All issues
Volume 33, Issue 1
Displaying 1-26 of 26 articles from this issue
- |<
- <
- 1
- >
- >|
-
Tadao OKUTANI, Akio SAKURAGAWA, Reppei UEMATSU1984 Volume 33 Issue 1 Pages 1-5
Published: January 05, 1984
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDetermination of anion using catalytic reaction between slightly hydrolyzed zirconium oxychloride and Xylenol Orange(XO) has been studied. It was also found that a micro amount of fluoride ion was catalytically determined by the use of zirconyl peroxide instead of slightly hydrolyzed zirconium oxychloride. The zirconyl peroxide solution can be permitted to stand for two months at ordinary temperature without any appreciable change. The recommended procedures were as follows: A sample solution containing less than 10 μg of fluoride ion, 1.0 cm3 of 3.0 mol dm-3 nitric acid, 1.0 cm3 of 5.0 × 10-4 mol dm-3 XO and 1.0 cm3 of 5.0 × 10-3 mol dm-3 cetyltrimethylammonium chloride as a surfactant were placed in a 25 cm3 volumetric flask. After 1.0 cm3 of zirconyl peroxide solution (5.0×10-4 mol dm-3 in Zr (IV), 0.20 mol dm-3 in hydrogen peroxide and 0.30 mol dm-3 in nitric acid) was added to the above sample, and the mixture was diluted to 25 cm3 with water. Then, the volumetric flask was placed in a water bath at 25°C. At 60 min after the addition of the zirconyl peroxide solution, the absorbance was measured at 605 nm against water as a reference. By this method, fluoride ion ranging from 1μg to 10 μg can be determined. Sulfate, phosphate, aluminum, and iron (III) showed interferences in this method. The proposed method was applied to the determination of fluoride ion separated from water samples (river-, lake-, and sea water) by a microdiffusion method using hexamethyldisiloxane.View full abstractDownload PDF (939K) -
Hajime KARATANI, Syotaro OKA1984 Volume 33 Issue 1 Pages 6-11
Published: January 05, 1984
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAn immobilized enzymatic post-column has been developed for the liquid chromatographic determination of bile acid. 3α-hydroxysteroid dehydrogenase (3α-HSD) was adopted for the immobilized enzyme, and it was fixed onto the surface of partially fluorinated gel-like glass particulates (ca. 100 μm, dia.) which were formed by hydrolysis of silicontetraethoxide to increase the efficiency of the immobilized enzyme reaction. In order to confirm the performance of the immobilized enzyme, this column has been applied to the high performance liquid chromatographic analysis. The working principle of the analytical method is essentially the flow injection analysis with a fluorometric detector, and the reduced nicotinamideadenine dinucleotide (NADH) which is produced by the enzymatic oxidation of bile acid in the presence of NAD is determined by means of the fluorometry. Calibration curves for each bile acid were linear in the range of 2 ng to 500 ng. The detection limit was 1 ng, and the coefficient of variation was within 5 % even at the smallest amount. The well-defined forms of chromatogram were obtained, and the chromatographic peak forms of each bile acid were clearly separated. In spite of the repeated measurements as many as over three hundred times on the 500 ng-cholic acid, no change of the detection sensitivity or degradation of the activity of the immobilized 3α-HSD was observed experimentally.View full abstractDownload PDF (991K) -
Takeo ADACHI, Hideyo YOSHIDA, Kimie IZAWA, Sorin KIHARA, Hiroshi HASHI ...1984 Volume 33 Issue 1 Pages 11-15
Published: January 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSWith the addition of boric acid to a dilute hydrofluoric acid solution, the free fluoride ion concentration is reduced to about one hundredth. In hydrofluoric acid(0.1 M to 1 M)-boric acid(0.4 M to 0.65 M) media, uranium(VI) forms a cationic fluoride complex, whereas zirconium(IV) exists as an anionic fluoride complex. And the free fluoride ion concentration is kept constant as the fluoride ion is supplied by the dissociation of the fluoroborate in the media, even if a considerable amount of the free fluoride ion is consumed by the complex formation with zirconium. By these characteristics of this media, a cation exchange separation method was developed for the determination of traces of uranium in zirconium and its alloys. By the proposed method, 0.5 ppm to 10 ppm of uranium was determined with the relative standard deviation of 10 % to 5 %. Iron, tin, chromium, nickel, and other metal elements usually included in zirconium alloys as the impurity did not interfere with the determination of uranium. About 2 g of sample was dissolved in 50 ml of 2.6 M hydrofluoric acid and 0.5 ml of hydrogen peroxide solution (30 %), and then, 1.25 g of boric acid was added. After the resulting solution was transferred to a cation exchange column (10 ml of Diaion SK#1, 10 mmφ × 120 mm), 100 ml of 1 M hydrofluoric acid-0.4 M boric acid solution was passed through the column at a flow rate of 1.2 ml min-1 to elute zirconium from the column. The remained uranium in the column was eluted by 50 ml of 1 M hydrofluoric acid solution. In order to remove the accompanying traces of zirconium, 1.25 g of boric acid was added to the effluent and the resulting solution was transferred to another cation exchange column (5 ml of Diaion SK #1). Then the separation procedure mentioned above was repeated. Uranium was determined by Arsenazo III spectrophotometry in 5 M perchloric acid after the effluent was evaporated to dryness.View full abstractDownload PDF (835K) -
Soei SATO, Hironobu OHSHIRO, Shigeyuki TANAKA1984 Volume 33 Issue 1 Pages 16-22
Published: January 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSSeparation behavior and composition analysis of organophosphorus compounds, which were used as additives for plastics and lubricating oil, was examined by gel permeation chromatography (GPC). Thirty three kinds of organophosphorus compounds such as orthophosphoric acid triesters, phosphorous acid di, triesters and diethyl phosphonic acid derivatives having alkyl and aryl groups as lipophilic moieties were used in this experiment. The correlation between the elution volume (Ve) and their molecular weight (Mw), molecular volume(Mv), and chemical structures of these compounds were discussed. The experiment was carried out using a model LC-07( Japan Anal. Ind. Co.) equipped with UV (254 nm) and RI detector. The GPC condition was as follows; column: 120 cm × 20 mm I. D. stainless steel column packed with JAI Gel lH (styrene-divinyl benzene copolymer, pore size 25 Å), eluent: CHCl3, flow rate: 3 ml/min. It was found that the elution volume of these compounds were closely related to their Mw, Mv, and chemical structures as follows: (1) In the case of aliphatic homologue compounds, the relation between the elution volume and logarithmic values of Mw or Mv were shown to be linear. (2) The elution volumes of organophosphorus compounds substituted with phenyl group or halogen atoms were greater than those of original compounds which have similar molecular structures. (3) Phosphorous acid triesters, especially having short alkyl chain, were partially decomposed to the diesters during the GPC process. Therefore, the elution volumes of organophosphorus compounds were influenced by the molecular weight, the molecular size including molecular forms, and the interaction with stationary phase gel. This method was applied to the composition analysis of organophosphorus compounds used as plastic additives, and satisfactory results were obtained.View full abstractDownload PDF (1148K) -
Yukio NAGAOSA, Toshikazu SANA1984 Volume 33 Issue 1 Pages 22-26
Published: January 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn anodic stripping voltammetric technique was developed for the determination of antimony(III) and (V) of the ng/ml and sub-ng/ml levels in the mining waste water. Both antimonies were extracted with acetonitrile by salting-out. The antimony gave a sharp stripping peak at -0.22 V vs. Ag/AgCl in the acetonitrile extract under the experimental conditions and was determined in the presence of 5000-fold excess copper(II). To an aliquot of solution containing antimony(III) and (V), 2.0 ml of ca. 12 N HCl was added and the total volume was made up to 10.0 ml with water (final acidity: 2.0 N HCl). The antimony was then extracted into the acetonitrile phase by adding 14.0 ml of 0.1 M tetrabutylammonium perchlorate solution in acetonitrile and 2.0 g of sodium chloride (Wako Junyaku). An 8.0 ml of the extract was transferred into an electrolytic cell and deoxygenated with nitrogen for 3 min. The deposition was carried out for 3 min at -0.35 V vs. Ag/AgCl. After 30 s, the differential pulse anodic stripping curves were recorded under a scan rate of 0.5 mV s-1 and a pulse amplitude of 10 mV. The peak height of the stripping curve at -0.22 V was proportional to the concentration prior to electrolysis of antimony(III) or (V) in the range of 0.2 ng/ml to 20 ng/ml. The lower limit of determination was 0.1 ng/ml at a deposition time of 10 min. The coefficient of variation was ca. 10 % for the ten replicate determinations of 1.0 ng/ml antimony (III) or (V). The effect of foreign ions on the determination of 5.0 ng/ml antimony(III) and 5.0 ng/ml antimony(V) was investigated(Table 1). The proposed method was applied to the determination of total concentration of antimony(III) and (V) in sodium chloride (Merck) and in the mining waste water (Nakatatsu).View full abstractDownload PDF (811K) -
Hiroshi TOKUNAGA, Toshio KIMURA, Jiro KAWAMURA1984 Volume 33 Issue 1 Pages 26-30
Published: January 05, 1984
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA determination of dihydroergotamine (DE) was established by high-performance liquid chromatography on a LiChrosorb RP-18 column maintained at 35°C using a mixture of acetonitrile and 0.1 M acetate buffer (pH 5.0) (45:55) containing 3 mM triethylamine. This method was applied to the assay and content uniformity test of DE methanesulfonate (DEM) tablets. The assay procedures were as follows; Twenty tablets were powdered and a portion of the powder containing 1 mg of DEM was placed in a glass-stoppered centrifuge tube. After adding 5.0 ml of 20 % methanol with 1 % tartaric acid, the tube was ultrasonicated for 10 min, then centrifuged at 3000 rpm. One ml of supernatant solution was mixed with 1.0 ml of 17α-hydroxyprogesterone solution (0.05 mg/ml) as internal standard in 70 % methanol with 1 % tartaric acid. A 20 μl aliquot was injected onto the column and the peak heights were measured. In the case of the content uniformity test, one tablet was placed in a glass-stoppered centrifuge tube, then treated as proposed assay procedures. The analytical values in 3 commercial tablets were 102.0 %, 103.0 %, and 108.1 %, respectively, and the averages of contents of each 10 tablet obtained by the content uniformity test were 104.9 %, 105.0 %, and 108.1 %, respectively. The method was also applied to the stability of DE (0.2 mg/ml) in 1 % tartaric acid solution. DE was very stable under irradiation with incandescent light of 30000 luces for 3 h. Heating at (80100)°C for 06 h, the degradation of DE follwed pseudo-first-order kinetics until (4060)% of residual concentration and the activation energy was 19.8 kcal/mol degree.View full abstractDownload PDF (742K) -
Shoji MOTOMIZU1984 Volume 33 Issue 1 Pages 31-36
Published: January 05, 1984
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSExtraction constant, Kex, for the chloroform extraction of ion associates from aqueous solution was divided into two parameters, C and A, assigned to the cation and the anion, respectively: logKex=C+A. In estimating the values of C or A for various ions, a hypothetical cation, -_??_-+ (long-chain alkyltrimethylammonium type), with no alkyl groups nor hydrogen atoms was chosen as a reference ion for which C=0. C value for long-chain alkyltrimethylammonium cations can be calculated from C=0.59n, where n is the number of carbons and 0.59 is the value of πCH2, contribution constant of methylene group to extraction constant. C values for other alkylammonium ions were determined experimentally and compared with those calculated on the assumption of additivity of contribution constants of functional groups. C values for other cationic groups were as follows: -1.20 for -_??_-+ (symmetrical tetraalkylammonium type), -0.56 for >-NH3+ 0.40 for NH2+, 1.29 for →NH+, 4.72 for -NH+, 7.53 for -+N-N=N-N(C2H5)2, and 10.74 for C(C6H4-)3+, respectively. By using these C values, A values for inorganic and organic anions were determined. A values for inorganic anions were as follows: -11.06 for F-, -9.07 for OH-, -8.11 for NO2-, -8.08 for Cl-, -7.05 for NO3-, -6.89 for Br-, -5.80 for BF4-, -5.32 for I-, -5.17 for SCN-, -5.03 for ClO4-, and -4.45 for ReO4-, respectively. A values for anionic groups were as follows: -9.08 for -SO3-, -10.73 for -COO-, and -7.38 for -OSO3-, respectively. By using the values of C and A, the extraction constants (logKex) for ion associate (C+·A-) were estimated and compared with those obtained experimentally. The differences between them were smaller than ±0.3 log unit.View full abstractDownload PDF (1042K) -
Masahiro KOMATSU, Minoru NAKAMIZO1984 Volume 33 Issue 1 Pages 37-43
Published: January 05, 1984
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAn infrared spectroscopic method was applied to the analysis of different types of organic sulfides in petroleum vacuum residue. Although sulfides have no characteristic infrared absorption band, their oxidized compounds, sulfones, show two strong absorptions associated with S=O stretching vibration in the (13001100) cm-1 region. The vibrational frequencies of S=O stretching modes are strongly dependent upon the chemical structure of the parent sulfides from which the sulfones are derived. The S=O absorption bands of aromatic sulfones appear near 1150 cm-1 and 1300 cm-1. On the other hand, the corresponding S=O absorptions for aliphatic sulfones occur at frequencies lower than those for aromatic sulfones and show a decrease in frequency with an increase in the number of carbon atom of alkyl group bonded with sulfur. The results obtained for these model compounds of sulfones were applied to the analysis of sulfides in the pyrolysis products of Khafji vacuum residue. Cracked oils obtained from the residues showed strong absorption bands at (11151120) cm-1, (11451150) cm-1, and (12981305) cm-1when oxidized with hydrogen peroxide and acetic acid, suggesting the presence of sulfur compounds with chemical structure of =_??_-S-_??_=, in addition to alkylarylsulfide, diarylsulfide or thiophene type sulfide. On the other hand, asphalt pitches showed two strong absorption bands at (11451150) cm-1 and (12951300) cm-1 when oxidized, suggesting the presence of alkylarylsulfide, diarylsulfide or thiophene type sulfide.View full abstractDownload PDF (1010K) -
Haruo TSUJI, Kimio NISHIMURA, Yuzo TAMARI, Yuzuru KUSAKA1984 Volume 33 Issue 1 Pages 43-48
Published: January 05, 1984
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSArsenic(III) and arsenic(V) in groundwaters at ppb levels are determined by a spectrophotometric method with silver diethyldithiocarbamate (SDDC), after preconcentration by means of coprecipitation with zirconium hydroxide, and sequential generation of arsine with sodium tetrahydroborate by pH adjustment of sample solution. Three milli liters of 3.53 % zirconium oxychloride solution (30 mg as Zr) is added to 1000 ml of sample solution containing (0.510)μg of arsenic, then the solution is adjusted to pH 9 with aqueous ammonia. After standing for a while, the precipitate is collected by centrifuging, dissolved in 1 ml of 6 N hydrochloric acid solution, and transferred to a reaction vessel. Then 5 ml of 25 % tartaric acid solution is added, and the solution is adjusted to pH 6 with aqueous ammonia. The solution is diluted to about 50 ml with water, and 2 ml of Tris buffer solution is addeed to the vessel. Into the reaction vessel, 3 ml of 4 % sodium tetrahydroborate solution is injected from a funnel, and argon is bubbled at the flow-rate of (60100) ml min-1 for 20 min. Arsine generated from arsenic(III) is trapped in a SDDC solution (1). Hence 5 ml of 6 N hydrochloric acid is added to the vessel to bring the pH of the solution to 01. Three milliliters of 4 % sodium tetrahydroborate solution is injected and argon is bubbled for 15 min to generate arsine from arsenic (V). Arsine is trapped in another fresh SDDC solution (2). The concentrations of arsenic in both SDDC solutions (1) and (2) are determined by spectrophotometry at 540 nm. The recoveries of arsenic (III) and arsenic (V) are quantitative and thier coefficients of variation are about 5 % ranging (2.0 10.0)μg of arsenic, and the detection limit of arsenic is about 0.5μg. This method is rapid and convenient for the determination of trace amounts of inorganic arsenic species in groundwaters.View full abstractDownload PDF (1088K) -
Chozo YOSHIMURA, Takayosi HUJINO1984 Volume 33 Issue 1 Pages 48-53
Published: January 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSNonaqueous conductometric titration of molybdenum in a lubricating oil was carried out by using N, N-dimethylformamide(DMF)-acid adduct as a titrant. The adduct was obtained by the reaction of hexafluorosilicic acid with DMF. Direct titration of ammonium molybdate with the adduct(H2SiF6-3DMF) in DMF was investigated by conductometric and photometric methods. The molar ratio of molybdenum(VI) and H2SiF6 at inflection points were found to be 2:1 and 1:1 by conductometric and 2:1 by photometric method, respectively. The reaction ratios were not influenced by water content of less than 1 percent. For an application of this method molybdenum in a lubricating oil was determined by the method after dissolving it in a mixture of DMSO-HNO3 and DMF-SO3 adducts. Molybdenum compound in organic substance soluble in organic solvents was found to be determined more rapidly by the proposed method as compared with the conventional method.View full abstractDownload PDF (916K) -
Hideo IMAI, Hisanobu YOSHIDA, Tsutomu MASUJIMA, Takuji OWA1984 Volume 33 Issue 1 Pages 54-57
Published: January 05, 1984
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDetermination of indole derivatives in aqueous solution was investigated by a flow injection method with chemiluminescence detection. It was found that indole derivatives oxidized beforehand by heating with potassium peroxodisulfate emitted light on mixing with 1, 3-dibromo-5, 5-dimethylhydantoin solution. The reaction was made to proceed in a flow injection system, and the chemiluminescence intensity was measured by a photon counter PM tube placed in front of the mixing cell with spiral channel. The optimum conditions selected were as follows; the concentration of potassium peroxodisulfate was 4.0 % (w/v), that of 1, 3-dibromo-5, 5-dimethylhydantoin was 0.7 % (w/v) in 0.1 N NaOH solution, and the optimum temperature of the oxidation reaction was 40 °C at the flow rate of 2.0 ml/min in a reaction coil of 1 mm i.d. and 6 m length. The linear range of the determination was (0.103.10) nmol with C.V. value of 1.8 % (within-run at 0.78 nmol) for tryptophan and (0.103.10) nmol with C.V. value of 3.4 % (within-run at 0.78 nmol) for tryptamine.View full abstractDownload PDF (614K) -
Shinya YAMAMOTO, Tadao OHTA, Yoshihiro MORIKAWA, Michio YOKOUCHI1984 Volume 33 Issue 1 Pages 58-62
Published: January 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSElectrophoretic behavior of sodium alginate (SA) has been studied to extend the application of capillary tube isotachophoresis in the polymer field. The weight average molecular weights of five specimens of SA ranged from 2.16 × 105 to 3.79 × 105. The delay of electrophoretic mobilities which had been proposed by the authors was confirmed with SA. The difference of the delay depending on the molecular weight of SA samples was also observed, though the difference of molecular weight was small compared with the case of sodium hyaluronate. The delay caused by 4 μg to 6.5 μg of samples was dependent on molecular weight, but not comparatively on sample size. The measurement of the electrophoretic delay have provided an information on the molecular weight of polyelectrolyte. In particular, this method is more useful for the high molecular weight of polyelectrolyte which elute in the exclusion limit in GPC. It was found that the precipitated SA moved to the anode in the leading electrolyte containing 40 % acetone and that the other ion moved with the same speed according to the Kohlrausch principle.View full abstractDownload PDF (620K) -
Shin-ichiro OKAWA, Bunshiro KOMINAMI, Akira KAWASE1984 Volume 33 Issue 1 Pages 63-65
Published: January 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS1-(2-Pyridylazo)-2-naphthol (PAN) reacts with zinc in an aqueous solution in the presence of a non-ionic surfactant, Brij 35, to form a soluble complex. The optimum condition for the EDTA titration of zinc with PAN indicator were studied. The formation constants of zinc-PAN chelate, and the acid dissociation constants of PAN in the presence of surface-active agent were investigated at 0.1 mo1/l (NaClO4) ionic strength and at 30 °C. The observed pH range to obtain sharp color change was decreased by pH 0.5 from calculated value by using the formation constants of zinc-EDTA chelate in the aqueous solution. The proposed procedure is as follows :To a sample solution containing of zinc (654 μg), add 20 ml of acetic acid-sodium acetate buffer (pH 6.3), 1 ml of Brij 35(0.1 g/ml) solution and 0.2 ml of PAN(10-3 mol/l), and then titrate with EDTA (10-2 mol/1).View full abstractDownload PDF (511K) -
Seiichiro HIGUCHI, Zegen ZHENG, Shigeyuki TANAKA1984 Volume 33 Issue 1 Pages 65-68
Published: January 05, 1984
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe microanalytical application of preresonance Raman effect has been examined for nitrobenzene and some para-substituted nitrobenzenes {p-OH, p-NH2, p-NHCH3, p-N(CH3)2}. The wavelengths of the maximum absorptions of UV bands of the samples are from 260 nm to 395 nm, and the wavelength of the excitation laser line is 488.0 nm. Under this condition, the detection limits of the samples by Raman spectrometry have been determined, using the NO2 symmetric stretching vibration band. Though, as is expected, the detection limit becomes lower in an orderly fashion as the wavelength of UV absorptions of samples approaches to that of the excitation source, it can roughly be said that it is about 10-6 M (from several hundreds to several tens ppb). This sensitivity is about two orders of magnitude lower, when compared with that for azo dye samples, for which the resonance condition is much more rigorous (the wavelength of the maximum absorption is about 500 nm). For all that, it can be concluded that the results obtained here give an useful guide in the microanalytical applications of Raman spectrometry to practical samples such as polycyclic aromatic nitrocompounds as air pollutants.View full abstractDownload PDF (770K) -
Binary mixture of crude oilsKunishige HIGASHI, Kazuyoshi HAGIWARA1984 Volume 33 Issue 1 Pages 68-70
Published: January 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn effect of mixing of two kinds of crude oils on a discrimination of the oils was studied by the pattern similarity method. A chromatogram was obtained by high performance gel permeation chromatography with ultraviolet absorption detector. Model chromatograms were calculated by mixing both section areas of chromatograms of the two oils. This model method was adopted to the discrimination of binary mixtures on fifteen crude oils. When the content of main component decreased, ratio of chromatograms which were discriminated as the crude oil of main component decreased.View full abstractDownload PDF (430K) -
1984 Volume 33 Issue 1 Pages e1a
Published: 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (60K) -
Yu YOKOYAMA, Mitsuru KOSUGI, Hisashi KANDA, Masaaki OZASA, Kazunori HO ...1984 Volume 33 Issue 1 Pages E1-E7
Published: January 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSPhotoacoustic signal intensities were measured at v3 band of sulfate ion on powdered sulfate/NaCl mixtures of a variety of particle sizes and sulfate compositions. It was found that (1) the slope of the calibration curves for potassium aluminum sulfate dodecahydrate was the steepest, then the next for calcium sulfate dihydrate, and the least for potassium sulfate, and that (2) the slope increased with decreasing particle size for sulfate compounds except for calcium sulfate dihydrate. The first result was shown to reflect the difference in molar concentration of sulfate ion in sulfate crystal, and the second result to come from the difference in crystal form among sulfate compounds.View full abstractDownload PDF (794K) -
Susumu NAKASHIMA, Masakazu YAGI1984 Volume 33 Issue 1 Pages T1-T3
Published: January 05, 1984
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA rapid and precise method has been developed for the determination of arsenic in natural waters, by employing flotation separation technique. The recommended procedures are as follows: Immediately after sampling, add 10 ml of hydrochloric acid per liter. Take one liter of sample (500 ml as for sea water sample) in a beaker and add 2 ml of iron(III) solution (5 mg/ml). Adjust the pH to 8.08.5 with aqueous ammonia solution to precipitate the iron(III) hydroxide and stir the solution for 15 min. Add 1 ml (2 ml for sea water) of sodium dodecyl sulfate solution (1 mg/ml in 99.5 % ethanol) and 1 ml of sodium oleate solution (1 mg/ml in 99.5% ethanol). Transfer the whole content of the beaker to a flotation cell with a filter (Millipore membrane filter: 0.45μm inpore size, 47 mm diameter) at the bottom. Pass air at 20 ml/min through a bubbler (No. 4-sintered glass disk) for about 2 min. Drain most of the mother liquor through the side arm of the cell and suck off the mother liquor completely through the filter. Rinse the precipitate with 30 ml of water and dissolve with 8 ml of 6 M hydrochloric acid. Collect the filtrate into a 20-ml calibrated flask, add the washings to the flask and dilute to 18 ml with water. Add 1 ml of KI solution (20 % w/v) and make up to 20 ml with water. The arsenic content was determined by atomic absorption spectrometry as arsine generated with NaBH4. Good agreements in the arsenic contents were obtained irrespective of whether the samples were pre-filtered through 0.45-μm Millipore filters, not.View full abstractDownload PDF (436K) -
Tatsuhiko TANAKA, Hiromi HASEGAWA, Kazuyoshi OISHI, Takayoshi YOSHIMOR ...1984 Volume 33 Issue 1 Pages E9-E15
Published: January 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSGallium(III) and indium(III) were determined precisely by coulometric complexometric titration. The ions were allowed to react with an excess EDTA of known purity, and the excess part of the reagent was back-titrated with zinc ion generated electrolytically from an amalgamated zinc anode. The results of the purity measurements of commercial high-purity gallium and indium metals (both nominally 5-nine) were 99.997 and 99.997%, with standard deviations of 0.003 and 0.009%, respectively. The proposed methods may be applicable to the evaluation of stoichiometric composition of the compound semiconductors such as gallium arsenide, indium phosphide, etc.View full abstractDownload PDF (753K) -
Chaman Lal SETHI, Bal Krishan PURI, Masatada SATAKE1984 Volume 33 Issue 1 Pages E17-E21
Published: January 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA new method has been proposed for the atomic absorption spectrophotometric determination of zinc, cadmium and lead after coprecipitation of their morpholine-4-carbodithioate complexes with microcrystalline naphthalene. They are easily coprecipitated over the pH range, Zn:3.7-9.4, Cd:3.3-11.0 and Pb:5.4-10.2. The compound coprecipitated with solid naphthalene is separated by filtration, dissolved in 2M nitric acid and made up to 25 ml with nitric acid. The metals are determined by measuring absorbance at 213.9, 228.8 and 217.0 nm for zinc, cadmium and lead respectively. Beer's law is obeyed up to Zn:23 μg, Cd:45 μg and Pb:200 μg per 25 ml of the final solution. Ten replicate determinations of a sample solution containing, Zn:10 μg, Cd:20 μg or Pb:50 μg gave mean absorbances of 0.105, 0.095 and 0.053 with relative standard deviations of 1.42, 1.57 and 2.20% respectively. The developed method has been applied to the determination of these metals in some standard samples.
Morpholine-4-carbodithioate has been used for the spectrophotometric and volumetric determination of some metal ions by a number of workers. Recently some gravimetric, thin layer and paper chromatographic separation of some metals with this reagent have been reported. In the present communication a simple atomic absorption spectrophotometric method has been developed for the determination of zinc, cadmium and lead using morpholine-4-carbodithioate as the complexing agent after coprecipitation of their complexes with microcrystalline naphthalene. The method is found to be sensitive in comparison to the extraction into molten naphthalene spectrophotometric method.View full abstractDownload PDF (477K) -
Yoshiaki ONOUE, Kiyotoshi MORISHIGE, Keizo HIRAKI, Yasuharu NISHIKAWA1984 Volume 33 Issue 1 Pages E23-E28
Published: January 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThermally activated delayed fluorometry (TADF) was applied to the trace analysis of zinc by using meso-tetraphenylporphinetri-sulfonic acid (TPPS3). Metalation of TPPS3 with zinc ion was accomplished in 0.5 mol dm-3 sodium hydroxide solution at 60°C for 30 min. After cooling the solution, the product was adsorbed on filter paper by dipping the paper in the reaction mixture. The TADF intensity of Zn-TPPS3 adsorbed on the filter paper which was dried at 60°C for 30 min was measured. A linear relationship between zinc concentration and TADF intensity was recognized in the wide range of 1 ppb to 162 ppb. The effects of foreign metal ions, Cd(II), Fe(III), Cr(III), Pb(II), In(III), Sn(II), Cu(II) and Ni(II), which are typical interfering metals on the determination of zinc by fluorometry and absorption spectroscopy, were studied, and it was found that twenty three fold amount of Cd(II) and forty six-fold amounts of Fe(III), Cr(III), Pb(II), In(III), Sn(II), Cu(II) and Ni(II) did not interfere with the determination of zinc.View full abstractDownload PDF (627K) -
Kazuo KUGA, Shizunori OOYU, Eiichi KITAZUME, Kanji TSUJII1984 Volume 33 Issue 1 Pages E29-E32
Published: January 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe semiconductor silicon surface is etched by mixed-acid (HF, HNO3, CH3COOH) solution and gallium in the etched solution is determined by graphite furnace atomic absorption spectrometry using a zirconium impregnated graphite tube. The depth of the silicon layer was ascertained by determination of the silicon content in the etched solution by inductively-coupled plasma atomic emission spectrometry. This method permits determination of gallium up to 1016 atoms in 200 nm sections of silicon slice with a diameter of 2.5 cm.View full abstractDownload PDF (395K) -
Yoshimi KITADA, Kikuo TAMASE, Munehiko MIZOBUCHI, Michiko SASAKI, Kaor ...1984 Volume 33 Issue 1 Pages E33-E35
Published: January 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple and rapid determination of tert-butylhydroquinone(TBHQ) in vegetable oils, butter, and margarine by using high-performance liquid chromatography(HPLC) is described. TBHQ was effectively separated, identified, and quantitated on LiChrosorb NH2 with hexaneethanol eluent. Detection was done at UV 293nm with 0.04AUFS.
p-Aminoacetophenone was used as an internal standard. The recovery of TBHQ added to oily foods was between 93.1-99.5% in the range of 100ppm of TBHQ.View full abstractDownload PDF (297K) -
Sunao YAMADA, Atsushi HINO, Teiichiro OGAWA1984 Volume 33 Issue 1 Pages E37-E40
Published: January 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn application of a double-beam method to a detector for liquid chromatography has achieved better detectability than the case of a single-beam method. The detection limit of pyrene in hexane was 2 pg.View full abstractDownload PDF (409K) -
EVALUATION OF ZERO OUTPUTShizuo FUJIWARA, Isao SAKAMA1984 Volume 33 Issue 1 Pages E41-E42
Published: January 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA novel method is proposed which allows the accumulation of the constant output of instrumental analyses. It will be useful for the identification of the nature of the zero output whether the latter is due to the absence of the objective substance or to the insufficient sensitivity of the instrument.View full abstractDownload PDF (217K) -
YUKIKAZU HATTORI, YOSHIO KUGE, MASAO NAKAMOTO1984 Volume 33 Issue 1 Pages E43-E46
Published: January 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn analytical procedure was described for the determination of tripropyltin chloride(TPTC) in the environmental water and sediment. TPTC was extracted into hexane with hydrochloric acid from water sample, and into methanolic hydrochloric acid from sediment sample and converted into hexane. After cleaning up of the extract by the aluminium oxide column with phosphoric acid, TPTC was measured by gas chromatograph with an electron-capture detector. Recoveries of TPTC were 90 to 97 % from water samples and 89 % from sediment samples. The detection limits were 0.30 μg/l in water and 0.015 μg/g in sediment samples.View full abstractDownload PDF (342K)
- |<
- <
- 1
- >
- >|