Analytical Sciences

Winter Conference on Flow Injection Analysis

Harald HANSEN

1989 Volume 5 Issue 2 Pages 127
Published: 1989
Released on J-STAGE: July 27, 2007

DOIhttps://doi.org/10.2116/analsci.5.127

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Chemical Analyses of Seawater for Trace Elements Recent Progress in Japan on Clean Sampling and Chemical Speciation of Trace Elements A Review

Eiichiro NAKAYAMA, Yoshimi SUZUKI, Kitao FUJIWARA, Yasushi KITANO

1989 Volume 5 Issue 2 Pages 129-139
Published: April 10, 1989
Released on J-STAGE: June 30, 2006

DOIhttps://doi.org/10.2116/analsci.5.129

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Progress in clean techniques that includes clean sampling, storage, treatment and analysis of seawater samples is essential for the exact determination of trace elements in seawater. Japanese marine chemists have worked vigorously to establish clean techniques and the accumulation of data. Results have met with a measured amount of success, as briefly shown in this review paper. The behavior and distribution of trace elements in seawater are dependent on multifaceted chemical, physical and biological processes occurring in the ocean. Thus, the chemical speciation of inorganic and organic species of trace elements in seawater has been eagerly studied. Specifically, the dissolved states of oxyacid elements such as Cr, I, Se, Te, As and Sb have been determined by using various procedures and methods developed by Japanese marine chemists. The present paper reviews the procedures of chemical speciation for inorganic species of Cr, I, Mn, Mo; W, Se, Te, As and Sb as well as those for organic species of Cr, Ge, I, Se, Hg, Fe and Cu in seawater. The difficulty in obtaining exact measurements of the total concentrations of trace elements in seawater is shown concerning Fe, Cu, Zn and Se as examples.

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Structure Identification Using the Nuclear Magnetic Resonance Spectral Database

Osamu YAMAMOTO, Kikuko HAYAMIZU, Masaru YANAGISAWA

1989 Volume 5 Issue 2 Pages 141-146
Published: April 10, 1989
Released on J-STAGE: June 30, 2006

DOIhttps://doi.org/10.2116/analsci.5.141

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A computer software system for structure identification using nuclear magnetic resonance (NMR) spectra is described. For this purpose search files are created from full spectral patterns. In the search files peak information is stored, including positions and intensities as well as other search items such molecular formula, molecular, weight, etc. in order to assist in identification. The¹H-NMR area intensity is used rather than the peak height intensity which is used in other spectroscopic methods. This enables us to utilize, in addition to peak positions, the ranges of peak positions for the complex patterns characteristic of¹H-NMR spectra as input data for the identification. The problems and limitations of the structure identification by¹H-NMR spectra relating to the frequency dependence are discussed. A brief description is given regarding structure identification by¹³C-NMR spectra in connection with¹H-NMR spectra.

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Laser Induced Photoacoustic Spectrometry with Single Particle Sample

Atsushi YOSHINAGA, Yu-Ming HSIEH, Tsuguo SAWADA, Yohichi GOHSHI

1989 Volume 5 Issue 2 Pages 147-149
Published: April 10, 1989
Released on J-STAGE: June 30, 2006

DOIhttps://doi.org/10.2116/analsci.5.147

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LIPAS (laser induced photoacoustic spectrometry) has been adopted for quantitative analysis of a single particle.To avoid the effects of the sample form (such as particle or coarse powder) upon the intensities of strong light absorption and strong light scattering, analysis using a single particle was carried out instead of diluting with optically transparent material. A solid adsorbent particle such as XAD-2 was used, on which trace elements in solutions were adsorbed in the form of metal-oxine (oxine=8-quinolinol) complexes. Here, 0.02-20ng zinc adsorbed on one XAD-2 particle could be detected quantitatively. Moreover, combination of LIPAS with both a single particle adsorbent and enrichment technique was found to be an excellent method for quantitative analysis for trace materials.

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Recycling Nebulization-Sample Introduction System for Indutively Coupled Plasma Atomic Emission Spectrometry

Kaneharu KATO, Kyoichiro TAKASHIMA

1989 Volume 5 Issue 2 Pages 151-156
Published: April 10, 1989
Released on J-STAGE: June 30, 2006

DOIhttps://doi.org/10.2116/analsci.5.151

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A recycling nebulization-sample introduction system which exhibits the long-term stability of analyte emission signals while consuming small sample volumes was constructed for inductively coupled plasma atomic emission spectrometry. The present system is composed of five main parts: i.e., a spherical cyclone spray chamber, two commercial concentric nebulizers, two 3-way stopcocks, an aerosol transport tube with heater, and a commercial concentric three-tube plasma torch. It is based on the spray chamber where the two nebulizers are mounted (twin-nebulizer configuration): one is for introduction of a sample or a rinse solution into the spray chamber, and the other one is for recycling nebulization of the solution introduced. The nebulizers are easily demountable symmetrically and horizontally outside the spray chamber. Analytical performance and nebulization characteristics are described in comparison with a conventional sample introduction system. A stable signal of analyte emission intensity was extended to 20min for 1ml of sample under the ordinary condition of 0.6l/min carrier gas flow rate.

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Determination of Sudan III, Sudan IV and Sudan Red 7B in Water by High Performance Liquid Chromatography after Mixing Extraction

Makoto NAGASE, Takahiko MATSUEDA, Yasuhiko OSAKI

1989 Volume 5 Issue 2 Pages 157-160
Published: April 10, 1989
Released on J-STAGE: June 30, 2006

DOIhttps://doi.org/10.2116/analsci.5.157

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A method is described for the determination of Sudan III, Sudan IV and Sudan Red 7B in river and seawaters. These dyes were extracted with hexane by mixing extraction from samples. The resulting materials were dried, dissolved in methanol and analyzed by high performance liquid chromatography with a variable-wavelength UV-VIS spectrophotometric detector. The separation of the dyes was possible using a LiChrosorb RP-18 column (25cm×4.0mm i.d.). The recoveries were 72.9-92.8% from river water and 94.6-98.1% from seawater, with the relative standard deviations below 4% (n=5) when 2μg of each dye was added to a 400-ml sample of water. The lower limits of determination were 4.4ng (0.55μg/l) for Sudan III, 5.3ng (0.66μg/l) for Sudan IV and 4.9ng (0.61μg/l) for Sudan Red 7B. This method allows simultaneous determination of the 3 dyes in water with simplicity, sufficients ensitivity and accuracy.

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Detection of Hydroxyl Radicals with Salicylic Acid

Yoshihiro YOSHIMURA, Kiyoshi OTSUKA, Katsumi UCHIYAMA, Hiroshi TANAKA, ...

1989 Volume 5 Issue 2 Pages 161-164
Published: April 10, 1989
Released on J-STAGE: June 30, 2006

DOIhttps://doi.org/10.2116/analsci.5.161

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Salicylate was hydroxylated by hydroxyl radicals formed in the system composed of hypoxanthine-xanthine oxidase and a ferrous iron salt. The hydroxylated products of salicylate, namely, 2, 3-dihydroxybenzoate, 2, 5-dihydroxybenzoate and 2, 6-dihydroxybenzoate, were identified by thin-layer chromatography and high performance liquid chromatography (HPLC). The relative standard deviation was 7.98% (n=5) and the detection limit for 2, 5-dihydroxybenzoate formed from salicylate was 0.555ng/ml (S/N=3). This method was employed for the detection of hydroxyl radicals generated in polymorphonuclear leukocytes during stimulation by opsonized zymosan. The generation of hydroxyl radicals increased with increasing incubation period up to 40min.

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Silver Ion-Selective Polymeric Membrane Electrode Based on Lipophilic Monothiacrown Ether

Masatoshi OUE, Kazuhiro AKAMA, Keiichi KIMURA, Minoru TANAKA, Toshiyuk ...

1989 Volume 5 Issue 2 Pages 165-169
Published: April 10, 1989
Released on J-STAGE: June 30, 2006

DOIhttps://doi.org/10.2116/analsci.5.165

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Dodecyl-monothia-16-crown-5, which contains one sulfur and four oxygen atoms, was synthesized and tested for its usefulness as a neutral carrier for Ag⁺-selective polymeric membrane electrodes. Employment of a Ag⁺-complex of the thiacrown ether as the membrane active material instead of the thiacrown ether itself allowed the better potential response. The resulted ion selective electrodes exhibited Nernstian response to Ag⁺ in a wide activity range. The ion selectivities against alkali, alkaline-earth, and heavy metal ions, NH₄⁺, and H⁺ were quite excellent. Silver ion in artificial samples was successfully determined by Ag⁺ potentiometric titration and Gran′s plot method with the Ag⁺ electrode.

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Electrolytic Generation of Cadmium(II) and Its Application to Coulometric Assays of Gallium and Indium

Tatsuhiko TANAKA

1989 Volume 5 Issue 2 Pages 171-174
Published: April 10, 1989
Released on J-STAGE: June 30, 2006

DOIhttps://doi.org/10.2116/analsci.5.171

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The current efficiency for the electrolytic generation of cadmium(II) from an amalgamated cadmium anode was investigated as a function of electrolyte composition and current density. The generation of cadmium(II) proceeded with 100% current efficiency over a wide range of current density, when both sodium chloride and sodium acetate concentrations were higher than 0.1M. Thus, the use of cadmium(II) instead of zinc(II) as a coulometric titrant for complexometry (T. Tanaka et al., Bunseki Kagaku, 33, E9 (1984)) reduced the error in amperometric indication of the end point. With 0.5M sodium chloride-0.5M sodium acetate medium of pH 5.5, high-purity gallium and indium were assayed coulometrically. The method was based on the reaction of the sample metal ion with a known excess of EDTA, the unconsumed EDTA being back-titrated with electrolytically generated cadmium(II). The relative standard deviation of the results was about 0.01% for both metals in the range of 200-300mg.

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Simultaneous Spectrophotometric Determination of Traces of Bromide and Iodide Based on Their Catalytic Effects on Pyrocatechol Violet-Hydrogen Peroxide Reaction

Norinobu YONEHARA, Tetsuya YAMANE, Takashi TOMIYASU, Hayao SAKAMOTO

1989 Volume 5 Issue 2 Pages 175-179
Published: April 10, 1989
Released on J-STAGE: June 30, 2006

DOIhttps://doi.org/10.2116/analsci.5.175

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A kinetic method is presented for the simultaneous determination of bromide and iodide based on the different catalytic behaviors during the oxidation of Pyrocatechol Violet by hydrogen peroxide in strongly acidic solution. The reaction is monitored spectrophotometrically at 492nm. The slope and the intercept at t=0 of the second-order plot are the parameters for the determination of iodide and bromide, respectively, which are simultaneously obtained by a single kinetic run. Mixture of these anions, in the ranges 0.01-0.1mg I-′ bromide and 0.005-0.05mg 1-′ iodide, can be determined within an error of ca .10%

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Electrothermal Atomic Absorption Spectrometric Determination of Germanium by Coprecipitation with Hafnium Hydroxide

Joichi UEDA, Toshio KITADANI

1989 Volume 5 Issue 2 Pages 181-184
Published: April 10, 1989
Released on J-STAGE: June 30, 2006

DOIhttps://doi.org/10.2116/analsci.5.181

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Various trace amounts of germanium in water were concentrated by the Coprecipitation technique with hafnium hydroxide, and determined by graphite furnace atomic absorption spectrometry. At pH 7.5-10.5, hafnium hydroxide coprecipitates almost completely 0.3-10μg of germanium from pure solution (less than 200ml) and more than 80% of germanium from natural waters (less than 200ml). The atomic absorbance of germanium is increased about 6 times by the presence of hafnium. The calibration curve is linear from 12 to 400ng ml-1 of germanium. The detection limit (signal/noise=2) was 0.3ng ml-1 of germanium in 200ml of the initial pure solution. This method was successfully applied to the determination of germanium in spring water, using the standard addition method.

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Adsorption Behavior of Copper Ion on Cellulose-Triacetate Polymer Containing α-Hydroxyoxime Compounds

Takehiro KOJIMA, Naruhito ONO, Yasumasa SHIGETOMI, Yuroku YAMAMOTO

1989 Volume 5 Issue 2 Pages 185-188
Published: April 10, 1989
Released on J-STAGE: June 30, 2006

DOIhttps://doi.org/10.2116/analsci.5.185

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A series of α-hydroxyoximes were synthesized and characterized. A new type of the adsorbent, cellulose triacetate (TAC) powder containing α-hydroxyoximes, has been prepared by dissolving cellulose triacetate with α-hydroxyoxime in 1, 2-dichloromethane, and pouring the mixture in hot water. The adsorption aspects of the TAC powder for the copper(II) ion from dilute aqueous solution were investigated for five kinds of α-hydroxyoximes. TAC powder containing α-hydroxyoximes was found to be useful for the preconcentration or the selective trapping of specific metal ions such as copper(II), nickel(II), at a low concentration level.

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Selective Recovery of Trace Scandium from Acid Aqueous Solution with (2-Ethylhexyl hydrogen 2-ethylhexylphosphonate)-Impregnated Resin

Yoshito WAKUI, Hideyuki MATSUNAGA, Toshishige M. SUZUKI

1989 Volume 5 Issue 2 Pages 189-193
Published: April 10, 1989
Released on J-STAGE: June 30, 2006

DOIhttps://doi.org/10.2116/analsci.5.189

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A reagent-impregnated resin prepared from 2-ethylhexyl hydrogen 2-ethylhexylphosphonate (PC-88A) and Amber-lite XAD-7 beads was examined in order to apply it to the selective recovery of scandium. The distribution ratio of scandium to the present resin is extremely high (log D_??_6), even in highly concentrated acids. The separation factors between Sc(III) and other common metal ions including Fe(III) are sufficiently large to allow effective separations. The selective recovery of Sc(III) from the acid-leached solutions of wolframite and tin slag has been carried out by using the present resin as the column stationary phase. The retained Sc(III) is released from the resin quantitatively by elution with 4-methyl-2-pentanone. Scandium has been isolated as a precipitate by treating Sc-PC-88A complex with oxalic acid in ethanol.

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Liquid-Liquid Distribution Behavior of Ion Association Complexes of Dihalogenocuprate(I) Anions with Azo-Dye Cations as Counter Ions

Koichi YAMAMOTO, Shoji MOTOMIZU

1989 Volume 5 Issue 2 Pages 195-200
Published: April 10, 1989
Released on J-STAGE: June 30, 2006

DOIhttps://doi.org/10.2116/analsci.5.195

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Separation of Palladium(II) from Aqueous Chloride Solution Using Tridodecylammonium Chloride in Toluene as Extractant

A. MASANA, M. HIDALGO, V. SALVADÓ, M. MUÑOZ, M. VALIENTE

1989 Volume 5 Issue 2 Pages 201-205
Published: April 10, 1989
Released on J-STAGE: June 30, 2006

DOIhttps://doi.org/10.2116/analsci.5.201

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A study on the separation of Pd(II) from chloride solutions by a solvent extraction process is presented. Organic solutions containing tridodecylammonium chloride (TLAHCl) in toluene were used as the extracting phase. The process determines the chemical species produced in the extraction reactions by analyzing, over a wide range of conditions, the equilibrium state of the system. The study, based on metal distribution measurements, includes the effect of aqueous chloride ion on the stability of the extracted species which affect the yield of palladium extraction. The extraction phenomena can be explained by assuming the following reactions: Pd²⁺+2Cl-+ TLAHCI_??_PdCl₂TLAHCl, Pd²⁺2Cl-+2TLAHCl_??_PdCl₂(TLAHCl)₂, Pd²⁺+2Cl-+3TLAHCl_??_PdCl₂(TLAHCI)₃. These reactions give the best fit to the experimental information. The results obtained at 1.0, 2.0 and 3.0mol dm^-3 of aqueous chloride have been correlated in terms of ionic interactions.

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Laser Ablation/Supersonic Jet/Fluorescence Spectrometry of Large Aromatic Hydrocarbon

Katsunori TANAKA, Totaro IMASAKA, Nobuhiko ISHIBASHI

1989 Volume 5 Issue 2 Pages 207-208
Published: 1989
Released on J-STAGE: July 27, 2007

DOIhttps://doi.org/10.2116/analsci.5.207

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Monodansyl Cadaverine as a Versatile Reagent for Fluorogenic Precolumn Derivatization of Carboxylic Acids

Yong-Moon LEE, Hiroshi NAKAMURA, Terumi NAKAJIMA

1989 Volume 5 Issue 2 Pages 209-210
Published: 1989
Released on J-STAGE: July 27, 2007

DOIhttps://doi.org/10.2116/analsci.5.209

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2, 6-Di-O-methylated Cyclodextrin-Bonded Stationary Phases for Liquid Chromatography

Minoru TANAKA, Hiroshi INADA, Yoshihiro KAWAGUCHI, Toshiyuki SHONO

1989 Volume 5 Issue 2 Pages 211-213
Published: 1989
Released on J-STAGE: July 27, 2007

DOIhttps://doi.org/10.2116/analsci.5.211

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Chromatography with pH-Gradient Elution of Dissolved Humic Substances in River Water

Kazuya OHCA, Yuji ARITOMI, Hiroshi OHTSU

1989 Volume 5 Issue 2 Pages 215-216
Published: 1989
Released on J-STAGE: July 27, 2007

DOIhttps://doi.org/10.2116/analsci.5.215

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Capillary Isotachophoretic Separation of Catechol and Its Derivatives Using the Reaction with Terminating Ion

Shunitz TANAKA, Takashi KANETA, Hitoshi YOSHIDA

1989 Volume 5 Issue 2 Pages 217-218
Published: 1989
Released on J-STAGE: July 27, 2007

DOIhttps://doi.org/10.2116/analsci.5.217

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Capillary Isotachophoretic Determination of Phosphate after Enrichment on Membrane Filter as Ion Pair of Molybdophosphate with Bis[2-(5-chloro-2-pyridylazo)-5-diethylaminophenolato]cobalt(III)

Mitsuhiko TACA, Masahiko KAN, Fumio KOMATSU, Shunitz TANAKA, Hitoshi Y ...

1989 Volume 5 Issue 2 Pages 219-220
Published: 1989
Released on J-STAGE: July 27, 2007

DOIhttps://doi.org/10.2116/analsci.5.219

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A Flow Injection System for the Simultaneous Determination of Two Components in a Single Injection and with a Single Detector

Takeshi YAMANE, Eiichi GOTO

1989 Volume 5 Issue 2 Pages 221-223
Published: 1989
Released on J-STAGE: July 27, 2007

DOIhttps://doi.org/10.2116/analsci.5.221

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Electroanalytical Aspects of Pulse Polarography for Determination of Germanium(IV)

Kiyoshi HASEBE, Satoshi HIKIMA, Teiji KAKIZAKI, Hitoshi YOSHIDA

1989 Volume 5 Issue 2 Pages 225-226
Published: 1989
Released on J-STAGE: July 27, 2007

DOIhttps://doi.org/10.2116/analsci.5.225

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Photochemical Decomposition for Detection of Tetrachloroethene in the Gas and Liquid Phase with Solid Silver/Silver Iodide Electrolyte-Sensor

Reinhard NIESSNER, Martin BACKER

1989 Volume 5 Issue 2 Pages 227-228
Published: 1989
Released on J-STAGE: July 27, 2007

DOIhttps://doi.org/10.2116/analsci.5.227

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Photodecomposition of Chlorinated Hydrocarbons by Titanium Dioxide for the Determination of Total Organochlorine Content in Water

Tsugio KOJIMA, Yasushi ASADA, Wei-Ping LI, Fujio MORISHITA

1989 Volume 5 Issue 2 Pages 229-230
Published: 1989
Released on J-STAGE: July 27, 2007

DOIhttps://doi.org/10.2116/analsci.5.229

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Role of Trioctylphosphine Oxide on Extraction Fluorometric Determination of Gallium(III) with 2, 2'-Dihydroxy-4, 4'-dimethylazobenzene

Kunihiro WATANABE, Massoud HOJJATIE, Takeshi SHIMA, IZUO AOKI

1989 Volume 5 Issue 2 Pages 231-233
Published: 1989
Released on J-STAGE: July 27, 2007

DOIhttps://doi.org/10.2116/analsci.5.231

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Simultaneous Determination of Total Phosphorus and Total Nitrogen by Flow Injection System

Masaya AOYAGI, Yoshiaki YASUMASA, Akemi NISHIDA

1989 Volume 5 Issue 2 Pages 235-236
Published: April 10, 1989
Released on J-STAGE: June 30, 2006

DOIhttps://doi.org/10.2116/analsci.5.235

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Crystal Structure of Benzoyldeoxyaconine Hydrobromide

Kimiko KOBAYASHI, Yasuo FUJIMOTO, Hongcheng WANG, Aina LAO, Tosio SAKU ...

1989 Volume 5 Issue 2 Pages 237-238
Published: April 10, 1989
Released on J-STAGE: June 30, 2006

DOIhttps://doi.org/10.2116/analsci.5.237

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