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Volume 35, Issue 12
Displaying 1-16 of 16 articles from this issue
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Tokishi HAYASHI, Mari KOMAKI, Hironori TSUCHIYA, Fumio MATSUDA, Hirosh ...1986 Volume 35 Issue 12 Pages 949-954
Published: December 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAlthough the gradient elution technique is very useful for HPLC separation of multi-component sample, a major bottleneck of its use especially in routine analysis might be the poor reproducibility. To overcome this problem, a new one-chamber continuous solvent programmer for HPLC was constructed using electromagnetic valves, a mixing chamber made of glass, a silicon rabber stopper, a magnetic stirrer, a vacuum pump, a programable controller etc. This system controlled by the programable controller permitted to prepare not only simple exponential curves but also more complex shaped gradient curves. The programmer also realized reproducible separations by the use of different types of reciprocating pumps with constant flow rate. The device was applied to an automated amino acid analyzer based on reversed phase ion pair chromatography. The separation was carried out with a stainless steel column (250×4mm i.d.) packed with NS-Gel C8 (5μm). Sodium lauryl sulfate was used as a counter ion. For the monitoring of amino acids eluted from the column, a fluorescence detection system using o- phathalaldehyde and 2-mercaptoethanol was used.View full abstractDownload PDF (855K) -
Mikita ISHII, Masaaki YAMADA, Shigetaka SUZUKI1986 Volume 35 Issue 12 Pages 955-960
Published: December 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSFlow injection analysis, with a new chemiluminescence (CL) detection, is used to determine trace amounts of cyanide ion (CN-) by means of the uranine-sodium hydroxide-didodecyldimethylammonium bromide (surfactant) system. The emission induced by CN-is efficiently sensitized by uranine in organized surfactant aggregate solution. The method permits selective determination of CN- with a detection limit of 3×10-10M for continuous sample flow or 2×10-9M (1pg) for 20μl sample injection. The linear range is 2 orders of magnitude, the sampling rate is 360h-1, and the relative standard deviation is 2.1% for 0.05 ngCN-(n=10). S2-, the strongest enhancer after CN-, provides a signal 0.1% of that for CN-. The present method is applicable to the determination of CN- in river water. Possible explanations of the CL emission are also discussed.View full abstractDownload PDF (1091K) -
Susumu NAKAMURA, Masaaki KUBOTA1986 Volume 35 Issue 12 Pages 961-965
Published: December 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn tungsten-ribbon furnace AAS, effects of alkali and alkaline earth salts on the absorbance signals of analytes, Cu and Fe, were investigated. To clarify whether the effects are due to chemical interference or not, activation energies of the analytes were calculated from signals and furnace temperatures using an atom formation equation. In the case of Cu, the coexistance of nitrates and/or perchlorates of alkali and alkaline earth elements is thought to cause chemical interference, because these salts decrease the activation energies as well ss the signal of the analyte. Whereas, no remarkable chemical interference occures with alkali and alkaline earth sulfates and/or chlorides. This suggests that the interference is not caused by chemical bonding between the analytes and the alkali and alkaline earth elements but between the analytes and the anion which separate from the alkali and alkaline earth elements at high temperatures.View full abstractDownload PDF (702K) -
Hiroki TAMURA, Kunimichi SASAKI, Tohru NAKAI, Noriaki KATAYAMA, Masaic ...1986 Volume 35 Issue 12 Pages 966-971
Published: December 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe behavior of adsorption of Zn2+ ions on Mn02 was investigated to establish the stoichiometry and the equilibrium conditions of the reaction. The concentrations of Zn2+ ions in solution were determined by AAS, and the amount of Zn2+ ions adsorbed was obtained from the difference between the concentrations before and after the adsorption. The surface concentration of adsorbed Zn2+ ions, Γ, increased with increasing pH and the concentration of Zn2+ ions in solution, [Zn2+].The adsorption is considered to occur by exchanging n protons in the acid hydroxyl groups on the surface of MnO2, ≡MnOHa, with a Zn2+ ion:
Zn2++(2-n)NO3-+n≡MnOHa_??_(≡MnO)nZn(2-n)+·(NO3-)2-n+nH+
……(1)
The reaction product is a surface complex with a charge of 2-n, to which NO3- ions are adsorbed as counter anions. The equilibrium condition of this reaction is given by
βn=Γ[H+]n/[Zn2+][NO3-]2-n[≡MnOHa]nexp(BΓ)
……(2)
where βn is the equilibrium constant and B is a constant. The exponential term expresses the retardation of adsorption by the adsorbed Zn2+ ions. By multiparametric curve-fitting, the values of βn, B, and n were determined to be: βn, =3.45×10-3 mol-0.79 m2.2, B=1.83×106 mol-1 m2, and n=1.21 for an ionic strength of 0.1(NaNO3) and at 25°C. Γ calculations from eq. (2) agreed well with the measured Γ over wide ranges of [Zn2+] and [H+].View full abstractDownload PDF (1051K) -
Hiroshi KAWAGUCHI, GuangYao ZHAN, Atsushi MIZUIKE1986 Volume 35 Issue 12 Pages 972-976
Published: December 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA V-shaped tungsten wire (0.2-mm dia., 9mm high) was used for the thermal vaporization of 10-μl sample solution. A glass vaporization chamber (volume ca. 1cm3) was connected to a torch with a Teflon tube of 1-mm i.d. The internal tube of a conventional torch was replaced by a quartz tube of 1.5-mm i.d. to reduce the dead volume. After the slovent was evaporated by heating the filament with a current of 3.23.6A, the filament was heated to high temperature by a discharging current of a capacitor (0.22F, 16W V) charged to an appropriate voltage (6.258.5V). Signal peaks were appeared within 0.2s from the start of the heating. Detection limits obtained for various elements were generally lower than those measured by either a similar method with a larger vaporization chamber or a graphite-rod atomization method reported previously. Matrix effects of potassium and calcium were examined and the latter showed much greater suppression effect than the former. The effect of calcium, however, were eliminated by the presence of potassium of 0.20.5mg/ml. The method was successfully applied to the direct determination of lead in urine.View full abstractDownload PDF (750K) -
Toru NOZAKI, Hiroshi YAMASHITA1986 Volume 35 Issue 12 Pages 977-981
Published: December 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA differential pulse polarographic method for the determination of nickel(II), zinc(II), cobalt(II) and manganese(II) has been studied in a 2-amino-2-methylpropanoic acid(AMP)-thiocyanate mixed system. Into a 50ml beaker, 10ml of a sample solution containing nickel(II), zinc (II), cobalt(II) and manganese (II) was placed, and 5ml each of the following was added; 0.1M AMP, 1.2M sodium thiocyanate and 4.0M sodium perchlorate. After the pH was adjusted to 6.9 with perchloric acid and sodium hydroxide, the solution was transferred to a 50ml measuring flask and diluted to the mark with water. The polarogram of the solution was recorded from -0.5 to -1.7 vs. SCE at 25°C, and the metals were determined from the peak heights of the calibration curves at -0.66, -0.99, -1.27 and -1.49 V vs. SCE, respectively. The lower limits for the determination of nickel(II), zinc (II), cobalt(II) and manganese(II) were 0.07, 0.03, 0.2 and 0.02μg/ml at pH 6.9, respectively, while the value for cobalt(II) was 0.04μg/ml at pH 8.0. The method was successfully applied to the determination of nickel, zinc and cobalt in manganese nodules, by changing the pH to 5.7 for nickel and zinc, and to 8.0 for cobalt, after the extraction of iron with methylisobutylketone.View full abstractDownload PDF (570K) -
Susumu NAKAMURA, Masaaki KUBOTA1986 Volume 35 Issue 12 Pages 982-984
Published: December 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSTungusten-strip electrothermal AAS using a fast response measurement system was applied to the determination of copper, iron, cadmium and zinc in biological samples. Based on the atom formation model function, activation energies of these elements at the atomization stage were measured to ascertain chemical interferences and select interference-free analytical conditions. Activation energies obtained for copper, iron and zinc metals in the absence of a matrix were in agreement with those obtained for these metals contained in NBS biological standard reference materials. Also, analytical values agreed well with the certified ones within the precision of the present method. These results demonstrate that chemical interferences are negligibly small under the analytical conditions selected.View full abstractDownload PDF (596K) -
Takeshi OMORI, Yuzo ISHIKAWA, Kunio AIKAWA, Hirao NAGAE1986 Volume 35 Issue 12 Pages 984-987
Published: December 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn automated system for carrying out the development of the thin-layer plate was assembled. The automated system consists of a conventional glass chamber, a mechanical unit for lifting the thin-layer plate and a double-beam optical sensor for detecting the solvent front. Development is stopped by lifting out the thin-layer plate from the glass chamber exactly after arrival of the solvent front at the pre-setted position monitored by the optical sensor. The reliable detection of the solvent front by the double-beam optical sensor offers reproducible results of development. By using this system, a laborious and time-consuming work in TLC can be significantly reduced.View full abstractDownload PDF (667K) -
Yutaka SAITO, Kumiko IWASAKI, Hideki OKUDA, Masaki MIFUNE, Junichi ODO ...1986 Volume 35 Issue 12 Pages 987-990
Published: December 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn order to reveal a functional group required to form an analytically valuable complex such as chrome Azurol S (CAS)-human serum albumin (HSA) complex, the absorption and fluorescence spectra of ten dyes related to CAS were examined in the presence of HSA. A red shift similar to that caused by HSA in the case of CAS was observed in the absorption spectrum only for the dyes containing carboxyl group. HSA also caused increase of fluorescence of these dyes, whereas the dyes free from carboxyl group exhibited weak or no fluorescence even in the presence of HSA. In particular, the increase of fluorescence intensity of Eriochrome Gyanine R (ECR) was found to be larger than that of CAS, and ECR may be superior to CAS for the determination of HSA. The increase of fluorescence may be attributed to ionization of carboxyl group and/or wear of planarity of the dye by binding to HSA. The results indicate that carboxyl group is essential to form an analytically valuable dye-HSA complex in contrast with the case of Bromcresol Green-HSA complex.View full abstractDownload PDF (639K) -
Chizuko OHTSUKA, Hiroko WADA, Yasukazu ASANO, Genkichi NAKAGAWA1986 Volume 35 Issue 12 Pages 990-993
Published: December 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe reversed phase chromatography of ten amino acids(serine, glutamic acid, glycine, alanine, valine, methionine, leucine, isoleucine, phenylalanine, proline) in Japanese sake was studied by using a copper(II) ion selective electrode as detector. Chromatographic conditions were: column, TSKgel ODS-120A (particle size 5μm, 4.6mm i.d.×25cm); mobile phase, waterethanol (95:5 v/v); flow rate, 0.23cm3min-1. The copper(II) reactant solution contained 10-5 mol dm-3 copper nitrate, 0.05mol dm-3 3-(N-morpholino) propanesulfate buffer(pH 7.0), 0.05 mol dm-3 ammonium acetate and 1%(w/v) potassium nitrate, and was delivered at the flow rate of 0.27cm3min-1. The change of copper(II) ion activity by the post-column reaction between copper(II) reactant solution and amino acid was monitored with a copper(II) ion selective electrode (DKK 7141). Eight peaks were obtained, serine, glycine and alanine were not resolved. Calibration curves of seven amino acids were linear for 0.21.5μg/10mm3. Amino acids in Japanese sake could be simply determined.View full abstractDownload PDF (557K) -
Shohgo SUZUKI, Kisayo MATUMOTO, Yukiko OKADA, Shoji HIRAI1986 Volume 35 Issue 12 Pages 993-995
Published: December 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThirty three elements in an environmental reference material Tea Leaves (NIES No.7) prepared by National Institute for Environmental Studies were determined by instrumental NAA. The Tea Leaves samples(ca. 401000mg) were irradiated by thermal neutron and epithermal neutron in Musashi Institute of Technology Research Reactor (MITRR). The cadmium cover of 1 mm thick was used for epithermal neutron irradiation. The gamma-ray measurements of irradiated samples were preformed using a coaxial Ge(Li) detector and 4096 channel pulse height analyzer. Thirty elements (Na, mg, Al, Cl, K, Ca, Sc, V, Cr, Mn, Fe, Co, Ni, Zn, Br, Rb, Sr, Sb, Hg, Cs, Ba, La, Ce, Sm, Eu, Tb, Yb, Hf, Ta and Th) were determined by measuring thermal neutron irradiated samples. While remaining 3 elements (As, Se and W) were determind by measuring epithermal neutron irradiated samples.View full abstractDownload PDF (494K) -
Akemi YASUI, Hideo KOIZUMI, Tadanao SUZUK, Chuichi TSUTSUMI1986 Volume 35 Issue 12 Pages T115-T119
Published: December 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA new dry ashing method using an aluminium foil cup as a vessel is proposed. Commercially available aluminium foil was cut and formed into a shape of cup. Cups were doubled and heated in a muffle furnace at 600°C for 23h. After the sample was ashed in the muffle furnace at 550°C, the inner cup was removed out and the bottom of the cup was destroyed with a glass rod so the ash dropped into a conical beaker, the inside of the cup was then washed with 1% hydrochloric acid. The washing solution was evaporated on a hot plate, and 5ml of 20% hydrochloric acid was added and subsequently evaporated on a hot plate. The residue was dried at 110°C oven for 1h and then dissolved with 1% hydrochloric acid. This method was applied to NBS SRM Oyster Tissue, Wheat Flour, Rice Flour, Orchard Leaves and Citrus Leaves. Potassium, magnesium, calcium, zinc, manganese, copper and iron were determined by AAS, and phosphorus was determined by the vanadomolybdate spectrophotometric method. The results obtained using this method agreed with the certified values and those obtained using platinum dish dry ashing method. The dry ashing method for pretreatment of a large number of samples can be performed economically by using the aluminium foil cup.View full abstractDownload PDF (855K) -
SeongBum LEE, Etsuro YOSHIMURA, Yukio TANAKA, Jun SAITOH, Sunao YAMAZA ...1986 Volume 35 Issue 12 Pages T120-T123
Published: December 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSTo determine trace metals (Ni, Cu and Mn) in oily foodstuffs, such as butter and margarine, an effective ashing procedure has been devised. Charring by heating with sulfuric acid and stepwise addition of nitric acid was found to. be best to prevent bumping of the decomposing solution. Final ashing of the carbonized sample was easily done in a muffle furnace. Suppression of metal-halide vaporization during dry ashing was examined using the model samples composed of the analytes and NaCl, and sufficient recoveries were given by addition of sulfuric acid. Reproducible results for the oily foodstuffs were obtained at the sample size up to 10g.View full abstractDownload PDF (654K) -
Eiko NAKAMURA, Hiroshi NAMIKI1986 Volume 35 Issue 12 Pages T124-T129
Published: December 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe effects of heating on the peroxodisulfate decomposition of phosphorus compounds for the determination of total phosphorus in water has been studied using adenosine-diphosphate (ADP), lecithin and tripolyphosphate as samples. Decomposition of ADP proceeded rapidly and completely at temperatures above 100°C in the absence of H2SO4, and at 100°C in the presence of H2SO4. In the presence of H2SO4, the complete decomposition of lecithin was difficult because lecithin was slowly decomposed while peroxodisulfate was rapidly consumed during thermal autolysis. Suitable amounts of acid was needed to hydrolyze tripolyphosphate, and the acid was supplied during the autolysis of peroxodisulfate. It was considered that the heating method which can elevate the temperature to above 100°C in a short time is suitable for the decomposition of the analytical samples.View full abstractDownload PDF (913K) -
Hiroshi KITANO, Hideki UCHIYAMA1986 Volume 35 Issue 12 Pages T130-T135
Published: December 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe pH value of a equimolal phosphate buffer solution has been accurately measured using a pH cell composed of a hydrogen and silver-silver chloride electrode. Four pairs of hydrogen and Ag-AgCl electrodes were prepared by an electrolytic method, and measurements of the electromotive force of the pH cell were repeated for each pair assembled in the cell. The pH cell was filled with buffer solutions KH2PO4, Na2HPO4 mixed with KCl at three different concentrations. The pH values of the buffer solution were calculated from the measured emf values in accordance with Bates-Guggenheim convention. In addition, the standard electrode potential(E°) of the Ag-AgCl electrode was precisely determined. The pH values obtained are 6.946±0.006, 6.864±0.003 and 6.838± 0.003, and the E° values also determined are 234.54± 0.14mV, 222.76±0.14mV and 204.64±0.13mV, at 5, 25 and 50°C respectively. These pH values agree with those of Bates et al. within 0.005, but the E° value shows a relatively large difference of 0.42mV from that of Bates et al. Consequently, it may be said that for the precise measurement of pH the E° value of each electrode must be measured to reduce the systematic error.View full abstractDownload PDF (1037K) -
Tsukasa SONODA, Susumu KAWAI, Makoto AKAMATSU1986 Volume 35 Issue 12 Pages T136-T140
Published: December 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSApplication of the fundamental parameter method to quantitative analysis of slags and rocks was studied. The program used for calculation is XRF-11. Pressed powder samples after screening at 44μm and glass beads of the dilution ratio (sample + flux/sample) of 11 were used for analysis of slags, and glass beads of the dilution ratio of 5 were used for analysis of rocks. Accuracies for each component obtained from the fundamental parameter method were equal to those from the calibration curve method except for the minor components in the powder samples and glass beads. The proposed method showed good reproducibility in slag and rock analysis. The relative standard deviation was in the range of 0.271.23% for each component in the slags and 0.231.78% in the rocks.View full abstractDownload PDF (819K)
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