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Volume 53, Issue 1
Displaying 1-11 of 11 articles from this issue
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Resarch Papers
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Hironobu KONISHI, Toshio TAKAYANAGI, Mitsuko OSHIMA, Shoji MOTOMIZU2004 Volume 53 Issue 1 Pages 1-6
Published: 2004
Released on J-STAGE: May 24, 2004
JOURNAL FREE ACCESSA flow titration analysis method based on flow ratiometry was developed in this study from the viewpoint of simplicity, rapidity, automation, and cost efficiency. Sample and titrant solutions react while the solutions are continuously propelled by individual pumps at different flow rates. The flow rates are accurately controlled and changed independently, and the color change of an indicator gives an equivalent point. The concentration of analyte was determined by using the ratio of the flow rate and the equivalent point. The fundamental properties of the flow titration method were evaluated through acid-base titration, and compared with the conventional manual titration. When Phenolphthalein or Cresol Red was used as an indicator added in either the sample solution or the titrant solution, linear calibration graphs were obtained for all titrations examined, including strong and weak acids. The proposed method was applied to the titration of carbonate salt using Bromocresol Green and Phenolphthalein. Two isolated end-points were obtained in one sequential measurement corresponding to carbonate and bicarbonate ions. The proposed titration method was applied to the analysis of commercial vinegar samples. The results agreed well with the ones obtained by the conventional titration method; the relative standard deviations for the end point were within 0.3%. The volume of wastewater per one measurement can be reduced down to about 100 μl by the proposed method, while a practical method requires about 50 ml.
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Kenichiro SUZUKI, Bunbunoshin TOMIYASU, Yoshimasa NIHEI2004 Volume 53 Issue 1 Pages 7-12
Published: 2004
Released on J-STAGE: May 24, 2004
JOURNAL FREE ACCESSWe made a close analysis of individual atmospheric particles sampled near to road traffic and a railroad with a personal air sampler using a field emission type scanning electron microscope. From the results of an electron microprobe analysis, the particles were classified into five types. Some particles had minute attachments on them. From comparisons of the X-ray spectra of the carrier particles and their attachments, we concluded that they were composite particles of a Fe carrier particle of railroad origin and the attached diesel exhaust particles.
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Technical Papers
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Yoshikazu NAKAMOTO2004 Volume 53 Issue 1 Pages 13-16
Published: 2004
Released on J-STAGE: May 24, 2004
JOURNAL FREE ACCESSA simple and rapid method was established for the direct determination of lead in thermally cracked gasoline using graphite-furnace AAS. Lead compounds in thermally cracked gasoline are known to be catalyst poisons in the aromatization process. Therefore, it is important to determine trace lead in thermally cracked gasoline. The volatilization of organic lead from the furnace was suppressed by the addition of iodine and the atomic absorption sensitivities of inorganic and organic lead compound became identical. Therefore, it was possible to use inorganic lead as a standard compound for the calibration curve. The detection limit and relative standard deviation were estimated to be 5 ng g−1 and 3.8% for lead determination (20 ng ml−1), respectively. The interference of thermally cracked gasolines and other metals were not observed. Analytical time of the proposed method was 20 min per one sample.
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Naoki FUJITA, Hideki KOBAYASHI, Toshiyuki ENAMI, Norikazu NAGAE, Noah ...2004 Volume 53 Issue 1 Pages 17-23
Published: 2004
Released on J-STAGE: May 24, 2004
JOURNAL FREE ACCESSA sensitive fluorometric method for the determination of aluminum has been developed using lumogallion [5-Chloro-2-hydroxy-3-(2,4-dihydroxy-phenylazo) benzenesulfonic acid]. Aluminum is known to form a fluorescent chelate with lumogallion. The aluminum-lumogallion complex was separated on a reversed-phase column within 6 minutes and detected by a fluorescence detector at 505 nm (excitation wavelength) and 574 nm (emission wavelength). The present method enabled detection down to 0.1 μg/l in an aqueous solution, and the relative standard deviation (RSD) at 50 μg/l of aluminum was less than 1%. We applied it to the determination of aluminum in not only parenteral solutions and injections including a matrix, such as vitamins, glucose and lipid, but also to amino acids as their ingredients. The recovery of this method was generally over 90%.
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Akinori ISOZAKI, Kenji YOSHIKAWA, Hisomu NAGASHIMA2004 Volume 53 Issue 1 Pages 25-30
Published: 2004
Released on J-STAGE: May 24, 2004
JOURNAL FREE ACCESSA method for the determination of 9 inorganic anions was investigated by ion chromatography using a poly(vinyl alcohol) column (Shodex IC SI-90 4E) with suppressed conductivity detection. The optimal mobile phase was 6.0 mM sodium tetraborate and 20.0 mM boric acid for the simultaneous determination a mixture of anions (F−, Cl−, NO2−, Br−, NO3−, SeO32−, HPO42−, SO42−, SeO42−) under the following conditions: flow rate, 0.8 ml/min; scavenger, 12.5 mM sulfuric acid; column temperature, 40°C. The 9 anions were efficiently separated in about 20 minutes. Calibration curves from the peak areas of 9 anions were linear with high correlation coefficients of more than 0.999, and the relative standard deviations (RSD) of the peak areas were about 1% from 10 repeated measurements. The limit of detection was from 1∼30 ng/ml for 7 anions, 28 ng/ml for SeO32− ion, and 17 ng/ml for SeO42− ion. This method was applied to the determination of selenium in organic selenium compounds. The content of selenium by this method was in good agreement with that calculated from the molecular formula. It was found that selenium in an absorbent from the combustion of a sample exists only in the selenite form.
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Notes
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Shigetomo MATSUYAMA, Jyunichi KUMON, Hisashi TAKAHAGI, Takeshi SAITO, ...2004 Volume 53 Issue 1 Pages 31-34
Published: 2004
Released on J-STAGE: May 24, 2004
JOURNAL FREE ACCESSAn accurate analysis of the amount of Bisphenol-A (BPA) in Polycarbonate (PC) was examined. BPA was extracted from PC under the Japanese food sanitation law (FSL). A new method was developed to determine the recovery under FSL by modifying the standard addition method. The recovery was determined to be 0.96 from this experiment. A comprehensive list of relevant sources of uncertainty under FSL operation was assembled. The uncertainty of the amount of BPA in PC was evaluated under the “guide to the expression of uncertainty in measurement (GUM)”. The amount of BPA in PC was evaluated: (38.89±1.59) μg/g (k = 2); here, k represents the coverage factor.
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Kazuaki WAGATSUMA2004 Volume 53 Issue 1 Pages 35-39
Published: 2004
Released on J-STAGE: May 24, 2004
JOURNAL FREE ACCESSA pulsed-voltage was applied to a glow discharge lamp for a modulation detection technique in d.c. glow discharge optical emission spectrometry. Emission signals from the glow discharge plasma were modulated by a cyclic variation in the discharge voltage so that only the desired signals would be detected without any noise with a lock-in amplifier. Molybdenum and vanadium determinations in a steel sample having contents of several 0.001 mass% was performed to estimate the analytical precision. The relative standard deviations of the intensities of the Mo I 379.65 nm and the V II 310.10 nm were 0.2∼0.6% in the modulation method, whereas they were 2.6∼3.6% in a conventional detection method. Compared with the result by the conventional detection method, the modulation method yielded a better precision in the analytical values. This technique contributes to the precise determination of minor elements alloyed in steels.
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Technical Letter
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Yuzo TAMARI, Kazuyuki TSUCHIYA2004 Volume 53 Issue 1 Pages 41-44
Published: 2004
Released on J-STAGE: May 24, 2004
JOURNAL FREE ACCESSLithium has been used as a medicine for the remedy and prevention of manic-depressive psychosis. It is, however, essential to monitor the blood lithium concentration of patients during their hospital-treatments, because the intake amount of lithium as a remedy is reflected in the blood lithium concentration, which is significantly close to a toxic level. Since continual lithium intake with daily meals is expected to prevent manic-depressive psychosis at an early stage, it is important to know the food lithium content. In this work, the effects of matrix constituents (Na+, K+, Ca2+, Mg2+ and PO43−) of food on the determination of lithium by flame photometry were studied. Since there was no interference of the matrix ions, the method was applied to food samples: fresh fish (30∼84 ng/g), dry-processed fish (731 and 1790 ng/g), table-salts (667∼2340 ng/g), infant formulas (120∼160 ng/g) and eastern medicines, such as mammalian bone and oyster-shell (18700 and 20200 ng/g).
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Satoshi NAKANO, Masako HIRANO, Bunbunoshin TOMIYASU, Yoshimasa NIHEI2004 Volume 53 Issue 1 Pages 45-48
Published: 2004
Released on J-STAGE: May 24, 2004
JOURNAL FREE ACCESSThe analysis of individual particles in a PM2.5 fraction of an urban air sample was carried out using scanning electron and electron microprobe analysis. Sampling was done using a portable cascade impactor with a silver substrate to obtain information about some lighter elements(C, N and O). It was found that particles in PM2.5 could be classified into 6 groups based on their shape and composition. Some of the groups could be attributed to specific anthropogenic origins. We observed a difference in the deformation of particles during the microprobe analysis, which might provide unique additional information concerning the classification protocols in the future.
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Kan-ichi MAKABE, Kunio TAKADA, Kazuaki WAGATSUMA2004 Volume 53 Issue 1 Pages 49-52
Published: 2004
Released on J-STAGE: May 24, 2004
JOURNAL FREE ACCESSThis paper describes a dissolution method for La-Sr-Ga-Nb (LSGN) oxide samples, which are hardly decomposed by conventional acid treatments. The LSGN oxides are not dissolved in any acid solution and do not undergo fusion with alkaline reagents, such as Na2CO3. However, the sample can undergo fusion with Na2B4O7 powder. A sample (50 mg) was fused with 1 g of Na2B4O7 in a Pt crucible, whose inside wall was covered with pre-melted Na2B4O7 (1 g). The melted product was cooled and then dissolved with a mixture of 30 ml HNO3 (1 : 1), 2.5 ml H2O2, and 1 g tartaric acid. After the addition of 1.5 ml of H2O2 and 5 ml of an Y solution (5 mg/ml) as an internal standard, the solution was diluted to 100 ml and measured by inductively coupled plasma-optical emission spectrometry. Two samples having different chemical compositions were analyzed to yield each in good agreement with the analytical values between two individual measurements.
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Yûetsu DANZAKI, Kazuaki WAGATSUMA2004 Volume 53 Issue 1 Pages 53-56
Published: 2004
Released on J-STAGE: May 24, 2004
JOURNAL FREE ACCESSFor the precise quantification of Ni-Pd-P alloys by inductively coupled plasma-optical emission spectrometry, non-spectral interferences of K should be corrected because the standard solution for P is usually prepared by using KH2PO4. An analytical method is suggested to correct the influence of K; after dissolution of the sample in HNO3-HCl, a standard solution of K is added to the sample solution so that the amount of K can be controlled to be the same as in the P standard solution with an error of ±1 mg.
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