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Volume 30, Issue 12
Displaying 1-20 of 20 articles from this issue
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Shigehiko HAYASHI, Kinuyo AOYAMA, Kumiko NOSAKA, Keiya KOTSUJI1981 Volume 30 Issue 12 Pages 761-765
Published: December 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA new ion exchanger called "xanthated Sephadex" (X-Sephadex) was prepared. Sephadex G-25(medium) was mixed with aqueous solution of sodium hydroxide and carbon disulfide, and allowed to stand for 5 d at 70°C under being stirred. The crude products were washed with acetone, (1:1) mixed solution of hydrochloric acid (pH 2) and methanol, then, with 50 % methanol, respectively, and dried. Mercury(II), copper(II), lead(II), cadmium(II), zinc(II), nickel(II) and cobalt(II) were collected quantitatively from 50 ml of 1×10-5 M solution of each metal salt with 0.1 g of the X-Sephadex over the pH range of 0.7 to 10.6, 2.1 to 10.8, 4.3 to 6.4, 4.5 to 10.4, 7.6 to 10.6, 9.9 to 10.8 and 10.2 to 11.0, respectively, by stirring the solution together with X-Sephadex for 30 min at room temperature. The collection of copper(II) from 1 M solution of sodium nitrate, magnesium nitrate, calcium nitrate and sodium bromide, respectively, and from 0.1 M solution of sodium iodide was complete at pH 4.7 to 5.2. The optimum pH range was shifted to the range of 2.6 to 10.8 when the collection was done from 1 M sodium chloride solution. Various complexing agents such as citrate, cyanide, thiocyanate and EDTA were found to interfere with the collection of copper(II). By the column system 1×10-4 mmol to 1×10-3 mmol of copper(II) in a 500 ml of 0.01 M sodium acetate solution was collected with 0.1 g to 0.2 g of the X-Sephadex. The X-Sephadex together with the collected copper was dissolved in 2 ml to 5 ml of conc. hydrochloric acid, the recovery of copper being satisfactory.View full abstractDownload PDF (771K) -
Toshiaki MIURA, Megumi KASHIWAMURA, Michiya KIMURA1981 Volume 30 Issue 12 Pages 765-770
Published: December 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSIt was found that 2, 3-naphthalenedicarbaldehyde(NA), a modified reagent of o-phthalaldehyde, specifically reacted with arginine in weak alkaline medium to produce a highly fluorescent adduct and the fluorescence intensity was greatly enhanced (about by 12 folds) by addition of β-cyclodextrin(β-CD). The procedure for a specific, simple and sensitive determination of arginine based on this fluorescence reaction was developed as follows. A 400 μl of sample containing arginine was diluted with 2.6 ml of 15 mM β-CD-0.2 M borate buffer (pH 9.3) and the reaction was initiated by addition of 100 μl of 30 mM NA solution in methanol. After incubation for 25 min at 20 °C, the fluorescence at 520 nm was measured using an excitation wavelength of 462 nm. Peptides containing arginine residue such as benzoylglycylarginine, angiotensin III and bradykinin, and 20 amino acids except cysteine did not interfere the analysis. Commonly occurring amines and guanidinium compounds in biological sample also had no appreciable effect on the determination, whereas thiol compounds such as glutathione and cysteine interfered with the analysis. However, the interference could be blocked by treating the sample with N-ethylmaleimide prior to the fluorescence reaction. The linear calibration curve was obtained over the concentration range (0.450) nmol arginine in 3 ml of the reaction mixture in the presence of (10100) nmol of each of 21 amino acids and glutathione. The coefficient of variation of this method was 3.8 % (n=16) for 1.0 nmol of arginine.View full abstractDownload PDF (936K) -
Tokuo SHIMIZU, Yoshio SHIJO, Kaoru SAKAI1981 Volume 30 Issue 12 Pages 770-774
Published: December 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA trace amount of cadmium in human urine was determined by graphite furnace atomic absorption spectrometry. A urine sample (25 ml) was digested with 5 ml of HNO3 and 30 ml of H2O2 in a long-neck flask on a hot-plate (200 °C), then diluted to 50 ml. The standard addition method was carried out before digesting. Ten μl of the resulted solution was injected into a tube treated with tungsten carbide, and the cadmium signal was measured with the ramp mode atomization. Interference induced by organic materials in urine was avoided by HNO3-H2O2 digestion. Interference induced by inorganic salts could be reduced by 2-fold dilution and tungsten carbide treatment. The cadmium signal was separated sufficiently from the molecular absorption due to NaCl etc. by the ramp mode atomization. Since the blank level of H2O2 was relatively high, the determination was limited to about 0.1 μg/l. The coefficient of variation was 1.76 % at 0.36 μg/l in 24 h human urine (n=4). The time required was (810) h. The precision of this method was higher than those of direct methods, and the reasonable values of urine levels of cadmium were obtained.View full abstractDownload PDF (811K) -
Kazuo TATEISHI, Keiichi FURUYA, Tadashi KIKUCHI, Hideyuki ISHIDA, Akir ...1981 Volume 30 Issue 12 Pages 774-779
Published: December 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSLaser Raman microprobe was applied for the analysis of anthophylite asbestos particles in environmental particulates. A Molecular Optics Laser Examiner (MOLE), Instrument S.A., was used for the experiment with use of Ar ion laser of 514.5 nm, output power=(300450) mW and slit of 1000 μm or 1100 μm in width, measurement range, Δv=(2001400) cm-1. Sample powder was dispersed with acetone on a non-fluorescence microscopic glass plate and was served for observation. In the analysis in punctual illumination mode, anthophylite asbestos and anthophilite nonfibrous particles were identified from a sediment dust on a beam in an abandoned asbestos factory building in Fukushima Prefecture. The existence of carbonate and phosphate minerals and alite component of cement was suggested from their Raman peaks. From a dust sample obtained from the back of a bench on a subway platform, no anthophylite Raman peaks were detected, but a spectrum of cellulose with a peak at 1090 cm-1 was observed. In the analysis in global illumination mode, Raman image at 674 cm-1 was obtained from anthophylite particle sample.View full abstractDownload PDF (3344K) -
Keizo HIRAKI, Norio SHIMIZU, Yasuharu NISHIKAWA, Tsunenobu SHIGEMATSU1981 Volume 30 Issue 12 Pages 780-784
Published: December 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe oxidation of ο-aminophenol by chlorate ion takes place in acidic milieu and is catalyzed by a trace amount of vanadium (V). Vanadium(V) oxidizes ο-aminophenol to 2-amino-3-phenoxazone, then the vanadium(IV) produced is reoxidized to vanadium(V) by the sodium chlorate. Further oxidation of ο-aminophenol proceeds by repetition of these reactions. The oxidation product (2-amino-3-phenoxazone) gives a intense fluorescence; under optimum conditions, the fluorescence intensity is proportional to the concentration of vanadium. The most suitable concentration of ο-aminophenol and sodium chlorate for the determination of vanadium(V) were found to be 0.02 M and 2 × 10-4 M, respectively. From 0.1 ppm to 5 ppm of vanadium(V) can be determined under the optimum conditions; reaction temperature 50 °C, reaction time 2 h, and at pH 2±0.2. If the reaction time is increased to 3 h at 55 °C, the method may be extended from 2 ppb to 15 ppb of vanadium. Interferences of diverse ions were tested, among which Fe(III) and Mn(VII) caused positive errors, and Cr(VI), Mo(VI) negative errors if present in 40 fold w/w ratio to V(V).View full abstractDownload PDF (623K) -
Evaluation of chromatographic profiles by pattern similarityKunishige HIGASHI, Kazuyoshi HAGIWARA1981 Volume 30 Issue 12 Pages 785-790
Published: December 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSEvaluation of chromatographic profiles was studied by one of pattern recognition procedures to establish an effective method for characterization of the oils. The chromatograms of fifteen crude oils (twelve from the Middle east and three from Indonesia) were obtained by measuring absorbance at 254 nm. Stationary and mobile phases were HSG-15 and tetrahydrofuran, respectively. Section areas of each chromatogram were printed out by a data processor. Pattern similarity (cosθ) on pair of chromatograms was calculated with the section areas by a computor. Where, θ is difined as the angle between two vectors in the multi-dimensional space formed by the data of the section areas. Similarity of fifteen crude oils was evaluated with the branching-tree diagram and the configuration chart of chromatographic pattern which were derived from the pattern similarity. Repeatability of the measurement, reproducibility among lots of the oils, effect of the weathering, and comparison among fuel oils were also studied. The proposed method was found to be effective and automatically estimable one for the discrimination of oils.View full abstractDownload PDF (871K) -
Takashi SAITO, Toru TAKASHINA, Saburo YANAGISAWA, Tsuneo SHIRAI1981 Volume 30 Issue 12 Pages 790-795
Published: December 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSLower fatty acids in the atmosphere were analyzed by gas chromatography using a glass capillary column. The fatty acids in the air were collected on filter paper impregnated with a 5 % sodium hydroxide solution. The flow rate of air was kept below 7 l/min. The filter paper which collected fatty acids was transferred in a separating funnel and 5 ml of distilled water and 1 ml of phosphoric acid were added. Free fatty acids in aqueous solution were extracted twice with 5 ml of ethylether. After concentration, a portion of 2 μl of the extract was injected into a gas chromatograph equipped with a flame ionization detector and the quantity fatty acids was determined. The present method was applied to the analysis of fatty acids in the atmosphere near horse barn and pigsty and in feces of horse and pig. Six fatty acids, acetic acid, propionic acid, butyric acid and isobutyric acid and valeric acid and isovaleric acid, were separated completely and these fatty acids in the atmosphere near animal barn were determined at a ppb level. In this method, the detection limits of acetic acid, propionic acid and n-butyric acid were 8.1 ppb, 2.1 ppb and 1.3 ppb, respectively, when 1 m3 of an air sample was taken. The coefficient of variation for determination of fatty acids was approximately 5 %.View full abstractDownload PDF (947K) -
Fumiaki GOSHIMA, Izumi ICHIHARA1981 Volume 30 Issue 12 Pages 796-800
Published: December 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA rapid and simple method for the determination of sulfite ion in water was investigated. The detector reagent was prepared as follows: cellulose powder that was impregnated with 0.2 % Na-CMC(sodium salt of carboxymethyl cellulose) was soaked in a mixed solution of 0.05 % Malachite Green-Magdalarot. After 10 min. the colored cellulose powder was filtered by suction and dried at 100 °C. And then, a portion of 0.1 g of the detector reagent was filled in a glass tube (about 1.8 mm inside diameter) to a length of 11 cm, and its both ends fixed with cotton stoppers. When this detector tube was soaked in a sample solution containing sulfite ion, the color changed from bluish purple to pink corresponding to the length of discolored zone of Malachite Green. The determination of sulfite ion was possible by measuring the length of the pink zone. By this method, the sulfite ion in the range from 10 ppm to 100 ppm {(0.040.40) mg/5 ml as sulfur dioxide} was determined. The variation coefficient was 6.7 % at the sulfite level of 0.20 mg SO2/5 ml. Dithionite, sulfide, disulfate and nitrite ions interfered with the determination of sulfite ion.View full abstractDownload PDF (742K) -
Kunihiro WATANABE, Masanori AWANO, Takashi NISHIYAMA, Kyozo KAWAGAKI1981 Volume 30 Issue 12 Pages 800-803
Published: December 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe extraction-spectrophotometric determination of bismuth with Bismuthiol II in the presence of acetic acid was studied. Bismuth(III) was extracted into chloroform as a ternary complex containing acetic acid. A constant absorbance at 335 nm (absorption maximum) is obtained in the pH range from 3.5 to 5.0, and the extraction efficiency is larger than 99 % in this pH range. Beer's law is obeyed up to 370 μg of bismuth in 10 ml chloroform. The molar extinction coefficient was 4.5 × 104 l mol-1 cm-1, the sensitivity being 4.65 × 10-3 μg/cm2 per 0.001 of absorbance. The composition ratio of the ternary bismuth complex extracted into chloroform was comfirmed to be 1:3:2 (Bi: Bismuthiol II: acetic acid). The recommended procedure is as follows: Take (1040) ml of sample solution containing less than 100 μg of bismuth into a beaker. Add 2 ml of a acetic acid (1+9), and adjust the pH to 4.5 with hydrochloric acid or ammonia. Add 2 ml of 0.1 % Bismuthiol II solution, and dilute to 50 ml with water. Then extract the bismuth complex with 10 ml chloroform by shaking for 3 min. Measure the absorbance at 335 nm against the reagent blank as the reference. Ag(I), Au(III), Fe(III), and Hg(II) which interfere with the determination could be masked by ascorbic acid, but copper(II) interferes significantly with the determination.View full abstractDownload PDF (406K) -
Atsuko SAI, Atsuko ONUKI, Kousaburo OHASHI, Kenji MOTOJIMA, Katsumi YA ...1981 Volume 30 Issue 12 Pages 804-808
Published: December 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe specific adsorption of molybdenum(VI) on activated carbon (Merck Co. Ltd.) and oxine-impregnated activated carbon {AC(HOx)} was studied by using a column method. The amount of molybdenum(VI) adsorbed on activated carbon and AC(HOx) were remarkably dependent on the value of pH. The optimum pH for the adsorption of molybdenum(VI) from 5.00 × 10-3 M molybdenum(VI) solution was 2.0 for activated carbon and AC(HOx) at the flow rate of 1.0 ml/min. The amount of molybdenum(VI) adsorbed on 5 g of the adsorbents was 1.15 g for activated carbon and 0.56 g for activated carbon impregnated with 0.5 g of oxine. The amounts of other metal ions such as copper(II), which were adsorbed on activated carbon and AC(HOx) at pH 2.0, were very small compared with that of molybdenum(VI). From 1.0 M HNO3 solution, 30 mg and 60 mg of molybdenum(VI) could be specifically adsorbed on 5.0 g of activated carbon and 5.0 g of AC(HOx) respectively, but copper(II), zinc(II), nickel(II), lead(II), manganese(II), cobalt(II), chromium(II), iron(III), and cadmium(II) were not adsorbed. The adsorbed quantity of molybdenum(VI) on activated carbon and AC(HOx) in 1.0 M acids increased in the order HNO3<H2SO4<HCl. Chloride and nitrate in concentrations up to 0.20 M showed little effect on the adsorption.View full abstractDownload PDF (797K) -
Shigeki ABE, Nobuo NAKAMURA, Tsutomu MATSUO1981 Volume 30 Issue 12 Pages 809-811
Published: December 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA catalytic photometric titration method has been developed for the determination of micromolar amounts of manganese(II). Manganese(II) catalyzed reaction between hydrogen peroxide and anthraquinone dye, Acid Blue-45 (C.I. 63010), was utilized for the indication of the end-point and the absorbance at 596 nm was followed spectrophotometrically. The recommended procedures are as follows : place 50 ml portion of 0.4 M sodium hydrogen carbonate solution containing known amounts of EDTA in the titration cell, add 0.5 ml of 0.05 % Acid Blue-45 and 1 ml of 3 % hydrogen peroxide, and then titrate the solution with manganese(II) solution {(10-340-4) M}. At the end-point, the catalytic oxidation of the dye proceeds and the absorbance of the solution decreases rapidly. Manganese(II) at micromolar levels was determined within a relative error of ±2 % and with a coefficient of variation of 0.4 %. The method has been applied to determine micromolar amounts of cobalt(II), nickel(II), copper(II), zinc(II) and cadmium(II) by back-titration of an excess of EDTA with standard manganese(II) solution.View full abstractDownload PDF (418K) -
Yukio MINAMI, Toshiyuki MITSUI, Yoshikazu FUJIMURA1981 Volume 30 Issue 12 Pages 811-813
Published: December 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSAlkaloids such as strychnine, quinine, emetine, procaine, tetracaine, and ephedrine were indirectly determined with good precision by atomic absorption spectrometry (A.A.S.). The recommended procedures are as follow. To (520) ml of each sample solution {(1.5100) μg/ml in N/10 HCl} is added with 1 ml of Reinecke salt solution (Ammonium tetrathiocyanodiammonochromate 6 mg/ml). After (510) ml of nitrobenzene is added, the mixture is shaken for about 2 min and then allowed to stand for 20 min. After the nitrobenzene layer is separated it is dehydrated and the chromium in the nitrobenzene solution is measured by A.A.S. Coexisting following ions, Cu2+, Co2+, Mg2+, Ca2+, Na+, Ni2+, K+, Pb2+, Cd2+, Fe3+, NH4+, Cl-, PO43-, Br-, and NO3- in the range of (137) fold (ions/strychnine, mol/mol) did not interfere with the determination. Sodium thiosulfate, monosodium glutamate, starch and sucrose also did not interfere when the amount is less than 200 fold (compounds/strychnine, mg/mg)View full abstractDownload PDF (342K) -
Morio TSUGE, Toshihiro SENBA1981 Volume 30 Issue 12 Pages 814-816
Published: December 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSResidual ethylene oxide in materials for medical devices was determined by gas chromatography using hexane as an internal standard. Ethylene oxide in about 2 g sample of polyvinyl chloride tube which contains dioctyl phthalate was extracted with 10 ml of ethanol in a vial of 50 ml capacity at (20±5)°C for 24 h. The analytical conditions were as follows; column : stainless steel column (3 m×3 mm I.D.) packed with Chromosorb W-AW (80/100 mesh) coated with poly(propylene glycol succinate) (15 %), column temperature : 50 °C, injection temperature : 70 °C, detector : FID, internal standard : hexane. 10 μl of ethanol extract was injected. It took about 20 min for the chromatographic procedure. The corrected coefficient for the slope of calibration curve was 3.16. The precision of the present extraction method was comparable to that of the direct injection method of the present sample dissolved in dimethylformamide, but the latter method can not be applied to insoluble samples such as silicon, polyethylene and fluorocarbon resins. The coefficient of variation of the present method was about 3.5 % and the detection limit about 1 ppm.View full abstractDownload PDF (511K) -
H. A. Laitinen1981 Volume 30 Issue 12 Pages S93-S97
Published: December 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSDownload PDF (635K) -
Shizuo FUJIWARA, Eiji SUGIMURA1981 Volume 30 Issue 12 Pages S99-S102
Published: December 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSDownload PDF (326K) -
T. S. West1981 Volume 30 Issue 12 Pages S103-S115
Published: December 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe trace elements B, Co, Cu, Fe, Mn, Mo and Zn have been shown to be essential for the growth of plants and, with the exception of B, for animals. Seven other elements, Cr, Ni, Se, Si, V, Br and I are biofunctional though not essential. The roles played in plants by these elements are reviewed and the effects produced by deficiency. The analytical problem is surveyed from the viewpoint of the range of these elements in soils, their forms of occurrence and the influence of factors that affect their uptake by plants. Finally the means by which plant uptake is simulated to permit preventive or corrective measures to be made are discussed and the role played by some of the techniques of analytical atomic spectroscopy.View full abstractDownload PDF (1634K) -
Kazuo WATANABE1981 Volume 30 Issue 12 Pages T103-T105
Published: December 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe sealed tube dissolution technique was studied for the complete conversion of sulfur in steels to sulfate. Isotope dilution mass spectrometry was used for the determination of sulfur in the sulfate. Sample (0.5 g) was dissolved in nitric acid (7 ml) and hydrochloric acid (3 ml) in a sealed borosilicate glass tube on being heated above 180 °C overnight. Nitrate ions were removed by repeated evaporation with hydrochloric acid. The residue was dissolved in hydrochloric acid. Sulfate was reduced with a mixture of hydrochloric, hydroiodic and hypophosphorous acids; hydrogen sulfide evolved was absorbed in cadmium acetate solution, then converted to silver sulfide, which was burned to sulfur dioxide in pure oxygen at low pressure, for isotopic analysis. Analytical blank in whole procedure was 0.8μg of sulfur. This technique was applied to the determination of sulfur in NBS low alloy steels. The principal cause of low values obtained by the open beaker dissolution technique was evaporation losses of sulfur as sulfur dioxide during the dissolution.View full abstractDownload PDF (517K) -
Takashi YAMASHIGE, Yasumasa SHIGETOMI1981 Volume 30 Issue 12 Pages T106-T110
Published: December 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA method is described for the determination of trace amounts of magnesium and calcium in ambient particulates by atomic absorption spectrometry using an air-acetylene flame. As a filter, quartz fiber (2500 QAST) made by Pallflex Co. Ltd. was suitable for the collection of the particulates as the content of magnesium and calcium in it was negligible and it allowed to pass easily much volume of air sample without dropping the aeration rate. The wet digestion with HF/HNO3/H2O2 was the most satisfactory for the extraction of magnesium and calcium from ambient particulates. Further, the interferences from Al(III), Ti(IV) and V(V) was overcame by the addition of 7000 μg/ml of strontium(II). The procedure is as follows; A given amount of particulates sample was taken in a teflon beaker. Five ml of 45 % hydrofluoric acid was added and the solution was evaporated to dryness on a hot plate. This process was repeated twice. The residue was dissolved in 20 ml of concentrated nitric acid together with a small amount of hydrogen peroxide by gentle heating. After filtering an insoluble residue off, the filtrate was evaporated to nearly dryness. The residue was dissolved again in 50 ml of 0.5 M hydrochloric acid containig 350 mg of strontium(II). The absorbances were measured at 285.2 nm (Mg) and 422.7 nm (Ca) with a Nippon Jarrell Ash Model AA-781 atomic absorption spectrophotometer. By the present method, (325) μg magnesium and (30300) μg of calcium in ambient particulates were determined satisfactory within an error of 5 %.View full abstractDownload PDF (763K) -
Sotaro ITO, Toshiko YAMAGUCHI1981 Volume 30 Issue 12 Pages T110-T114
Published: December 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe purpose of this work is to clarify the effect of the sample volume on the COD values (JIS K 0102 13, acidic permanganate method at 100 °C) using three kinds of the standard samples (No. 10, 11 and 12) prepared by Japan Environmental Measurement and Chemical Analysis Association. In the range of titrant volume(a) from 2.15 to 7.87 ml, the following full logarithmic linear relationship was found to hold with correlation coefficients above 0.997, log a=logk+ n log V, where V stands for the sample volume (ml) and k and n are constants. The n values for the standard samples No. 10, 11 and 12 are 0.90±0.014, 0.90±0.027 and 0.88±0.031, respectively. The observed n values less than unity indicate that the COD values for these samples are sensitive to the sample volume. A possible contribution of the effect of sample volume to the COD values reported previously from 38 laboratories was discussed in detail.View full abstractDownload PDF (771K) -
G. Horvai, K. Tóth, E. Pungor1981 Volume 30 Issue 12 Pages S117-S124
Published: December 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSWidespread use of ion-selective electrodes and the growing possibility of using sophisticated computer technique in conjunction with the electrodes has made necessary to investigate the degree of precision attainable by potentiometric techniques. Results obtained by applying error propagation statistics to various potentiometric methodologies, like calibration, single and multiple standard addition, titration, etc. have been critically reviewed.View full abstractDownload PDF (858K)
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