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Volume 38, Issue 9
Displaying 1-16 of 16 articles from this issue
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Osamu SAKURADA, Hideaki TAKAHASHI, Mitsuhiko TAGA1989 Volume 38 Issue 9 Pages 407-412
Published: September 05, 1989
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA mechanism of stabilization of Pb with a palladium matrix modifier in graphite furnace AAS has been investigated by XPS. The effect of Pb amounts added as PdCl2 on the Pb atomic absorption profile was examined by AAS. Small amounts of PbCl2 or PbCl2/PdCl2 were deposited on graphite plates and, as a function of heating temperature, the changes in the amounts and valence states of Pb, Pd and Cl remaining on the graphite surface were measured by XPS. It was shown by AAS that the addition of more than 20ng of Pd causes a significant increase of a 2ng-Pb absorption peak, and that the addition of more than 200ng Pd causes shift of the absorption peak to a higher temperature. The XPS of PbCl2-deposited graphite showed that Pb 4f and Cl 2p spectra remain unchanged during heating up to 400°C and disappear at 600°C, indicating that Pb evaporates as PbCl2 above 400°C. By the addition of PdCl2, Pb(II)and Pd(II) were found to be reduced to the metallic states at 200°C and to remain even at 600°C, after chlorine had disappeared. The enhancement of Pb absorption signal in AAS with a Pd modifier is discussed in terms of Pb reduction and alloy formation with Pd.View full abstractDownload PDF (820K) -
Fusao SHIRATO, Yoshiaki OKAJIMA, Chiaki MAEKOYA, Yoshinori TAKATA1989 Volume 38 Issue 9 Pages 413-418
Published: September 05, 1989
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA FIA system was developed for the rapid and continuous determination of nitrite, nitrate and ammonium nitrogens in soil by spectrophotometry. Nitrite nitrogen was determined by using of N-(1-naphthyl)ethylenediamine. The reagent and sample solutions were injected in the order of reagent (40 μl), sample (40 μl) and reagent (40 μl) by a 16-port injection valve in carrier solution (deionized water). Ten meters long Teflon tubing (0.5 mm i.d.) was used as a reaction coil and maintained at 90°C. Nitrate ion was reduced to nitrite ion with a Cu-Cd column and determined by the same method as that for nitrite nitrogen. For determination of ammonium nitrogen, molecular ammonia was liberated by 1 M NaOH which was injected in both sides of sample solution. Molecular ammonia was separated by means of a tubular microporous poly(tetrafluoroethylene) membrane into a mixed reagent stream in the inner tube and determined by indophenol method. The method developed has been successfully applied to the analyses of soil extracts. The linear relationship between the signal and concentration were obtained for nitrite, nitrate and ammonium nitrogens in the range of 0.17, 120 and 1150 ppm, respectively. The relative standard deviation was 0.30.5%. The analysis time required for one sample was about 10 min.View full abstractDownload PDF (841K) -
Masashi GOTO, Wenzhi HU, Daido ISHII1989 Volume 38 Issue 9 Pages 419-423
Published: September 05, 1989
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA continuous monitoring method was developed for the automatic determination of trace silicon in industrial water, based on the molybdenum blue absorption spectrophotometry. A sample, a molybdic acid reagent and a reducing reagent are continuously pumped with a peristaltic pump at a flow rate of ca. 75μl/min. The sample is mixed with the molybdic acid reagent in a mixing joint and then introduced into a reaction tube made of Teflon tubing (0.5mm inner diameter, 8m length) in an aluminium block bath at 23°C, in which the molybdosilicic acid is formed. A platinum wire with a diameter of 0.2mm is inserted into the reaction tube to assist the mixing of sample with reagent. The stream from the reaction tube is mixed with a stream of the reducing reaget to form the molybdenum blue, which is then introduced into a flow cell (10mm light pass length, 8μl volume) of a spectrophotometer. The absorbance at 815nm based on the molybdenum blue is continuously recorded to measure the trace silicon in samples. The method was successfully applied to the determination of trace silicon in commercial pure waters and to the continuous monitoring of trace silicon (22000ppb) in water.View full abstractDownload PDF (721K) -
Michio ZENKI, Keiichiro SAI, Yiwen YE, Kyoji TÔEI1989 Volume 38 Issue 9 Pages 424-428
Published: September 05, 1989
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe lanthanum(III), thorium(IV) and uranium(VI) complexes of Arsenazo III were investigated as the reagent for the determination of fluoride by FIA. Optimum conditions for FIA system, for example, Arsenazo III concentration, metal ion concentration, pH, reaction coil length and sample volume were examined and compared with each other. Arsenazo III-uranium-(VI) complex was selected because of the high sensitivity. A 4.8×10-5M Arsenazo III solution containing the same concentration of uranium (pH 2.8) was used as a reagent solution, and distilled water as a carrier solution. Two streams were propelled at the same flow rate of 0.5ml min-1 by using a double plunger micropump. Sample solution (196μl) was injected into the carrier solution and twenty centimeter long Teflon tubing (0.5mm i.d.) was used as a reaction coil. The decrease in absorbance of Arsenazo III-uranium complex with fluoride was measured at 606nm using a flow cell (8μl, 1cm long). The interference of cations such as calcium and iron were eliminated by using a cation exchange column (Dowex 50WX2, 100200 mesh, NH+4form, 2 mmi.d.×40cm long), which was installed just behind the sample injection valve. A calibration curve was linear up to 1.5ppm fluoride, and the detection limit corresponding to S/N =2 was 50ppb. The relative standard deviation was 0.45% for the determination of 0.5ppm fluoride (n=10). The method was applicable to the determination of fluoride in well waters.View full abstractDownload PDF (567K) -
Shinya SAKAE, Norio TERAMAE, Tsuguo SAWADA1989 Volume 38 Issue 9 Pages 429-433
Published: September 05, 1989
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSMn, Fe, Zn and Cu in plant samples were determined by flame AAS after alkali fusion with lithium tetraborate and sodium carbonate (2:1). After fusion at about 700°C for 10 min, the fused product was dissolved in 4 M HCl solution and heated for 15 min on a hot plate. After extraction with APDC, Mn, Fe, Zn and Cu in MIBK were determined by flame AAS. The proposed method was applied to the determination of the elements in Orchard Leaves (NBS-SRM 1571) and Tomato Leaves (NBS-SRM 1573). The analytical values obtained were within the certified values. Losses of the elements during the fusion treatment were not significant.View full abstractDownload PDF (691K) -
Atsushi UZAWA, Shinji MITA, Yoko IWAMOTO, Wataru YOSHIMURA, Tadao OKUT ...1989 Volume 38 Issue 9 Pages 434-437
Published: September 05, 1989
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSPreconcentration of Pd from aqueous solution for metal furnace AAS determination was studied using activated carbon impregnated with 1, 2-cyclohexanediondioxime (AC-DOx). Pd of 0.050.25 μg in the sample solutions (100cm3 to 1000cm3) were completely collected over the pH range of 1.04.0 by stirring with 25 mg AC-DOx for 15 min. Aliquots (10 μl) of AC-DOx-suspention, which was prepared by adding 5.0 cm3 of water to the AC-DOx adsorbed Pd, were introduced into a tungsten ribbon atomizer. The detection limit was 0.012 ng/cm3 and relative standard deviation was 3.5% (n=5). The proposed method has been applied to the determination of Pd in wastewater from a plating factory.View full abstractDownload PDF (577K) -
Takeji OZAKI, Kazuo HIRAYAMA, Nobuyuki UNOHARA1989 Volume 38 Issue 9 Pages 438-442
Published: September 05, 1989
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA cyclic voltammetry was applied to the determination of chloride ion by the four electrodes method. A designed apparatus can concurrently measure the working electrode potential regulation and bipolar current, by using the gold working and platinum counter electrodes against the current-carrying electrodes as a bipolar electrode. As the result of scanning potential in the anodic direction in 0.1 M potassium nitrite at pH 2.9 as the supporting electrolytes, the correlation between the peak current at about +1.0 V (vs. Ag/AgCl) and chloride concentration was linear. Chloride ion, ranging from 2 to 900 mg/l, can be determined by scanning several times in the narrow range from +0.5 to +1.3 V at a rate of 5 V/min. A small amount of silver, mercury, iodide and bromide ions interferes the determination of chloride, while most heavy metal ions do not interfere.View full abstractDownload PDF (778K) -
Kikuko YOSHIMURA, Mayumi ASHIDA, Yumi NISHIMOTO, Asako SAKAI, Tatsuya ...1989 Volume 38 Issue 9 Pages 443-448
Published: September 05, 1989
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSSilica gel powder was coated with plasma polymer produced in a glow discharge of propargyl alcohol (PA) or 60% water-containing PA (PW), and a hexane-suspended slurry of the material was applied to TLC. Individual Rf-values of azo dyes, amino acids and cholesterols on the proposed plates were compared with those of uncoated or PA plasma-coated silica gel plate which had been briefly described in this journal. Relatively high Rf-values appeared in cases of organic compounds containing polar functional groups such as hydroxyl group. The ratio of Rf-value (coated/uncoated) was generally higher by nonpolar developing solvent than polar one. It was also found that the TLC plate using plasma-coated silica gel powder appeared a similar behavior of migration to the previously described plasma-coated silica gel plate. Somewhat different behavior of migration between PA plasma-coated plate and PW plasma-coated one was elucidated by X-ray photoelectron spectroscopy which revealed a difference of element composition (Si, O, C) at the surface of plasma-coated silica gel powder. These results suggested that the chromatographic behavior could be widely altered by changing the monomer sources and the operating conditions for the plasma polymerization.View full abstractDownload PDF (909K) -
Study on identification of soot IIIMasahisa TAKATSU, Tadahiro YAMAMOTO1989 Volume 38 Issue 9 Pages 449-453
Published: September 05, 1989
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSBasic experiments for identifying the intact material of soot before combustion were carried out by using trace amount of soot produced from eight aromatic hydrocarbons ; benzene, toluene, o-, m-, p-, xylene, ethylbenzene, styrene and cumene. The soot was collected with glass fiber filter paper that was out of contact with diffusion flame. The contents in the soot were determined by Curie point pyrolysis GC, at both pyrolysis temperatures 358°C and 590°C. Though little amount of intact materials such as benzene was detected in a lot of soot at 358°C, the detectable amount of characteristic content such as benzene, toluene, o-, m-, p-xylene, styrene and biphenyl increased and the difference between pyrograms became more clear at 590°C. Especially, xylene in xylene soot and biphenyl in benzene soot were useful content to identify its soot. These contents could be found even in the soot aged one year after the preparation.View full abstractDownload PDF (602K) -
Hiroaki KUBO, Yuesheng HUANG, Toshio KINOSHITA, Hiroyuki NAKAZAWA1989 Volume 38 Issue 9 Pages 454-457
Published: September 05, 1989
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method for the sensitive determination of proteins has been developed using FIA with coulometric detection. The redox reaction of copper(II) was coupled with the reducing ability of proteins in alkaline solution (pH 12.0) at high temperature. This system is comprised of the delivery pump of a carrier reaction reagent solution, sample injector, reaction coil (0.5mm i.d.×5m, 95°C), cooling coil (0.5 mm i.d.×1m, 10°C) and a coulometer. The applied potential on the working electrode of the coulometer was fixed at 0.7V. The flow rate of the carrier reaction reagent solution containing of 0.3M phosphate buffer (pH 12.0) in which was included 1mM copper(II) sulfate and 20mM ammonia was 1.5ml/min. The injected sample volume was 5μl. Linear calibration curves were obtained from 10ng up to 100ng of proteins such as bovine serum albumin (BSA), human serum albumin, human-γ-globulins and ovalbumin. Relative standard deviations for 10ng (n=10) and 25ng (n=10) of BSA were 3.5% and 3.1 %, respectively. The detection limit (S/N = 2) for BSA was 2.5ng. Although glucose, glycine and alanine could not be found in quantities as much as 50ng, histidine, cysteine, tryptophan and tyrosine were sensitively detected by the present method.View full abstractDownload PDF (464K) -
Kunihiro WATANABE, Katumi YOKOO, Izuo AOKI1989 Volume 38 Issue 9 Pages 458-461
Published: September 05, 1989
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS2, 2'-Dihydroxazobenzene (DHAB) and 4, 4'-dimethyl derivative (DDAB) react with aluminium(III) in an aqueous solution to form fluorescent 1 : 1(metal-DHAB or DDAB) complexes. We studied the effects of anions and neutral ligands on the extraction/fluorometric determination of aluminium by using these complexes. The aluminium-DHAB complex was extracted with tributyl phosphate (TBP), and with benzene by adding trioctylphosphine oxide (TOPO). A large amount of appropriate anions i.e. acetate, propionate, thiocyanate and perchlorate, was required for the extraction of the complex. Especially the addition of propionate and thiocyanate gave a strong fluorescence. TBP and TOPO acted as neutral adductants and remarkably increased both the extractability and fluorescence quantum yield of the complex. TOPO also acted as a catalyst for the reaction between aluminium and DDAB. The ratio of the composition of the extracted complexes Al-(DHAB or DDAB)-(anion)-(TBP or TOPO) was 1 : 1: 1: 2 in the presence of acetate, and 1 : 1 : 1 : 3 in the presence of perchlorate.View full abstractDownload PDF (570K) -
Michio ZENKI, Hiroshi KOGAWA, Kazuko NOSE, Kyoji TÔEI1989 Volume 38 Issue 9 Pages T129-T133
Published: September 05, 1989
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSGlyoxal bis(2-hydroxyanil) (GBHA) reacts with calcium to form a red complex in alkaline solution. On the basis of this color reaction, FIA is proposed for the simple and rapid determination of calcium in natural waters. Three streams, a reagent solution (0.05% GBHA), a buffer solution (0.20 M NaOH) and a carrier solution (water) were propelled at the same flow rate of 0.6 ml min-1 by using plunger micropumps. Sample solution (290 μl) was injected into the carrier solution and an eight meter long Teflon tubing (0.5 mm i.d.) was used as the reaction coil. The absorbance of Ca-GBHA complex was measured at 520 nm using a flow cell (8 μl, 1 cm long). The calibration curve was linear up to 1.2 ppm Ca, and the detection limit corresponding to S/N =2 was 5 ppb Ca. At the sampling rate of 20 samples per hour, the relative standard deviations were 1.2 and 0.22% (n =10) for the determination of 0.4 and 1 ppm Ca respectively. The results for the analysis of natural waters (rain, river, tap and well waters) agreed well with those obtained by AAS (JIS method).View full abstractDownload PDF (517K) -
Hiroyasu YOSHIKAWA, Hideo IWATA, Hideo SENO, Takeshi MISUMI1989 Volume 38 Issue 9 Pages T134-T139
Published: September 05, 1989
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe amount of phosphorus in nonferrous metal alloys containing tungsten was determined by phosphomolybdate blue spectrophotometric method with beryllium hydroxide coprecipitation technique. Results obtained were as follows : (1) More than 4 mg of beryllium hydroxide was required for the quantitative coprecipitaion of phosphorus. (2) Nickel and cobalt could be masked by EDTA for the quantitative separation of phosphorus. (3) Chromium was vaporized as chromium dichloridedioxide (CrO2Cl2). (4) Molybdenum and zirconium showed no interference in the present method. However, the presence of above 1% of zirconium together with above 2% of tungsten interfered. (5) The solvent extraction method with 1-pentanol was also studied, and the extraction condition could be determined. The extraction was completed in 30 s, and the extracted complex was stable at least for 120 min. (6) The limit of determination for phosphomolybdate blue spectrophotometric method and the solvent extraction method were 20 ppm and 1 ppm, respectively.View full abstractDownload PDF (690K) -
Masao UMEMOTO, Wataru TANI, Koji HAYASHII, Katsuhiko KUWA1989 Volume 38 Issue 9 Pages T140-T142
Published: September 05, 1989
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAccuracy of the determination of potassium in serum by flame emission spectrometry (FES) using lithium as an internal standard (IS) is studied. Potassium in serum was determined with a Hitachi 710, following the procedure described in NBS Special Publication 260-63. In order to examine the accuracy of FES, certified reference materials (NBS SRM 909 Human Serum and Japanese certified reference serum for ion selective electrode 88-1) were used. When potassium standard solutions containing lithium as an IS were used for calibration, the deviation of the measured values from the certified values were approximately +5 %. On the other hand, when calibration was made with certified reference serum 88-1 having three concentration levels of potassium, the deviation from the certified values were only +0.4%. Errors associated with serum matrix effects can be eliminated by using the certified reference serum as the calibration standards.View full abstractDownload PDF (474K) -
Shoji MOTOMIZU, Katsuhiko KORECHIKA1989 Volume 38 Issue 9 Pages T143-T148
Published: September 05, 1989
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSFIA of anionic surfactants was examined by using a double-line system in respect to practical application. A reagent solution and an extraction solvent were propelled by a double-plunger pump. Sample solutions were injected into a reagent solution stream, which was marged in a extraction solvent stream. An improved segmentor with an outlet of 0.25-mm bore and 13-μl space made smaller segments (averaged length, 2 mm), which enabled to have higher peaks. The efficiency of the smaller segments on the peak height was higher when the extraction tubing was shorter than 1 m. Three kinds of reagent solutions were examined ; one comprised 1-methyl-4-(4-diethylaminophenylazo) pyridinium (MEP) chloride (extraction solvent, chloroform ; MEP · Cl method), another an iodide of MEP (extraction solvent, chloroform ; MEP· I method) and the other methylene blue (extraction solvent, ο-dichlorobenzene ; MB method). By the MEP· I method, negative peaks were obtained in the range below 10-6 M of anionic surfactants. The highest peaks were obtained by the MB method. The peak height, the standard deviation and the relative standard deviation obtained by 10 times injection of 10-6 M laurylsulfate (LS- ) were 200.6 mm, 0.8 mm and 0.4%, respectively, by the MB method ; 121.1 mm, 0.3 mm and 0.3%, respectively, by the MEP·Cl method. The detection limit corresponding to a signal to noise ratio (S/N) of 3 was about 1 × 10-8 M of LS- by the MB and MEP·Cl methods. This method was capable of analyzing 2030 samples per hour.View full abstractDownload PDF (719K) -
Akiharu HIOKI, Noriko FUDAGAWA, Masaaki KUBOTA, Akira KAWASE1989 Volume 38 Issue 9 Pages T149-T155
Published: September 05, 1989
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSTo establish the traceability of metal standard solutions of Zn, Cd, Co, Cu, Pb and Mn, the concentration of each metal standard solution (Cs) measured by EDTA chelatometric titration was compared with that (C) calculated from the weight of the dissolved metal. The EDTA solution was standardized with a high-purity Zn solution. The intersection of both the tangent at an inflection point and φ(indicator transition) =1 was adopted as an end point of titration. The inflection point was calculated from experimental data near the point with the approximation as a curve of the third order. The difference between Cs and C was within ±0.1% for each metal standard solution. The traceability of the metal standard solutions of Zn, Cd, Co, Cu, Pb and Mn was thus confirmed.View full abstractDownload PDF (947K)
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