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Keihei UENO
1986 年 2 巻 1 号 p.
1
発行日: 1986年
公開日: 2007/07/27
ジャーナル
フリー
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Genya CHIBA
1986 年 2 巻 1 号 p.
2
発行日: 1986年
公開日: 2007/07/27
ジャーナル
フリー
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Kozo MATSUMOTO, Shin TSUGE, Yukio HIRATA
1986 年 2 巻 1 号 p.
3-7
発行日: 1986年
公開日: 2006/06/23
ジャーナル
フリー
Supercritical fluid chromatograph (SFC) with a fused silica separation column (0.5mm I.D.×70cm) packed with ODS-Q3 (30-50μm) was directly coupled with a quadrupole mass spectrometer (MS) through a vacuum nebulizing interface originally developed for the combination of high performance liquid chromathograph (HPLC) with MS. Mixtures of hexane and ethanol were used as the mobile phase for SFC at a flow rate of 40μl/min (50kg/cm
2). The column temperatures were maintained above the critical ones of the mobile phase between 260 and 280°C. Introduction of line filters to remove possible small particles in the SFC effluent and the subtle control of the optimum flow and/or the pressure for the SFC column enabled fairly long term stable operation for this SFC-MS system. Thus developed new system was successfully applied to the analysis of various samples such as styrene oligomers, phthalates, triglycerides, and polyethylene glycol derivatives.
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Kazuo IMAEDA, Keiko OHSAWA, Katsumi UCHIYAMA, Shigeru NAKAMURA, Tsunem ...
1986 年 2 巻 1 号 p.
9-13
発行日: 1986年
公開日: 2006/06/23
ジャーナル
フリー
A photoacoustic cell which can accommodate a thin-layer plate of 26×76mm is described. A high-power light emitting diode was used as a visible light source to scan the plate surface to obtain a densitogram of each material. Protein dissolved in a 2M NaCl solution was spotted onto the thin-layer plate; staining with amidoblack 10B followed. The protein (
e.g. bovine serum albumin, hemoglobin, myoglobin) spotted onto slica-gel thin-layer plate was determined using the apparatus. The detection limit of bovine serum albumin stained with amidoblack 10B was about 25ng, with a signal/noise ratio of 2. A densitogram of rat serum protein seperated with polyacrylamide gel electrophoresis was obtained by use of the apparatus.
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T. GARAI, Z. NAGY, F. FAGIOLI, C. LOCATELLI
1986 年 2 巻 1 号 p.
15-19
発行日: 1986年
公開日: 2006/06/23
ジャーナル
フリー
A relationship was derived for the resolution of differential pulse polarography as a function of the pulse amplitude and various parameters of the electrode reaction of the simultaneously present components(number of electrons exchanged in the electrode reaction, half-wave potentials). The resolution was found to be higher at small pulse amplitudes and large difference in the half-wave potentials. Resolution is higher when the number of electrons involved in the electrode reaction of both the measured and the interfering species are larger and it is mainly affected by the latter. The resolution of differential pulse polarography was found to be inferior to that of fundamental harmonic and second harmonic a.c. polarography.
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Masashi HOJO, Yoshihiko IMAI
1986 年 2 巻 1 号 p.
21-23
発行日: 1986年
公開日: 2006/06/23
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フリー
A new anodic wave in polarography other than the original anodic wave or waves from each acyclic polyamine (ethylenediamine to tetraethylenepentamine) appeared by the addition of HClO
4 or
p-toluenesulfonic acid. Successive cathodic waves were given by the conjugate acids from a polyamine. A good linearity was observed between
E1/2 of the conjugate acids and the protonation constants of a polyamine (diethylenetriamine, triethylenetetramine, tetraethylenepentamine), except the first protonation step.
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Toshio SUZKI, Hiroyuki OZAKI, Kiyoshi SAWADA
1986 年 2 巻 1 号 p.
25-29
発行日: 1986年
公開日: 2006/06/23
ジャーナル
フリー
A method based on solvent extraction with capriquat(trioctyl methylammonium chloride) and subsequent graphite furnace atomic absorption spectrometry of antimony has been described. Antimony(III) and antimony(V) are quantitatively extracted with 1%(w/v) capriquat in xylene from 0.1M potassium iodide and 0.5M sulfuric acid solution. The presence of chloride, sulfate, nitrate and perchlorate ions does not interfere with the extraction of antimony. A 20 μl aliquot of the organic phase containing antimony was injected into the carbon tube in the graphite furnace atomizer and the optimum conditions of ashing and atomizing were studied. The addition of copper(II) ion and ascorbic acid gave an excellent lineality for the calibration curve and better sensitivity for the determination of antimony. The present method has been applied to the determination of antimony in NBS SRM 1571, Orchard Leaves. The result obtained agreed well with the certified value.
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Tetsu KUMAGAI, Katsuya UESUGI, Masakazu MATSUI
1986 年 2 巻 1 号 p.
31-35
発行日: 1986年
公開日: 2006/06/23
ジャーナル
フリー
The cation exchange method has been used to investigate the distribution equilibria between zinc bromide or zinc iodide complexes and the resin in aqueous acetone solutions. Formation constants of zinc bromide or iodide have been calculated from the distribution coefficients of zinc in aqueous acetone solutions containing 10, 20 and 30v/v% water. In 10v/v% aqueous acetone, β
Br1=4.98, β
Br2=8.81 and β
Br3=11.55 for zinc bromide, β
l1=3.97, β
l2=5.55 and β
l3=7.71 for zinc iodide, and in 20v/v% aqueous acetone β
Br1=3.77, β
Br2=5.97, β
Br3=7.61, for zinc bromide and β
l1=2.61, β
l2=4.14 for zinc iodide, and in 30 v/v% aqueous acetone, β
Br1=2.33 and β
Br2=4.07 for zinc bromide.
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Shiro GOHDA, Hideo YAMAZAKI, Tsunenobu SHIGEMATSU
1986 年 2 巻 1 号 p.
37-42
発行日: 1986年
公開日: 2006/06/23
ジャーナル
フリー
A rapid, sensitive and selective method is described for the determination of molybdenum in natural waters and environmental materials by polarized Zeeman atomic absorption spectrometry with a pyrolytic graphite-coated graphite furnace. For the separation and concentration of trace amounts of molybdenum(VI ), the extraction behavior of molybdenum(VI)-8-quinolinolate complex with diisobutyl ketone(DIBK) was investigated. The high extractability of molybdenum with DIBK allows molybdenum to be concentrated about 200fold or more with a single extraction at pH 3.5. The molybdenum absorbance was measured at the wavelength of 313.3nm by using 20mm
3 of organic phase. The optimum conditions obtained at heating stages were as follows: drying for 30s programmed from 1.50 to 200°C, charring at 500°C for 30s, atomizing at 2800°C for 15s and cleaning at 2900°C for 10s. The detection limit, defined as twice the standard deviation of the blank value, was found to be 0.05ng of molybdenum and the relative standard deviation was 1.5% for 2ng of molybdenum. Interferences of many metal ions can be effectively reduced by masking with EDTA and sodium fluoride.
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Yasoo ITOH, Hiroshi KAWAMOTO, Hideo AKAIWA
1986 年 2 巻 1 号 p.
43-46
発行日: 1986年
公開日: 2006/06/23
ジャーナル
フリー
A simple preconcentration method for cobalt(II) in natural waters based on synergistic extraction is proposed. Cobalt(II) is extracted as the ternary complex, Co(II)-dithizone-tributylphosphine oxide, from 300cm
3 of a water sample into 3cm
3 of carbon tetrachloride at pH 5. The method was applied to a river water sample. Using this method, cobalt(II) in natural waters with levels below μg dm
-3 range could be determined by the atomic absorption spectrometry, an aliquot of the organic extract being injected into a graphite furnace.
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Shigeya SATO, Sumio UCHIKAWA
1986 年 2 巻 1 号 p.
47-51
発行日: 1986年
公開日: 2006/06/23
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フリー
A very simple and sensitive method for the extraction-spectrophotometric determination of antimony(V) and (III) was developed. It was found that antimony(V) reacts with 2-hydroxyisocaproic acid in weak acidic aqueous solution on heating for 15min at 45°C and that the complex anion formed can be extracted into chlorobenzene with Malachite Green. Antimony(III) reacts quickly irrespective of the temperature. However, the Sb(III)-complex anion formed can not be extracted in the presence of citrate, whereas Sb(V)-complex anion can be extracted and determined under the same condition. This significant difference in reactivity between citrate and these two species was applied to the differential determination of antimony(III) and antimony(V). The calibration graph was linear over the range 0.19-11.5μg for antimony(V), and 0.15-8.1μg for antimony(III).
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Isao YOSHIDA, Ryo'ichi TAKESHITA, Keihei UENO, Makoto TAKAGI
1986 年 2 巻 1 号 p.
53-56
発行日: 1986年
公開日: 2006/06/23
ジャーナル
フリー
Solvent extraction of lanthanoid and yttrium ions(M
3+) was investigated in a water-dichloroethane system using poly(oxyethylene)-type nonionic surfactants such as Triton X-100 and Triton X-405(L) and picrate ion(A
-) as extraction agent and pairing anion, respectively. The result of extraction studies at various extraction agent concentrations and at various picrate ion concentrations, suggested that the composition of the extracted species was MLA
3. Among the lanthanoid ions investigated, the ions such as Nd
3+, Sm
3+, Eu
3+, and Gd
3+ gave relatively larger distribution ratios than the other lanthanoid ions, while the yttrium ion was the least extractable among the metal ions investigated. The distribution ratio with extraction agent Triton X-405 was about ten times larger than those with Triton X-100.
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Susumu OSAKI, Yasuhiro KUROKI, Naoshi MANNEN, Yoshimasa TAKASHIMA
1986 年 2 巻 1 号 p.
57-60
発行日: 1986年
公開日: 2006/06/23
ジャーナル
フリー
The reactive iron contents of fresh water samples filtered with membrane and ultrafiltration filters were determined by an isotope dilution method using the solvent extraction of 4, 7-diphenyl-1, 10-phenanthroline(bathophenanthroline)- Fe complex into 3-methyl-1-butanol (isoamyl alcohol). The total iron contents were determined in the same manner after digestion and dissolution with perchloric acid and hydrofluoric acid. Only small amounts of reactive iron were found in water samples collected upstream, at the reservoir and underground. It is noted that almost all iron in these water samples is present as stable forms. Considerable amounts of reactive iron were found in downstream water, especially as surface species on particulates larger than 5μm.
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Shigenori NAKANO, Chisato YAMADA, Masahiko SAKAI, Takuji KAWASHIMA
1986 年 2 巻 1 号 p.
61-65
発行日: 1986年
公開日: 2006/06/23
ジャーナル
フリー
A catalytic photometric method for determining a nanogram level of vanadium(IV) and vanadium(V) is proposed. The method is based on their catalytic effect on the oxidative coupling reaction of 4-aminoantipyrine with
N,
N-dimethylaniline in the presence of bromate and sulfosalycilic acid. The vanadium concentrations as low as 10
-9M can be easily determined by measuring the absorbance of dye formed at a fixed time. The reproducibility of the method is satisfactory with the relative standard deviations of less than 3% and there are few interfering ions. The method has been applied to the determination of vanadium in natural waters.
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Yoshiaki YOSHITAKE, Kikuko KAKIUCHI, Kiyotoshi MORISHIGE, Shiro GOHDA, ...
1986 年 2 巻 1 号 p.
67-69
発行日: 1986年
公開日: 2006/06/23
ジャーナル
フリー
A narrow baseline method for the simultaneous determination of pheophorbide a and methylpheophorbide a in core sediment samples has been developed by high performance liquid chromatography. A linear relationship between the concentration of methylpheophorbide a and the peak height on the narrow baseline was obtained. The relative standard deviation of measurement was found to be 2.4% (n=6) for samples containing 8.1×10
-8mol dm
-3 ofmethylpheophorbide a.
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Tetsuo UCHIDA, Bert L. VALLEE
1986 年 2 巻 1 号 p.
71-75
発行日: 1986年
公開日: 2006/06/23
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フリー
A method for the determination of low level manganese in serum by graphite furnace atomic absorption spectrometry was established. Serum was diluted two-fold with Triton X-100 without deproteinization. The final concentration of the detergent was 0.2%. Manganese was measured twice by 20μl injection of sample solution by a standard addition method. For the serum manganese of 0.52ng/ml, the relative standard deviation was below 5%. Special precautions for sampling of serum and some sources of contamination are also described.
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Tadahiro TETSUMI, Masao SUMI, Minoru TANAKA, Toshiyuki SHONO
1986 年 2 巻 1 号 p.
77-80
発行日: 1986年
公開日: 2006/06/23
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フリー
A simple and reliable method is described for the determination of sodium dialkyldithiocarbamates (R
2NCS
2Na:R=CH
3, C
2H
5, n-C
3H
7, and n-C
4H
9) by high performance liquid chromatography. They were injected onto a column packed with the strongly basic anion exchanger and separated with an eluent of acetonitrile-phosphate buffer containing no ion-pairing reagent. This method was applied to the analysis of commercially available R
2NCS
2Na. It was demonstrated that the results are in good agreement with those obtained by the potentiometric titration.
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Ichiro KOSHIISHI, Junko ISONO, Toshio IMANARI
1986 年 2 巻 1 号 p.
81-85
発行日: 1986年
公開日: 2006/06/23
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A sensitive and specific high performance liquid chromatographic method for the simultaneous determination of cyanate and Carbamyl phosphate was established. The chromatographic conditions were as follows: column, TSK gel SAX (4mm I.D.×50mm); eluent, 0.075M NaCl; column temperature, 20°C. The detection was based on the indophenol reaction of ammonia which was released by the hydrolysis of cyanate or carbamyl phosphate. To suppress their hydrolysis during the sample preparation, the deproteinization of biological samples with trichloroacetic acid was carried out at 0°C, and the interval between addition of trichloroacetic acid and neutralization was restricted to 20s. Taking advantages of the sensitivity and precision of the present method, we developed a procedure that permits measurement of concentrations of cyanate as low as 0.8μM and those of carbamyl phosphate as low as 0.5μM in samples of whole blood and liver extract.
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Shizuo FUJIWARA, Izumi HAYASHI, Yayoi SAITO
1986 年 2 巻 1 号 p.
87-88
発行日: 1986年
公開日: 2007/07/27
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フリー
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Shuzo TOKUNAGA
1986 年 2 巻 1 号 p.
89-90
発行日: 1986年
公開日: 2007/07/27
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Shin-ichi NAKATA, Sachio ASAOKA, Hiromitsu TAKAHASHI, Kenzo DEGUCHI
1986 年 2 巻 1 号 p.
91-93
発行日: 1986年
公開日: 2007/07/27
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Shin-ichi NAKATA, Kohji NAGAOKA, Sachio ASAOKA, Hiromitsu TAKAHASHI
1986 年 2 巻 1 号 p.
95-96
発行日: 1986年
公開日: 2007/07/27
ジャーナル
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Liquid Particle Chromatography
Hideyuki NISHIZAWA, Yoshihiro ABE
1986 年 2 巻 1 号 p.
97-98
発行日: 1986年
公開日: 2007/07/27
ジャーナル
フリー
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Atsuko TSUNODA, Hiroki HARAGUCHI, Keiichiro FUWA, Kazuko MATSUMOTO
1986 年 2 巻 1 号 p.
99-100
発行日: 1986年
公開日: 2006/06/23
ジャーナル
フリー