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Volume 30, Issue 3
Displaying 1-16 of 16 articles from this issue
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Kousaburo OHASHI, Masuji OZAKI, Henry FREISER1981 Volume 30 Issue 3 Pages 139-143
Published: March 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe exchange reaction of nickel(II) in nickel (II)-dithizone {Ni(Dz)2} complex with mercury (II) was studied by means of atomic absorption spectrophotometry. The stoichiometry for the reaction is as follows: Ni(Dz)2o+Hg(II)w→Hg(Dz)2o+Ni(II)w where the abbreviations, o and w represent organic and aqueous phase respectively. The optimum pH range for the exchange reaction is between 1.0 and 3.0. Nickel (II) in the complex is quantitatively released by shaking Ni(Dz)2 complex in chloroform with an aqueous solution of mercury (II) at pH 2.0 for 5 min at room temperature. Mercury (II) can be determined in the concentration range of 0.20 to 8.00 μg Hg(II)/ml by measuring the replaced nickel(II) concentration in an aqueous solution using a nickel (II) cathode lamp at 232 nm. Metal ions, Cu (II), Cd(II), Al(III), Fe(III), Cr(III), Mo(VI), U(VI), Th(IV) in molor amounts up to 100-fold, ten-fold Ni(II), and an equimolar Co(II) do not interfere. The interference of Ag(I) can be masked by the addition of chloride ions. The reactivity of copper (II) toward Ni(Dz)2 is different from that of mercury (II), though mercury (II) and copper(II) are quantitatively extracted with dithizone at pH 2. This may suggest that the exchange reaction of Ni(Dz)2 with these metal ions would be affected by the difference in the softness of metal ions.View full abstractDownload PDF (730K) -
Michiko NAMIKI, Kichinosuke HIROKAWA1981 Volume 30 Issue 3 Pages 143-148
Published: March 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSDetermination of metallic cobalt, a 0.1 g of sample was dissolved in 2 % silver nitrate solution under nitrogen atmosphere at 50°C for 1 h. Cobalt oxides and silver precipitate were filtered off with all together and the filtrate was submitted to the spectrophotometric determination of the cobalt aquo complex at 510 nm. Determination of cobalt (III), metallic cobalt in the sample was dissolved in 0.9 N sulfuric acid-0.03 N iron (III) ammonium sulfate solution under nitrogen atmosphere at 70°C. The residue (cobalt oxides) filtered through filter paper was put again into the original flask together with the filter paper, and then dissolved in a definite volume of 2.5 N hydrochloric acid-0.1 N iron (II) chloride solution under nitrogen atmosphere at 70°C for 2 h. Remaining iron(II) was titrated with 0.1 N potassium dichromate solution, thus, cobalt (III) was determined. Determination of total cobalt, a sample was dissolved with nitric acid (1+1) and hydrochloric acid (1+1), and evaporated to dryness. The residue was dissolved in 2.4 N hydrochloric acid and the absorbance of the solution was measured at 510 nm. Cobalt (II) was estimated by the subtraction of the values of metallic cobalt and cobalt (III) from that of total cobalt. The procedure established was applied to the analysis of samples of metallic cobalt-cobalt oxides mixtures and also surface oxidized cobalt metals. The coefficient of variation for the analysis of a surface oxidized cobalt was 0.86 % for metallic cobalt, 2.04 % for cobalt monoxide, 5.6 % for tricobalt tetraoxide and 0.2 % for total cobalt.View full abstractDownload PDF (993K) -
Koichi NAKAGAWA, Toshio OGATA, Kensaku HARAGUCHI, Saburo ITO1981 Volume 30 Issue 3 Pages 149-153
Published: March 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSSimultaneous kinetic determination of cadmium and manganese, on the basis on the difference of the rate of ligand substitution reaction between 1-(2-pyridylazo)-2-naphthol (PAN) chelate and EDTA in ammonia buffer solution, has been studied. Although the difference of the rate of the ligand substitution reaction between cadmium chelate and manganese chelate is small in the absence of ammonia, it becomes sufficiently large enough for simultaneous determination by an addition of ammonia because of an accelation of the reaction of cadmium chelate caused by a catalytic effect of the ammonia. PAN and its chelates were solubilized in water with nonionic surfactant, Triton X-100, and with a small amount of methanol to measure the rate of the reaction by a stopped-flow technique. The procedures are as follows; Take a sample solution containing less than 28 μg of cadmium and 14 μg of manganese into 50 cm3 volumetric flask, add 10 mg of ascorbic acid and 5 cm3 of 4.0×10-3 mol dm-3 PAN solution (10 % Triton X-100, 10 % methanol), and adjust the pH of the solution to 8.8 with 10 cm3 of 2.0 mol dm-3 ammonia buffer and then dilute to the make with water. The reaction of this solution with 2.0×10-3 mol dm-3 EDTA solution (pH 8.8 with ammonia buffer) was observed by a stopped-flow apparatus at 25°C. Change in the absorbance at 554 nm as a function of the reaction time was recorded and the concentration of cadmium and manganese were determined by linear extrapolation method from the reaction curves. The present method is free of interferences with other metal ions and anions, and applicable for the determination of cadmium and manganese in mining waste and treated water.View full abstractDownload PDF (790K) -
Akira OKAHIRA, Hiroshi KOBATAKE, Hideo KUSHIDA1981 Volume 30 Issue 3 Pages 154-159
Published: March 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSIn order to presume relative retention times of unknown alditol acetates in gas-liquid chromatography, we investigated the correlation between their molecular structures and retention indices. Retention indices of alditol acetates tested were given by the equation
I=100×log TRX-log TRG/logTRI-log TRG
where TRX, TRG and TRI mean relative retention times of sample, glycerol acetate and iditol acetate respectively. To calculate the retention indices of alditol acetates, four index units were adopted according to the direction of acetyl substituents in zigzag formula, namely same and opposite direction of every other position of acetyl groups. Relative retention times of the acetates were experimentally obtained on four generally used columns (10 % SE-30 Chromosorb W, 3 % ECNSS-M/Gas Chrom Q, 3 % Silar-10C/Chromosorb W, and Tabsorb®) at 190°C, and then calculated values were also obtained using the four index units. Since the index units had additively of the configurational contribution, we found it possible to apply the units to the other acetates of alditols such as heptitols, methylated alditols and deoxy alditols. Using several indices calculated, relative retention times of unknown alditol acetates were presumed.View full abstractDownload PDF (917K) -
Reiko YODA, Kazuya AKIYAMA, Yuichi YAMAMOTO, Yukio MURAKAMI1981 Volume 30 Issue 3 Pages 160-164
Published: March 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA method for the solvent extraction-spectrophotometric determination of palladium(II) with a new reagent, N, N-dimethyl-N'-(4-phenyl-2-thiazolyl)-thiourea (DPTT), has been studied, In acidic solutions, DPTT easily reacts with palladium(II) to form a chelate extractable into chloroform. The apparent molar absorption coeffiicient of the Pd-chelate in chloroform was 3.85×104 l mol-1 cm-1 at 290 nm. The excessive reagent, which has an absorption maximum at 270 nm and gave a positive error in the determination of palladium, could easily be removed by scrubbing the chloroform extract with 1 N sodium hydroxide solution without decomposition of the Pdchelate. The optimum concentration range for the determination, defined by Ringbom, was (5.919.3) μg Pd/10 ml. The molar ratio of palladium to DPTT in the extracted chelate was found to be 1:2 by the male ratio method. The existence of a 1:2 Pd DPTT chelate was confirmed by elemental analysis and mass spectrometry of the isolated compound. The method can successfully be applied to the determination of palladium in palladium-asbestos.View full abstractDownload PDF (848K) -
Kazuo KUGA, Eiichi KITAZUME1981 Volume 30 Issue 3 Pages 164-169
Published: March 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSIndirect determination of trace amounts of phosphorus by graphite furnace atomic absorption spectrometry of antimony and molybdenum after extraction of the molybdoantimonylphosphoric acid (PSb2-Mo10O40) complex with butyl acetate has beeen studied. The procedure is as follows. Put an aliquot of sample solution {containing (0.012)μg of phosphorus} into a separatory funnel. Add 1 ml of a mixed reagent solution (0.85 w/v % in sodium molybdate, 0.27 w/v % in potassium antimony tartrate and 1.5 M in sulfuric acid) and 1 ml of 1 w/v % ascorbic acid solution into the separatory funnel, and dilute to about 10 ml with water. Allow to stand for about 10 min to form the heteropoly-blue complex of molybdoantimonylphosphoric acid. Add 5 ml of butyl acetate and shake for 2 min. Allow the phases to separate and eliminated the lower aqueous phase. Wash the organic phase by shaking with two 10 ml portions of a wash solution (0.3 N sulfuric acid saturated with butyl acetate) for 1 min each time and discard the aqueous layer. Inject 10 μl of the organic layer into the graphite furnace with a micropipette and measure the atomic absorption of molybdenum (wavelength: 313.3 nm, ashing: 1400°C-45 s and atomizing: 2700°C-15 s) and antimony (217.6 nm, 450°C-45 s, 2100°C-8 s). The working curve for phosphorus is linear over the range of (0.010.15)μg (molybdenum measurement) or (0.12) μg (antimony measurement) of phosphorus. Interferences from Bi, Ca, Co, Fe (III), Mn (II), Ni, Pb, Se (IV), Si, Te (VI) and Zn were almost negligible when the amounts of those were 1000 times of phosphorus, but As (III), Ge and Cr (VI) interfered seriously. This method was applied for the determination of phosphorus in silicon and phosphosilicate glass with satisfactory results.View full abstractDownload PDF (895K) -
Keijiro MORITA, Masao MISHIMA1981 Volume 30 Issue 3 Pages 170-174
Published: March 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSAntimony and selenium in whole blood were determined by graphite furnace atomic absorption spectrophotometry after extraction of the chloro-complexes of antimony and selenium from 6 N hydrochloric acid. solution with methyl isobutyl ketone (MIBK). Organic materials in blood were decomposed with nitric acid and perchloric acid. The solution was evaporated to fumes of perchloric acid and transferred to a separatory funnel. The volume was made up to 5 ml with water. After the addition of 5 ml of 36 % hydrochloric acid, the solution was shaken with 10 ml of MIBK for 2 min. The aqueous phase was discarded. The organic phase was shaken twice with two 10 ml portions of 0.1 N hydrochloric acid for back extraction of iron. Then, 10 μl of the organic phase was introduced into the graphite furnace and the atomic absorption signals were measured. The calibration lines were straight up to 0.1 μg of antimony and up to 0.5 tig of selenium. The coefficients of variation (11 runs) in the determination of 0.191.μg antimony and (0.601.52)μg selenium were 3.2 % and (9.84.5)%, respectively.View full abstractDownload PDF (751K) -
Masanori KURODA, Kiyokatsu KUDO1981 Volume 30 Issue 3 Pages 174-178
Published: March 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSEpoxy resin was analyzed by thin layer chroma-tography (TLC) and the influence of solvent polarity, its mixing ratio, and particle size distribution in solid support on the separation of the resin was investigated. The stationary phase of TLC plates used in the experiments was prepared with wet sieving and sedimentation. It is found that the particle size distribution and solvent polarity show a significant effect on the separation, and that there is a suitable condition for TLC of Epoxy resin. It is confirmed that each spot on TLC plate corresponds to a constant n values ranging from 0 to 7. It is evident that THF-chloroform solvent system is applicable to the separation of epoxy resin by liquid chromatography (LC) with gradient technique, because the system shows no absorption in UV spectra region.View full abstractDownload PDF (656K) -
Toshiaki NOMURA, Osamu HATTORI1981 Volume 30 Issue 3 Pages 179-181
Published: March 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSIn the presence of hydrogen peroxide cyanide reacted with a gold electrode of a quartz oscillator to form cyano gold complex, and the dissolution of the gold resulted in the frequency change of the quartz oscillator. A minute amount of cyanide in solution could be determined by this method. Cyanide sample solution (50 ml, pH 10, 30 °C) containing 0.3 % hydrogen peroxide was flowed out on the both gold electrodes of the quartz oscillator at the rate of 2.50 ml/min with a peristaltic pump. After 20 min, the quartz oscillator was washed with water and acetone, and dried by flowing nitrogen gas, and the change of the frequency of the oscillator, F (Hz), was measured. The calibration curve was linear over the range of (2.0×10-74.0×10-6) M, and the relationship was given by an equation, [CN-]=(F/19.2)×10-7 M. The standard deviation was 11.7 Hz (3.5 %) for 5 determinations of 2.0×10-6 M cyanide.View full abstractDownload PDF (454K) -
Motohisa FURUSAWA, Masaki TACHIBANA, Yoshihiro FUJIMORI1981 Volume 30 Issue 3 Pages 181-184
Published: March 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSCommercially available carbazole contains 2, 3-benzocarbazole as an impurity. For the fluorometric determination of anthracene in the carbazole, it is necessary to remove carbazole and 2, 3-benzocarbazole from the sample prior to the determination. The carbazoles were effectively and rapidly removed by the reaction with formaldehyde in the presence of sulfuric acid and thiourea. Complete recovery of anthracene could be attained by adding thiourea. Two milligrams of the sample was dissolved in 20 ml of cyclohexane. The solution was shaken for 5 min with a mixture of 10 ml of 74 % sulfuric acid containing 200 mg of thiourea and 0.1 ml of formalin. Anthracene could be determined by measuring the relative fluorescence intensity of the cyclohexane layer at 400 nm with excitation at 375 nm. As a standard, 0.1 g/ml solution of anthracene was used. The determination limit of anthracene in carbazole was 0.005 %. The carbazoles could be removed in about 6 min.View full abstractDownload PDF (630K) -
Toshio YAO, Soichiro MUSHA1981 Volume 30 Issue 3 Pages 184-187
Published: March 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSLactate dehydrogenase and alcohol dehydrogenase were chemically immobilized on the surface of nylon tube and silica gel, by undergoing a variety of surface synthetic reactions. The dehydrogenases immobilized in a continuous-flow system, converted the oxidized form of nicotinamide adenine dinucleotide (NAD+) to its reduced form (NADH) which was detected by the electrochemical oxidation at 0.7 V vs. SCE. In this manner, the activities of these enzymes were determined by the steady-state currents of NADH, produced by the reaction catalyzed by their respective immobilized dehydrogenases. These immobilized dehydrogenases were relatively stable; no noticeable deterioration in activity has been observed over 2 months being stored in a refrigerator at 5 °C when not in use. Consequently, such immobilized-enzymes have fairly great practical value and can be readily adapted to more specific continuous-flow detection system.View full abstractDownload PDF (602K) -
Kazuko MATSUMOTO, Keiichiro FUWA1981 Volume 30 Issue 3 Pages 188-190
Published: March 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA hydride generation technique for phosphorus has been applied to inductively coupled plasma emission spectroscopy. The generation technique was as follows : phosphate was reduced to calcium phosphide with aluminum powder, followed by the reaction with 2.7 N hydrochloric acid to generate phosphine gas in a graphite furnace atomizer as a recation vessel. Phosphine generation was investigated using Ca3(PO4)2 powder and phosphate solution in the presence of calcium (II). Phosphine gas evolved was introduced into an inductively coupled argon plasma. Phosphorus atomic line 213.6 mn was observed. Almost linear calibration curves were obtained in the concentration range from 20 μg to 200μg P for Ca3(PO4)2 powder and from 2 μg/min to 200 μg/ml for 10μl phosphate solution, respectively. The detection limit was about an order of magnitude higher than that obtained by direct neblization, but the use of a larger furnace as a reaction vessel, which can contain ml levels of the solution, might improve the detection limit.View full abstractDownload PDF (426K) -
Hui-kang KIM, Tsunehiko OTOSHI, Yoshikazu HASHIMOTO1981 Volume 30 Issue 3 Pages T23-T25
Published: March 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSPerformances of filters were evaluated for the collection of ammonium salts in the atmosphere. Two kinds of glass filters, two kinds of quartz filters and one kind of polycarbonate membrane filter were examined. The field study confirmed that the amount of ammonium salts collected on the polycarbonate membrane filter was larger than those collected on quartz or glass fiber filters. The indoor adsorption tests confirmed that the amount of ammonia adsorbed on quartz filter was larger than those on polycarbonate and glass filters. The amount of ammonia collected on filters were increased and decreased by the existence of sulfur dioxide and nitrogen dioxide, respectively. Ammonium salts collected on the glass filter in the field sampling were desorbed by passing clean air through the filter. The authors concluded from their experimental results that (1) the adsorption amount of ammonia was related to the pH of filters, (2) polycarbonate membrane filter, which was inert and neutral, was the most suitable one among various filter materials tested for the collection of ammonium salts in the atmosphere.View full abstractDownload PDF (502K) -
Tetsuo MAKINO1981 Volume 30 Issue 3 Pages T26-T29
Published: March 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSFor the determination of trace metals in biological materials, apparatus for acid-washing of sample cups {(40100) cups/rack} was made. The apparatus (in polyvinylchloride) consisted of two parts, a rack for acid-washing (drying and sefekeeping) of cups (a: centrifuge tube type, b: teacup type) and a stand for the rack (Separate-rack system). The rack consist of a plate for put the cups on, the cups, a top plate (bored) for covering the cups, and a clip for holding the two plates (Sandwich form). The two plates were bored for the cups, clip, and bar of mixer (only cup a), respectively. The cup together with the rack was soaked in acid. The stand for cup a was designed as push up the cup when put the rack on this stand. The stand for cup b was also designed as keep off metal contamination from a dust and concentration (evaporation) of sample. Mixer (Vortextype) was improved as could be mixing cup a together with the rack and then deproteinization agent adding to the cup. Elimination effect of metal contamination and reproducibility of mixing by the apparatuses were tested, and were obtained the fairly good results. By use of the apparatuses, the time of acid-washing and deproteinization procedure has been shortened into below a quarter of until now.View full abstractDownload PDF (539K) -
Kiyoshi IWASAKI, Katsu TANAKA, Osami MORI, Fumio ADACHI1981 Volume 30 Issue 3 Pages T30-T35
Published: March 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSX-Ray fluorescence (x. r. f.) method was described for the determination of heavy metals in size-separated particulate matters collected from a stationary source by an Andersen stack sampler equipped with eight collecting plates. On each of the plate, an aluminum foil was placed tightly, and the particulate matters were collected on this foil. The sample (15) mg was taken up from the foil, dissolved with conc. HNO3-30 % H2O2, conc. HCl-30 % H2O2 or aqua regia, and if necessary, was fused with KHSO4. From the solution thus obtained, metals were extracted as their diethyldithiocarbamates into 5 ml of chloroform after the pH of the solution being adjusted to 5 with ammonia water in the presence of tartrate. The chloroform layer was transfered dropwise onto a filter paper (15 cm diameter), and concurrently a gentle stream of warm air was blown over the surface of the paper to speed up evaporation of chloroform. The metal complexes were then concentrated as a spot in a small central area by allowing chloroform to permeate from the edge towards the center of the paper. The spot was exposed to the primary X-ray beam from a tungsten-target tube for X-ray fluorescence measurement. The standard samples were prepared from the standard solutions of metals. The elements determined were Cu and Zn for the particulate emissions from a metal-melting furnace, Cu, Zn, Pb, Cd, Ni and Fe for those from a glass-melting furnace, and Cu, Zn, Pb and Fe for the dust from a garbage burning plant. The results by x. r. f. method were in good agreement with those obtained by other analytical techniques, namely, by atomic absorption spectrometry and spectrophotometry. The applicability of this method to the determination of (0.11) % level of multi-elements in 0.5 mg of sample was discussed.View full abstractDownload PDF (928K) -
Studies on analytical methods by amperometric titrations using a rotating platinum electrode. XLIIISanae IKEDA, Hiromu SATAKE, Hideaki SHINOHARA, Kazutaka TAKEICHI1981 Volume 30 Issue 3 Pages T35-T39
Published: March 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA simple method for the rapid determination of selenious acid in the presence of sodium nitrate was investigated by means of amperometric titration with silver nitrate using a rotating platinum electrode (+0.15 V vs. SCE). Selenious acid {(10-410-2)M}and metallic selenium (3180)mg were determined with a coefficient of variation about 0.1 %. Sodium nitrate did not interfere with the titration. The recommended procedure is as follows. (1) Determination of selenious acid in the presence of sodium nitrate. Place 5 ml each of 10-2 M selenious acid and 1 M sodium nitrate into the titration cell. Add 0.5 ml of 5 % poly (vinylpyrolydone) and dilute to 50 ml with water after adjusting the pH to 9 with 10-1 M sodium hydroxide and 10-2 M sodium tetra-borate. Titrate the resultant solution with 10-2 M silver nitrate solution amperometrically. (2) Determination of metallic selenium. Dissolve powdered selenium (370) mg with 1 ml of concentrated nitric acid in a 20 ml weighing bottle at (90100)°C using a water bath {(56)min}. Dilute the solution to 100 ml with water. Analyze an aliquot of the solution in the same manner as discribed in (1).View full abstractDownload PDF (629K)
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