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Tomohiro URAMOTO, Shin'ichi NAGAYAMA, Hironobu MATSUDA, Fumio SAGARA, ...
1992 Volume 8 Issue 2 Pages
125-130
Published: April 10, 1992
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Femtomole fluorescers such as perylene or 5, 12-bis(phenylethynyl)naphthacence (PEN) were detected photographicallythrough the peroxyoxalate chemiluminescence reaction (CL). With the use of X-ray film, the CL emissions from 9.6× 10
-14mol fluorescers were recorded as black-and-white spots, while they are recorded as color spots on color films such as instant color films (ISO 80-100) or high speed 35mm roll films (ISO 400 and 3200) with the detection limit of 9.6× 10
-13mol. This technique has been applied to the detection of albumin labeled with fluorescer. As little as 0.30μg of pyrene labeled bovine serum albumin or 2.4μg of tetramethylrhodamine labeled albumin was detected by this technique.
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Andreas MANDELIS, Ryoichi TAKAUE, Zhuohui CHEN, Joanna SZURMAK, W. Dou ...
1992 Volume 8 Issue 2 Pages
131-136
Published: April 10, 1992
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Purely concentration-gradient driven liquid-liquid interface laser beam deflection detection was studied theoretically and used experimentally to monitor the kinetics of diffusion between water and sugar as a simple model system. The combination of data from both sides of the interface was used to determine the initial position of the interface plane. The developed one-dimensional model of the dependence of the laser beam deflection on the diffusion parameters was found to be in good agreement with the experimental data, especially at early interdiffusion times. The model was thus able to yield the values for the diffusion coefficient D
Sof sugar in water, and for the refractive index gradient
∂n/
∂C
S.
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Jun HAGINAKA, Junko WAKAI
1992 Volume 8 Issue 2 Pages
137-140
Published: April 10, 1992
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β-Cyclodextrin (CD)/diol phase silica materials have been designed for direct serum injection assays of drug enantiomers. The mixed functional phase (MFP) materials having β-CD and diol phases were synthesized in four steps: introduction of a 3-chloropropyl phase, introduction of a β-CD phase by ether linkage, introduction of a 3- glycidoxypropyl phase and hydrolysis of the oxirange ring to a diol phase. The obtained MFP materials were more stable against continuous flow of an eluent including phosphate buffer and organic solvent and/or acid hydrolysis than only β-CD-bonded materials were. These MFP materials could be used for direct serum injection assays of drug enantiomers. The recovery of drug enantiomers from serum was almost 100%.
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Jun HAGINAKA, Junko WAKAI
1992 Volume 8 Issue 2 Pages
141-144
Published: April 10, 1992
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An improved preparation method for mixed functional phase (MFP) silica packing materials has been developed for direct injection analysis of drugs in serum. The MFP materials were synthesized from a porous silica gel having 9-nm pore-size in two steps: introduction of a phenyl phase and introduction of a glycerylpropyl (
i.e. diol) phase. Bovine serum albumin was completely recovered from the MFP materials at the first injection of the protein sample. The MFP materials prepared by two steps were superior to those prepared by three or four steps [J. Chromatogr., 535, 163 (1990)] in column efficiency and in batch-to-batch reproducibility. The MFP packing materials can be used for direct injection analysis of hydrophobic and hydrophilic drugs in serum.
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Ryoichi KIZU, Manabu KANEDA, Motoichi MIYAZAKI
1992 Volume 8 Issue 2 Pages
145-150
Published: April 10, 1992
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Iproplatin [
cis-dichloro-trans-dihydroxo-bis(isopropylamine)platinum(IV), CHIP] is a potent antitumor platinum complex with axial hydroxy ligands. The high-performance liquid chromatographic behavior of CHIP was investigated on a poly(styrene-divinylbenzene)-based cation exchange column with a dipotassium hydrogen phosphate eluent and an octadecylsilica column with a phosphate buffer/methanol eluent containing a sodium alkylsulfonate. On both cation exchange and octadecylsilica columns, the capacity factor of CHIP increased, the lower was the eluent pH. However, this was not found to be the case in the absence of an alkylsulfonate. Using the cation exchange column, the CHIP capacity factors at various pH values were plotted (on log-log graph paper) as a function of the eluent potassium concentration. Straight lines were obtained with slopes of-O.65 at pH 4.0 and-0.81 at pH 2.5. The observed charges on CHIP evaluated from these slopes were 0.65 at pH 4.0 and 0.81 at pH 2.5, indicating that a large portion of CHIP was present as a monovalent cation in both cases. This study shows that CHIP is protonated and, consequently, can be chromatographed on cation exchange and octadecylsilica columns as a cationic compound, under acidic conditions.
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Shigeori TAKENAKA, Kunihiko DOHTSU, Makoto TAKAGI
1992 Volume 8 Issue 2 Pages
151-156
Published: April 10, 1992
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Intercalator-like aromatics-loaded columns were prepared by modifying silica with benzoic acids m-substituted with the nitro (NBA column), hydrogen (BA), methyl (MBA), methoxy (MOBA), and dimethylamino (DABA) groups. These chromatographic supports constitute a hydrophobic stationary phase; they were used for the separation of mono-, di-, and tetranucleotides under isocratic conditions in HPLC. The retention of nucleotides on these column correlated with the π-electron density of the aromatic moiety of these supports, suggesting the importance of stacking interactions of the aromatic rings with the nucleic base. The base-selective separation of nucleoties, CCGG and GGCC, was achieved with the MBA column.
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Kenji NAKAMURA, Shinji SATOMURA, Takumi TANAKA, Shuji MATSUURA
1992 Volume 8 Issue 2 Pages
157-160
Published: April 10, 1992
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A simple and convenient method for the analysis of antigen-antibody reactions using high-performance liquid chromatography is described. A mixture of human serum albumin and anti-albumin monoclonal antibody in a buffer was analyzed on a gel filtration column. After the free albumin and antibody were rapidly separated from the antibody- antigen immune complex, the three amounts in the mixture were directly calculated from the peak heights. The concentration of the antigen and antibody as well as other reaction conditions were easily varied by this method. The effects of the reaction time, the concentrations of albumin or antibodies, and the pH were examined. The reactivities of the antigen binding sites of immunoglobulin G, pepsin digested fragment F(ab′)
2and reduced monomeric form Fab′ were studied; the results suggest that the Fc region of IgG may participate in the antigen-antibody interaction at those binding sites. Epitope typing of monoclonal antibodies was also carried out with a combination of two antibodies. This represents a new immunochemical technique for characterizing antibodies and for the quantitative assay of protein antigens.
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Kouichi KASAI, Nobuyuki YAMAJI
1992 Volume 8 Issue 2 Pages
161-164
Published: April 10, 1992
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Two novel Nacetyl-β-D-glucosaminides, resorufinyl-(
1) and resazurinyl-Nacetyl-β-D-glucosaminides (
2), were synthesized by a coupling reaction of 1-chloro-l-deoxy-2, 3, 4, 6-tetraacetyl-α-D-glucosamine with resorufin derivatives followed by deprotection of the sugar moiety. Compounds
1 and
2 were hydrolyzed by
N-acetyl-β-D-glucosaminidase to give products showing high absorbance at a long absorption wavelength (575 and 610nm) under rate-assay conditions of a weakly acidic pH. Though these two compounds are considered to be potential chromogenic substrates,
1 is the more favorable substrate for the rate-assay of
N-acetyl-β-D-glucosaminidase.
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Satoshi HIKIMA, Kiyoshi HASEBE, Teiji KAKIZAKI
1992 Volume 8 Issue 2 Pages
165-168
Published: April 10, 1992
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A sensitive flow injection system for L-lactate with polarographic detection is described. The system mainly utilizes saturated dissolved oxygen in samples for enzymatic reactions to convert L-lactate and oxygen to pyruvate and hydrogen peroxide; and then, any excess amount of dissolved, electroreducible oxygen which is not consumed in the enzymatic reaction can be retarded by an ODS-column to separate it from the pyruvate and hydrogen peroxide. After that, both the pyruvate and hydrogen peroxide are measured by the polarographic method using a static mercury drop electrode. The enzyme, lactate oxidase, was covalently immobilized on Chitopearl® composed of chitosan, and packed into a reactor. The detection limit under this system was 9.9×10
-6M and the relative standard deviation at 2.O×10
-4M L-lactate was 2.8%.
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Kunishige NAITO, Kazuho KUDO, Shinsuke TAKEI
1992 Volume 8 Issue 2 Pages
169-172
Published: April 10, 1992
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A chemically bonded phase was prepared from alumina by modifying with β-phenethyltrichlorosilane. The amounts of surface-bonded β-phenethyl groups were easily controlled by adjusting the initial amount of the silane upon reaction. Using a column packed with chemically bonded alumina, some aliphatic hydrocarbons, benzene and t-butyl methyl ether were eluted as symmetric or slightly skewed peaks. Increasing the number of surface-bonded, β-phenethyl groups decreased the reduced retention volume of a given solute with improved peak shape and linearly reduced the specific surface area of the chemically bonded alumina. The mixed retention mechanism was used for understanding this dependence of the reduced retention volume and the specific surface area upon the amount of surface-bonded β-phenethyl groups.
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Hiromi ARIMOTO, Kaori OZAKI, Koichi SHIOMI, Naoki HAMADA
1992 Volume 8 Issue 2 Pages
173-177
Published: April 10, 1992
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The response characteristics of flame thermionic detectors (FTDs) to sulfur compounds were studied. The optimum flow rates of air and hydrogen were obtained by investigating changes in the detector response and selectivity for hydrocarbons with respect to changes in the air and hydrogen flow rates. From these investigations, the response for sulfur compounds shows a high sensitivity at an air flow rate of about 6ml min
-1, as well as 100ml min
-1 or 16ml min
-1. Investigations were carried out concerning the detection limit, response linearity and selectivity for representative sulfur compounds (under these set of operational conditions). Disulfides were detected at especially high sensitivity, under 16ml min
-1 air flow rate conditions. The detection limit of dimethyl disulfides was 1.78×10
-10g s
-1 (
S/N=2), and the selectivity for hydrocarbons was 1.7×10
3gC/gS. Exact details concerning the negative surface ionization process on alkali metal surface are not completely known. The presumed ionization process for organic sulfur compounds is discussed in this paper.
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Yosikazu KIKUTA, Holger JENETT
1992 Volume 8 Issue 2 Pages
179-182
Published: April 10, 1992
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Some instrumental effects on sensitivity factors in SNMS (secondary or sputtered neutral mass spectrometer) have been investigated with :III-V semiconductors, viz., GaAs, GaP and InP. There is a large variation of sensitivity factors, affected by target potential, ion optics setting and multiplier voltage, which is related to the mass difference between component elements. But relatively small variation of sensitivity factors by plasma conditions was found.
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Mitsuru EBIHARA, Naomi SAITO, Hideo AKAIWA, Kenji TOMURA
1992 Volume 8 Issue 2 Pages
183-187
Published: April 10, 1992
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For determining trace amounts of iodine in geological samples (igneous and sedimentary rocks), applicabilities of instrumental and radiochemical neutron activation analyses (NAA) using a short-lived nuclide
128I were examined. Instrumental NAA using a TRIGA-type reactor and Cd metal or boron carbide as an absorbing filter of thermal neutron could be applied for the determination of iodine in ppm level in sedimentary rocks. Further, radiochemical NAA (RNAA) could lower the detection limit down to several ppb for igneous rock samples. Even though RNAA was employed, at least 6 samples could be routinely analyzed a day (6h in reactor operation) using the analytical procedures reported in this work.
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Ambrogio MAZZUCOTELLI, Fabio DE PAZ, Emanuele MAGI, Roberto FRACHE
1992 Volume 8 Issue 2 Pages
189-193
Published: April 10, 1992
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A study concerning the nature of the interference of sodium, potassium, calcium and iron in the determination of rare earth elements by ICP has been carried out. The studied elements are the most common constituents of naturally occurring samples and severally interfere in the spectrochemical determination of the analytes. The physico-chemical and spectral Interferences are not negligible and cause a strong depression or enhancement of the emission intensity of the rare earth elements (REE). Although the best analytical line for every rare earth element is also suggested, separating the analyte from the complex matrix is often necessary.
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Akinori JYO, Isao HIWATASHI, Rudolf WEBER, Hiroaki EGAWA
1992 Volume 8 Issue 2 Pages
195-200
Published: April 10, 1992
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Chelating resins containing a macrocyclic ligand, 1, 4, 8, 11-tetraazacyclotetradecane-5, 7-dione, were prepared by ligand reactions with two different crosslinked copolymer beads of the macroreticular type: chloromethylated styrene- divinylbenzene (RCS) and glycidyl methacrylate-divinylbenzene (RG) copolymers. Although both resins have nearly equal amounts of the fixed ligand, the RG-based resin (RGD) shows a much higher uptake of Cu(II) than does the RCS- based resin (RCSD). This indicates that the complexing ability of the fixed ligand is strongly influenced by copolymer matrices. A further detailed study of RGD revealed that the characteristics of RGD include high selectivity toward Cu(II) and a rapid elution rate of Cu(II) with an aqueous solution of strong acid. The usefulness of RGD in the separation of Cu(II) has been demonstrated by means of column operation.
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Corrado SARZANINI, Ornella ABOLLINO, Massimo De LUCA, Edoardo MENTASTI
1992 Volume 8 Issue 2 Pages
201-206
Published: April 10, 1992
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If sulfonato ligands are to be used in metal ion preconcentration techniques based on ion-exchange, the chelate stability constant must be available. An ion-exchange procedure is described for the determination of the stability constants for some metal-Plasmocorinth B complexes. The results are compared with those obtained spectrophotometrically. log
K values are in good agreement for two methods. The enrichment of anionic complexes is obtained with an ion-exchange procedure.
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Takaho WATANABE, Chang Qing LIN, Shu Ming CHEN, Yoshihiro YOSHIMURA, K ...
1992 Volume 8 Issue 2 Pages
207-211
Published: April 10, 1992
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Trace amounts of chlorine dioxide in water were detected by a fluorophotometric method that was based on the quenching of fluorescence of Chromotropic acid (CA). The interference by various ions in the determination was examined. In addition, the mechanism of the quenching of fluorescence was studied. Chlorine dioxide reacted with CA at a stoichiometric ratio of 1:1 at pH 3. Moreover, the quenching constant of the reaction system, suggested that the quenching of the fluorescence is dynamic. A linear relationship was found between the fluorescence intensity and the amount of chlorine dioxide in water over a range from 0.55ppb to 1.4ppm. The reaction of CA with chlorine dioxide was not influenced very much by metal ions, such as sodium, potassium, magnesium, zinc, lead, cupric and manganese ions, nor by the sulfurous ion. The limit of detection was 0.55 ppb, a value that corresponds to the amount of 3σ from the blank level.
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Stanislaw KUS, Norbert OBARSKI, Zygmunt MARCZENKO
1992 Volume 8 Issue 2 Pages
213-218
Published: April 10, 1992
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Derivative spectrophotometry of the 3rd-order was used to determine microgram amounts of Th, U(VI) and Zr with Arsenazo III. Complexes of these metals with the reagent form in a strongly acidic (4M HClO
4) and 2-propanol-water (25%(v/v)) medium. Optimal apparatus parameters and the way of obtaining derivative spectra were established. A determination of the Th and Zr sum is possible after measuring the derivative value at 673.4nm (where the derivative spectrum of the U(VI)-Arsenazo III complex crosses the zero line). When oxalic acid masks Zr, the value of the derivative at 673.4nm is a measure of the Th concentration, and at 659.2nm-U. The proposed method allows the determination up to 30μg of U, 20μg of Th and 5μg of Zr, in various relations, without any separation step, with good precision and accuracy.
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Tomozo KOH, Noriaki TAKAHASHI
1992 Volume 8 Issue 2 Pages
219-223
Published: April 10, 1992
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Excess silver(I) from its reaction with sulfide was extracted into 1, 2-dichloroethane using Methylene Blue; the extract was measured spectrophotometrically at 657nm for the determination of sulfide. Hydrogen sulfide, separated from sample matrices, was introduced into a solution in which the hydrogen sulfide was completely converted into silver sulfide. A linear calibration graph with a negative slope was obtained over the range 8.0×10
-8-4.5×10
-6M (M=mol dm
-3) sulfide (0.026-1.44μg of S
2- in 10ml(ml=cm
3)) and the relative standard deviation was 0.93% at the 2.5 ×10
-6M sulfide level when applied to hot-spring water samples. The effective molar desorptivity for sulfide is -1.99×10
5l mol
-1 cm
-1.Good recoveries of sulfide from hot-spring waters were achieved using the proposed method.
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Birsen DEMIRATA, Huseyin AFSAR
1992 Volume 8 Issue 2 Pages
225-227
Published: April 10, 1992
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A spectrophotometric method for microdetermination of S
2O
32- has been developed. The method is based on the oxidation of thiosulfate with chlorine (Cl
2) and the residual chlorine is determined by the color reactions with o-tolidine (3, 3′-dimethylbenzidine). A linear calibration graph (0-8×10
-6M S
2O
32-) is obtained under optimum reaction conditions at room temperature and pH 11. The stoichiometric mole ratio of chlorine, Cl
2, to thiosulfate is 4. The effective molar absorptivity for thiosulfate with o-tolidine is 2.15×10
5M
-1 cm
-1 at pH 1.6. The lower limit of determination is 4.65×10
-8 or 5.21ppb (0.026μg thiosulfate in 5ml).
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M. T. M. ZAKI, F. M. El-ZAWAWY, A. A. GHORAB, M. A. ESMAILE
1992 Volume 8 Issue 2 Pages
229-232
Published: April 10, 1992
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Iron was determined spectrophotometrically in water samples and boiler scale by extracting the ion-associate formed between iron(II)-Bathophenanthroline cationic complex and Eosin anion into chloroform. The ion-associate was formed in the pH range 3.6-5.2. The method was highly sensitive and selective. The extracted species had an apparent molar absorptivity of (1.32±0.02)×10
5l mol
-1 cm
-1 at 542nm with a sensitivity index of 0.42ng cm
-2. Beer′s law was valid up to 0.42μg ml
-1 of iron in the aqueous phase. The composition of iron: Bathophenanthroline : Eosin ion- associate was 1:3:2. EDTA was used to mask Cd
2+, Co
2+, Cu
2+, Ni
2+ and Zn
2+.
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Ms. Mayuri N. GANDHI, Shripad M. KHOPKAR
1992 Volume 8 Issue 2 Pages
233-236
Published: April 10, 1992
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A rapid method has been developed for the solvent extraction separation of manganese(II). At pH 5-8, 2.5×10
-3mol/l Cryptand 221 in chloroform quantitatively extracts manganese with 1.5×10
-3mol/l Erythrosin as the counter ion. From the organic phase it was stripped with 0.5mol/l hydrochloric acid, and was determined by atomic absorption spectroscopy at 279.5nm in an air-acetylene flame. Manganese was separated from iron(III), zinc, cadmium, lead, cobalt, nickel, thallium(I), which were generally encountered in an aquatic environment. The method was extended for analysis of manganese from aerosols, sediments and effluents.
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Manjusha A. KARVE, Shripad M. KHOPKAR
1992 Volume 8 Issue 2 Pages
237-241
Published: April 10, 1992
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Zirconium and hafnuim were extracted with 0.1M of Aliquat 336S in toluene from 0.005M of ascorbic acid at pH 4.0. Both of the metals were stripped with 2M hydrochloric acid. Zirconium from the aqueous phase was determined spectrophotometrically with Arsenazo III at 650nm, while hafnium was determined with Xylenol Orange at 540nm. The separation of zirconium from hafnium was achieved by stripping hafnium with 9M hydrochloric acid followed by stripping zirconium with 2M hydrochloric acid. They were also separated from associated elements in multicomponent mixtures.
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Anoop Kumar CHHAKKAR, L. R. KAKKAR
1992 Volume 8 Issue 2 Pages
243-246
Published: April 10, 1992
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A highly simple, sensitive and selective method of determination of palladium in trace amounts is developed which is based on the reaction of α-isonitroso-2-acetonaphthone with the metal ion. The colored complex formed is quantitatively extractable into chloroform, whose λ
max lies at 430nm. The procedure eliminates the interference of several metal ions, especially the other platinum metals which adversely affect most of the determination methods of palladium. It obeys Beer′s law in the range of 0-4μgPd/ml with a Sandell′s sensitivity of 0.0026μgPd cm
-2.
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Masanori SAWAJI, Hiroshi YAMASHITA, Takashi MAEKAWA
1992 Volume 8 Issue 2 Pages
247-250
Published: April 10, 1992
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The ion flotation of rare-earth and another fifteen metal ions was investigated using octadecyliminobismethylenebisphos- phonic acid (OIMBP) as an anionic surfactant having the ability to form complexes with metal ions. The efficiency of flotation was greater than that with dodecyliminobismethylenebisphosphonic acid (DIMBP) due to its low p
Ka1, value, as well as the hydrophobic property of the alkyl chain of OIMBP. The rare-earth ions were classified into three groups according to their flotation behavior. A successive flotation procedure used to separate rare-earth ions was then proposed.
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Hiroshi YAMASHITA, Norihiko MATSUMOTO, Toshifumi OTSUBO, Hiroshi OCHI, ...
1992 Volume 8 Issue 2 Pages
251-254
Published: April 10, 1992
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The flotation of metal ions was investigated using diphenyl- and diethyl dithiophosphoric acids. From their flotation behavior, the metal ions were classified into three groups. The ions of first group [Au(III), Pd(II), Sb(III), In(III), Cd(II), Bi(III), Cu(II) and Pb(II)] floated effectively under acidic conditions. The maximum yields of the ions of second group [Zn(II), Co(II) and Ni(II)] appeared at around pH=10. On the other hand, the floatability of ions belonging to the third group [Fe(III), Ga(III), Cr(III), Cr(VI), Ti(IV), Hf(IV), Al(III) and U(VI)] was lower than those of the first and second groups. These results could be fairly well understood in terms of HSAB (hard and soft acids and bases) prediction.
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Xing-dong YAO, Jin-Chun LIU, Jie-ke CHENG, Yun'e ZENG
1992 Volume 8 Issue 2 Pages
255-258
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Using dithizone as a precolumn derivatization reagent, four species of Hg were quantitatively separated and determined by RP-HPLC. The method described has high analytical sensitivity, it can be applied for speciation analysis of Hg in natural water. The retention mechanism of Hg-Dz chelates was also investigated.
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Toshiaki KOGA, Hirofumi KAWAZUMI, Toshihiko NAGAMURA, Teiichiro OGAWA
1992 Volume 8 Issue 2 Pages
259-260
Published: April 10, 1992
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Shotaro KASHIWAGI, Kazuhiro OHMORI, Mizuo MAEDA, Makoto TAKAGI
1992 Volume 8 Issue 2 Pages
261-263
Published: April 10, 1992
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Hiroshi KAWAMOTO, Satoshi YAMAZAKI, Eiji KATOH, Kin-ichi TSUNODA, Hide ...
1992 Volume 8 Issue 2 Pages
265-266
Published: April 10, 1992
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Nobuya NAGASHIMA, Chiaki SANO, Tetsuya KAWAKITA, Yoichi IITAKA
1992 Volume 8 Issue 2 Pages
267-269
Published: April 10, 1992
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