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Volume 45, Issue 11
Displaying 1-14 of 14 articles from this issue
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Kazuhiko TSUKAGOSHI, Mizuo MAEDA, Makoto TAKAGI1996 Volume 45 Issue 11 Pages 975-986
Published: November 05, 1996
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSA concept of "Surface Imprinting" has been proposed by the present authors. First, we prepared a metal ion-imprinted microsphere on the basis of the concept. The imprinted microspheres as a new metal ion-selective adsorbent were synthesized by seeded emulsion polymerization of divinylbenzene, styrene, butyl acrylate, and methacrylic acid. The imprinted structure was introduced on the carboxylated microsphere by Surface-Imprinting, in which the carboxyl groups were reorganized through complexation with metal ions on the surface, and then fixed by crosslinking polymerization in their specific orientation. Cu(II), Ni(II), and Co(II)-imprinted microspheres were obtained as submicron particles with average diameters of 0.550.60 μm.They were immediately used as a metal ion-selective adsorbent without any further treatment, such as grinding or sieving. The adsorption behaviors of metal ions {Cu(II), Ni(II), and Co(II)} were examined, and the imprinted effects were verified on these imprinted microspheres. The imprinted microspheres adsorbed the corresponding guest ion more effectively than did unimprinted ones. Furthermore, a Cu(II)-imprinted microsphere was studied in detail in order to obtain information about the origin of the imprinting effect. Unimprinted and Cu(II)-imprinted microspheres were prepared under several pH (4.0, 5.0, 5.6, or 6.0) conditions in the imprinting step. The obtained microspheres were characterized for particle form, size-distribution pattern, average diameter, Cu(II)adsorption behavior, and so on. Spectroscopic studies were also performed on Cu(II)-loaded microspheres.The collected data indicate that the origin of the imprinting effect on a Cu(II)-imprinted microsphere is an interaction between Cu(II)and the carboxylate group at the aqueous-organic interface, supporting the concept of Surface Imprinting.View full abstractDownload PDF (2181K) -
Kunihiro WATANABE, Satoru TAKAHASHI, Masayuki ITAGAKI1996 Volume 45 Issue 11 Pages 987-991
Published: November 05, 1996
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSCatalytic analysis of Mn(II)in tap water using 2-hydroxy-1-(2-hydroxy-4-sulfo-1-naphthylazo)-3-naphthoic acid (NANA)has been described. The decomposition reaction of NANA with hydrogen peroxide was catalyzed by Mn(II)in alkaline medium. The sensitivity of the method was very high;however, the selectivity was not sufficiently high for the determination of Mn(II)in tap water. Therefore, the effect of some masking agents was examined. Triethanolamine was selected in spite of decreasing the sensitivity for Mn(II). The optimum conditions for Mn(II)determination in the presence of triethanolamine were as follows : pH 10.4, CAPS (0.02 M) as buffer reagent, NANA (6.85×10-5 M), triethanolamine (0.27 M), hydrogen peroxide (0.5%), and temperature 30°C. As the result, the RSD was 5.4% (n=6) at 0 ppb of Mn(II). The detection limit was 0.06 ppb (S/N=3). A calibration curve was made between ln (A1/A6)and Mn(II)concentration, where A1 and A6 were the absorbances of NANA at 1 min and 6 min after the start of the decomposition reaction, respectively. The determination range was 0.2 ppb to 1.0 ppb. Diversions, e.g., Fe(III)up to 100-fold, and Cu(II)and Zn(II)up to 125-fold the Mn(II)concentration (0.8 ppb), were tolerated for the determination of Mn(II)by using triethanolamine as the masking agent. The results of trace Mn(II)determination in tap water showed good agreement with the values obtained by graphite furnace AAS.View full abstractDownload PDF (696K) -
Tomonori TSUBOI, Takahiro NAKAMURA, Akiko MATSUKURA, Shoji MOTOMIZU1996 Volume 45 Issue 11 Pages 993-998
Published: November 05, 1996
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSTrace amounts of hydrazine in boiler feed water were determined by a flow injectionspectrophotometric method with p-dimethylaminobenzaldehyde (DMBA). The DMBA solution for the color development was prepared by dissolving it in diluted hydrochloric acid without using any organic solvents such as alcohols. The reagent solution proposed in this work had several advantages, compared with the alcoholic solution usually used in the batchwise spectrophotometric method. The solution was easily prepared with hydrochloric acid and water, stable for longer times and did not evolve when the solution was mixed with sample solutions, and the waste treatment was easier than for the alcoholic solution. A carrier (H2O)and the reagent solution were propelled at flow rates of 1.0 ml min-1 and 0.6 ml min-1, respectively. They were merged to flow into a reaction coil (0.6 mm i.d.×6 m) kept in a temperature-controlled air bath at 80°C.Samples were injected into the carrier stream, and the reaction product was measured at 458 nm. Metal ions and ammonia did not interfere with the determination of hydrazine. The calibration graph was linear up to 100 ppb of hydrazine, and the detection limit corresponding to a signal to noise ratio of 3 was 0.2 ppb.Relative standard deviations for seven replicates of 5, 50 and 100 ppb of hydrazine were 1.1, 0.9 and 0.4%, respectively. The proposed method was applied to the determination of hydrazine in boiler feed water samples.View full abstractDownload PDF (774K) -
Jun OJIMA1996 Volume 45 Issue 11 Pages 999-1004
Published: November 05, 1996
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSTo evaluate air contamination of living and working environments with dust, information on particle size of the dust is essentially needed. Therefore, a convenient method to determine particle size distribution is valuable for an assessment of pollution. In this study, an infrared spectrometry was applied to measuring particle size distribution of quartz dust.The estimation of size distribution is based on dependence of infrared absorbance on the particle size of sample dust. Application of multiple regression analysis allowed calculation of the particle sizes with a vector of the absorbance peaks and regression coefficients. The particle size distribution was gotten as a vector of cumulative weight percent. The particle size distribution of standard quartz determined by the infrared method was in good agreement with that of the same quartz sample determined by a centrifugal particle size analyzer, and the validity of this method was proved.View full abstractDownload PDF (952K) -
Yoshisuke NAKAMURA, Katsuyuki TAKAHASHI, Ryosuke HASEGAWA1996 Volume 45 Issue 11 Pages 1005-1012
Published: November 05, 1996
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSAnalytical performance of a long torch for axially (end-on) viewed horizontal inductively coupled plasma atomic emission spectrometry (ICP-AES) was examined using a high resolution echelle spectrometer with wavelength modulation and second derivative detection.Optimum operating conditions were studied for 24 elements having spectral lines between 210 and 770 nm. Compared to conventional torch measurement, net emission intensities of the elements increased by 2040% and background intensities of water blanks decreased by 3050%. The values of S/σ (S:signal intensity of an analyte, σ:standard deviation of the background intensities) and BEC(background equivalent concentration) were improved for all of the elements.Limits of detection were improved by 1.5-fold (Be) and 6.9-fold (Al). Repeatability given by the relative standard deviation of the net emission intensities was also improved for each element. The dynamic range for each element was about five orders of magnitude. The emission line (427.673 nm) of Ca showed interference by Na of above 50mg dm-3, but was scarcely affected by phosphoric acid of below 3 v/v%. Determination of the main and trace elements of the standard reference material, NIST SRM 1643c (water), gave analytical values which agreed well with its certified values.View full abstractDownload PDF (1180K) -
Kiwao KADOKAMI, Kenji SATO, Tomomi IWAMURA, Yoshifumi HANADA1996 Volume 45 Issue 11 Pages 1013-1018
Published: November 05, 1996
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSThe authors have developed an analytical method for hydrophilic alcohols, 1-propanol, 2-propanol, 1-butanol, 2-butanol and tert-butanol, in water and sediment samples by solid-phase microextraction coupled with GC/MS. Extraction efficiencies of the alcohols from water were dramatically improved by adding potassium carbonate as a salting-out reagent.The mean recovery of the alcohols from water at concentrations of 15 to 1.0 μg/l was 94%, and the mean relative standard deviation was 12%. The detection limits of the alcohols ranged from 0.63 to 4.3 μg/l.In order to analyze sediment samples, the alcohols were first extracted with water and the following procedures were carried out in the same manner as for water samples. The mean recovery of the alcohols from sediment samples at 20 μg/kg was 94%, and the mean relative standard deviation was 21%. The detection limits of the alcohols ranged from 6.9 to 84μg/kg(wet). Analysis of real environmental samples from a sea sediment detected 1-propanol and 2-propanol at 140 and 500 μg/kg(dry), respectively.View full abstractDownload PDF (1029K) -
Tatsushi WAKISAKA, Naoki MORITA, Shoji TANAKA, Taketoshi NAKAHARA1996 Volume 45 Issue 11 Pages 1019-1023
Published: November 05, 1996
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSEnergy-dispersive X-ray fluorescence (EDXRF) measurements using the monochromatic excitation of a Mo-Kα X-ray tube (17.44 keV) have been established for the direct determination of trace arsenic.A detection limit of 0.08μg g-1 in light-element matrices was obtained, and the relative standard deviation for ten determinations of 2μg g-1arsenic is 1.2%.The application of the proposed method to the arsenic limit test (Japanese Pharmacopoeia, Japanese Standards of Cosmetic Ingredients) was investigated.The recoveries of arsenic in various samples were satisfactory.Compared with the conventional arsenic limit test, the proposed method is much easier to operate because sample preparation is unnecessary;furthermore, the detection limit, reproducibility and recovery are higher.The EDXRF method is useful as a rapid substitute method (30 min) of the arsenic limit test.View full abstractDownload PDF (927K) -
Tatsushi WAKISAKA, Naoki MORITA, Shoji TANAKA, Taketoshi NAKAHARA1996 Volume 45 Issue 11 Pages 1025-1031
Published: November 05, 1996
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSEnergy-dispersive X-ray fluorescence (EDXRF) measurements using three monochromatic excitations (W-Lβ 9.7 keV, Mo-Kα: 17.4 keV and W-continuum: 40 keV) have been established for the direct determination of trace heavy metals in light-element matrices. The detection limits are 0.080.64μg g-1 (Pb;0.25μg g-1, mean value;0.35μg g-1), ascertained for the 26 elements examined (VPb and Bi). The precisions were found to be within 1% R. S. D. at 20μg g-1 for all of the elements. The application of this method to the heavy metals limit test (Japanese Pharmacopoeia, Japanese Standards of Cosmetic Ingredients) was investigated.The recoveries of Pb and heavy metals in various standard samples were satisfactory. Compared with the conventional heavy metals limit test, the proposed method is much easier to operate without sample preparation;furthermore, the detection limit, reproducibility and recovery are higher. The present EDXRF is useful as a rapid and simple substitute method(3060 min)of the heavy metals limit test.View full abstractDownload PDF (1205K) -
Tadao SAKAI, Shio WATANABE, Noriko OHNO1996 Volume 45 Issue 11 Pages 1033-1039
Published: November 05, 1996
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSMolecular tetrabromophenolphthalein ethyl ester (H·TBPE), a triphenylmethane dye, reacts with aliphatic alkylamines to form red charge-transfer complexes in 1, 2-dichloroethane. Its association is based on the basicity of amines and a hydrogen bridge between the nitrogen atom in alkylamines and the phenol group in the TBPE molecule. The primary, secondary and/or tertiary alkylamines form RH2N·H·TBPE, R2HN·H·TBPE and R3N·H·TBPE.The association constants for each amine were determined. On the other hand, all of the charge-transfer complexes studied showed thermochromism with a change in the measuring temperature at 20 and 60°C. The thermodynamic characteristics for each amine family were specific. The thermochromism can be applied to fractional analyses for tertiary amines and secondary amines in the presence of a primary amine.View full abstractDownload PDF (1019K) -
Hisatake NARASAKI, Kumiko HAYASHI, Atsuko HOSHINA1996 Volume 45 Issue 11 Pages 1041-1044
Published: November 05, 1996
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSStibine, generated by mixing a 0.7 M sulfuric acid solution of antimony(III)with a 2% sodium tetrahydroborate solution in a mixing coil for 30 s, was separated from solution in a gas-liquid separator, and then swept into an electrically heated quartz furnace by manipulating electromagnetic relays and timers.Sharp peaks were recorded on a recorder. The detection limit (three times signal to noise ratio) for antimony(III)was 0.6 ng ml-1.It took five minutes for one sample measurement.Interference from transition metals could eliminated by Chelex 100 separation.Antimony(V)was reduced by using a 0.1 M potassium iodide solution. The accuracy, checked with a biological standard reference material obtained from the National Institute of Standard and Technology (NIST) of USA, was within the certified value. Antimony in river water was determined by the present method.View full abstractDownload PDF (505K) -
Shigeo SAWADA, Toshiyuki OSAKAI, Mitsugi SENDA1996 Volume 45 Issue 11 Pages 1045-1049
Published: November 05, 1996
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA small-type electrolytic cell for polarographic studies of ion-transfer at the oil/water interface with an ascending water electrode was constructed and its performance was examined. A small orifice for channeling ascending water drops into the oil phase was drilled in the center of a Teflon disk (10mm diameter, 5mm thickness), which was then incorporated into a three-electrode type electrolytic cell requiring only 0.5 cm3of the oil phase. This electrolytic cell was tentatively applied to study some ion transfer processes at the nitobenzene/water interface, viz. (1) the transfer of tetramethylammonium ion, and (2) the facilitated transfer of K+ by valinomycin. The current-potential curves due to the ion transfer processes were as well-defined as those obtained with a conventional, large-type electrolytic cell. For the transfer process (2), the current maximum appeared around the limiting current, but it was suppressed effectively by the addition of Span®20 (sorbitan monolaurate) in the nitrobenzene phase.View full abstractDownload PDF (912K) -
Shigeru TERASHIMA, Masahiro TANIGUCHI1996 Volume 45 Issue 11 Pages 1051-1058
Published: November 05, 1996
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA method to determine the chemical forms of As and Sb in geological reference samples is described. It combines a sequential extraction procedure with hydride generation and AAS. The sequential extraction solutions were classified into the following five types: 1) 1 M magnesium nitrate of pH 7 for the ion exchange and adsorbed fraction; 2)0.05 M ethylendiaminetetraacetic acid disodium salt(EDTA)for the EDTA soluble fraction; 3) a mixture of 0.2 M ammonium oxalate, 0.2 M oxalic acid, 0.1 M ascorbic acid and 0.01 M HCl for the oxide fraction; 4) 0.7 M sodium hypochlorite for the sulfide fraction;and 5) a mixture of HF, HNO3, HClO4 and KMnO4 for the residual fraction.For samples treated with the 0.05 M EDTA, almost all of the As and Sb in the carbonate minerals and small amounts of both elements in the oxide phases were extracted. In some cases sulfides such as As2S3 and Sb2S3 were changed to oxides and/or EDTA soluble forms during sample processing. In the speciation of As and Sb in geological reference samples, igneous rocks are dominated by residual forms reflecting their mineral composition, whereas sediments and sedimentary rocks are generally richer in oxide forms. This method was successfully applied to the speciation of As and Sb in a variety of geological reference samples.View full abstractDownload PDF (1307K) -
Katsumi UCHIYAMA, Chikahiro TERADA, Keiko OHSAWA, Kazuo IMAEDA1996 Volume 45 Issue 11 Pages 1059-1062
Published: November 05, 1996
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSPhotoacoustic spectrometry (PAS) was applied to the determination of thermal diffusivity of polyacrylamide gel (7.5% gel concentration), which was previously dried to film. Carbon black was placed on the polyacrylamide gel surface and then stuck onto a piece of double side adhesive tape, the other side being previously stuck to a sample holder for the photoacoustic cell.By phase variation of PAS, thermal diffusivity (α) of the gel was obtained at 2.02.4× 10-3 cm2/s. Ovalbumin electrophoresed on a slab of polyacrylamide gel was silver-stained and then the depth of silver deposition from the surface was determined by photoacoustic amplitude examination. Photoacoustic amplitude was plotted against thermal diffusion length μs, which was defined as μs=(2α/ω)1/2by varing the frequency (ω) of the laser beam. The silver stained layer was determined to be 18-20 μm to give an inflection point of the photoacoustic amplitude vs. thermal diffusion length of the gel. The value obtained by this method was smaller than the one obtained by microscopic observation.View full abstractDownload PDF (608K) -
Syuji OKUYAMA1996 Volume 45 Issue 11 Pages 1063-1064
Published: November 05, 1996
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSMultivariate analyses (quantification IV, cluster analysis and principal component analysis) were applied to some signals obtained from the X-ray diffraction method, the spectrophotometric method, Fourier transform infrared spectroscopy and gas chromatography. The reproducibility and accuracy of an analysis of the desired components in binary and ternary systems were investigated. Multivariate analyses are particularly useful, because in forensic science the amount of sample is usually too small to measure repeatedly. In the conventional calibration method, one peak in one sample was generally used for the determination, and the peak for the determination was arbitrarily selected by the analyst. In this method, many peaks in one sample were selected according to a definite rule, and were used for the determination by multivariate analyses. By this method, the analysis of inorganic and organic substances could be accomplished with a high degree of reproducibility and accuracy.View full abstractDownload PDF (293K)
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