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Keiichiro HOZUMI
1993 Volume 9 Issue 2 Pages
167-177
Published: April 10, 1993
Released on J-STAGE: July 04, 2006
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Automatic instrumentation has been developed for the microdetermination of various elements in organic samples ranging from 2 to 3mg. The author has devised a microanalyzer for carbon, hydrogen and nitrogen which embodies a pump system for collecting the combustion gas; this device operates on the principle of thermal conductometry for determining the three elements. The pump system is also useful for the microdetermination of organic oxygen in collecting equivalent carbon monoxide, which is then determined by infrared photometry. Organic halogen and sulfur compounds are mineralized in the conventional oxygen flask combustion and the resulting halide and sulfate ions are titrated potentiometrically with standard silver nitrate or barium chloride by means of an ion-selective glass electrode for getting the end point. Equivalence points are characterized by extremely sharp points of inflection; i.e. short lengths on the steeply rising sections of the titration curve. Ultramicrodetermination of elements in 0.5mg organic sample or less
are vital in the field of biochemistry. Dry combustion in a sealed tube has been proposed to minimize the blank value and to eliminate loss of reaction products. Accurate determination of nitrogen and later of carbon, hydrogen and nitrogen simultaneously has become possible. This approach has been further extended to the determination of halogen and sulfur.
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Jun KAWAI, Kuniko MAEDA, Takahisa YAMANE
1993 Volume 9 Issue 2 Pages
179-184
Published: April 10, 1993
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This is the first report concerning the use of an imaging plate for the X-ray detector of an X-ray spectrometer. The particle-induced X-ray emission (PIXE) spectra of the Fe KL
n-L
n+1series are recorded using an imaging plate in a flat-crystal type Bragg spectrometer. It is demonstrated that the imaging plate has potential to be used as a position-sensitive X-ray detector of a high-resolution heavy-ion PIXE spectrometer. The imaging-plate X-ray spectrometer has the following advantages: (1) the measuring time is short; (2) only a small amount of the specimen is required; (3) the simultaneous detection of many spectral lines is possible; (4) the X-ray spectra are treated as digital data; and (5) high energy-resolution is achievable.
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Chushiro YONEZAWA
1993 Volume 9 Issue 2 Pages
185-193
Published: April 10, 1993
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Basic examination of elemental analysis by a reactor-neutron-induced prompt γ-ray analysis (PGA) using a system installed at the JRR-3M (upgraded Japan Research Reactor No. 3) cold and thermal neutron beam guides is reported. Analytical sensitivities and detection limits for 71 elements were measured. Boron, Gd, Sm, and Cd are the most sensitive elements with detection limits down to 1 to 7ng. The decay γ-rays of some elements such as F, Al, V, Eu, and Hf have a higher analytical sensitivity compared to their respective prompt γ-rays. In addition, the analytical sensitivity of several heavy elements through detection of characteristic X-rays was higher than through the prompt γ-ray detection. The present system is useful for the determination of, for example, ppb level of B in graphite and Be, ppb level of Gd, Sm, Eu, and Dy in high purity cerium(IV) oxide, and ppm to % level of H and Hf in Zr and zircaloy. This system is also applicable to trace determination of Cd and Hg in environmental samples and also to major and minor elements
determination in various kinds of samples that cannot be destroyed or dissolved.
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Yusuke KUNO, Soichi SATO, Eiichi OHNO, Jinichi MASUI
1993 Volume 9 Issue 2 Pages
195-198
Published: April 10, 1993
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This report describes the rapid determination of
90Sr in highly radioactive solutions from a nuclear fuel reprocessing plant. The majority of fission products (FPs) including
90Y are precipitated in an alkaline medium, leaving
90Sr in the supernatant in the presence of inactive strontium as the hold-back carrier.
90Y freshly grown-in from the
90Sr is measured by utilizing a Cerenkov radiation counting technique with stainless steel shielding 0.2mm thick that cuts off any low energy β-particles, after strontium is recovered as a carbonate precipitate from the supernatant. Only two hours is sufficient for
90Y grow-in because large amount of
90Sr can be present in the final precipitation. The concentration of
90Sr is calculated from the
90Y detected and its grow-in time. The nuclides potentially interfering with this method,
106Ru,
134Cs,
137Cs,
144Ce,
144Pr,
147Pm,
154Eu,
123Sn and
125Sb, are quantitatively removed by coprecipitation with iron(II) hydroxide during the alkaline precipitation stage. The relative standard deviation (
n=5) is better than 5%. The time required for one determination is less than 3h.
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Hiroaki TAIRA, Koji NAKANO, Mizuo MAEDA, Makoto TAKAGI
1993 Volume 9 Issue 2 Pages
199-206
Published: April 10, 1993
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A long-chain, dialkyl disulfide having a terminal dinitrophenyl (DNP) group was newly synthesized for modification of a surface of gold with chemisorbed, self-assembled organic monolayers. The resulting monolayer was characterized by infrared spectroscopy of reflection absorption spectroscopy mode, by cyclic voltammetric measurement and by electrical impedance measurement. Coupled with impedance measurements, a possible application of the modified electrode system to impedimetric immunosensors was demonstrated. The sensor gave electrical response to anti-DNP antibody at 10-10
3ng cm
-3 concentration.
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Yukihiro ESAKA, Kenji KANO, Masatoshi SUKEGUCHI, Masashi GOTO
1993 Volume 9 Issue 2 Pages
207-211
Published: April 10, 1993
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Coenzyme pyrroloquinoline quinone (PQQ) was electrochemically detected with high sensitivity and high selectivity by employing its redox catalytic function in reversed-phase high-performance liquid chromatography. This catalytic reaction involves oxidative decarboxylation of glycine by PQQ and the reoxidation of the reduced PQQ by Fe(CN)
63- to accumulate Fe(CN)
64-, of which the electrochemical detection allows amplified detection of PQQ. Increase by two orders of magnitude of the current was achieved as compared with a direct reductive detection, at a reaction time of 3min and a reaction temperature of 25°C. The detection limit was 0.2pmol (10-8M, 20μl). The present method was applied to quantification of PQQ in table vinegar, milk, and swine serum.
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Masahiko NANAMI, Kiyoshi ZAITSU, Yosuke OHKURA
1993 Volume 9 Issue 2 Pages
213-216
Published: April 10, 1993
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A solid-phase fluoroimmunoassay of insulin is described. The assay uses Gly(A1)- and Lys(B29)-[
S-(4-sulfobenzoxadiazol-7-yl)-thioglycoloyl]-insulins which have a fluorescent sulfobenzoxadiazolyl group at a definite position, respectively. The immunoreactivities of these labeled insulins with a mouse anti-porcine insulin monoclonal antibody coated on polyacrylamide beads were compared using porcine insulin. The former labeled insulin provides 1.6-times greater immunoreactivity than does the latter and, thus, can afford a higher sensitivity in the assay.
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Mutsuko OHTA, Masatake IWASAKI, Masaaki KAI, Yosuke OHKURA
1993 Volume 9 Issue 2 Pages
217-220
Published: April 10, 1993
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A sensitive method is described for determining a biguanide drug, metformin, by high-performance liquid chromatography with precolumn fluorescence derivatization. Metformin and phenylguanidine, as an internal standard, react with a novel fluorogenic reagent, desyl chloride, or benzoin to afford the corresponding fluorescent derivatives, which are separated by reversed-phase chromatography on a TSKgel ODS-120T column with linear-gradient elution. The applicability of the method to the determination of metformin in human serum is also demonstrated. The calibration curve of metformin was linear over the range of 0-100nmol ml
-1 in human serum. The detection limit (
S/N=3) was 1.3pmol per 20-μl injection volume.
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Yoshiya ODA, Nariyasu MANO, Naoki ASAKAWA, Yutaka YOSHIDA, Tadashi SAT ...
1993 Volume 9 Issue 2 Pages
221-228
Published: April 10, 1993
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The effects of the pH, organic modifiers and buffer salt of the mobile phase upon the retention and separation characteristics of avidin- and ovomucoid-bonded silica columns as proteinous chiral stationary phases for HPLC were investigated. The enantioselectivity was greatly affected by changing the mobile-phase composition, possibly because of induced alterations in the protein conformation. Hydrophobic and Coulombic interactions play major roles in the retention, and there are some similarities between the avidin column and the ovomucoid column. However, the stereoselectivity does not necessarily reflect the retention processes on these columns. No significant decrease in the retention or enantioselectivity was observed, even after the injection of 200 samples.
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Akira TERAKITA, Akimasa SHIBUKAWA, Terumichi NAKAGAWA
1993 Volume 9 Issue 2 Pages
229-232
Published: April 10, 1993
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Micro high-performance frontal analysis (MHPFA) method has been developed for the simultaneous determination of unbound and total carbamazepine (CBZ) concentrations in protein binding equilibrium. When a 300-μl portion of 4-12μg/ml CBZ and 593μM human serum albumin (HSA) mixed solution was directly injected into a small bore ISRP column (10cm×2.0mm i.d.), CBZ gave a trapezoidal peak with a plateau separated from HSA. The CBZ concentration calculated from the plateau height agreed well with the unbound concentration determined by the conventional ultrafiltration-HPLC method, while the CBZ concentration calculated from the peak area coincided with the total (bound plus unbound) concentration. The within-run and day-to-day reproducibilities were satisfactory (relative standard deviation, <1.27%,
n=5). Compared with the injection volume (1.4ml) required for the HPFA using a conventional size (15cm×4.6mm i.d.) ISRP column, MHPFA could reduce the sample size to about one-fifth (300μl).
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Yoichi OHNO, Toshiyuki HOBO, Masaki SUYAMA, Risako TAMURA, Mikita ISHI ...
1993 Volume 9 Issue 2 Pages
233-237
Published: April 10, 1993
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A new chemiluminescence reaction system using hydrogen peroxide/sodium hydroxide/brilliant sulfoflavine was successfully applied to a flow-injection analysis (FIA) for the specific determination of adenosine-5′-triphosphate (ATP). The analytical system comprised two flow lines (L
1 and L
2) with a 20μl injector; 5% hydrogen peroxide and 5.O×10
-3M (mol/l) sodium hydroxide/1.O×10
-3M brilliant sulfoflavine were passed through the L
1 and L
2 at a flow rate of 4.5ml/min, respectively. The analytical properties of ATP were as follows: the lower detection limit was 1.0×10
-5M (
S/N=2); the determination range, 1.0×10
-5-5.0×10
-3M; the analytical time required, 8s; the reproducibility, 2.1% in terms of the relative standard deviation in 5 repeated runs for 5×10
-3M ATP. Regarding the selectivity, the CL intensity for 1.0×10
-3M ATP was not interfered with by other nucleotides coexisting at 100-times higher concentration than ATP. A recovery test of ATP in a human urine matrix was also performed.
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Yasuhiko NISHIKAWA
1993 Volume 9 Issue 2 Pages
239-244
Published: April 10, 1993
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The retention behavior of organophosphorus pesticides on five stationary phases in capillary supercritical fluid chromatography was evaluated using two parameters: the conventional steric parameter of polarizability and a parameter based on an organic conceptual diagram, the Inorganicity/organicity ratio. The former parameter, which is often effective for polycyclic aromatic hydrocarbons, gave poor results for the relationship between the capacity factor of the organophosphorus pesticides investigated and their polarizability through all of the stationary phases; however, satisfactory correlation coefficients were obtained between the capacity factor and the inorganicity/organicity ratio. Thermodynamic considerations based on the definitions of the inorganicity, organicity and separation coefficient supported the validity of the linearity. Also, an interesting retention behavior was observed for solutes on the
homologous series line of organic conceptual diagrams with an increasing stationary phase polarity. This descriptor was useful for evaluating the retention behavior of complex-structure chemicals as well as the polarities of stationary phases.
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Yoshio IIDA, Shigeki DAISHIMA, Fujihiro KANDA
1993 Volume 9 Issue 2 Pages
245-249
Published: April 10, 1993
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Flash desorption and negative ion chemical ionization (NCI) mass spectrometry have been combined to study the detection of polycyclic aromatic hydrocarbons, such as benzo[a]pyrene, at high sensitivity. Such detection below pg orders can be readily accomplished by modifying the ionization chamber to increase the seal, and also by employing rapid heating of the sample loaded filament at a rate of 1000°C/s. This method enabled a several-fold sensitivity increase over both flash desorption with electron ionization and GC/MS with NCI. Furthermore, by setting the sampling points to 20 per second to cope with rapid ionization, a repeatability of within 10% was achieved, thereby allowing quantification utilizing an internal standard. Despite isomeric influences, simultaneous detection of homologs was also possible.
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M. BILLAH, Takaharu HONJO, Kikuo TERADA
1993 Volume 9 Issue 2 Pages
251-254
Published: April 10, 1993
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A new method for the preconcentration and determination of trace amounts of manganese at the ppb-sub ppb level in natural water is described. The method is based on the formation of the thenoyltrifluoroacetone (TTA) complex with dibenzo-18-crown-6 (DB18C6) by means of synergistic extraction and back extraction combined with atomic absorption spectrometry. The effect of various factors (pH, shaking time, preconcentration factor and foreign ions
etc.) on the extraction and back extraction of manganese has been investigated. The manganese TTA chelate in o-dichlorobenzene forms stable adducts with DB18C6 [Mn(TTA)
2•nDB18C6,
n=1-2]; the stability constants (β
n) of the adducts were determined by a curve-fitting method as log β
1=4.43 and log β
2=6.85. The amount of manganese in Sai river (Kanazawa City) and Asano river (Kanazawa City) was found to be 2.4±0.3 and 12.2±0.8ng/ml, respectively.
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Jun'ichiro MIURA, Mitsuhisa YOSHITOME, Itsuji GOTO, Yoshiharu NAKAMURA ...
1993 Volume 9 Issue 2 Pages
255-260
Published: April 10, 1993
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he solubilization equilibria of 2-(2-thiazolylazo)-4-methylphenol (TAC) and 2-(2-thiazolylazo)-5-dimethylaminophenol (TAM) in aqueous micellar solutions of nonionic surfactants were investigated according to a distribution model between the micellar and aqueous phases. The distribution constants of TAC and TAM, thus obtained, decreased with an increase in the oxyethylene chain length of nonionic surfactants, indicating the possibility of controlling the distribution of TAC and TAM into micelles. Based on this finding, we tested the micellar reversed-phase high-performance liquid chromatography (micellar RP-HPLC) of vanadium(V)-TAM chelate, which was hardly separated from free TAM in conventional RP-HPLC. Micellar RP-HPLC was effective in preferentially eluting the vanadium(V) chelate in advance of free TAM when a nonionic surfactant with a longer oxyethylene chain was employed.
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Masatoshi ICHIKAWA, Naomi NONAKA, Ichiro TAKADA, Sigeru ISHIMORI
1993 Volume 9 Issue 2 Pages
261-266
Published: April 10, 1993
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A method to estimate the octane number of motor gasoline by mass spectrometry (MS) has been studied, by first examining whether the octane number can be estimated from its mass spectrum (MS). The MS of 29 different regular gasolines and 32 premium gasolines, sampled in the market from spring to autumn, were measured. We studied whether it is possible to extract any available parameters for clearly distinguishing between regular and premium gasolines, by applying both feature-selection and pattern-recognition methods to MS. It was found that a clear distinction between regular and premium gasolines could be made using MS information.
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Masahisa TAKATSU, Tadahiro YAMAMOTO
1993 Volume 9 Issue 2 Pages
267-271
Published: April 10, 1993
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Soot samples produced by the combustion of benzene, toluene,
o-,
m-, and
p-xylene, ethylbenzene, styrene and cumene were pyrolyzed at 590°C and evaluated by gas chromatography/mass spectrometry (GC/MS). Various materials were identified:the residual fuels, dealkylation products, elimination products of the fuels such as styrene and phenylacetylene, and oxygenated compounds such as cresol, xylenols, benzaldehyde, tolualdehydes, phenylacetaldehyde and acetophenone. In addition to these small compounds, coupling compounds such as biphenyl, diphenylmethane, diphenylethane, diphenylethene, their mono- and dialkylated homologues, terphenyls and polycyclic aromatic hydrocarbons (PAHs) were identified. The profiles of these compounds obtained during pyrolyzing the eight types of soot characteristically changed in accordance with the chemical structures of the original alkylbenzenes. This pyrolysis GC/MS analysis should be useful for identifying unknown alkylbenzene fuels from a trace amount of the soot.
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Wilfried DIRKX, Ryszard LOBINSKI, Freddy C. ADAMS
1993 Volume 9 Issue 2 Pages
273-278
Published: April 10, 1993
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Two techniques, megabore column gas chromatography quartz furnace atomic absorption spetrometry (MCGC-QFAAS) and MCGC graphite furnace AAS (MCGC-GFAAS), were developed for the determination of pentylated organotin species and compared with the existing techniques, packed column (PC) GC AAS and capillary column (CC) GC-atomic emission spectrometry (AES). Particular attention was given to the design of the interface between a GC column and the detector cell (GF or QF) as well as optimization of the operational variables of the interface and detector. The accuracy of the developed techniques is discussed on the basis of an intermethod comparison analysis of 15 water samples.
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Dongjin Pyo, Ken-ichi HARADA
1993 Volume 9 Issue 2 Pages
279-283
Published: April 10, 1993
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As gas chromatography/infrared spectrometry (GC/IR) becomes routinely available, methods must be developed to contend with the large amount of data produced. We demonstrate computer methods that can be used to determine the proper ranges of frequencies within which characteristic patterns of absorbances for a given functional group can be found. The methods can be applied to Chemigram calculations for selecting aromatic compounds from collected GC/IR data. The computer acts as a functional-group selective detector.
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Maciej JAROSZ, Slawomir OSZWALDOWSKI
1993 Volume 9 Issue 2 Pages
285-288
Published: April 10, 1993
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A sensitive method for the spectrophotometric determination of niobium(V) based on the formation of its complex with 2-(5-Bromo-2-pyridylazo)-5-diethylaminophenol in the presence of hydrogen peroxide has been developed. The molar absorptivity at 591nm is 7.43×10
4l mol
-1 cm
-1 at pH 4.0±1.0. This method becomes selective for niobium(V) after a preliminary extraction of its complex with α-benzoin oxime from 5-9M hydrochloric acid, thus permitting the determination of traces of niobium in the presence of a large amount of other ions. It has been applied to the determination of niobium in materials of certified Nb content: steel and apatite samples.
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Manabu FUJIWARA, Takayuki MATSUSHITA, Shigero IKEDA
1993 Volume 9 Issue 2 Pages
289-291
Published: 1993
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Manabu FUJIWARA, Takayuki MATSUSHITA, Shigero IKEDA
1993 Volume 9 Issue 2 Pages
293-295
Published: 1993
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Kazuhiro MASUDA, Takanori INOUE, To-oru YASUDA, Keiji NAKASHIMA, Teiic ...
1993 Volume 9 Issue 2 Pages
297-298
Published: 1993
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Soichi OTSUKI, Kimihiro ADACHI
1993 Volume 9 Issue 2 Pages
299-301
Published: April 10, 1993
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Hidehiko FUJII, Mitsuhiro HASHIMOTO
1993 Volume 9 Issue 2 Pages
303-307
Published: April 10, 1993
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Hirofumi KAWAZUMI, To-oru YASUDA, Teiichiro OGAWA
1993 Volume 9 Issue 2 Pages
309-310
Published: April 10, 1993
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Yasuto TSURUTA, Hiroshi TONOGAITO, Yuuko DATE, Eiichi SUGINO, Kazuya K ...
1993 Volume 9 Issue 2 Pages
311-313
Published: April 10, 1993
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Yoshio SHIJO, Kohsuke TAKADA, Nobuo UEHARA
1993 Volume 9 Issue 2 Pages
315-317
Published: April 10, 1993
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Junichi ISHIDA, Shinji SONEZAKI, Masatoshi YAMAGUCHI, Takashi YOSHITAK ...
1993 Volume 9 Issue 2 Pages
319-322
Published: April 10, 1993
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