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Volume 30, Issue 8
Displaying 1-16 of 16 articles from this issue
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Toru NOZAKI, Masatomi SAKAMOTO, Keiko OKAMURA1981 Volume 30 Issue 8 Pages 489-493
Published: August 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA square-wave polarographic method for simultaneous determination of zinc(II) and cobalt(II) has been studied with glycine as a complexing agent. Into a 50 ml beaker 5 ml of 0.1 M glycine and 10 ml of 2.0 M sodium perchlorate were taken and added 10 ml of a sample solution containing zinc(II) and cobalt(II). After the pH was adjusted to 5.25.3 with perchloric acid and sodium hydroxide, the solution was transferred to 50 ml measuring flask and diluted to the mark with water. The polarogram of the solution was recorded from -0.8 V to -1.6 V vs. SCE at 25°C, and zinc and cobalt were determined from the calibration curves, where the wave height due to zinc was substracted from the peak height of cobalt(II) at -1.27 V vs. SCE. The lower limits of detection of zinc and cobalt were 0.07 μg/ml and 0.3 μg/ml, respectively. The following amounts (μg/ml) of diverse ions were allowed for the determination of 0.65 μg/ml of zinc(II) and 0.59 μg/ml of cobalt(II) : Co(II) 5.9 for the determination of Zn(II), Zn(II) 1.3 for Co(II), Fe(III) 1.1, Mn(II) 54.9. Nickel(II) interferred seriously, whereas copper(II), lead(II) and cadmium(II) did not. This method was successfully applied to the determination of zinc and cobalt in manganese nodules, after the extraction of iron with methylisobutylketone and removing of nickel and the majority of manganese by an anion-exchanger.View full abstractDownload PDF (771K) -
Toshiaki NOMURA, Takashi NAGAMUNE, Kosuke IZUTSU, Thomas Summers WEST1981 Volume 30 Issue 8 Pages 494-499
Published: August 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA new electrolytic method, in which metal ions in flowing aqueous solutions were electrodeposited on the platinum electrode of a piezoelectric quartz crystal (cathode) by using a silver-silver chloride electrode (Ag/AgCl) as the counter electrode, and the frequency changes of the crystal during electrolysis were measured, was developed. For some metals, the difference (ΔF, Hz) between frequencies of the crystal just before and after the electrodeposition was proportional to the concentration of the metal ion in the solution. Selective determination of copper(II) was performed as follows: A sample solution of copper(II) containing 1 × 10-3 M potassium chloride and 0.01 M acetate buffer (pH 4.7) was made to flow through the cell at the rate of 9.4 ml/min, and electrolyzed at -0.7V vs. Ag/AgCl for 5 min. The frequency difference (ΔF, Hz) of the crystal between just before and after the electrodeposition was applied to the calibration curve prepared by the same method. Copper(II) solution from 1 × 10-6 to 1 × 10-4M could be determined with good reproducibility having 4.97 Hz (1.74 %) standard deviation for the 6 determinations of 2 × 10-5 M copper(II).View full abstractDownload PDF (1164K) -
Nobuaki MATSUOKA, Masaki OKAMURA, Eiji HIRAI, Naosuke SHIRAISHI, Noriy ...1981 Volume 30 Issue 8 Pages 499-503
Published: August 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA simple method for the determination of 222Rn and 220Rn in air with a liquid scintillation counter (LSC) was investigated. With a simple absorption apparatus, Rn in air was concentrated into the liquid scintillator solution(LS) consisting mainly of toluene or p-xylene according to the distribution equilibrium. After removal of humidity and particulates, the sampled. air passed through the absorption vessel which contained 100 ml of LS, for 40 min at the rate of 200 ml/min. After establishment of radioactive equilibrium, CLS (the concentration of Rn in LS) was measured with a LSC. It was found experimentally that the concentration of Rn in air was approximately equal to CLS/K, where K was the distribution coefficient of Rn and could be known from various literatures. The detection limit became low by using an improved integral counting method based on the concept of quenching correction. The detection limit for 222Rn was 0.1 pCi/l (twice the standard deviation of counting). When the concentration of 220Rn was much higher than that of 222Rn, both 222Rn and 220Rn could be determined simultaneously by use of Bunney plot. The concentration of 222Rn in air at 1 m above the ground was (0.10.4) pCi/l. The concentrations of 222Rn and 220Rn in a geothermal gas were 3.1 × 10-11 Ci/l and 1.37 × 10-8 Ci/l respectively. The results obtained by the present method were in good agreement with other methods. The present method is very suitable for a field survey, because the analytical procedure is simple and a number of samples can be determined successively.View full abstractDownload PDF (741K) -
Masahiko TAKASUGI, Noriyuki WATANABE, Eiji NIKI1981 Volume 30 Issue 8 Pages 504-508
Published: August 05, 1981
Released on J-STAGE: January 19, 2010
JOURNAL FREE ACCESSCarbon-13 NMR spectra and spin-lattice relaxation times (T1) of toluene, benzene, ethylbenzene, 7 kinds of amines and 4 kinds of carboxylic acids were observed both in adsorbed and liquid states. Each carbon of aniline derivatives adsorbed on silica gel showed characteristic chemical shifts. The ring carbon substituted with amino groups and its meta carbons gave upper field shifts, whereas ortho and para carbons gave lower field shifts. Carbonyl carbons of carboxylic acids showed upper field shifts. These results suggest that the hydrogen bond was formed between amines or carboxylic acids and surface silanole groups (≡Si-OH). Adsorption of amines or carboxylic acids on the surface of the silica gel resulted in the decrease of T1. The methyl carbon of the adsorbed species kept still rather long T1, owing to its remaining free rotation. It was proved that measurements of T1 for adsorbed molecules were powerfully useful in assignment of close peaks for the ring carbons in the case of ο-ethylaniline.View full abstractDownload PDF (646K) -
Hiroshi NISHIDA1981 Volume 30 Issue 8 Pages 509-513
Published: August 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSIn the spectrophotometric determination of beryllium with Chromazurol S (CAS) in the presence of zephiramine, the absorbance of the complex was dependent on concentration of diverse anions like as chloride and sulfate. In the pH range from 5 to 5.7, the absorbance of the complex was increased with the increase of the anion concentration and became constant at anion concentrations higher than 0.15 mol dm-3. The effect by the anions appeared larger with chloride ion than with sulfate ion. These facts observed on formation equilibria of the beryllium complex were successfully explained by introducing certain side reactions such as hydrolysis of beryllium ion, ion-pair formation between zephiramine and the diverse anions, and dissociation of CAS. According to the results, it was recommended that, in the spectrophotometric determination of beryllium, the composition of diverse anions in the samples should be kept as constant as possible by adding extra salts in an excess.View full abstractDownload PDF (672K) -
Shigeru TAGUCHI, Issei KASAHARA, Katsumi GOTO1981 Volume 30 Issue 8 Pages 513-518
Published: August 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSSeveral cobalt(III) complexes of 2-(2-pyridylazo)-5-aminophenol derivatives were synthesized. Since these complexes are inert univalent cobalt chelate cations, they can be used as the counter ions for the extraction of anionic surfactants in water. The ionpairs can be extracted even into low dielectric solvents such as benzene, toluene and xylene, which are usually classified as poor solvents for such ion-pair extractions. The extraction constants (Kex) of these ion-pairs into benzene were studied. The Kex values for the 5-diethylaminophenolato cobalt (Co-PADAP) series are higher than those for the 5-dimethylaminophenolato cobalt (Co-DMPAP) series. Modification of 5-position of the pyridylazo group with chloro, bromo and methyl groups enhances the extractability of the ionpairs. An addition of one methylene unit into the carbon chain of the surfactants increases the log Kex values by approximately 0.6 for the series C8C14 of the alkylsulfonate. Among the surfactants having the same alkyl chain, extractability decreases in the order of sulfate>sulfonate>carboxylate.View full abstractDownload PDF (984K) -
I. Iron and manganeseKazuo ITOH1981 Volume 30 Issue 8 Pages 518-524
Published: August 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSSelective leaching experiments were carried out in order to determine chemical forms of iron and manganese in estuarine sediments. Manganese nodule was used as the reference material for the leaching test. The leaching solutions were classified into the following five types, according with their chemical and physical properties toward metals; type 1. 0.1 M acetate buffer with pH 5.0 used for ion exchange leaching, type 2. 5×10-2 M ethylenediaminetetraacetic acid for chelate formation, type 3. 2.5 % and 25 % acetic acid for acidic solubilization, type 4. 3 % hydrogen peroxide in 25 % acetic acid for oxidizable, and solubilization, type 5. 0.1 M ascorbic acid in 2.5 % acetic acid for reducible solubilization. The leaching solution of 0.1 M ascorbic acid in 2.5 % acetic acid was more suitable for extracting oxide and hydroxide of iron and manganese from estuarine sediments rather than 1 M hydroxylamine in 25 % acetic acid. Because the later solution, having a low pH of 1.2, may cause decomposition of silicate structures in clay. The solution of 5 × 10-2 M ethylenediaminetetraacetic acid was effective to strip off whole metals from estuarine sediments. Pyrite was separated with the 3 % hydrogen peroxide in 25 % acetic acid. The proposed leaching solutions were proved to be useful for the speciation of iron and manganese in estuarine sediments.View full abstractDownload PDF (1000K) -
Mikita ISHII, Keiji KAJI, Toshiyuki HOBO, Shigetaka SUZUKI1981 Volume 30 Issue 8 Pages 524-528
Published: August 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSDetermination of total hemoglobin in human blood has been investigated by high performance aqueous gel permeation chromatography (HPAGPC). Separations were effected on two G3000SW columns and two G2000SW columns (Toyo Soda, Tokyo) connected in series using M/15 phosphate buffer solution (pH 7.3) as the mobile phase. The detectors were a refractive index detector and an atomic absorption detector. These two detectors were connected through an interface when it is desired to monitor iron compounds. First, preparation of standard hemoglobin was attempted from ICN-NBC Laboratories, Inc. (NBC) human hemoglobin samples, which showed two impurity peaks besides the hemoglobin peak on the chromatogram. Through injecting the solutions of NBC hemoglobins for fifteen times and collecting those fractions corresponding to hemoglobin, the pure standard hemoglobin was obtained which could be used for the quantitative analysis. The calibration curve for hemoglobin obtained by the standard sample was linear up to 5.0 g/l. Collection was done at the same time on the other two impurity peaks, and their response factors against hemoglobin could be determined. Thereafter, the concentration of pure hemoglobin in NBC hemoglobin preparation could be determined through measuring the peak areas on the chromatogram. And the NBC hemoglobin whose purity was previously checked could be used as a standard sample for the determination of total hemoglobin in blood. The concentration of total hemoglobin in blood samples determined by the proposed method agreed well with those obtained by other two methods, namely cyanmethemoglobin method and azidemethemoglobin method. The coefficient of variation of the proposed method was within 1.8 %. The time required for the analysis was less than 120 min.View full abstractDownload PDF (644K) -
Kazuo KUGA1981 Volume 30 Issue 8 Pages 529-534
Published: August 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSDetermination of trace amounts of gallium by using a zirconium-impregnated graphite tube has been studied. The zirconium-impregnated tube was made as follows; a conventional graphite tube (Nippon Carbon Corp. EG-36H internal diameter: 6.0 mm, external diameter: 8.0 mm, length: 32 mm) was soaked in a 2 % zirconium nitrate solution under reduced pressure for 60 min. Then the tube was dried at 100°C for 60 min and was heated at 500 °C for 30 s in air and 2700 °C for 3 min in argon. The process was repeated 2 times. The life-time of the tube increased about 2 times longer than that obtained with conventional untreated tube (2500 °C-6 s operation) and the sensitivity of gallium increased to about 6 fold. The optimal measuring conditions of gallium were established for practical analysis. A10μl volume sample solution was injected with micropipette into the furnace and the atomic absorption signals were measured (wavelength : 287.4 nm, drying : 100 °C-30 s, ashing : 1000 °C-30 s, atomizing : 2500 °C-6s). The working curve for gallium was linear over the range of (0.010.6)μg/ml{(0.16) ng/10μl}.The detection limit (S/N=2) obtained was 0.015ng/10μl and the relative standard deviation (n=10) of this method was 2.5 % for 0.1 ng. Interference by Al, Ca, Co, Cu, Ge, In, K, Mn, Na, Sb, Tl and Zn was almost negligible when the amounts of these elements were 1000 times of gallium (0.1μg/ml) but Ag, B, Ba, and Cr interfered. This method was applied to the determination of gallium in indium metals, aluminum and aluminum alloys and the results were satisfactory.View full abstractDownload PDF (1059K) -
Kazuo HIROWATARI, Yoshihiro KOUMURA, Kazuo KUMAMOTO, Korehiro HATTORI, ...1981 Volume 30 Issue 8 Pages 534-537
Published: August 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe liquid chromatographic separation of ethylenediaminetetraacetic acid (EDTA)-chelates of bismuth(III), iron(III) and copper(II) was established by reversed phase paired-ion chromatography. The EDTA-chelates in aqueous solution were separated on a column (4 mm i.d. × 30 cm) packed with ODS-Hypersil. A 1 : 9 mixture of acetonitrile and water containing 0.01 M ammonium dihydrogen phosphate and 0.01 M tetrabutylammonium bromide (pH 3.0) was used as a mobile phase at a flow rate of 1 ml/min. The EDTA-chelates in the elute were detected at 254 nm. From the peak area of the elution curve, the amount of each EDTA-chelate could be determined. This method provided the linear working curves in the concentration range of (20 to 200) μg/ml for each EDTA-chelate and the detection limits (S/N=3) were 4 ng, 2 ng and 40 ng for Bi(III), Fe(III) and Cu(II)-chelates. The coefficient of variation was within 1.2 %.View full abstractDownload PDF (633K) -
Hideko YASUDA, Tanenori SASAKI, Kazuo SAITO1981 Volume 30 Issue 8 Pages 538-544
Published: August 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSWhen the sample is atomized at high temperature the graphite cuvettes will deteriorate. The effects of this deterioration to the measurement is described in this report. Whole blood was diluted to 14-fold of the blood volume with 0.1 N HCl containing manganese. The absorption by manganese was measured using the cup-type cuvette with Zeeman type atomic absorption spectrophotometer (Hitachi 170-70 type). The time required to dry up the sample, and the weight loss, revelation temperature, and the temperature-current characteristic of cuvettes were investigated. The weight of cuvettes decreased linearly with increasing the frequency of measurements by the sublimation and the oxidation of graphite cuvettes loaded at high temperature. The weight loss of an cuvette was about 0.36 mg on average at every atomization of the sample. The electric resistance of cuvettes increased with increasing the weight loss. In spite of setting the same current, the revelation temperature of cuvettes increased with increasing the number of measurements. The heights of peak in absorbance also increased. This reason may be considered as follows: the more the frequency of measurements are, the higher the atomization temperature rises up. At the same time, the number of atoms atomized at the stage of atomization increases. As the cuvettes had different weights, these showed different revelation temperatures under the same condition for measurements respectively. Heavy cuvettes indicated the lower revelation temperatures.View full abstractDownload PDF (998K) -
Masahiko IKEDA, Jiro NISHIBE, Taketoshi NAKAHARA1981 Volume 30 Issue 8 Pages 545-548
Published: August 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSFlameless atomic absorption spectrometry using an electrically heated quartz cell atomizer has been developed for the determination of antimony, tin, selenium and bismuth in combination with an automated hydride generation system which enable the gaseous hydrides produced by sodium borohydride to be introduced into the atomizer continuously. Some fundamental parameters affecting their production and introduction have been investigated. Of the metal hydrides studied, hydrogen selenide was the most unstable and the most soluble or reactive with water. Therefore, such a direct transfer mode as used in this study is exceedingly preferable especially for selenium to a collection mode. Under the optimum conditions, the detection limits (S/N=2) were 3 ng/ml, 3 ng/ml, 2 ng/ml and 1 ng/ml for antimony, tin, selenium and bismuth respectively and the reproducibilities (RSD's) of the present method based on ten replicate determinations of the elements at the concentrations of 20 times greater than their detection limits were within 1 %.View full abstractDownload PDF (522K) -
Masahiko IKEDA, Jiro NISHIBE, Taketoshi NAKAHARA1981 Volume 30 Issue 8 Pages 548-550
Published: August 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSAtomic absorption spectrophotometry with a premixed argon (entrained air)-hydrogen flame has been developed for the determination of germanium in combination with a continuous hydride generation system which enables the gaseous germanium hydride (GeH4, "germane") produced from the acidified solutions with tartaric acid by sodium borohydride introduced into the flame continuously. Several fundamental parameters affecting its production and stability were investigated. Tartaric acid is superior with respect to interference to hydrochloric acid which is usually used for other hydride-forming elements. Of the elements investigated, some elements, such as copper, cobalt and nickel, have shown a large depressing interference with the determination. Under the optimum experimental conditions, a sensitivity (1 % absorption) of 0.02 μg Ge/ml and a detection limit (S/N=2) of 0.01μg Ge/ml were obtained. A reproducibility (as RSD) of the present method, which is calculated from ten replicate determinations of the element at the concentration of 20 times greater than the detection limit is approximately 1 %.View full abstractDownload PDF (510K) -
Yoshihiro SAKAI, Yasuhiko KASAI1981 Volume 30 Issue 8 Pages 550-552
Published: August 05, 1981
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSAn indirect method is described for the determination of N, N'-dicyclohexylcarbodiimide(DCC), which is based on the reaction of DCC with oxalic acid and the subsequent iodometric determination of the unreacted oxalic acid. The procedure is as follows: to a mixture of DCC (about 70 mg) and methylene chloride (25 ml) in a 300-ml iodine-flask, add 10 ml of 1.0 w/v % oxalic acid and reflux in a water bath {(7580)°C} for 30 min. After cooling to room temperature, add 10 ml each of 10 w/v % potassium iodide, 10 w/v % barium chloride, and 0.1 M potassium iodate, and 100 ml of distilled water. After 10 min, titrate the iodine liberated with 0.1 N sodium thiosulfate. The coefficient of variation was (0.100.32) %.View full abstractDownload PDF (428K) -
Naobumi OI, Tadashi DOI, Hajimu KITAHARA, Yoko INDA1981 Volume 30 Issue 8 Pages 552-555
Published: August 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSAmide derivatives of three optically active carboxylic acids, N-(S)-2-(4-chlorophenyl)isovaleroyl laurylamine [I], N-(1R, 3R)-trans-chrysanthemoyl laurylamine[II] and N-(1R, 3S)-cis-chrysanthemoyl laurylamine[III] were synthesized and their properties as stationary phases for the separation of chiral compounds by gas chromatography were examined. These phases showed enantioselectivity for some enantiomers of N-trifluoroacetyl (TFA) amino acid esters, N-TFA-amines and carboxylic acid amides. Rather high separation factors were obtained for some carboxylic acid amide enantiomers. For example, racemic 2-ethyl-3, 3-dimethylbutyric acid t-butylamide was separated (α=1.037, 100 °C) with [I] and racemic trans-chrysanthemic acid t-butylamide was separated (α=1.074, 100 °C) with [II], respectively. It was noticeable that these two carboxylic acid amides were hardly separated with N, N', N″-[2, 4, 6-(1, 3, 5-triazine) triyl]-tris-(L-valine isopropylester), N, N'-[2, 4-(6-ethoxy-1, 3, 5-triazine)diyl]-bis-(L-valyl-L-valine isopropylester), N-lauroyl-L-valine t-butylamide and N-lauroyl-(R)-1-(α-naphthyl)ethylamine, which were proved to be excellent chiral phases for the separation of amino acid and amine enantiomers. In conclusion these optically active carboxylic acid amides are specifically effective as the stationary phase for the separation of some chiral carboxylic acid amides.View full abstractDownload PDF (480K) -
Yûetsu DANZAKI, Masahiko SASE, Jin KIMURA1981 Volume 30 Issue 8 Pages T81-T84
Published: August 05, 1981
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSComposition of Chevrel phase compound Pb1-xSn1.2xMo6.35S8 is determined without preliminary separation. i) Sulfur-Sample has been fused with sodium carbonate and sodium peroxide mixture, the melt is leached with water, and lead precipitate formed is filtered off. Sulfur is determined by the gravimetric method as barium sulfate after masking of tin(IV) with tartaric acid and of molybdenum(VI) with EDTA and hydroxylamine hydrochloride. ii) Lead-Sample is dissolved in a mixture of hydrochloric acid and nitric acid. After tin(IV) has been masked with tartaric acid, lead is determined complexometrically at pH 10. iii) Tin-Sample is dissolved in a mixture of hydrochloric acid and nitric acid, and then sulfuric acid is added. The solution is heated, and evaporated. to SO3 fume. After oxidizing partially reduced molybdenum with nitric acid, tin(IV) is determined complexometrically with bismuth nitrate solution at pH 1.31.7. iv) Tin and molybdenum-Sample is dissolved in a mixture of hydrochloric acid and nitric acid, and then sulfuric acid is added. The solution is heated, and evaporated to SO3 fume. After adding EDTA and hydroxylamine sulfate, and adjusting pH to about 2, the solution is boiled and then cooled. Sum of tin(IV) and molybdenum(VI) is determined complexometrically with bismuth nitrate solution at pH 1.31.7.View full abstractDownload PDF (487K)
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