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Volume 19, Issue 7
Displaying 1-19 of 19 articles from this issue
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Tetsuo FUJITA, Tsunenobu SHIGEMATSU1970 Volume 19 Issue 7 Pages 893-899
Published: July 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA method for the determination of strontium, calcium and magnesium in seaweeds by atomic absorption spectrochemical analysis has been examined.
For the simultaneous determination of these elements in one solution of a sample, the standard addition method was suitable for strontium and the calibrationline method was recommended for calcium and magnesium. Addition of 500 ppm of strontium and 250 ppm of calcium was effective for the elimination of influence of coexisting elements and acid for the determination of calcium and magnesium.
The condition recommended for strontium, calcium and magnesium were, respectively, wavelength 4607Å, 4227Å and 2852Å, hollow cathod lamp current 13 mA, 6 mA and 7 mA, slit with 100μ, 100μ and 100 μ, hydrogen pressure 0.5 kg/cm2, 0.5 kg/cm2 and 0.4 kg/cm2 and air pressure 1.0 kg/cm2, 1.2 kg/cm2 and 1.0 kg/cm2. The instrument used was Nippon Jarrell ash atomic absorption spectrophotometer model AA-1.View full abstractDownload PDF (817K) -
Isao TAKEMURA1970 Volume 19 Issue 7 Pages 899-902
Published: July 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe oxidation dyes and the intermediates for hair dyes and rinses were analyzed qualitatively by thin layer chromatography.
As the adsorbent, silica gel was better than aluminum oxide, because the oxidation dyes and the intermediates were separated well and moreover silica gel reduced spot tailing and developing time. The spots were distinguished clearly when the developing solvent was n-butyl acetate+benzene (2:1) and the color former was 1% p-dimethylaminobenzaldehydechloroform solution.
The procedure was applied to commercial products and ingredients of the dyes were separated well and identified easily without any pre-treatment.View full abstractDownload PDF (685K) -
Hitoo KAKIYAMA, Masahiro KOMATSU1970 Volume 19 Issue 7 Pages 902-907
Published: July 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA method of square wave polarography was applied to the determination of sulphur ions in industrial water. Sodium hydroxide was used as a supporting electrolyte. The peak potential of sulphur ion was the same as that of lead ion, which was contained in special grade reagent of sodium hydroxide as an impurity.
To separate the wave of lead ion from that of sulphur ion, EDTA-4Na was added to the supporting electrolyte. The calibration curves of sulphur ion were obtained for 1 × 10-61 × 10-5M and 1 × 10-51 × 10-4M in 0.09M EDTA-4Na and 1.0M NaOH solution. This method was not interfered from foreign anions, such as SO42-, SO32-, S2O32-, SCN-, I-, Br- and Cl-, even if these anions were contained as 100 times as sulphur ion in analyzing water. The coefficient of variation was about ±3%.View full abstractDownload PDF (833K) -
Nobuta HAYASHI, Shigeo INOUE, Keiji TAKEUCHI1970 Volume 19 Issue 7 Pages 907-918
Published: July 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe surface structures of several kinds of commercially available diatomaceous earth supports including Celite 545, C-22, Chromosorb W, Chromosorb P, Anakrom U and Gas Chrom S and column packing were observed by using scanning electron microscopy.
The correlation between their surface structures and gas chromatographic performances were examined.
The supports were roughly classified into three groups having microstructures composed of either fragmentary of complete remains of diatomaceae.
Celite 545 and Chromosorb W have similar microstructures mainly composed of amorphous and small fragmentary remains.
C-22 and Chromosorb P are composed of net work fragments of diatomaceae. On the other hand Anakrom U and Gas Chrom S are composed of complete net work cylindrical remains.
These surface structural classification of supports approximately correlates with their gas chromato graphic performances represented by separation efficiency and retention time.
The column efficiency of these supports represented by separation efficiency between methyl stearate and methyl oleate were; in case of 30% (w/w) D. E.G. S.- support, C-22 and Chromosorb P> Celite 545 and Chromosorb W> Anakrom U and Gas Chrom S, in case of 10% (w/v), Celite 545 and Chromosorb W> C-22> Anakrom U and Gas Chrom S> Chromosorb P, and in case of 5% (w/w), Anakrom U, Celite 545 and Gas Chrom S> C-22, Chromosorb W and -P and by the ratio of the retention time of methyl stearate against it of Celite 545 were divided into three groups; Celite 545 and Chromosorb W, C-22 and Chromosorb P, and Anakrom U and Gas Chrom S.
The washing of supports with an acid did not give deformation of those surface structures. The mode of distribution of a stationary liquid-D. E. G. S. (diethylene glycol succinate polyester)- on these supports gave characteristic pattern in accordance with the coating methods, namely evaporating dish method, rotary evaporator method, filter method and in-place method.View full abstractDownload PDF (5295K) -
Nobuta HAYASHI, Shigeo INOUE, Keiji TAKEUCHI1970 Volume 19 Issue 7 Pages 919-925
Published: July 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe behavior of stationary liquid of DEGS (diethylene glycol succinate polyester)-packed column in gas chromatography was investigated and informations on aging of packing materials were obtained.
The surface of used packing materials was observed to be resinificated under a scanning electron microscope.
About half of stationary liquid disappeared from the column by evaporation and most of the remainder was heat-denatured to be insoluble in organic solvents.
The heterogeneous redistribution of stationary liquid occured in the used column with characteristic periodicity, which depended on the oven structure of the column, i. e. the distribution of temperature in the oven.
This heterogeneous redistribution, which is regarded as the chief cause of lowering the column efficiency, may be avoided to a certain extent by improving the oven structure of gas chromatograph.View full abstractDownload PDF (1471K) -
Influence of solvent vapor in thin-layer chromatography. ITsugio TAKEUCHI, Yoshihito SUZUKI, Yutaka YAMAZAKI1970 Volume 19 Issue 7 Pages 926-931
Published: July 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSIn thin-layer chromatography (TLC) with binary solvent, solvent vapor adsorption (V. Ad.) and solvent absorption (S. Ab.) to silica gel layer have been measured by gas-chromatography.
Quantities of solvent constituents contained in 1 g of layer are as follows.
(1) Benzene-cyclohexane (8:2, v/v), (BC system)
Benzene: V. Ad.=0.32 g S. Ab.=0.89 g
Cyclohexane:=0.07 g =0.21 g
(2) Cyclohexane-acetone (7:3, v/v), (CA system)
Cyclohexane: V. Ad.=0.18 g S. Ab.=0.57 g
Acetone:=0.15 g =0.23 g
Quantities of solvent permeation by capillary action of the layer are shown approximately by the difference between S. Ab. and V. Ad.
In BC system, TLC layer absorbs benzene-cyclohexane mixture. In CA system, only cyclohexane is soaked into the layer, and pre-adsorbed acetone vapor acts as the spots carrier in TLC.
Putting the data mentioned above together with Rf values, we found a remarkable influence of solvent vapor on TLC separation with polar-nonpolar solvent. Solvent vapor gives only a minor effect on TLC with nonpolar-nonpolar solvent.
Further discussion on TLC mechanism has been given.View full abstractDownload PDF (1009K) -
Minoru OTA1970 Volume 19 Issue 7 Pages 931-935
Published: July 05, 1970
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSBoth iron and gold can be extracted with TBP from their hydrochloric acid solution and their mutual separation is achieved only by passing their TBP solution through a silicagel column without any backextraction. The distribution ratio of iron between TBP and HCl is reduced markedly by lowering the acid concentration below 4M but that of gold is not. Their mutual separation is hence carried out as follows: in a glass tube is packed 8 g of silicagel, containing, 53.8, 43.9 and 4.9% of water, respectively, and 1 ml of the TBP containing iron as tetrachloroferrate (III) and gold as tetrachloroaurate (III) is poured onto the column. Then the eluent that is pure TBP pre-equilibrated with 1M HCl is flowed down through the column. Iron is retained entirely on the column, whereas gold is eluted down in the first fraction of the effluent.View full abstractDownload PDF (846K) -
Kenji MOTOJIMA, Tadashi YAMAMOTO, Hiroshi MUTO, Yoshiharu KATO1970 Volume 19 Issue 7 Pages 935-938
Published: July 05, 1970
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSA spectrophotometric method is described for determination of thorium. In 0.3M nitric acid, thorium forms a coloured complex with carboxyarsenazo {2-(2-carboxyphenylazo)-7-(2-arsonophenylazo)-chromotropic acid}. The complex has absorption maxima at 630 and 675 mμ. The molar absorptivity at 675 mμ is ca. 3.5×104, and Beer's law holds over the range of 06.0 μg Th/ml. Zirconium interferes, but less than 1 mg of uranium or rare earth elements does not interfere with the determination of 100 μg of thorium.View full abstractDownload PDF (613K) -
Takeshi ISHII, Sôichirô MUSHA1970 Volume 19 Issue 7 Pages 938-941
Published: July 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA method for the alternating current polarographic determination of lead and zinc in commercial lubricating oil were established.
Lead and zinc in commercial lubricating oil can be determined polarographically after extracting the sample in perchloric acid-hydrochloric acid. Calibrating solutions can be prepared by dissolving commercially available lead (zinc) metals of special grade in perchloric acid-hydrochloric acid.
The alternating current polarogram in region of applied potential from 0 to -1.5 volt vs. mercury pool anode after bubbling for 15 min. with nitrogen is recorded, and lead (zinc) are determined by referring to a calibration curves.
The method is rapid and has accuracies nearly comparable to those attained by conventional ashing method.View full abstractDownload PDF (630K) -
Polarographic studies on pharmaceuticals. IITadayuki OMURA, Shukuro MORISHITA, Yoshihiko UEDA1970 Volume 19 Issue 7 Pages 941-946
Published: July 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThimerosal (sodium ethylmercurithiosalicylate), commonly used as an antiseptic and a preservative, showed a well-defined a. c. polarographic wave in 0.1M sodium perchlorate supporting electrolyte solution. Thimerosal produced two a. c. polarographic peaks, the summit potentials of which were ca. +0.07V and ca.-0.73V vs. Hg pool respectively.
A. c. wave of thimerosal seemed to have both faradaic and non-faradaic nature, and the substances, such as chlorpheniramine maleate and dibucaine hydrochloride, which are absorbed at the dropping mercury electrode stronger than thimerosal, decrease the peak height of thimerosal (Table II, Fig. 6).
A sensitive and selective a. c. polarographic method for the determination of 0.00020.003 w/v% of thimerosal in commercially available eye lotions is described.
The determination is carried out without prior separation of thimerosal and is based on standard addition method measuring the peak height at ca. -0.73V vs. Hg pool (the second peak) on the a. c. polarogram recorded with sample in 0.1M sodium perchlorate supporting electrolyte solution at pH 9.
Results, reproducible to within 1.57% coefficient of variation, were obtained on an eye lotion sample containing 0.002 w/v% of thimerosal (Table IV).View full abstractDownload PDF (1021K) -
Analytical studies on pesticides and related compounds. IAstushi MURANO1970 Volume 19 Issue 7 Pages 946-950
Published: July 05, 1970
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSA quantitative analytical method for some technical and several formulations has been developed by using thin layer chromatographic separation and ultraviolet spectrophotometry. A solution of carbamate sample was applied to silica gel plate, developed with n-hexane-ethyl acetate-formic acid (80+20+1), eluted with methanol and hydrolyzed with potassium hydroxide. The corresponding phenol produced was determined by its absorbance at maximum wavelength between 290 mμ and 300 mμ. 3, 4-Dimethylphenyl N-methylcarbamate, 3-methylphenyl N-methylcarbamate, 3, 5-dimethylphenyl N-methylcarbamate and 2-sec-butylphenyl N-methylcarbamate could be determined with standard deviation of about 0.4%.View full abstractDownload PDF (822K) -
Hidetsuru MATSUSHITA, Yoshio ESUMI, Kunio YAMADA1970 Volume 19 Issue 7 Pages 951-966
Published: July 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThis paper presents a method for the identification of polynuclear hydrocarbons in particulates suspending in urban air. The method consists of collection of suspended particulates by Hi-volume sampler, extraction of polynuclear compounds in them by means of vacuum sublimation, separation of the extract into each component by two-dimensional dual band thin-layer chromatography, solvent extraction of the each component and identification of the extracted solution by means of spectrofluorometry or spectrophotometry.
Suspended particulates from Kawasaki air were analysed by this method. The vacuum sublimation extract of the particulates was separated by the thin-layer chromatography into 76 fluorescent spots which corresponded to those of polynuclear hydrocarbons and their related compounds. Fifty-nine spots in these spots were analysed by spectrofluorometry and spectrophotometry, and 30 polynuclear hydrocarbons and 1 aza-heterocyclic hydrocarbon were identified. The identified compounds included the following 14 polynuclear hydrocarbons which were newly detected from urban air: 5, 12-dihydrotetracene, 13H-naphtho-(2, 3-b) fluorene, 11H-naphtho (2, 1-a) fluorene, indeno-(1, 2, 3-cd) pyrene, picene, tetracene, benzo (b) chrysene, tribenzo (a, c, j) tetracene, tribenzo (a, e, i) pyrene, dibenzo (a, i) pyrene, dibenzo (a, h) pyrene, benzo (g) chrysene, 1, 2, 3, 5, 6, 7-hexahydrotriangulene and naphtho-(2, 3-k) fluoranthene. It was also proved that 12 active or suspected carcinogens were included in the air pollutants.View full abstractDownload PDF (2323K) -
Masahiro TSUBOUCHI, Yuroku YAMAMOTO1970 Volume 19 Issue 7 Pages 966-971
Published: July 05, 1970
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSA new method for the determination of perchlorate ions by solvent extraction is proposed. It is found that a small amount of perchlorate ion is extracted into nitrobenzene as ion-pair formed between neutral red cation and perchlorate anion. The best extractant is nitrobenzene. The absorbance maximum of the extracted species is at 552 mμ. Perchlorate can be determined spectrophotometrically by measuring the absorbance of the extract at this wavelength.
The recommended procedure is as follows: A series of solutions is prepared by pipetting ml of 2 × 10-5M perchlorate solution, 5 ml of sodium citrate-sulfuric acid buffer solution (0.4M citrate, pH 1.9), and 5 ml of 4 × 10-4M neutral red solution into 100 ml separatory funnels. These solutions were brought to volume (25 ml) with water. After adding 10 ml of nitrobenzene to each separatory funnel, the contents were shaken for 2 min. The absorbance of the organic layer is measured at 552 mμ against the reagent blank. Beer's law is followed over the range of 1.6 × 10-68.0 × 10-6M of perchlorate in the aqueous solution, with molar absorptivity of 9.39 × 104 mole-1 cm-1 liter.View full abstractDownload PDF (1072K) -
Hiroshi NISHIDA1970 Volume 19 Issue 7 Pages 972-980
Published: July 05, 1970
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSChromazurol S (CAS, H4L) in the presence of an excess of aluminum formed AlHL with an absorption maximum at 570 mμ in the range of pH below 3, and in the presence of an excess of CAS formed AlL25- and a 1:3 complex with an absorption maximum, respectively, at 545 mμ and 585 mμ in the range of pH above 4. They had the structures in which aluminum coordinated to the phenol-carboxylate sites of CAS. As the 1:2 complex together with the 1:3 complex were formed in the presence of an excess of CAS, the calibration curve at 545 mμ did not obey Beer's law. But the 1:3 complex was exclusively formed in 3.42 × 10-4M CAS at pH 5.6 and Beer's law held for 0.020.4 ppm of aluminum. Its molar absorptivity at 585 mμ was 5.1 × 104.
The 1:1 complexes of CAS with aluminum, beryllium and scandium had the same structures, but the 1:1 complexes with transition metals such as copper, nickel and cobalt had the structures in which they coordinated to the carbonyl-carboxylate sites of CAS in acidic media.View full abstractDownload PDF (1180K) -
Takao YOTSUYANAGI, Ryuji YAMASHITA, Kazuo AOMURA1970 Volume 19 Issue 7 Pages 981-982
Published: July 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe chelates of 4-(2-pyridylazo)-resorcin with iron (II), cobalt, nickel and vanadium (V) react with quaternary ammonium salts (tetradecyl-dimethylbenzyl ammonium chloride) to form red association complexes soluble in chloroform in the presence of a large excess of polyaminocarboxylic acid (PC) such as EDTA (for Ni2+, Co2+ and Fe2+) and CDTA (for V5+). The EDTA and CDTA not only act as masking agents for interfering metals, but also increase the molar absorption coefficient, ε, of the complexes in the organic phase. The numerical value of ε varies as a function of PC concentration at [PC] <10-3M (for example, εNi2+ has a maximum value of 1.2×105 at [PC]=5×10-4M, pH=9.3, 505 mμ), however, the ε valule is constant at [PC]>10-3M (εNi2+=7.65×104 at 505 mμ; pH=9.3, εCo2+=5.9×104 at 520 mμ; pH=8.3, εFe2+=4.0×104 at 522 mμ; pH=10, εV5+=4.3×104 at 560 mμ; pH=6.8).
Based on these results, a highly selective and sensitive method for the determination of Ni2+, Co2+, Fe2+ and V5+ has been proposed. The mechanism of the increase in ε by polyaminocarboxylate is also discussed.View full abstractDownload PDF (273K) -
[in Japanese]1970 Volume 19 Issue 7 Pages 983-996
Published: July 05, 1970
Released on J-STAGE: May 29, 2009
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[in Japanese], [in Japanese], [in Japanese]1970 Volume 19 Issue 7 Pages 996-1001
Published: July 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDownload PDF (902K) -
[in Japanese]1970 Volume 19 Issue 7 Pages 1002-1009
Published: July 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDownload PDF (1662K) -
[in Japanese]1970 Volume 19 Issue 7 Pages 1010-1017
Published: July 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDownload PDF (1504K)
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