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Motoji IKEYA
1989 Volume 5 Issue 1 Pages
5-12
Published: February 10, 1989
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Uses of electron spin resonance (ESR) techniques in chronology and radiation dosimetry are reviewed, especially the special distribution of ESR intensities with imaging techniques. This will stimulate the use of these analytical techniques in interdisciplinary fields including nuclear science, medicine, biology, earth science, archaeology, history and forensic science. The principle of "chemical ESR dating" is to detect unpaired electrons created by oxidizing or deterioration reactions, while that of "physical ESR dating" is the measurement of the total accumulated dose of natural radiation. The age is determined by radiation assessment. The spatial imaging of the age and dose can be made with the ESR imaging techniques or with ESR microscopes. The procedures of ESR microscopy are described.
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Akiko TAKATSU, Sueo NISHI
1989 Volume 5 Issue 1 Pages
13-17
Published: February 10, 1989
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Determination of serum glucose by isotope dilution mass spectrometry with liquid chromatography is described. After adding uniformly labeled glucose to the serum, serum protein was removed. Glucose was separated using high performance liquid chromatography and measured by electron impact or chemical ionization mass spectrometry with a direct insertion device. Analytical results of NBS SRM serum showed satisfactory agreement with the certified value; relative standard deviations of about 1% were obtained.
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Junichi GOTO, Gang SHAO, Hiroya MIURA, Toshio NAMBARA
1989 Volume 5 Issue 1 Pages
19-22
Published: February 10, 1989
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A method for the separation of C-25 epimers of 3α, 7α-dihydroxy-and 3α, 7α, 12α-trihydroxy-5β-cholestanoic acids by reversed-phase high performance liquid chromatography (HPLC) is described. The 5β-cholestanoic acids and their glycine and taurine conjugates were derivatized quantitatively into fluorescent compounds through the 3α- hydroxyl group by treatment with 1-anthroyl nitrile in the presence of quinuclidine in acetonitrile. Subsequent resolution into each epimer was attained by HPLC on a Cosmosil 5C
18column using a 0.3% potassium phosphate buffer (pH7.0)-methanol(1:4 or 1:5) as a mobile phase. The 3-(1-anthroyl) derivatives of C-25 epimeric 5β-cholestanoic acids were monitored by fluorescence detection (excitation wavelength 370nm; emission wavelength 470nm), the limit of detection being 40fmol. The effect of pH of the mobile phase on chromatographic behaviors of 5β-cholestanoic acids is also discussed.
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Steven A. SOPER, Susan M. LUNTE, Theodore KUWANA
1989 Volume 5 Issue 1 Pages
23-29
Published: February 10, 1989
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The development of a convenient, low cost, low power He-Cd laser-induced fluorescence (LIF) detection system for HPLC is described. The system was developed for the detection of primary amines derivatized with naphthalenedialdehyde (NDA). The LIF system incorporates a fiber optic cell similar to the cell developed by Yeung and coworkers, which was modified in order to improve the
S/
Nratio. The LIF system exhibited detection limits of 0.75-1.2fmol which was comparable to the detection limits obtained for the derivatized amino acids with a high power argon ion LIF system and demonstrated a tenfold improvement in comparison to a commercial fluorescence detector. In addition, the LIF cell, collection optics and photomultiplier tube were mounted on a standard laboratory ringstand, which allowed the system to be easily moved. The applicability of the LIF system was demonstrated by derivatizing a human tear sample with NDA and subjecting it to HPLC analysis with LIF detection. Several amino acids were identified in the resulting chromatogram.
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Shigeru NARITA, Takayasu KITAGAWA
1989 Volume 5 Issue 1 Pages
31-34
Published: February 10, 1989
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2-[
p-(5, 6-Methylenedioxy-2
H-benzotriazol-2-yl)]phenethylamine (MBPA; 1) and two related compounds (2 and 3) were synthesized as highly sensitive fluorescence derivatization reagents for carboxylic acids. We investigated the fluorescence characteristics and the chromatographic behavior of their benzamide derivatives produced by the reaction with benzoic acid. Among them, MBPA was found to be the best reagent for use in high performance liquid chromatography (HPLC). Thus it was applied to the determination of ibuprofen in human serum. MBPA reacted with ibuprofen in the presence of 2-bromo-1-ethylpyridinium tetrafluoroborate to give the corresponding fluorescent amide at room temperature. Linear relationships were found between the peak areas and the concentrations of ibuprofen in the range of 5-100ng/ml and 0.5-5ng/ml with relative standard deviations of 7.49% and 15.02%, respectively. The detection limit for ibuprofen in serum was 1.5pg per injection.
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Masatoshi YAMAGUCHI, Shuuji HARA, Yasuyo TAKEMORI, Masaru NAKAMURA
1989 Volume 5 Issue 1 Pages
35-38
Published: February 10, 1989
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A highly sensitive and simple high performance liquid chromatographic method with fluorescence detection for the determination of monosialogangliosides is described. The gangliosides are converted into the corresponding fluorescent derivatives by reaction with 3-bromomethyl-6, 7-methylenedioxy-1-methyl-2(1
H)-quinoxalinone in dimethylformamide. The derivatives are separated isocratically on a normal-phase column (Radial PAK Silica cartridge) and detected fluorimetrically. The detection limits for gangliosides GM
1, GM
2 and GM
3 are 4.0, 1.1 and 0.4ng, respectively, in a 10-μl injection volume at a signal-to-noise ratio of 3. The method was applied to the determination of ganglioside GM
3 in plasma from normal subjects and from gastric cancer patients.
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Shinobu KUDOH, Hiroshi NAKAMURA
1989 Volume 5 Issue 1 Pages
39-42
Published: February 10, 1989
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A high performance liquid chromatographic (HPLC) method employing a column-switching technique was developed to determine the plasma levels of Cromakalim, a novel antihypertensive agent. The plasma sample is first introduced onto a precolumn of two-phase gel where the hydrophobic drug, having a chroman skeleton, is well retained while biological macromolecules such as proteins and nucleic acids are not. The retained Cromakalim is subsequently transferred to an analytical column of octadecyl silica (ODS) using a column-switching technique, followed by fluorescence detection (Ex 254nm, Em 306nm). This system has realized a highly sensitive determination of Cromakalim in human plasma without prolonged pretreatment procedures such as solvent extraction. In tests, calibration curves were linear over the range 0.3 to 20ng ml
-1 with a detection limit of 0.07ng ml
-1. The relative standard deviations (
n=3 each) for spiked plasma samples at 1 and 20ng ml
-1 were 3.33 and 1.21 %, respectively.
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Shinzo TANABE, Chiaki ISE, Takayoshi KOSUGI, Koji KAWANABE
1989 Volume 5 Issue 1 Pages
43-47
Published: February 10, 1989
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Phenanthro[9, 10-
d]imidazole-2-
N-chloroimide (PI-NCl) was synthesized as a new color reagent for phenolic compounds and its reactivity was examined in detail. The color reaction to phenolic compounds occurs at alkaline pH and does not require any oxidants. Among phenolic compounds tested, PI-NCl especially showed a strong coloration for 1, 3-diphenols, 1-naphthol and dialkylphenols substituted in the 2- and 5- or 6-positions at a strongly alkaline condition: the apparent molar absorptivities of resorcinol, 1-naphthol and 2, 6-xylenol were 3.00×10
4, 3.65×10
4 and 4.02×10
4, respectively. 1, 3-Diphenols substituted with carboxy or methylketo group in the position 6, however, did not react with the reagent at all. PI-NCl reacted slightly or not at all with monosubstituted phenols. The analytical conditions for the above three compounds as obtained by the present method were also investigated.
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Hirofumi ISOYAMA, Tetsuo UCHIDA, Chuzo IIDA, Genkichi NAKAGAWA, Yoichi ...
1989 Volume 5 Issue 1 Pages
49-53
Published: February 10, 1989
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A pseudo-simultaneous background correction system was constructed to enable alternate measurements of the peak and background in the single channel ICP-AES to be performed with discrete nebulization technique. The quartz refraction plate inserted in an optical pass was vibrated at 150ms intervals with a square wave; thus the center and wing of the spectral line could be measured alternately. The effects of sampling frequency on background correction were examined with regard to the precisions of peak height and peak area measurements. The present system was applied to the aluminum and iron determinations in NIES-CRM Pepperbush.
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I. M. KENAWY, M. A. H. HAFEZ
1989 Volume 5 Issue 1 Pages
55-60
Published: February 10, 1989
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The use of a cellulose ion-exchanger (Hyphan) for the isolation of the rare earth elements (REE′s) yttrium and scandium from aqueous solution is described. After preconcentration, the cations under investigation were determined using a wall stabilized plasma arc in atomic emission spectroscopy (DCP-OAES). The detection limits for Sc, Y, La, Nd, Gd, Yb and Lu were determined (0.02-0.31μg ml
-1). The distribution coefficient for the investigated cations were determined as a function of pH. The order of selectivity is the following sequences, Yb>Lu>Gd>Y>La>Sc>Nd at pH of 7.15-9.04. The distribution coefficient obtained is in the range 10
2-10
5ml/g. Such order of selectivity was also confirmed by thermal analysis technique. Moreover, the lanthanoid complexes formed by the chelating ion exchanger were characterized by reflectance and infrared spectrometry. Alkali and alkaline earth cations did not interfere at 50-100μg ml
-1.
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Ryusuke KOBAYASHI, Keishichiro IMAIZUMI
1989 Volume 5 Issue 1 Pages
61-64
Published: February 10, 1989
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Trace antimony in urine was determined by atomic absorption spectrometry using a graphite furnace atomizer. The urine was concentrated and digested with HNO
3-HClO
4-H
2SO
4 in a Teflon beaker. The bulk of the salts and interfering elements was removed by cation exchange and the ammonium pyrrolidinedithiocarbamate-2-methyl-4- pentanone extraction procedure, and finally the organic phase was analyzed by graphite furnace atomic absorption spectrometry. Results of Sb in the NBS reference material agreed with its certified value. Relative standard deviation were about 8.4% at the 1-μg level. Antimony contents in urine ranged from 0.3 to 1.3μg l-1.
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Yoshio SHIJO, Tokuo SHIMIZU, Takatoshi TSUNODA
1989 Volume 5 Issue 1 Pages
65-68
Published: February 10, 1989
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A method is presented for the determination of silver in seawater by graphite furnace atomic absorption spectrometry after solvent extraction and microscale back-extraction. Silver is quantitatively extracted with 2× 10
-4mol l
-1 dithizone-benzene from seawater, and back-extracted with 100μl of nitric acid. The aqueous phase is taken by a fine glass tube; then a 10μl aliquot of the solution is injected into the graphite tube. This procedure has been applied to the determination of silver in coastal seawater.
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Shigenori NAKANO, Mutsuo TAGO, Takuji KAWASHIMA
1989 Volume 5 Issue 1 Pages
69-72
Published: February 10, 1989
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A catalytic-photometric method with a continuous-flow system is presented for the determination of nanogram amounts of vanadium in natural water. It is based on the catalytic effect of vanadium(V) on the oxidative coupling reaction of 4-aminoantipyrine with
N,
N-dimethylaniline in the presence of bromate. A higher sensitivity can be attained by using 1, 2-dihydroxybenzene-3, 5-disulfonic acid (Tiron) as an activator; vanadium(IV, V) at the 0.05- 2.0ng ml
-1 level can be determined at a rate of 30 samples h
-1. The method suffers few interferences and can be applied successfully to the determination of vanadium in natural water.
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Kousaburo OHASHI, Mitsuko ARAMAKI, Masahiro KAISE, Katsumi YAMAMOTO
1989 Volume 5 Issue 1 Pages
73-77
Published: February 10, 1989
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Spectrophotometric and electron spin resonance (ESR) studies on the formation of chromium(IV, V)-ethylene- diamine-
N,
N,
N′,
N′-tetraacetate (EDTA) and the spectrophotometric determination of chromium(VI) and cobalt(II) are described. Chromium(V)-EDTA, formed by the oxidation of cobalt(II)-EDTA with chromium(VI) in the presence of excess EDTA and chromium(VI), gives two narrow ESR absorption lines with a g-value of 1.969 and intense absorption at 550nm. The formation of chromium(IV, V)-EDTA depended to a fair degree on the solution pH and the concentration of free excess EDTA. Chromium(IV, V)-EDTA is stable for at least 30min under optimal conditions. The color system obeyed Beer′s law up to 3.8μg/cm
3 Co(II) and 3.4μg/cm
3 Cr(VI).
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Tomozo KOH, Yasuyuki MIURA, Masahiro ISHIMORI, Norihito YAMAMURO
1989 Volume 5 Issue 1 Pages
79-84
Published: February 10, 1989
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The proposed method consists of four procedures; excess iodine for reactions with thiosulfate and/or sulfite under Procedures I, II and III, and the thiocyanate formed under Procedure IV are measured spectrophotometrically after proper chemical treatments. The absorbance obtained by Procedure I corresponds to the sum of the amount of tetrathionate and that of thiosulfate in the mixture. The absorbance obtained by Procedure II corresponds only to the amount of thiosulfate in the mixture. The absorbance obtained by Procedure III corresponds to the sum of the amount of thiosulfate and twice that of sulfite in the mixture. The absorbance obtained by Procedure IV corresponds to the sum of the amount of both thiosulfate and trithionate and twice that of tetrathionate in the mixture. The proposed method was applied to the determination of tetrathionate, thiosulfate, sulfite and trithionate mixed in various ratios in amounts of more than 0.05μmol with an error below ±0.02μmol.
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Shoji MOTOMIZU, Mitsuko OSHIMA, Yuka OJIMA
1989 Volume 5 Issue 1 Pages
85-88
Published: February 10, 1989
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On the basis of the coloration formed with molybdosilicate and Malachite Green in aqueous solution, trace amounts of silicate were determined. In an acidic medium, silicate reacted with molybdate to form molybdosilicate, which reacted with Malachite Green to form a colored ion association complex. The color was stabilized by adding poly(vinyl alcohol). The molar absorptivity was 1.0×10
5mol
-1 cm
-1 at 595nm, and the absorbance of the reagent blank was 0.089. The recommended concentration range of silicon was 0.1-5μg and the limit of detection was 0.01μg of silicon. Silicate in river and tap waters was determined.
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Hasan AYDIN, Güler SOMER
1989 Volume 5 Issue 1 Pages
89-93
Published: February 10, 1989
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A method for a direct determination of trace quantities of selenium by anodic stripping voltammetry has been developed. A mercury-coated graphite wax electrode was used for this determination. It is possible to determine 2×10
-9M Se with a relative standard deviation (
n=6) of 3.7% in solutions containing copper (up to 10% of the concentration of selenium). The presence of other elements, including tellurium, does not interfere. The presence of copper appears to be critical in the application of this method; in this case, if the quantity of selenium falls into the range 1.8_??_
r_??_11, where r is the Cu/Se concentration ratio, selenium can be determined from the Cu-Se peak, which belongs to an intermetallic compound between copper and selenium. Considering that the known methods generally require an elimination of copper from the solution, the present method enables one to make such a determination in the presence of copper, even though it is within a short interval (1.8_??_r_??_11).
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Hiroyuki KUTSUMI, Takayoshi YOSHIMORI, Tatsuhiko TANAKA
1989 Volume 5 Issue 1 Pages
95-100
Published: February 10, 1989
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A method for the determination of mcroamounts of carbon in metals which do not achieve complete combustion has been developed. This method is based on wet chemical dissolution with a mixture of 280ml of 5 to 10M sulfuric acid and 16g of potassium dichromate, with and without the addition of a small amount of copper(II) sulfate in a stream of oxygen, and on nonaqueous coulometric photometric titration of the evolved carbon dioxide. The reagents used for the wet chemical method were highly purified in order to lower the blank value. Microamounts of carbon in sucrose could be determined with good precision and accuracy. Trace amounts of carbon (0.8-166ppm) in iron, low-carbon steels, titanium alloy, indium and gallium were determined precisely and accurately. The blank value and determination limit obtained by the proposed method are lower than those previously obtained by wet chemical dissolution and volumetric titrimetry.
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Takashi HAYASHITA, Hisashi OKA, Hiroaki NOGUCHI, Manabu IGAWA
1989 Volume 5 Issue 1 Pages
101-103
Published: February 10, 1989
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The sorption behavior of Cd(II) and Pb(II) chloride complexes on DB18C6 resin was investigated. The Pb(II) sorption increased with the chloride concentration regardless of the counter cation species. But the Cd(II) sorption was significantly affected by the binding property of counter cations with the crown ether matrix. According to analysis of the sorption equilibrium, Pb(II) was found to complex directly with the crown ether matrix to sorb in the form of PbCl
2 (metal-chelating sorption), but Cd(II) was found to sorb in the ion- association form of R
+-CdCl
3- (anion-exchange sorption). In the latter sorption, DB18C6 resin was found to behave as a "dynamic" anion exchanger.
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Hiroyuki FUJINO, Shujiro GOYA
1989 Volume 5 Issue 1 Pages
105-106
Published: 1989
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Yasuyuki SHIBATA, Masatoshi MORITA
1989 Volume 5 Issue 1 Pages
107-109
Published: 1989
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Nobuo UEHARA, Yukiko ANNOH, Tokuo SHIMIZU, Yoshio SHIJO
1989 Volume 5 Issue 1 Pages
111-112
Published: 1989
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Katsuyuki AOKI, Yasuo WAKATSUKI, Hiroshi YAMAZAKI
1989 Volume 5 Issue 1 Pages
113-114
Published: February 10, 1989
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Sei TSUBOYAMA, Naoyuki SAITOH, Kimiko KOBAYASHI, Kaoru TSUBOYAMA, Tosi ...
1989 Volume 5 Issue 1 Pages
115-116
Published: February 10, 1989
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Tomohiro SATO
1989 Volume 5 Issue 1 Pages
117-118
Published: February 10, 1989
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Yoshiharu NAWATA, Yohko KURIKI, Masatoshi HANEDA, Kiyoshige OCHI, Taka ...
1989 Volume 5 Issue 1 Pages
119-120
Published: February 10, 1989
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Chiaki SANO, Nobuya NAGASHIMA, Tetsuya KAWAKITA, Yoichi IITAKA
1989 Volume 5 Issue 1 Pages
121-122
Published: February 10, 1989
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Takao MATSUZAKI, Yasuko T. OSANO
1989 Volume 5 Issue 1 Pages
123-124
Published: February 10, 1989
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