    Absorption spectrum through a 10 mm layer of sample solution (properly diluted by methanol) is conveniently used, and with the estimation of light absorbancy at 260.2 mμ and 268.2 mμ, 0.01 to 0.5% of benzene and toluene can be determined simultaneously with an accuracy of ±10%-relative at 95% reliability.
    The limit of detection is 0.005%, but 0.001 to 0.002% when benzene or toluene is contained separately.
    Download PDF (705K)
  • Studies on spectrophotometric determination of trace amounts of metals. I
    Fumito NAKASHIMA, Kaoru SAKAI
    1961 Volume 10 Issue 2 Pages 89-93
    Published: February 05, 1961
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A rapid spectrophotometric method has been developed for the determination of trace iron by using bathophenanthroline. Bathophenanthroline and ferrous ion form an intensely red colored complex insoluble in water but soluble in ethanolwater mixture. At maximum absorption, 533 mμ, the molecular extinction coefficient of the complex in 10% ethanol is 22, 400. It has been confirmed that the spectrophotometric measurement of the color intensity developed in 10% ethanol offers a rapid and sensitive method for the determination of iron, and the analytical procedure is simpler than in the extraction method.
    The color is very stable and the intensity does not change provided the pH range is 26. The absorbancy obeys Beer's law, and 5 ppb of iron can be detected when a 100 mm light path is used. Results of water analysis show a standard deviation of less than 2.3%. Among the diverse ions tested, only copper, cobalt, cyanide and citrate have interfering effects.
    Download PDF (855K)
  • Studies on spectrophotometric determination of trace amounts of metals. II
    Fumito NAKASHIMA, Kaoru SAKAI
    1961 Volume 10 Issue 2 Pages 94-98
    Published: February 05, 1961
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Although the red colored complex of ferrous ion and bathophenanthroline is used extensively for the determination of iron, the composition and the stability constant thereof have hitherto been left undetermined. In the present paper, the spectrophotometric study on the ferrous-bathophenanthroline complex in 10% ethanol solution has been carried out.
    The composition of the complex is determined by both the continuous variation method and Molland's method. Since the combining ratio of ferrous ion and bathophenanthroline is one to three in buffered solutions of pH 2 to 6, the red complex is considered to be tris- (4, 7-diphenyl-1, 10-phenanthroline) -iron (II). Following the discussion on the effect of pH on absorbancy, the stability constant of the complex is evaluated to be 1021.8 at 18°C. Bathophenanthroline behaves as a mono-acid base in the solution, and the acidity constant of bathophenanthrolium ion is spectrophotometrically estimated to be 10-4.80 at 18°C.
    Download PDF (759K)
  • Studies on the analytical methods of trace impurities in high purity substances. V
    Masuo MIYAMOTO
    1961 Volume 10 Issue 2 Pages 98-102
    Published: February 05, 1961
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Chemical analysis of Al in high purity selenium was studied, whereby oxine-chloroform extraction method for determination of micro amounts of Al after the preliminary removing of interfering ions by diethyldithiocarbamate-chloroform extraction have been established.
    Se is eliminated by evaporation, after decomposition of sample by nitric acid and sulfuric acid. The residue, treated with hydrofluoric acid, is dissolved in acetate-acetic acid buffer solution. To this solution, diethyldithiocarbamate is added and its complex is extracted away by chloroform. Then Al is extracted by chloroform solution of oxine and determined spectrophotometrically.
    The method is sensitive and rapid. Provided that contamination from apparatus or reagents can be avoided, it is possible to determine Al down to a content of 0.1 ppm within about 3 hours.
    Download PDF (1007K)
  • Studies on the analytical methods of trace impurities in high purity substances. VI
    Masuo MIYAMOTO
    1961 Volume 10 Issue 2 Pages 102-106
    Published: February 05, 1961
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Chemical analysis of T1 in high purity selenium was studied, whereby the most simple and sensitive method for separation and determination of micro amounts of T1 is established.
    Sample is decomposed by nitric acid, sulfuric acid and potassium sulfate, and Se is eliminated by evaporation. The residue is dissolved in hydrobromic acid and T1 is extracted by isopropylether. From the extract, to which is added an aqueous solution of rhodamine B and fully shaken, T1 determined spectrophotometrically.
    Determination of T1 down to a content of 0.1 ppm is easily carried out within about 2 hours.
    Download PDF (898K)
  • Determiation of impurities in thorium. I
    Tomoyuki MUKOYAMA, Norio ICHINOSE
    1961 Volume 10 Issue 2 Pages 107-111
    Published: February 05, 1961
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A method has been studied for the photometric determination of copper (> ca. 0.2 ppm) in thorium oxides or nitrates of the reactor grade. A sample (12.5 g as ThO2) is dissolved in 10 ml nitric acid (1 + 1) and 3 drops of hydrofluoric acid using 50 ml platinum dish and evaporated to dryness on a steam bath. The residue is dissolved in 1 ml nitric acid (1 + 1) and several ml of water by gentle heating, and transfered in a 50 ml tall-beaker. Five ml of 50% citric acid and 8 to 12 ml of ammonium hydroxide (1 + 1) are added with stirring. After the solution is transfered in a 100 ml separating funnel, 4 ml of 1% EDTA is added and the solution is diluted to about 40 ml. The pH should be about 9 against thymol blue paper. One ml of 0.2% sodium diethyldithiocarbamate is then added, and the solution is shaken with 5.00 ml of iso-amyl acetate for about 2 minutes. The extract is filtered through a small dry paper, and the absorbancy is measured at 430 mμ. A reagent blank is run through the whole procedure. The calibration curve is derived from an experimental curve plotted using the procedure and a standard series of copper solutions in which is added about the same amount of thorium compound as the sample itself, by subtracting the effect of inevitable trace of Cu in the added thorium compound withan aid of vertical translocation of the curve.
    Download PDF (948K)
  • Seiichiro HIKIME, Hitoshi YOSHIDA, Masahiro YAMAMOTO
    1961 Volume 10 Issue 2 Pages 112-115
    Published: February 05, 1961
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Tellurium forms, with sodium diethyldithiocarbamate, a colored complex soluble in the acetone-water medium. The coloration is applied to the spectrophotometric determination of tellurium, and the conditions for the determination have been studied. The complex has an absorption. maximum at about 424 mμ in the medium consisting of water and 60% (v/v) acetone. It shows constant absorbance in the pH range of 6.39.0. While the complex is unstable in the daylight, tellurium can be determined accurately and rapidly when colored glass vessel is used and the absorbance measurement is carried out avoiding ultraviolet light immediately after the color development. The calibration curve for the determination of tellurium at 420 mμ shows linearity for 120 ppm of tellurium. The molar absorption coefficient at this wave length is ca. 3200, and the sensitivity of the recommended method is 0.04γ Te/cm2. In this method, the presence of Fe (III), Cu (II) or Bi gives a disturbing influence. In the presence of EDTA, however, 40 ppm of Co, Hg (II), Ni or W (VI), 200 ppm of Al or Ba, and a large amount of As (III), Ca, Cd, Mg, Mn (II), Mo (VI), Pb, Se (IV) and Zn do not disturb the determination.
    Download PDF (683K)
  • Chemical studies on radioactive indicators. XXIII
    Masayoshi ISHIBASHI, Taitiro FUJINAGA, Mutsuo KOYAMA, Taiji NAITO
    1961 Volume 10 Issue 2 Pages 116-119
    Published: February 05, 1961
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Ion exchange separation of Rb and Cs was investigated by the batch and the column methods using 36Rb and 137Cs as radioactive indicators. Dowex 50-X8 (200400 mesh) was used as the exchange resin and HCl solutions were employed for the eluant. From the values of both elements determined by the batch method, it was shown that the lower concentration of the eluant would give the more effective separation. By the column method, elution curves for each element were taken automatically using a recording rate-meter. The effects of the amounts of the salts in question and of the concentration of HCl to the elution curves were examined. From the results of the foregoing experiments, Cs and Rb from trace quantities to 0.058 m mole could be separated using 0.5N HCl as the eluant with the column of 25.5 cm×φ 0.6 cm.
    Effects of Na, K and NH3 to the elution curve of carrier free 137Cs were investigated and the separation of them from 137Cs was made.
    Download PDF (694K)
  • Kameji SHIMASAKI, Kimiyoshi ONO, Susumu SHINDO
    1961 Volume 10 Issue 2 Pages 119-124
    Published: February 05, 1961
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    In order to make the vacuum fusion technique for the determination of oxygen in titanium practical, it is essential to establish an economical procedure for recovering platinum from the used platinum bath. The authors have established the following method.
    Platinum containing about 10% titanium is dissolved in mixed acid (HCl 5+HNO3 1), and heated. Most of titanium in the solution is removed after it is hydrolyzed by boiling. Hydrochloric acid is added to the acidic platinum solution which contains a little titanium, and the solution is evaporated by heating to convert all platinum to chloro-platinic acid. The solution is treated with water and hydrochloric acid, and reduced by metallic magnesium to obtain platinum precipitate. The precipitate is dried and ignited at 1000°C. The obtained gray crude platinum sponge is melted and refined by the cupellation at 1800°C to pure platinum metal.
    Results of the spectroscopic inspection and the blank test using the vacuum fusion bath proved that quality of the recovered platinum by the recommended method is as high as that of commercial pure platinum for which 99% minimum purity is guaranteed. The recovering yield of platinum by the method is 95% or more.
    Download PDF (7702K)
  • Application of selective adsorbent resin to analytical chemistry. III
    Hiroshi IMOTO
    1961 Volume 10 Issue 2 Pages 124-129
    Published: February 05, 1961
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Micro-determination of manganese in alkalichloride brine, industrial salt and caustic soda was tested by using Dowex A-1(Na form). After some fundamental studies on the titration curve for the resin (Fig. 2), on the optimum pH for adsorption (Fig. 3) and on the effects of salt concentration vs. adsorption (Fig. 4), an analytical procedure was carried out as follows:
    The sample solution containing manganese was adjusted to pH 67, then 10 grams of the wet resin were added to it, and when the solution was subjected to agitation by batch process for one hour, the adsorption of manganese took place. Then, the resin was filtered off to separate it from large amounts of NaCl, and the resin was eluted with 12N H2SO4. The effluent was oxidized by heating with KIO4 as an oxidizing agent the resultant MnO4- was determined photometrically. Satisfactory results were obtained as indicated in Tables IV, V and VI.
    Download PDF (1069K)
  • Masayoshi TATSUZAWA
    1961 Volume 10 Issue 2 Pages 129-133
    Published: February 05, 1961
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    The method depends on the addition of excess of Nessler reagent to the solution of isoniazide, and the back-titration of the excess of Hg with sodium diethyldithiocarbamate standard solution using CuSO4 as an indicator. The recommended procedure is as follows: transfer an accurately weighed portion of the sample powder, corresponding to about 20 mg of isoniazide, to a centrifuge tube. Add 10 ml of methyl alcohol (aldehyde-free), and shake the mixture for 10 minutes mechanically, centrifuge, pipet 10 ml of the alcoholic solution into a 25 ml Erlenmeyer flask, and evaporate to dryness on a steam bath. The residue is dissolved in 10 ml water, and transferred with washings into a 50 ml measuring flask. Add 5 ml of Nessler reagent and warm on a steam bath for 10 minutes.Cool to room temperature and dilute with water to the mark. Filter, discard the first 10 ml and pipet 10 ml from the subsequent filtrate into a 100 ml conical flask. Add 20 ml of water, 10 ml of pyridine, 3 ml of 0.1M EDTA, 1 ml of 20% tartaric acid and 1 drop of 0.1M CuSO4. Titrate with 0.02M sodium diethyldithiocarbamate until a stable yellow-brown coloration appears. Carry out a blank determination.
    p-Aminosalicylate compounds do not interfere with the titration, while the presence of lactose, dextrose, and sugar etc. should be avoided.
    Download PDF (1056K)
  • Microdetermination of impurities in monosodium glutamate with high-sensitivity polarograph. I
    Jutaroh SETO
    1961 Volume 10 Issue 2 Pages 133-137
    Published: February 05, 1961
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Monosodium glutamate (M. S. G.) often contains L-cystine which shows a prominent peak in the high-sensitivity square wave A. C. polarogram. The cystine in M.S.G. was confirmed by comparing its summit potential with that of the standard cystine solution in the supporting electrolyte of high-purity M.S.G. The summit potential of cysteine wave observed after the reduction of cystine with sodium sulfite also coincided well with that of pure cysteine added to M.S.G. By the method of standard addition the cystine content in a commercial M.S.G. was found to be 00.12%. Trace of lead did not interfere with the determination.
    Download PDF (905K)
  • Shiro USAMI
    1961 Volume 10 Issue 2 Pages 137-141
    Published: February 05, 1961
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    For the determination of diphenylamine, a polarographic method of utilizing its nitroso derivative has been used, as well as the colorimetry, the gravimetry, and the infrared spectrometry. The author found that a simple quantitative determination of diphenylamine was possible by using a polarogram of p-anilino-phenylquicksilveracetate formed from the reaction of diphenylamine and mercuric acetate.34 m mols mercuric acetate and diphenylamine less than 0.6 part of the mercuric acetate in the molar ratio were reacted in 10% acetic acid-90% methanolic solution for 7.5 hr at 50°C, resulting in a quantitative formation of mercury addition compound of diphenylamine. This mercury addition compound gave a two-step wave in the polarogram at around -0.3and-0.8V when Triton X-100 as a maximum suppressing agent and 0.1 mol sodium nitrate as a supporting salt were used. There were proportional relationships between the heights of the first and the second waves, and the concentration of diphenylamine. The second wave was used for quantitative determination since it was more stable than the first wave. Analytical data were obtained with the coefficient of variation 1.11.8%. The time required for completion of the reaction of diphenylamine with mercuric acetate can be shortened by decreasing the concentration of acetic acid in the solution or by reducing the molar ratio of diphenylamine/mercuric acetate.
    Download PDF (894K)
  • Shiro USAMI
    1961 Volume 10 Issue 2 Pages 141-146
    Published: February 05, 1961
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Industrial vinyl acetate usually contains, as the impurities, minute amounts of acetaldehyde, crotonaldehyde, methyl acetate, acetone, methanol and benzene. Gaschromatographic determination of these impurities has been investigated by the authors.
    Acetaldehyde, methanol, acetone and methyl acetate in vinyl acetate can be determined separately by using a column of DM-13A with silicone oil DC-510 (85%) and stearic acid (15%) (column No. 1). The lower limit of detection is 0.006vol% for acetaldehyde, 0. 007vol% for methanol, 0.015vol% for acetone, and 0.018vol% for methyl acetate. The peak of methanol by the column No. 1 is disturbed by the peaks of water and acetaldehyde when vinyl acetate contains Comparative qantity of water and acetaldehyde, while methanol can be separately determined by using a column of DM-13A with glycerin (column No. 2) even when much water and acetaldehyde are contained in the sample. The determination of crotonaldehyde is also possible by the 2nd column. The lower limit of detection is 0.031 vol% for crotonaldehyde, and 0.013vol% for methanol. Benzene can be determined by using a combination of the 1st and 2nd columns, the limit of detection being 0. 024vol%.
    Download PDF (964K)
  • Studies on the techno-analytical method by means of S. W. polarograph. II
    Nobuo TAJIMA, Moriji KUROBE
    1961 Volume 10 Issue 2 Pages 146-151
    Published: February 05, 1961
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A method of quantitative determination of several percent of copper and 0.11% of iron and zinc in aluminum alloy by means of S. W. polarography has been investigated. Copper and zinc in 0.1g sample is dissolved in hydrochloric acid-nitric acid mixture, evaporated to dryness and the residue is dissolved in 5 ml hydrochloric acid. This is made up to 50 ml with water and a portion is used for taking polarogram. Copper and zinc are determined by the waves at -0.25V and 1.05V respectively (mercury pool is used in each case). For determination of iron, another portion of the sample solution is evaporated to dryness and the residue is dissolved in hydrochloric acid (1 : 1). This in a separatory funnel is extracted with MIBK. The solvent layer is treated with water to back-extract the iron. The extract is concentrated to about 2 ml for driving off the solvent. This is made up to 25 ml with water, neutralized with 0.5N sodium hydroxide, using methyl red-methylene blue indicator, acidified with 1 ml hydrochloric acid (1 : 10), 7.5g sodium citrate is added, the solution is made up to 50 ml with water and a part of it is used for taking polarogram at -0.3V (against mercury pool) for the determination of iron from the wave height. This method is less affected by the presence of coexisting ions and the determination can be carried out within 1 hour.
    Download PDF (1038K)
  • Determination of trace impurities in uranium metal. XIV
    Ken SAITO, Tsugio TAKEUCHI
    1961 Volume 10 Issue 2 Pages 152-156
    Published: February 05, 1961
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    The sample was dissolved in hydrochloric acid and hydrogen peroxide. For the extraction of trace amount of lead from large amount of uranium, dithizone-benzene solution was used. To mask the trace impurities as Cu, Ni, Fe, Zn in uranium on during the extracting procedure, ammonium citrate, sodium sulfite, potassium cyanide, and ammonium hydroxide were added preliminarily to the sample solution. The lead extracted into the dithizone-benzene solution was shaken with and transfered into 0.45N perchloric acid, and determined by the A. C. polarography.
    In the case of spectrophotometric determination, the absorbancy of the extracted dithizone-benzene solution was measured at 520 mμ.
    Good agreement was obtained between the results from the two methods.
    Download PDF (875K)
  • Determination of traces of impurities in uranium metal. XV
    Takayoshi YOSHIMORI, Yoshirô TOMIDA, Tsugio TAKEUCHI
    1961 Volume 10 Issue 2 Pages 156-160
    Published: February 05, 1961
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A simplified procedure for the colorimetric determination of iron in metallic uranium was proposed. Iron in uranium chloride solution of 7.5N hydrochloric acid was extracted into butyl acetate, and the solvent layer was washed twice with 7.5N hydrochloric acid. The same volume of methyl-isobutyl-ketone was added to the solvent, and the mixed solvent layer was shaken with 20% aqueous solution of ammonium thiocyanate. The color developed in the solvent layer was measured, using a 520 mμ filter. 120γ of iron in 0.11g of uranium could be determined with satisfactory results.
    Download PDF (952K)
  • D. C. and A. C. method
    Hiroya TAKAO, Soichiro MUSHA
    1961 Volume 10 Issue 2 Pages 160-165
    Published: February 05, 1961
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    The polarographic behavior of titanium EDTA complex has been studied in various solutions for the purpose of applying the complex to the determination of titanium.
    The quantitative formation of titanium EDTA complex depends on pH of the solution.
    In view of the facts that titanium reacts quantitatively with EDTA at pH 2 and the complex gives satisfactory half wave potential (E1/2= -0.22V vs.S.C.E.), the direct titration of titanium with standard EDTA solution has been studied.
    Besides, in this report, the A. C.-amperometric method which uses both D. C. applied voltage and 20 mV sine wave has been proposed. It has been found that titanium having the concentration range of 1070 ppm is determined by the latter method and 50130 ppm by the former one. In both cases the errors are less than ±2.0%.
    Download PDF (948K)
  • Hiroshi HATA, Kiyoshi OKADA
    1961 Volume 10 Issue 2 Pages 165-168
    Published: February 05, 1961
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Quantitative determination of a small amount (00.1%) of acetaldehyde in acrylonitrile, was investigated, and it was found that by using a suitable amount of fuchsin reagent the determination was not affected by the presence of impurities, and the lower limit for the estimation was 0.001% with an error of ± 0. 002%. Also, the estimation of methyl vinyl ketone (00.02%) was carried out by a m-phenylenediamine method with the lower limit for determination 0.0003%, and with an error ±0.0006%.
    Those methods showed higher accuracies than the methods of R. L. Maute et al., and were applicable for the quality inspection of acrylonitrile to be used as a raw material for synthetic fiber.
    Download PDF (644K)
  • Nakaaki ODA, Goro TSUCHIHASHI, Shigeo ONO
    1961 Volume 10 Issue 2 Pages 168-171
    Published: February 05, 1961
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    By use of a combustion tube to the overlid of which is attached an internal tube (Fig. 1), an analytical method of determination of carbon and hydrogen in organic compounds, with easier and faster operation than the present methods, has been established.
    In the proposed method, a boat holding the sample is placed at an end of the internal tube, and while passing the oxygen through this tube, the whole is promptly inserted into the combustion tube preliminary heated at 800850°C. The operation from placing of a sample to sweeping off the combustion gas can be finished within 5 minutes. Since the combustion tube is closed simultaneously with the inserting of the sample, and the sample is protected from the instantaneous violence of heat by a rather large heat capacity of the internal tube itself, the combustion of sample is proceeded smoothly and rapidly without scattering of sample or backflow of combustion gases.
    The operation of the new method is easier and faster without sacrificing the accuracy.
    Download PDF (743K)
  • Studies on flame photometry by organic solvent extraction method. II
    Hidehiro GOTÔ, Emiko SUDÔ
    1961 Volume 10 Issue 2 Pages 171-174
    Published: February 05, 1961
    Released on J-STAGE: May 07, 2010
    JOURNAL FREE ACCESS
    In determining trace elements by flame photometry, an extraction techinique with organic solvent has been introduced in order to eliminate the interferences of the other elements and to increase the sensitivity of the method.
    In the present work, calcium oxinate was extracted with methyl isobutylketone and the microquantity of it in the extract was determined by flame photometry. The measurement of emission intensity of calcium was made at the wave length of 554 mμ or 622 mμ, under the hydrogen pressure of 2.0 1b/in2 and oxygen pressure of 25.0 1b/in2.
    Barium and Na which interfered the flame photometric determination of Ca by aqueous solution did not disturb in this case.
    The permissible amount of P was larger than in the case of aqueous solution.
    Applying the present method to the determination of Ca in iron and steel, Ca could be determined down to 0.001 percent. In the present method the sensitivity for calcium was about 10 times higher than that obtained by flame photometry of aqueous solution.
    Download PDF (616K)
  • Studies on flame photometry by organic solvents extraction method. III.
    Hidehiro GOTÔ, Emiko SUDÔ
    1961 Volume 10 Issue 2 Pages 175-181
    Published: February 05, 1961
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Micro-determination of metals was made by flame photometric method, in which metals were changed into oxin complex and the extracted complex with organic solvent was directly derived into the flame.
    The method was not only useful in removing of disturbing elements, but also effective for increasing the line intensity by a direct excitation of organic solvent in the oxygen-hydrogen flame and the sensitivity was much higher than in the case of aqueous solution. The oxin complex of manganese or copper was extracted with organic solvent, such as methyl isobutyl ketone, amylacetate, ethyl acetate or chloroform, the extract was derived into oxygen-hydrogen flame, and the line intensity of manganese was measured at 403.5 mμ and that of copper at 324.8 mμ. The intensities of flame under various conditions have been investigated for each solvent, and it was confirmed that the sensitivity could be increased 2030 times in case of manganese and 68 times in case of copper than in the case of aqueous solution by selecting optimal gaseous pressure for each solvent.
    Download PDF (1039K)
  • [in Japanese], [in Japanese]
    1961 Volume 10 Issue 2 Pages 182-183
    Published: February 05, 1961
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
  • [in Japanese]
    1961 Volume 10 Issue 2 Pages 183-185
    Published: February 05, 1961
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Download PDF (573K)
  • [in Japanese], [in Japanese]
    1961 Volume 10 Issue 2 Pages 185-187
    Published: February 05, 1961
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
  • [in Japanese], [in Japanese], [in Japanese]
    1961 Volume 10 Issue 2 Pages 187-188
    Published: February 05, 1961
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Download PDF (407K)
  • [in Japanese]
    1961 Volume 10 Issue 2 Pages 189-190
    Published: February 05, 1961
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
  • [in Japanese]
    1961 Volume 10 Issue 2 Pages 190
    Published: February 05, 1961
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
  • [in Japanese], [in Japanese], [in Japanese]
    1961 Volume 10 Issue 2 Pages 191-193
    Published: February 05, 1961
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
  • [in Japanese]
    1961 Volume 10 Issue 2 Pages 193-194
    Published: February 05, 1961
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
  • [in Japanese]
    1961 Volume 10 Issue 2 Pages 194-196
    Published: February 05, 1961
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Download PDF (519K)
  • [in Japanese], [in Japanese]
    1961 Volume 10 Issue 2 Pages 196-198
    Published: February 05, 1961
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
  • [in Japanese]
    1961 Volume 10 Issue 2 Pages 199-204
    Published: February 05, 1961
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
feedback
Top