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Volume 24, Issue 5
Displaying 1-12 of 12 articles from this issue
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Koreharu OGATA, Takeichi SAKAGUCHI, Yoshiko ICHIKAWA, Fumiko DEGUCHI, ...1975 Volume 24 Issue 5 Pages 279-283
Published: May 10, 1975
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSIon pair compounds between tetrabromophenolphthalein ethylester (TBPE) and tertiary amine derivatives were extracted from the alkaline aqueous solution into 1, 2-dichloroethane (DCE) phase and determined colorimetrically of the maximum absorption at about 600 nm. The analysis was carried out as follows ; 5 ml of standard pH buffer solution (0.5M sodium phosphate+ 0.1M borax), 0.25 ml of methyliodide and 2.0 ml of sample solution were mixed in a 100 ml colorimetric tube or a separatory funnel being shaken for 30 seconds. Then 2.0 ml of 10-3M TBPE ethanol solution was added and the solution was diluted to 25 ml with water.
To this solution was added 10 ml of DCE and the solution was shaken for 2 min. The mixture was settled for 5 min. The fraction of the organic phase was separated with a filter paper and the colorimetric measurement was made by using DCE as a reference. The sample solution was taken so as the final concentration fell in the range of 10-7 to 10-4M. The binding ratio of the dye to amines such as 4, 4-diethylaminoethoxy-α, β-diethyldiphenyl-ethane 2HCl, 10-diethylaminopropyl phenothiazine and 3-phenyl-5-diethylaminoethyl-1, 2, 4-oxadiazol citrate was 2/1, 1/1, and 1/1, respectively. However, in both compounds of 3- diethylaminoethoxy-carbonyl pyridine citrate and 3-(β-diethylaminoethyl)-4-methyl-7-carboethoxy-2-oxo- (1, 2-choromene) HCl, the ratio was found as 0.6 which did not show multiple constitution for a pairing complex. In order to study the composition of the latter product colored crystalline compound was prepared as a model compound with TBPE and triethylamine. The latter product was crystallized from ethyl acetate solution. Similarly, crystalline products were obtained from tertiaryamines and sulfophthalein series dyes. The infrared, absorption spectra of the latter two compounds suggested the similar mechanism of ionic binding at quinoid carbonyl, and furthermore, the mass spectra of the latter two compounds revealed the same conclusion. Hence, it was concluded that the colored products were ion pair compounds and the binding mechanism in this color reaction was also based on ion pairing reaction.View full abstractDownload PDF (585K) -
Sadato SAKURAI, Eiji NIKI1975 Volume 24 Issue 5 Pages 283-288
Published: May 10, 1975
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSIn digital polarography, the diffusion current (peak current) in DC (SW) polarography is digitized and accumulated in a 100 channel pulse height analyzer (PHA) by repeating the scanning. The coefficient of variation of the diffusion current decreases by 1/√n, where n is the number of scanning. With cadmium ion (reversible system), the coefficient of variation of the diffusion current in DC polarography is nearly equal to that of the peak current in SW polarography in the range 5×10-6M to 10-3M. With nickel ion (irreversible system) the coefficient of variation of the peak current in SW polarography increases more rapidly than that of the diffusion current in DC polarography with decreasing concentration, due to the lower peak current. The variation of the diffusion current measured on different days was not significantly (at the 5% level) different from that measured on the same day (for 10-3M Cd2+, Ni2+). However, the variation of the peak current among different preparations of sample solutions of the same concentration was significantly (at the 1% level) larger than that among the repeated measurements of the same single sample solution (for 5×10-4M Cd2+).
Indium (III) ion in the presence of cadmium(II) ion (concentration ratio 1 : 5) could be determined with the coefficient of variation of 0.2% by using the differential method.View full abstractDownload PDF (1012K) -
Toshiyuki HOBO, Takeshi OGURA, Shigetaka SUZUKI, Shun ARAKI1975 Volume 24 Issue 5 Pages 288-293
Published: May 10, 1975
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA new method for concentration of methyl mercuric chloride (MMC) in water is proposed. It is based upon the foam separation in the presence of potassium n-butylxanthate (n-BuXn) and cetyltrimethylammonium bromide (CTAB). The apparatus was devised and the effects of pH, amount of CTAB, concentra-of n-BuXn and nitrogen gas volume on MMC recovery were investigated. The standard condition was settled as follows : pH; 9.0, n-BuXn concentration; 5.6×10-5g/ml, the addition of CTAB (7.5×10-4 g/ml) ; 2 ml at the beginning and then 1 ml at every 5 min, N2 flow rate; 60 ml/min, time for separation; 20 min. The foam was continuously collected in the glass receiver which contained 0.1 ml of n-butanol. The MMC concentrated in the receiver was extracted with benzene and analyzed by GC. As the heavy metals caused decrease in the MMC recovery, they were removed by an ion-exchange column packed with Amberlite IR-120A and Amberlite IR-4B. The MMC recovery was higher than 95%, when Cu2+ +Hg2+ was 10 ppm.View full abstractDownload PDF (784K) -
Analyses of harmful chemicals in household necessities. IShigeo KOJIMA, Takuma OBA1975 Volume 24 Issue 5 Pages 294-298
Published: May 10, 1975
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSDetermination of free formaldehyde in underwears was investigated. This investigation was undertaken because free formaldehyde in underwears could be one of the cause of the skin troubles. For the determination, it is necessary to avoid the decomposition of resins and formation of additional formaldehyde during extraction and color development. The extraction temperature was set at 40°C, because the decomposition of urea-formaldehyde resin was assumed to be accelerated with increasing temperature and moreover this temperature was the one where underwears were in contact with the skin. A 1 g chopped sample was immersed in 100 ml of water for 1 hour at 40°C, and the extract was filtered through a glass filter (G2). The formaldehyde in the extract was determined by the photometric acetylacetone method. With formaldehyde standard solutions, the color reaction was completed by heating for 30 minutes at 40°C as well as for 10 minutes at 60°C after addition of the acetylacetone reagent. With N, N'-dimethylolurea solutions and extracts of underwears treated with ureaformaldehyde resin, however, the former condition was superior to the latter. Commercial underwears were analysed by the proposed method and high levels of formaldehyde were found in (1) cupra treated with urea-formaldehyde resin, (2) shirts, especially their paddings, and (3) brassieres, especially their non-woven fabrics.View full abstractDownload PDF (713K) -
Masao KANDA, Yoshiki HORI, Isao MATSUMOTO1975 Volume 24 Issue 5 Pages 299-303
Published: May 10, 1975
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSSeveral analytical conditions have been examinated to determine rapidly a trace amount of lead in titanium dioxide with little pretreatment. A quantitative profile of lead absorption was obtained by introducing directly the mixture of sample and carbon powder into a graphite atomizer (Fig. 4).
The procedure was as follows : 50 to 100 mg of sample was weighed. Carbon powder, 5 to 9 times as much amount as the sample, accurately weighed, added to the sample and mixed well in an agate mortar for 10 minutes. One to five mg of the mixture was introduced into a graphite atomizer, the amount being controlled by the lead content of the sample. The lead content of the sample was calculated from the calibration curve which was introduced 20 μl of the standard lead solution containing lead from 0.025μg/ml to 0.3μg/ml into a graphite atomizer.
Interference from coexisting metals such as K, Ca, Al, Mn, Mg, Fe and Zn was studied in 500 times as much amount as 0.2 ppm of lead, there were little problems except K. But K was also found little problem by arring out with a background corrector. The time required for an analysis was about 15 minutes and the coefficients of variation was 3.1% for 5 ppm of lead and 2.4% for 30 ppm of lead in titanium dioxide.View full abstractDownload PDF (729K) -
Hiroshi HASHITANI, Takeo ADACHI1975 Volume 24 Issue 5 Pages 303-307
Published: May 10, 1975
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA sensitive photometric method for the determination of trace of niobium in tantalum with sulfochlorophenol S is proposed. Tantalum was quantitatively separated by an anion-exchange method from nitric acid-hydrofluoric acid medium. Prior to the color development, these acids were removed by fuming with perchloric acid. Sulfuric acid (0.04 to 0.2M) was necessary for the color development. A maximum absorbance was obtained when the solution was kept for 60 minutes at room temperature, or 5 minutes at 60°C.
Niobium down to 1 ppm in tantalum can be determined (ε=4.2×104) according to the following procedure. Not more than 1 g of tantalum is dissolved in 8 ml of hydrofluoric acid (1:1) and 2 ml of nitric acid (1:1) by heating. The solution is transferred to a column containing 10 ml of strongly basic anion-exchange resin (Diaion SA#100) in a polyethylene tube, with three 10-ml portions of a mixture of 1M nitric acid-5M hydrofluoric acid. Niobium is eluted with 100 ml of a mixture of 5M nitric acid-0.2M hydrofluoric acid. The effluent is evaporated to fumes with 1.5 ml of perchloric acid in the presence of 2 ml of sulfuric acid (1:19). The solution is transferred to a volumetric flask with 5 ml of hydrochloric acid (1:1) and small portions of water. Two ml of 0.05% sulfochlorophenol S solution and 2.5 ml of acetone are then added, and the resulting solution is diluted to 25 ml with water. After 60 minutes, the absorbance is measured at 650 nm with a blank as reference.View full abstractDownload PDF (769K) -
Katsuta NAKAGAWA, Shigeaki ASHITANI, Yumiko KOZAKI, Shinya KITAHARA1975 Volume 24 Issue 5 Pages 308-310
Published: May 10, 1975
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe column (1 m × 2.1 mm of internal diameter) was packed with Zipax-strong cation exchange resin (1%) and was operated at 25°C with M/15 KH2PO4 (pH 4.50) as eluent (flow rate : 1.2 ml/min). 1 μl of the sample solution in methanol was injected and the effluent was monitored at 254 nm. These conditions permitted the separation of the isomers of chloroanilines; ο-chloroaniline (elution time 1.5 min), m-chloroaniline (3.8 min), p-chloroaniline (7.0 min), and p-anisidine (13.0 min). p-Anisidine proved to be the best internal standard for the determination of the isomers of chloroaniline. The limit of detection was 0.1 mg/ml.
The coefficients of variations were 1.6% (the determination of p-derivative in ο-chloroaniline) and 1.5% (ο-derivative in p-chloroaniline) for commercial samples.View full abstractDownload PDF (374K) -
Studies on oxygen determination by carrier gas methods. VIIITakeo KURIKI, Keiko OHSAWA, Kazuo IMAEDA1975 Volume 24 Issue 5 Pages 311-314
Published: May 10, 1975
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSOrganic acid salts of indium, such as bis(benzoate-O)hydroxy indium, bis(2-methyl benzoate-O)hydroxy indium and bis(trichloro acetate-O)hydroxy indium, and indium complexes, such as tris (2-methyl-8-quinolinolate)indium, tris(2, 4-pentane-dionate-O, O')indium and tris (8-quinolinolato) indium, were used as samples. Oxygen in these samples was determined precisely by the usual method. Oxygen in indium, chloride with crystal water was also determined precisely by the same method. On the other hand, the amount of oxygen in indium oxide, indium hydroxide and indium nitrate was determined as less than the calculated value by a factor of (814) %. For the compounds whose total oxygen could not be determined precisely with the usual method, the authors designed the reaction-gas-addition-carrier-gas-method. In this paper hydrogen was used as a reaction gas. The results of oxygen determination in indium oxide, indium hydroxide and indium nitrate were in good agreement with those of their calculated values with this method. One analysis required approximately 40 min.View full abstractDownload PDF (638K) -
Studies on the hydrazone derivatives in fluorometric analysis. VHirokazu TANIGUCHI, Kazue TESHIMA, Keiko TSUGE, Saburo NAKANO1975 Volume 24 Issue 5 Pages 314-318
Published: May 10, 1975
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe fluorophotometric titration of copper(II) with 2-hydroxy-1-naphthaldehyde benzoic acid hydrazone-(HNBH) was investigated.
Copper(II) reacted with HNBH to produce nonfluorescent Cu-HNBH complex, whereas scandium(III) yield a fluorescent Sc(III)-HNBH complex which had an excitation maximum at 440 nm and an emission maximum at 500 nm in dimethylformamide(DMF)-acetate buffer (pH 4.5) mixture.
When HNBH was gradually added to the mixture solution of copper(II) and scandium(III) salt, nonfluorescent Cu-HNBH complex was initially formed, subsequently fluorescent Sc(III)-HNBH complex was formed. This phenomenon could be applied to the fluorophotometric titration of copper(II).
The recomended procedure for the determination of copper(II) is as follows: To 5 ml of a sample solution containing copper(II) are added 2 ml of 1 M acetate buffer solution(pH 4.5) and 7 ml of DMF. The solution is cooled to room temperature, and subsequently 0.5 ml of 0.6% Sc(NO3)3· 4H2O solution is added. This solution is titrated with 10-4M HNBH solution in 50% DMF until the yellowish green fluorescence comes out.
The presence of iron gave a large effect on the determination of copper(II), but its interference could be eliminated by extracting Fe-cupferron complex with ether. The range of determination was (0.2100) μg of copper(II) per ml and the coefficient of variation was 1.1%.View full abstractDownload PDF (780K) -
Shigeru TERASHIMA1975 Volume 24 Issue 5 Pages 319-321
Published: May 10, 1975
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA method is proposed for the determination of tin in silicates by atomic absorption spectrometry after extracting tin (IV) iodide with benzene. Take 0.1 to 0.5g of sample in a platinum dish, add 10 ml of HF, 5ml of HClO4, and 3 ml of HNO3, and evaporate the solution to dryness. Dissolve the residue by heating with 5 ml of HCl (1+1). Transfer the solution into a separatory funnel, add 10 ml of HClO4, 0.5 ml of 50% sodium hypophosphite, 5 ml of 5M NaI, and extract tin for 3 min with 10 ml of benzene. Wash the organic phase with 16 ml of 5.5M HClO4-0.3M NaI solution. Shake the organic phase for 3min with 10 ml of 0.6M HCl-0.004M MgCl2, and withdraw the aqueous phase into a beaker. Cover the beaker, immerse in boiling water for about 15 min to remove the dissolved benzene, and introduce this solution into a premix type slot burner. The sensitivity is 0.02 μg/ml/1% abs., and the limit of detection 0.4 ppm of tin in rock samples. The relative standard deviation in the determination of 2 to 100μg tin is 2 to 9%. The time required for 10 samples is about 4 hours. The method is satisfactorily applied to the standard silicate samples.View full abstractDownload PDF (496K) -
Kiyotoshi MORISIGE, Sakae SASAKI, Keizo HIRAKI, Yasuharu NISHIKAWA1975 Volume 24 Issue 5 Pages 321-324
Published: May 10, 1975
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSScandium in several minerals { (0.0020.3) % Sc} was determined by the fluorometric method. The procedure is as follows : (0.050.1)g of mineral sample is treated with 30 ml of concentrated sulfuric acid for 3 hrs on a sand bath, and the solution is evaporated to dryness. The residue is dissolved in (35)ml of concentrated hydrochloric acid, and the solution is diluted to (7080)ml with water and filtered. Seventy milligrams of Ca2+ as a carrier and oxalic acid solution are added and the pH of the solution is adjusted to 2.0. After the solution has stood for ten minutes, the precipitate is centrifuged and decomposed by evaporating with perchloric acid to dryness. The residue is dissolved in 5 ml of 6M HCl. Scandium is separated by extracting at pH 1.6 with 10 ml of 0.2M TTA-benzene followed by backextracting with 10 ml of 1M HCl. The solution is made up to 25 ml, and an aliquot of the solution is taken. Two ml of 0.1% 2, 4-dihydroxybenzaldehyde-semicarbazone solution, 2 ml of 20% ammonium acetate solution are added, and the pH of the solution is adjusted to 6 with hydrochloric acid or ammonia, and the solution was diluted to 25 ml with water. The fluorescence intensity of the solution is measured (λexcitation360nm, λemission 425 nm).
In this procedure, the recovery of scandium was found to be about 95%. Several mineral samples (naegite, allanite, yamaguchilite, lepidomelane, hokutolite) were analyzed.View full abstractDownload PDF (573K) -
Hiroshi UCHIDA, Fumio ADACHI, Osami MORI, Ryokichi NEGISHI1975 Volume 24 Issue 5 Pages 325-326
Published: May 10, 1975
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSMultielement analysis of individual air-borne particulates is nesessary for air-pollution research (e. g., search for their origins). Particles are collected on a Mylar film by a cascade impactor at a flow-rate of 9 liter per minute for 1 hour. The Mylar film is supported on a hollow tube after drying. A particle suitable for analysis is selected microscopically, evaporated by a laser beam emitted from neodymium glass, and excited by a high voltage spark discharge (100 μH, 6 μF, 1 Ω, and 2.5 kV). Magnesium, aluminium, silicon, calcium, iron, copper, and zinc are detected in particles of 4, 6, 8, and 10 μm diam. The content of light elements seems to be greater than that of heavy elements. The amount of each element increases with increasing particle size. The chemical composition of each particle differs in spite of the same diameter, and the variation of spectral line intensity of heavy elements seems to be slightly larger than that of light elements.View full abstractDownload PDF (241K)
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