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Volume 19, Issue 4
Displaying 1-32 of 32 articles from this issue
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Tsutomu FUKASAWA, Osamu TSUNEKAWA, Atsushi MIZUIKE1970 Volume 19 Issue 4 Pages 443-450
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA simple and rapid method has been developed for the simultaneous concentration and subsequent X-ray fluorescence determination of parts per million quantities of iron, manganese, zinc and copper in aluminum. The metal is dissolved in sodium hydroxide solution, and, after the addition of sodium sulfide, the solution is cooled until partial freezing occurs. The resulting precipitate is filtered on a Millipore filter, and the intensity ratios of the Kα fluorescence to the scattered X-ray are measured on the dried filter holding the precipitate. The lower limit of determination and the precision of the present method are about 1 ppm of each element in aluminum and about 2% at the 50 ppm level, respectively. The time required for a determination is 1.5 to 2 hrs.View full abstractDownload PDF (1354K) -
Kouichiro UMEMOTO, Kayo INOUE, Akemi NISHII1970 Volume 19 Issue 4 Pages 450-454
Published: April 05, 1970
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSAn accurate titration method has been introduced for the determination of sulfate ion in connection with microdetermination of organic sulfur using the flask combustion and photometric titration.
Sulfonazo III, Dimethylsulfonazo III and especially Arsenazo III have shown sufficient reproducibility as they were used as an indicator the photometric titration with barium perchlorate in the nonaqueous medium. Its application to the flask combustion method for organic sulfur was successfully achieved with sufficient accuracy, the standard deviation being about 0.1 (%) from a series of analytical data.View full abstractDownload PDF (791K) -
Itsuo MORI1970 Volume 19 Issue 4 Pages 455-458
Published: April 05, 1970
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSSn(IV) with gallein in the presence of an excessive cetylpyridinium bromide (CPB) at pH <2.0 formed a water soluble red complex. By the addition of CPB, the reagent blank of gallein decreased and the sensitivity for the determination of tin increased.
To the solution containing 020.0 μg of Sn (IV), each 2 ml of 1.0×10-2M CPB and 1.0×10-3M gallein solutions were added, and the solution was made up to 10.0 ml and at pH <2.0 with 3% sulfuric acid and water. After 60 min. standing at 15°C, the absorbance at 530 mμ was measured against the reagent blank. Bi(III), Sb(III), Th(IV), Zr(IV), Fe(III) and Al(III) interfered seriously.View full abstractDownload PDF (603K) -
Isamu TSUBAKI1970 Volume 19 Issue 4 Pages 458-462
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSHomologous elements in periodic table increase their number of electrons with increasing atomic number. The oxidizing power of the elements was then strengthened as seen in their values of ionization potential, standard oxidation potential and standard free energy of formation. This general tendency was perceived in many practical reactions especially in analytica-chemical reactions, but the oxidizing power decreased exceptionally with increasing atomic number in IV B group involving Ti, Zr and Hf, V B group involving V, Nb and Ta and VI B group involving Cr, Mo and W. In VII B group involving Mn, Tc and Re the oxidizing power was in the order Tc>Mn>Re, and in VI A group involving S, Se and Te the oxidizing power was in the order Se>Te>S. The relation between oxidizing power and atomic number was not seen in those groups.View full abstractDownload PDF (862K) -
Tomihito KAMBARA, Shiyo MATSUMAE, Kiyoshi HASEBE1970 Volume 19 Issue 4 Pages 462-466
Published: April 05, 1970
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESS8-Hydroxyquinoline-5-sulfonic acid (H2QS) reacts with Fe(III) in the presence of zephiramine (ZCl, tetradecyl-dimethyl-benzyl-ammonium chloride) and forms a dark green association complex. The complex is completely extractable into chloroform at pH 4.58.5 and has the absorption maxima at 465 mμ and 595 mμ.
Beer's law is obeyed within the range of the final iron concentrations from 0.14 to 1.26 μg/ml, the molar absorptivity being 3.12×103. The composition of the extracted species is estimated to be [Fe3+(QS2-·Z+)3], and the logarithm of the equilibrium constant for the reaction shown by equation (2) is found to be: log K=39.51±2.49.View full abstractDownload PDF (752K) -
Hitoshi KOHARA, Nobuhiko ISHIBASHI, Toshiaki MASUZAKI1970 Volume 19 Issue 4 Pages 467-477
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe interaction between acidic dye molecule and positive charges on the micelle surface has been investigated. The protolytic dissociation of acidic dye molecule containing a hydroxyl group on one end of the conjugated system and nitro or carbonyl group on the other end is promoted on the micelle surface. The interaction between dipole of acidic dye molecule and positive charges on the micelle surface causes a transfer of an electron from the electron-donating group to the electron-attracting group. The influence of quaternary ammonium salt on the interaction increases with the incsrease of the dissociation constant of hydroxyl group on the dye molecule. Enthalpyerm is predominant for change in free energy of protolytic dissociation of dye molecule on the micelle surface. With the quaternary ammonium salt, the lower the critical micelle concentration, the stronger is the interaction between dye molecule and micelle. Acidic dye molecule or organic ligands involving -SO3H group are liable to be absorbed on the micelle surface. The increase of ionic strength and the decrease of dielectric constant weaken the interaction. Behavior of organic ligands such as Eriochrome Black T, Pyrocatechol Violet, Eriochrome Cyanine R and Xylenol Orange in aqueous solution containing micelle ions have been also explained.View full abstractDownload PDF (1882K) -
Voltammetry at solid electrode. IVToyokichi KITAGAWA, Yasuhiro MARUYAMA1970 Volume 19 Issue 4 Pages 477-481
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSAnodic oxidation of Tl(I) on a solid electrode by chronopotentiometry and voltammetry with linearly varing potential was investigated by using carbon paste electrode(CPE) or glassy carbon electrode(GCE).
Chronopotentiometric transition time constant was 862 and was almost independent of the current densities in 1M KNO3+0.1N NaOH aqueous solution. The plot of log (√τ-√t)/√τ vs. potential (vs. SCE) was linear with the reciprocal slope 88 mV. Electrode reaction is supposed to be 2Tl(I)+60H-=Tl203+3H2O+4e.
Tl(I) ion in the range of 0.01 to 0.2 mM was determined successfully in 1M KNO3+0.1N NaOH aqueous solution, although the theoretical value of the peak current at CPE or GCE by the voltammetry with linearly varing potential did not accord with the experimental value.
Anodic oxidation of Tl(I) in 0.1M KNO3+3 mM EDTA was also investigated. In this case, the electrode reaction is Tl(I)EDTA= Tl(III)EDTA+2e in the range of pH 1011. The peak current was linear with the concentration of Tl(I) ion in the range of 0.2 to 0.5 mM, although the sensitivity was very low because of the low values of the diffusion coefficients of Tl(I)-EDTA and Tl(III)EDTA.View full abstractDownload PDF (772K) -
Voltammetry at solid electrode. VToyokichi KITAGAWA, Yoichi KANEI1970 Volume 19 Issue 4 Pages 482-487
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe anodic oxidation of Ni(II)EDTA chelate containing excess of Ni(II) ions in a 0.1M CH3COOH-0.1M CH3COONa buffer solution with 0.005% polyacrylamide was investigated at the carbon paste electrode. The value of transition time constant for the oxidation of Ni(II)EDTA was 403 μA·sec1/2/mM·cm2. As the diffusion coefficients of most metal EDTA chelates are about 5.5×10-6cm2/sec, the electrode reaction for the oxidation of Ni(II)EDTA is supposed to be a two-electron irreversible oxidation process.
EDTA in the range of 0.05 to 0.5 mM was determined successfully in the supporting electrolytes of 1.5 mM NiSO4, 0.1M CH3COOH, and 0.1M CH3COONa containing 0.005% polyacrylamide by the voltammetry with linearly varing potential using carbon paste electrode. This method is very convenient for the determination of small amounts of EDTA, because the presence of large excess of halide ions does not interfere. The anodic wave of EDTA at the dropping mercury electrode, which is due to the formation of stable chelates with mercury(II), is affected by the small amounts of halide ions. The electrode reaction mechanism for the anodic oxidation of Ni(II)EDTA was discussed by the method of controlled potential electrolysis, polarography at the dropping mercury electrode and spectrophotometry.View full abstractDownload PDF (911K) -
Shun ARAKI, Shigetaka SUZUKI, Masaru KITANO1970 Volume 19 Issue 4 Pages 488-492
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA new reaction equipment for rapid determination of alkoxyl groups by gas chromatography had been reported by the authors {This journal, 18, 608 (1969)}.
In this paper, the same equipment was used for the determination of N-alkyl groups, and experimental conditions for the differentiating determination of alkoxyl and N-alkyl groups was also investigated. The less volatile reagent, KI-H3PO4, was recommended for the formation of tertiary ammonium salt of the sample and its pyrolysis in the closed system.
Following procedures are recommended, and analytical results are shown in Table II.
(1) Samples containing N-alkyl groups alone: Immerse the pre-column III in Fig. 2 into a Dewar bottle containing liquid oxygen. Weigh sample (25 mg) accurately into the reaction vessel, and add successively 400 mg of KI, 0.05 ml of H3PO4 and 2μl of methyl cyclohexane as an internal standard. Assemble the reaction vessel to the equipment as shown in Fig. 2. Heat the vessel stepwise as follows : at 250°C for 30 min., at 300°C for 10 min., and at 350°C for 5 min. After each heating step, collect the reaction products in the pre-column III by turning the four-way cock. Remove the Dewar bottle and heat the pre-column at about 120130°C. Introduce the collected reaction products into a gas chromatograph. Calculate each alkyl iodide content by using the internal standard method.
(2) Samples containing both alkoxyl and N-alkyl groups: Heat the pre-column III at 120130°C. Weigh sample and add KI-H3PO4 and methyl cyclohexane as described above. Heat the reaction vessel at 140150°C for 20 min. After heating, turn the four-way cock and introduce alkyl iodide formed from alkoxyl group with carrier gas into a gas chromatograph. After one minute, turn the cock, and cool the pre-column III with liquid oxygen. Heat the reaction vessel. at 300°C for 20 min. and then at 350°C for 10 min.
Procedures after heating are the same as in (1).View full abstractDownload PDF (809K) -
Use of double jet type hydrogen flame ionization detectorShun ARAKI, Shigetaka SUZUKI, Toshiyuki HOBO, Masaaki YAMADA1970 Volume 19 Issue 4 Pages 493-501
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA new auto-ion exchange chromatograph was designed and the hydrogen flame ionization detector was improved to be suited for the chromatograph. The improved detector has two jets for hydrogen flame as shown in Fig. 1. Salts of alkali and alkaline earth metals were evaporated in the lower flame and responses corresponding to ionization of these metals were measured in the upper flame. As each flame could be adjusted to suitable temperature for evaporation and ionization, the noise level of this double jet detector was lower than that of the single jet type {This journal, 17, 847 (1968)} and also it showed higher sensitivity and much improved linear dynamic range (Refer to Fig. 7 and Table III).
An auto-ion exchange chromatograph was composed of an ion exchange column, a motor driven turntable, a photo-electric monitor, a heater chamber for evaporation of eluate and the detector (Fig. 13). The turntable had 47 platinum sample holders. When a drop of effluent from the column fell on a sample holder, the motor began to rotate with signal from the monitor and drove turntable to rotate clockwise until the next sample holder was positioned just below the column. In this manner, a drop of effluent on the holder moved intermittently entering into the heater chamber. In the heating zone, the eluate was thorooughly evaporated only remaining a metal salt on the sample holder. When the metal salt was inserted into the evaporating flame, a response from the collector electrode was obtained and recorded. Thus the elution chromatogram was obtained. By using 1M ammonium chloride as eluate, separation and detection of sodium and cesium ions by auto-ion exchange chromatograph was carried out as shown in Fig. 17.View full abstractDownload PDF (3005K) -
Tadaharu TAMAI, Tetsuo HASHIMOTO, Rokuji MATSUSHITA, Shiro IWATA1970 Volume 19 Issue 4 Pages 502-507
Published: April 05, 1970
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSCarrier free iodine-131 can be produced by the neutron irradiation of tellurium followed by subsequent β-decay. If tellurium compounds used as target material contain some quantity of iodine as impurity, the specific activity of iodine-131 obtained will be decreased. Thus the determination of iodine content in various tellurium compounds was investigated by the nondestructive reactor neutron activation analysis with a Ge(Li) detector, with which two gamma photopeaks, 441 keV from 128I and 453 keV from 131Te, were easily resoluble. A new method is proposed by using the activity ratio of the photopeaks and compared with the ordinary calibration curve method at 441 keV photopeak. From the application of these methods, it was found that the iodine quantity of 1100 ppm could be determined in tellurium compound and that the detection limit of these methods was about 1 ppm. These two methods were conveniently applied to the analysis of some commercial tellurium compounds.View full abstractDownload PDF (938K) -
Tetsuo HASHIMOTO1970 Volume 19 Issue 4 Pages 508-513
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSIt is well known that the most of actinide nuclides decay by emitting alpha particle and cause the fission reaction by the absorption of neutron. The author has proposed, in his previous paper, a new useful method based on the count of alpha particle tracks for the detection of natural alpha nuclides on electromigrating paper by the use of celluloid film.
In this experiment, the fission track method using muscovite was investigated for the detection of uranium and thorium. Sample solutions in various concentrations were electromigrated on a filter paper and subjected to the detection of fission track after the irradiation with reactor neutron by combining with the chemical etching of muscovite surface. This method was satisfactory for the study of uranium distribution on migrated paper. In the case of thorium, the sensitivity of this method was poor as expected from the cross section value.
The comparison of fission track method and alpha track method was done by calculation on the published data under an appropriate condition, i. e. 1 day for the exposure time for alpha track recording and 4.21×1016 n/cm2 for the total flux of thermal neutron for fission track experiment. The ratios between alpha tracks and fission tracks were shown in Fig. 3, as functions of specific activity for each actinide nuclide. One can easily select from this figure the optimum method for the detection of object nuclides, which in this report were classified as follows :
The method recommended Nuclide
(1) Fission track {235U, 233U, 245Cm, 239Pu, 229Th,
249Cf, 237Np, and spontaneous fissile nuclides (250Cf, 252Cf,
253Es, 254mEs)
(2) Alpha track {226Ra, 228Th, 242Cm, 223Ra, 227Ac,
230Th, 231Pa, 240Pu, 243Am, 241Am,
238Pu, 227Th, 232U, and other alpha nuclides.
(3) Fission or alpha }243Cm, 234U, 242Pu.
(4) Colorimetric method }232Th, 238U.View full abstractDownload PDF (3167K) -
Toyozo UNO, Koichiro MIYAJIMA, Terumichi NAKAGAWA1970 Volume 19 Issue 4 Pages 513-517
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe pyrolysis of N-n-alkyl-N, N-dimethyl anilinium bromide was carried out at 250°C in a sealed glass tube and, alternatively, in the flash heater chamber of a gas chromatograph. Both methods gave identical pyrolyzates, i. e., n-alkyl bromide, N, N-dimethyl aniline and N-n-alkyl-N-methyl aniline which were identified with the authentic samples by IR spectroscopy and gas chromatography. The temperature dependences of the pyrolytic reactions of N, N, N-trimethyl anilinium bromide and N-benzyl-N, N-dimethyl anilinium chloride were also investigated. Judging from these observations together with the results of the pyrolysis of benzalkonium salts and alkyl pyridinium salts, which already had been reported, the thermal decomposition reaction of the quaternary ammonium salts was reviewed and the applicability of the pyrolysis gas chromatography to the analysis of cationic surfactants was discussed.View full abstractDownload PDF (759K) -
Zenzo TAMURA, Chang-Shu KIM, Nobuko HOSODA, Shoji TAKITANI, Masao SUZU ...1970 Volume 19 Issue 4 Pages 518-524
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThree kinds of inorganic fluorescent substances, which differed from each other in excitation spectrum and in fluorescent color (blue, green and red), were selected from those listed in Fig. 2 and properly mixed. Some typical examples of the mixed fluorescent substances thus prepared are shown in Table I. Although they fluoresced white by irradiating with an improved light source giving a spectrum shown in Fig. 1, they showed various colors when irradiated with monochromatic ultraviolet light as shown in Photo. 1.
Combination of a screen made of the mixed fluorescent substance and the improved light source made it possible to utilize them as a detector of ultraviolet absorbing compounds on the paper chromatogram as in Photo. 2. Colors of spots depended on the absorption spectra of the compounds. The screen was also used for a viewer in Fig. 3.
An adsorbent containing 510% of the mixed fluorescent substance was also useful for thin-layer chromatography (Photo. 3) and for column chromatography (Photo. 4), though in the latter case a quartz tubing was required for making column.
As such detection method usually keeps sample compounds intact, it will be used widely for analysis and purification of natural products, biological substances, drugs etc.View full abstractDownload PDF (3380K) -
Studies on the atomic absorption by the double aspiration method. IMitsutomo TSUHAKO, Eiichi SEKIDO1970 Volume 19 Issue 4 Pages 525-530
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe influence of phosphoric and sulfuric acid on the atomic absorption of calcium and magnesium was studied by using a glass atomization chamber equipped with two atomizers.
The intensity of atomic absorption of calcium and magnesium was increased considerably by supplying calcium or magnesium solution from one atomizer and phosphoric or sulfuric acid from the other.
The enhancing effect observed by this double aspiration method could not be ascribed to physical factors, such as viscosity and surface tension of the solution, acetylene pressure and characteristics of aspiration chamber, but to some chemical reactions occurring in the flame.
The depressing effect of phosphoric or sulfuric acid on the ordinary atomic absorption of calcium or magnesium was considered to be caused by the formation of phosphate or sulfate in solution which would then give refractory substances in the acetylene flame.View full abstractDownload PDF (958K) -
Studies on the atomic absorption by the double aspiration method. IIMitsutomo TSUHAKO, Eiichi SEKIDO1970 Volume 19 Issue 4 Pages 531-536
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe effects on the atomic absorption intensity of calcium or magnesium of the various substances such as acids, alkalies, salts and alcohols, were examined by using a glass chamber equipped with two atomizers.
It was found that concentrated HClO4, NaOH, NaCl, NH4Cl, NH4NO3 and alcohols multiplied the atomic absorption intensity twice at least, and that the sensitivity was increased considerably by raising the flow rate of acetylene.
Such an increase of sensitivity was also found in the atomic absorption of zinc and iron and in the flame emission of calcium and magnesium, corresponding to an increase of the atom density in the flame.
Experimental results indicated that the increase of atomic absorption intensity was given by the complicated effects of various factors including (1) the facility to dehydration of hydrated metal ion, (2) the enhancement of thermal decomposition of molecules containing the metal atom and (3) depression of the metal oxide formation or reduction of the oxide in the flame by the second substances.View full abstractDownload PDF (1018K) -
Yoshinobu WAKAMATSU, Makoto OTOMO1970 Volume 19 Issue 4 Pages 537-541
Published: April 05, 1970
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSA new sensitive method is described for the spectrophotometric determination of iron(III) which is based on the extraction of iron(III)-indoferron chelate into chloroform in the presence of 1, 3-diphenylguanidine. The extracted species shows an absorption maximum at about 635 mμ, having the composition of 1 : 2 : 2 in metal-ligand-amine ratio.
An addition of sodium chloride is effective for complete extraction of the chelate. Under the optimum condition, a linear relationship between absorbance of organic phase and iron(III) content of aqueous phase is obtained in the range from 3.1 to 19.5μg Fe(III) per 20.0 ml.
The sensitivity of the reaction is 0.003 μg Fe(III) per cm2. Titanium(IV), thorium(IV), vanadium(IV) and chelating agents such as NTA, EDTA and CyDTA interfere with the determination.View full abstractDownload PDF (783K) -
Hiroo SASUGA, Katsuhiro KATO, Yasuhiro ASAOKA1970 Volume 19 Issue 4 Pages 542-546
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSMetallic iron in many samples of reduced iron was incompletely dissolved by bromine-methanol method. The conditions for selective dissolution of metallic iron with methanolic bromine were investigated by means of chemical analysis, X-ray diffraction and infrared absorption. Metallic iron was dissolved preferrably in the presence of some reaction products of alcohol and bromine such as ketone, aldehyde and bromic acid. An addition of acetone to methanolic bromine was very effective for complete dissolution of metallic iron, which could be then titrated successfully by EDTA solution. Results of analysis by this procedure for a number of samples of reduced iron agreed closely with those by X-ray diffraction analysis.View full abstractDownload PDF (852K) -
Spectrophotometric determination with Arsenazo III.Hiroshi ONISHI, Keiichi SEKINE1970 Volume 19 Issue 4 Pages 547-550
Published: April 05, 1970
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSA method has been developed for the separation and determination of microgram quantities of thorium and uranium(VI). Thorium is extracted with 0.15M TTA (thenoyltrifluoroacetone) in benzene at pH 1.0. Uranium remains in the aqueous phase. Thorium and uranium are then determined spectrophotometrically with Arsenazo III. In the presence of oxalic acid (0.1 g per 25 ml of aqueous phase), thorium can be separated from uranium by extraction with TTA at pH 5.5.
Repeated analyses of samples containing 10 μg of thorium and 20 μg of uranium gave average recoveries of 94% for thorium (relative standard deviation was 1.2%) and 100% for uranium (1.5%). In the presence of oxalic acid, average recoveries were 97% for thorium (1.5%) and 94% for uranium (2.4%).View full abstractDownload PDF (619K) -
Masking of ferric iron with ο-phenanthrolineTsunenobu SHIGEMATSU, Yasuharu NISHIKAWA, Keizo HIRAKI, Noriko NAGANO1970 Volume 19 Issue 4 Pages 551-554
Published: April 05, 1970
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSLumogallion was found as a superior reagent for the fluorometric determination of aluminum in sea water [This Journal, 17, 1092 (1968)]. Up to 30 μg of F- and 1000 μg of PO43- are tolerable in this procedure. Interfering ions were Fe3+, Cu2+, Ti4+, VO3- and Ga3+; the concentration of each of these except ferric iron in sea water was negligible. Ferric iron interfered in this procedure. It was found that ο-phenanthlorine prevented interference by up to 10 μg of ferric iron.
Sample water containing 0.0032 μg of aluminum was treated with 2 ml of 4% hydroxylamine hydrochloride solution. After standing for 15 min., 1 ml of 1% ο-phenanthroline solution and 0.5 ml of 0.01% lumogallion solution were added to the solution, and pH was adjusted to 5.0(CH3COONH4-CH3COOH buffer). It was heated at 80°C for 20 min., and the fluorescence intensity of the solution was measured.
The method may be applied to the samples of natural water containing ≥0.05 μg of aluminum per liter.View full abstractDownload PDF (637K) -
Hideaki HIGASHIKUZE, Yuzuru KIDAKA1970 Volume 19 Issue 4 Pages 554-557
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSGas chromatographic analysis of hygroscopic water in clay minerals was studied by using Shimadzu gas chromatograph Model GC-4APT, Shimadzu pyrolyzer Model PYR-1A and Disc chart integrator Model MI-1B. The optimum operational condition was ;
Column : 1.5 m×3 mm, Porapak Q (80100 mesh).
Carrier gas : helium.
Column temperature : 80°C.
Detector : thermal conductivity detector.
Every experiments were conducted by an identical analytical method.
The results obtained were in good agreement with those by thermal gravimetric analysis. The advantages of this method are rapidity, simplicity and good accuracy.
Contents of hygroscopic water in Filtrol-58, Elutriated Yamagata. Bentonite, Pyrophyllite and Filtrol-47 were determined.View full abstractDownload PDF (586K) -
Takeshi ISHII, Sôichirô MUSHA1970 Volume 19 Issue 4 Pages 558-562
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA method for the alternating current polarographic determination of zinc in commercial vulcanizates was established.
Zinc in commercial vulcanizates can be determined polarographically after extracting the sample in ethyl acetoacetate (EAA). Calibrating solutions can be prepared by dissolving commercially available zinc metal of special grade (purity 99.999%) in EAA.
The alternating current polarogram in the region of applied potential from 0 to -2.0 volt vs. mercury pool anode after bubbling for 15 min. with nitrogen is recorded, and zinc is determined by referring to a calibration curve.
The method is rapid and has accuracies nearly comparable to those attained by the conventional ashing method followed by JIS.View full abstractDownload PDF (686K) -
Kazuyoshi HAGIWARA1970 Volume 19 Issue 4 Pages 563-565
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSIt has been found that arsenic is extracted quantitatively into benzene from comparatively high concentration of sulfuric acid solution (9M) containing small amounts of chloride (0.5 M) while lead remains in the aqueous phase. Arsenic in the organic phase is back-extracted into water and is determined by the square-wave polarography using 2M hydrochloric acid as a supporting electrolyte. Lead remaining in the aqueous phase is determined directly by the square-wave polarography.
The sample is decomposed with a mixture of 10 ml of sulfuric acid and 3040 ml of nitric acid in a Kjeldahl flask by heating to fumes of sulfuric acid. The solution after the decomposition is transferred into a 100 ml beaker and 0.2 g of hydrazine sulfate is added. It is heated again to fumes of sulfuric acid and the heating is continued for about 10 min to reduce the arsenic. The solution is transferred into a separatory funnel and 10 ml of water containing about 0.5 g of ammonium chloride is added. Arsenic is extracted twice into 10 ml and 5 ml of benzene and determined after back-extraction into water as described above. Lead in the aqueous phase is also determined directly after the solution is transferred into a 20 ml volumetric flask.
Arsenic (0.3 to 7 ppm) and lead ( 1 to 20 ppm) in rinds of some apples were able to be determined by the proposed method.View full abstractDownload PDF (514K) -
Takao TSUDA, Daido ISHII1970 Volume 19 Issue 4 Pages 565-568
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSGas chromatography and infrared spectroscophy were connected by using a flow liquid cell to be applied. for a unit process in rapid analysis. By using tetrachloroethylene as the organic vapor instead of carbon tetrachloride, the application of this GC-IR combination method was extended to high boiling substances such as methyl benzoate, dimethyl adipate, methyl myristate, decanol, diphenyl ether etc. As every GC fraction was passing through the cell, consecutive scans were taken, or a portion of every sample was once trapped in the cell for measuring its infrared absorption in the range of 4000650 cm-1. This new simple device permits the rapid spectrometric examination of GC effluents.View full abstractDownload PDF (556K) -
Yoshitaka YOICHI, Masakazu UENO, Kazuo KAKEMI1970 Volume 19 Issue 4 Pages 568-570
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSCytosine arabinoside is in some circumstances e.g. by heating, converted into uracil arabinoside. A paper chromatographic method was recommended for the determination of cytosine arabinoside in the presence of uracil arabinoside in which a mixture of ethyl acetate, iso-propanol and water (2:2:1) was used as the developing solvent on Toyo No. 5B or Whatman No. 1 filter paper (3 cm×20 cm). The method was rapid and accurate, and the calibration formula for cytosine arabinoside was 18.28A282-0.06 and that for uracil arabinoside was 23.70A264+ 0.09.
The recovery of cytosine arabinoside in 2% aqueous solution after 6 hours heating in boiling water was:
pH cytosine arabinoside %
5.4 94.6
7.6 97.9
9.2 97.4View full abstractDownload PDF (456K) -
Nobuyoshi YAMAGUCHI, Minoru HASEGAWA1970 Volume 19 Issue 4 Pages 571-573
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA rapid spectrophotometric determination of phosphours in ferrovanadium using solvent mixture (n-butanol+chloroform) has been carried out as follows.
Take up 0.250.50 g of sample with nitric acid and sulfuric acid, and evaporate to fumes of sulfuric acid. After cooling add ferrous ammonium sulfate to reduce vanadium and then ammonium molybdate immediately. The phosphomolybdic acid was extracted with a solvent mixture and was reduced with stannous chloride. The absorbance of the molybdenum blue produced was measured at wavelength of around 700 nm to determine the phosphorous content. The time required was about 40 minutes.View full abstractDownload PDF (397K) -
Motohisa FURUSAWA, Yoshiichi SATO, Sumiko YAMADA, Tsugio TAKEUCHI1970 Volume 19 Issue 4 Pages 573-575
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSXanthydrol forms violet colored product with carbazole in glacial acetic acid medium in the presence of hydrochloric acid and the reaction is applied to the determination of carbazol. The authors have proposed a modified method which is more precise than the previous method. The recommended procedure is as follows. A sample containing about 100 μg of carbazole is dissolved in 10 ml of glacial acetic acid. Five milliliters of glacial acetic acid solution of xanthydrol (1 mg/ml) and 0.5 ml of conc. hydrochloric acid are added. The solution is heated at 80°C for 45 minutes, cooled to room temperature and diluted to 25 ml with glacial acetic acid. The absorbance of the solution is measured at 570 mμ against the reagent blank.View full abstractDownload PDF (362K) -
[in Japanese]1970 Volume 19 Issue 4 Pages 576-580
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDownload PDF (1003K) -
[in Japanese]1970 Volume 19 Issue 4 Pages 580-589
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
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[in Japanese]1970 Volume 19 Issue 4 Pages 589-595
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
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[in Japanese]1970 Volume 19 Issue 4 Pages 595-614
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESS -
[in Japanese], [in Japanese]1970 Volume 19 Issue 4 Pages 615-624
Published: April 05, 1970
Released on J-STAGE: May 29, 2009
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