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Volume 33, Issue 9
Displaying 1-23 of 23 articles from this issue
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Takeo ADACHI, Hideyo YOSHIDA, Kimie IZAWA, Hiroshi HASHITANI1984 Volume 33 Issue 9 Pages 455-459
Published: September 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSWith the addition of boric acid to a dilute hydrofluoric acid solution, titanium(IV) and aluminum(III) form cationic fluoride complexes due to the reduction of the free fluoride ion concentration, whereas zirconium(IV) exists as an anionic fluoride complex. As fluoride ion is supplied by the dissociation of the fluoroborate in the media, the free fluoride ion concentration is kept constant even if a considerable amount of the free fluoride ion is consumed by the complex formation with zirconium. On the basis of the above characteristics, a cation exchange separation method was developed for the successive determination of micro quantities of titanium and aluminum in zirconium and its alloys. By the following proposed method, more than 3 ppm of titanium and more than 2 ppm of aluminum can be determined. About 0.5 g of sample was dissolved in 12 ml of 2.6 M hydrofluoric acid and 0.5 ml of concentrated nitric acid. A few ml of potassium permanganate solution(1%) and 2 g of boric acid were added and the solution was diluted with water to 50 ml. After transferring the resulting solution to a-cation exchange column (10 ml of Diaion SK # 1, 120 mm×10 mm φ), 100 ml of 0.2 M hydrofluoric acid 0.65 M boric acid solution was passed through the column at a flow rate of 1.2 ml min-1 to elute zirconium from the column. The remained titanium and aluminum, respectively, were successively eluted with 50 ml each of 0.5 M hydrofluoric acid-0.4 M boric acid solution and 0.1 M hydrofluoric acid solution. In order to eliminate the accompanying traces of zirconium, 1.25 g of boric acid was added to the effluent containing aluminum, and the resulting solution was transferred to another cation exchange column(5 ml of resin). After washing the column with 30 ml of 0.5 M hydrofluoric acid-0.4 M boric acid solution, aluminum was eluted with 30 ml of 0.1 M hydrofluoric acid solution. Titanium and aluminum, respectively, were determined by diantipyrylmethane spectrophotometry and 8-quinolinol extraction spectrophotometry.View full abstractDownload PDF (835K) -
Instrumentation of classification system and application to dextran particlesYasuyuki KUROSU, Kaoru YASUKAWA, Hiroshi KAWASAKI, Nobuharu TAKAI, Tsu ...1984 Volume 33 Issue 9 Pages 460-465
Published: September 05, 1984
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe size classification of low density particles e.g. dextran or agarose (dp=1.001.05) is relatively difficult compared to that of ion exchange resin (dp= 1.2). In this paper, the concept of hydrodynamic chromatography is introduced for the size classification of low density particles. Aqueous solution containing 10% 2-propanol was used to inhibit aggregation of particles. The classification was made for the suspension using the long range of laminar flow. Elution time (tf) of particles can be predicted using the following equation:
tf =ηl /[vcη - 1.960×10-3(dp - df) a2]
tf : elution time (h), η : viscosity of eluent (g/cm s), l : length of laminar flow layer (cm), vc : counter flow rate (cm/h), dp: density of particle (g/cm3), df: density of eluent (g/cm3), a: diameter of particle (μm). Sephadex G-200 was classified using this method by the following conditions: column size; 155×5.5 cm I.D., counter flow rate; 4.4 cm/h, eluent; 10 % 2-propanol. For the given size of classified particles, the elution time was found to be approximately identical with that predicted by the equation. Particles of 10 and 20 μm were flowed out within 48 h (the predicted time is 34.6 h) and 96 h (the predicted time is 71.6 h) respectively.View full abstractDownload PDF (1042K) -
Osamu FUJINO, Yoshinobu KOMETANI, Masahito SUGIYAMA, Masakazu MATSUI1984 Volume 33 Issue 9 Pages 465-471
Published: September 05, 1984
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSInductively coupled plasma atomic emission spectrometry (ICP-AES) was applied to the determination of samarium in calcium apatite minerals. The detection limits(S/N=3) of samarium in distilled water and in cyclooctane were 0.66μg/ml and 0.30 μg/ml, respectively. The effect of coexisting elements other than the matrix components on the samarium emission intensity was scarcely observed at 443.43 nm. However, a large amount of calcium phosphate showed high spectral interference and signal suppression. Hence, the separation of samarium from the matrix by solvent extraction was studied with alkanes and cycloalkanes as solvents. Cyclohexane, a more commonly used solvent, was useless in this case, because it extinguished the ICP flame soon after the introduction. The ICP operating conditions with the organic solvents were 2.0 kW R.F. power, 0.481/min carrier gas, 201/min coolant gas, and 1.21/min plasma gas. The experimental results showed that the stability of the ICP flame is higher for higher hydrocarbons. Thus, cyclooctane was used as an extraction solvent in the present work. The apatite minerals(1 g) were dissolved in hot nitric acid, evaporated to dryness, and dissolved in perchloric acid (1011 M, 100 ml). Samarium was then extracted into cyclooctane containing 0.1 M-HDEHP, and determined by ICP-AES. The samarium content in the apatite minerals was found to be (0.261.81)×10-3 %.View full abstractDownload PDF (1143K) -
Tamotsu WASA, Kengo AKIMOTO, Koichi UEDA, Toshio YAO1984 Volume 33 Issue 9 Pages 471-476
Published: September 05, 1984
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSChemically modified enzyme membrane electrode for L-ascorbic acid was prepared by cross-linking ascorbate oxidase(EC 1. 10. 3. 3, Cucumber) with bovine serum albumin(BSA) by using glutaraldehyde onto the surface of epoxy resin impregnated RVC(Reticulated Vitrious Carbon) electrode. Electrochemical behavior of BSA membrane electrode and analytical characteristics of enzyme membrane electrode were investigated by voltammetric and amperometric techniques. Voltammetric response of BSA membrane electrode for several electroactive compounds showed mostly sigmoid current and its limiting current varied inversely proportional to the square root of molecular weight of the depolarizers, it seemed to suggest that the current attributed to the mass transfer restricted by permiability of the BSA membrane on the electrode surface. Amperometric response of ascorbate oxidase electrode was monitored by the decrease of oxygen cathodic current at -0.7 V vs. SCE, which was attributable to the enzyme reaction (L-ascorbate +1/2 O2 → dehydro-L-ascorbate+H2O) at the electrode surface. The current response was linearly related to the L-ascorbic acid concentration in the range 20800 μM {Δi (μA) =6.58 c (mM) - 0.08; r=0.9996}. The response time was less than 5 s in rigorously stirred(1430 rpm) McIlvaine buffer solution(pH 6.5) at 30 °C. The ascorbate oxidase electrode responded to D-isoascorbic acid(about 100 %) and triose-reductone(about 30 %), but did not respond to amino acids, carbohydrates, organic acids, etc.. The enzyme electrode could be applied to the determination of L-ascorbic acid in orange juices and drugs with satisfactory precision (RSD <2 %). The enzyme electrodes retained about 80 % of their original activities after repetitive use for more than 3 months, by being stored in 0.1 M phosphate buffer solution(pH 6.5) at 5 °C, being not in use.View full abstractDownload PDF (1080K) -
Eiko ONISHI, Toshio YAMADA, Kazuo YAMADA, Hajime INOUE, Yoshiyuki SEYA ...1984 Volume 33 Issue 9 Pages 477-481
Published: September 05, 1984
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAmygdalin, a cyanoglycoside contained in Kyonin (Armenia semen) and Tonin (Persicae semen), is potentially hazardous when administered in large amount as the crude drug because of the side effects of cyanide. Thus, strict quality control of the drug should be made. No specific and sensitive assay method of amygdalin has so far been reported. In the present study, separation and quantitative assay methods of amygdalin were developed by using HPLC with a reversed phase column. Kyonin, Tonin, and the crude drugs containing these two substances were extracted with methanol to prepare the samples for the assay. Amygdalin and its decomposed products were separated on a reversed phase partition column of LiChrosorb RP-8, 10μm in diameter, and 250 × 4.0 mm. Acetonitrile and water, or methanol and water was used as the mobile phase. The effect of pH onthe separation was also studied. Amygdalin in the compounded crude drugs could be efficiently separated on the above column with 8 % aqueous acetonitrile with sufficient sensitivity. It was confirmed that benzaldehyde which was a decomposition product of amygdalin could be determined in 20 min. Amygdalin as well as its decomposed products may be simultaneously determined without special purification by HPLC in the present study. It is suggested that this method may be used for the quality control of amygdalin contained in crude drugs.View full abstractDownload PDF (764K) -
Zong Yin QIU, De Ying HUANG, Souji ROKUSHIKA, Hiroyuki HATANO1984 Volume 33 Issue 9 Pages 481-485
Published: September 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSPoly(ethyleneimine) (PEI 6) was coated on porous silica gel beads in a methanol solution and packed into a stainless steel tube (140220 mm × 0.8 mm i.d.) by a slurry packing method. The surface coated PEI 6 was cross-linked with ethyleneglycole diglycidylether. A Shimadzu Model LC 5A liquid chromatograph with a SPD-2AM UV detector was used. PEI 6 was coated on a Develosil 5 (5 μm, Nomura Chemicals, Japan) or LiChrospher SI 100 (10 μm, E. Merck, F. R. G.). Phenolic, benzoic, and benzenesulfonic compounds were chromatographed with 2.515 mM carbonate or phosphate eluents. This column showed an excellent separation of o-, m-, and p-isomers of above compounds. The capacity factors, k', and chromatograms of over 30 compounds eluted from the column are reported. The k' values of dinitrophenols increased with the eluent pH at low pH range and had maximum values between pH 4 and 5, above this pH range, the values decreased with increasing pH of the eluent. This may be explained by the complex effects of the dissociation of solute molecules, counter ions in the eluent and secondary or tertiary ammonium residues in the stationary phase. By cross-linking of the coated PEI 6 on the silica gel, retention of nitrophenols was increased and elution order or isomers was altered. The cross-linked PEI 6 coated silica gel column will be useful for the separation of isomeric phenols and aromatic acids. This column was stable and good reproducibility was obtained after continuous operation of about three months.View full abstractDownload PDF (702K) -
Toshio ISHIZUKA, Yoshinori UWAMINO, Akira TSUGE1984 Volume 33 Issue 9 Pages 486-490
Published: September 05, 1984
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSImpurities (twenty elements) in silicon nitride powder samples were determined by inductively coupled plasma emission spectrometry (ICP-ES). Silicon nitride (0.5 g) was decomposed by 10 ml-hydrofluoric acid and 2 ml-nitric acid in a Teflon pressure vessel at 170°C during 16 h. The obtained sample solution was diluted to 100 ml with distilled water, followed by ICP-ES determination. The spectrometer was equipped with a crossflow platinum nebulizer and a polypropylene spray chamber for the analysis of the sample solutions containing hydrofluoric acid. The recovery of boron was 97101 % in the acid decomposition procedure, suggesting that the leakage of boron from the vessel as boron fluoride was negligibly small. The presence of ammonium ion as matrix component in the sample solution (0.26 %) little affected the emission intensities of the elements. Hexafluorosilicate as matrix component (1.52 %) reduced the emission intensities by 38%, and increased the background levels for several elements of which analytical lines are below 250 nm. Because of this matrix effect, the detection limits of the elementswere somewhat higher in solutions containing hexafluorosilicate than in solutions containing no silicate. The calibration curves for each element were established from a series of solutions containing silicate as a matrix component and were successfully used for the determination of impurities in silicon nitride samples.View full abstractDownload PDF (807K) -
Tsutomu SHIBATA, Sakae HAMADA, Yuji OKUYAMA, Yoshitaka KASHIO, Akihiro ...1984 Volume 33 Issue 9 Pages 491-495
Published: September 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDetermination of calcium in steels by conventional emission spectrometry is difficult. This is because calcium is present in complex oxides such as CaO·SiO2·Al2O3 or complex sulfide-oxides in which the complex oxides are surrounded by sulfides, (Fe, Mn)S, and during the measurement preferential discharge occurs at these inclusions. Thus, the data obtained by conventional emission spectrometry are always different from those determined by chemical analysis. In the present investigation, (a) short time-high energy discharges or (b) long time-low energy discharges were applied to the sample surface of the steels before the conventional spectroscopic measurements with low energy discharge. Both pretreatments were effective to disperse homogeneously the oxide and sulfide-oxide inclusions in the matrices, thus giving reliable analytical data. It was demonstrated that the spectroscopy with pretreatment of short time-high energy discharge was superior to that with pretreatment long time-low energy discharges in both rapidity and accuracy.View full abstractDownload PDF (888K) -
Shozaburoh HIRAOKA, Toshiyuki SHINONAGA, Takashi ASO, Daijiro YAMAMOTO1984 Volume 33 Issue 9 Pages 496-497
Published: September 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSSpectrophotometric determination of ultratrace amount of copper (II) was reported on our previous paper. A highly sensitive spectrophotometric method is proposed for the determination of manganese(II). This method is based on the accelerating effect of manganese(II) ion on the coloration of potassium trithiocarbonate (K2TTC). By this method, ultratrace amount of manganese(II) can be determined. The recommended procedure is as follows: To a sample solution (4 cm3), containing manganese(II) less than 140 ng, was added alkaline solution of pH 12.2 (12 cm3: containing 0.01 w/v % sodium citrate and 1.8 × 10-3 mol dm-3 potassium cyanide). The mixed solution was cooled with ice, and then added a precooled 0.5 w/v% K2TTC solution (4 cm3). The reaction was allowed to continue for 1 h at 40°C in a dark room. The absorbance of solution was measured at 390 nm against the reagent blank. This accelerating effect was facilitated with an increase in temperature, but the reaction product was decomposed rapidly at above 45 °C. Serious interferences from bismuth(III), copper (II), iron(II), iron(III), and nickel(II) ions can be eliminated by the addition of sodium citrate and potassium cyanide. The R.S.D. (n = 5) of determination for the standard reference material (NIES No. 1 Pepper-Bush) was 3.9 %. This method is highly sensitive with the apparent molar absorptivity of 9 × 106 dm3 mol-1 cm-1, and enables the facile determination of manganese (II) at ppb level.View full abstractDownload PDF (398K) -
Seiji YASUDA, Hitoo KAKIYAMA1984 Volume 33 Issue 9 Pages 498-500
Published: September 05, 1984
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe spectral changes in the Lα2, Lα1, Lβ1, Lβ4, Lβ3, Lβ2, 15, and Lγ1 lines were measured for various compounds of tin and antimony using a two-crystal X-ray spectrometer. The chemical shift was observed in the Lβ2, 15 and Lγ1 lines depending on different oxidation states of tin and antimony. The shifts of both lines were almost comparable to each other for every compound tested. The compounds in lower oxidation states of Sn(II) and Sb(III) exhibited the positive shifts in Lβ2, 15 and Lγ1 lines relative to the respective lines from their metallic state, while those with the higher oxidation states of Sn(IV) and Sb(V) had the negative shifts of these lines. This fact suggests that oxidation state of tin and antimony can be readily distinguished by the measurements of their Lβ2, 15 and Lγ1 shifts. The chemical shifts in other L lines of both elements did not exceed the experimental error of about ±0.02 eV.View full abstractDownload PDF (538K) -
Chizuko SATO, Mitsuhiko TAGA1984 Volume 33 Issue 9 Pages 500-503
Published: September 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method is described for separation and concentration of trace amount (<20μg) of Mn(II), Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Cd(II), and Pb(II) coexisting with large amount of Ca(II), Mg(II), Na(I), and K(I) using chelating resin Unicellex B. The pH of sample solution obtained by digestion of food is adjusted to 5 in 0.1 mol dm-3 acetate buffer solution, then passed through the Unicellex B column for retention of heavy metals except Fe(III). Ca(II) and Mg (II), which were retained on the column at pH 5, are previously eluted with 0.5 mol dm-3 malate buffer solution(pH 5) and then heavy metals are eluted with 3 mol dm-3 HCl. Otherwise only Fe(III) and Cu(II) are retained on the column at pH 2 in 0.1 mol dm-3 maleate buffer solution and eluted with 3 mol dm-3 HCl. Heavy metals in the effluent are determined by Zeeman atomic absorption spectrophotometry. According to the procedure, 520μg of heavy metals in 1 dm3 of synthetic sample solution containing each 1 g of Ca(II), Mg(II), Na(I), and K(I) were quantitatively recovered in 10 cm3 of the effluent except Mn(II). The proposed method was applied to the determination of the heavy metals in NBS 1571 Orchard Leaves and some foods successfully.View full abstractDownload PDF (652K) -
Kiyokatsu JINNO, Tsuyoshi FUKUTA1984 Volume 33 Issue 9 Pages T73-T77
Published: September 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA BASIC program has been developed to predict the main features of gamma-ray spectra for thermal neutron activation analysis using a Ge-detector. By inputting the approximate major and minor elements included in the sample matrix, the predicted gamma-ray spectrum resulting from thermal neutron activation of the elements of interest may be calculated. The program is designed to accept any selected irradiation, decay, and counting conditions. The calculations are rapid. while using only a 16-bit microcomputer. A comparison of predicted spectra with those experimentally observed showed satisfactory results. Although incomplete, the existing program may be used as an excellent guide for selecting optimum parameters for subsequent experiments.View full abstractDownload PDF (769K) -
Kazuo HIIRO1984 Volume 33 Issue 9 Pages T77-T80
Published: September 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSCross check tests were carried out by the members of Association for Environmental Analysis in Osaka, Japan for the purpose of comparison of analytical methods of nitrate and nitrite, ammonia, organic and total nitrogens in environmental water samples. Twenty of authentic samples were prepared, some of them were synthesized by mixing the standard solutions and spiking the standards to natural waters. Eight samples were used for the determination of nitrate and nitrite, four for ammonia and eight for organic and total nitrogens. These samples were distributed to 53 laboratories and the results were compared with respect to mean values, relative standard deviations and accuracy. The following results were obtained by these cross check tests. (1) Good results on nitrate were obtained when the copper-cadmium column reduction method was adopted. However, samples should be diluted before the reduction when they might contain a considerable amount of foreign substances like as silicate. (2) Accurate and precise analytical results were obtained for nitrite and ammonia. Higher results, however, were obtained when the calibration curve was made after the distillation of ammonia. (3) The results on organic nitrogen diversed due to variation in the recovery of nitrogen compounds from their rate of digestion. The satisfied results were obtained when commercial total nitrogen analyzers were used.View full abstractDownload PDF (803K) -
Kiyoshi NOMURA, Yusuke UJIHIRA1984 Volume 33 Issue 9 Pages T81-T87
Published: September 05, 1984
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSTwo types of gas flow propotional counters were fabricated for the use in conversion electron Mossbauer spectrometry (GEMS), and their working characteristics were investigated from the practical viewpoint. The one was a hexagonal pillar type detector, by which angular dependent (90°and 45°incident γ-ray to sample surface) CEM spectrum can be measured. The other was a thin plate type detector, which was designed to reduce the background. The variation of energy distribution of electrons reemitted from 57Fe enriched stainless steel was examined as a function of the distance between the anode wire of the detector and the sample steel surface. With the increase in the distance between γ-ray source and the detector, the FWHM of peaks became independent of the Doppler velocity and the back ground became flatter. The incident angle of γ-ray changed the electron energy distribution and the peak shape of CEM spectrum. The peak height/background ratio at 45°was larger than that at 90°. When high energy electrons were detected with the flow of Q gas, asymmetric peaks appeared in CEM spectrum due to the count loss of electrons. The phenomenon was explained by the space charge effect coupled with the scanning speed of time scaler of multichannel pulse height analyzer.View full abstractDownload PDF (741K) -
Kazuo FUJIWARA, Yutaka TAMAURA, Takashi KATSURA1984 Volume 33 Issue 9 Pages T87-T91
Published: September 05, 1984
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA rapid and sensitive method for determination of methyl mercuric chloride at a low concentration (5μg/l) has been developed by gas chromatography-mass spectrometry. An extracted benzene solution (200 μl) was injected into the GC/MS system. Methyl mercuric chloride was trapped and concentrated on the inlet part of a glass column packed with 20 % DEGS-Hg on Chromosorb W at 40 °C (a herium carrier gas flow rate: 60 ml/min). The benzene solvent was first desorbed by increasing the column temperature to 70 °C and holding that temperature for 1 min. Then the methyl mercuric chloride was desorbed by increasing the column temperature to 160 °C at a rate of 30 °C/ min. Quantitative and qualitative analysis was achieved by the selected ion monitoring set at m/z 202 (Hg) and m/z 252(CH3HgCl). The determination limit in the present method was 5μg/l in the case of 200 μl injection.View full abstractDownload PDF (653K) -
Kozo NAGASHIMA, Yoshiko YANO, Miho HAMADA1984 Volume 33 Issue 9 Pages T91-T94
Published: September 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSComplete analyses of multiple oxide minerals such as pyrochlore A2B2O7, betafite AB2O7, and samarskite ABO4, where A represents Ca, Fe, Y, U, Th, etc. and B does Nb, Ta, Ti, etc. by ICP-AES were made with excellent reproducibility. Seventeen elements which occur as major components of above mineral groups, K, Na, Mg, Mn, Fe, Ca, Pb, Y, Zr, Th, U, Al, Sb, Ti, Nb, Ta, and W, were examined. The mineral samples were decomposed with a mixture of sulfuric and hydrofluoric acids, and diluted with dilute sulfuric acid containing hydrogen peroxide. The suppression effect of sulfuric acid on the emission intensity was minimized by keeping the acid-concentration of sample and standard solution the same. The standard solution containing either 6 or 17 elements was used for the calibration. Both have two series of the concentration of each element; 5 ppm and 30 ppm. Corrections for spectral interferences from coexisting elements were made by subtracting the predicted emission intensities due to the interfering elements from the total intensity at the wavelength of the elements to be analyzed. Procedure: Take 510 mg sample into a tared Pt crucible. Add 9 ml of sulfuric acid (1 : 1) and several ml of hydrofluoric acid. Heat to the sulfuric acid fume, cool and weigh the crucible to know the amount of the remaining sulfuric acid. Add necessary sulfuric acid to make the final concentration to be 5 %. Add 2 ml of 30 % hydrogen peroxide and dilute the solution to 100 ml, determine the spectral intensities of elements and apply the necessary corrections.View full abstractDownload PDF (575K) -
Yuzo TAMARI, Haruo TSUJI, Yuzuru KUSAKA1984 Volume 33 Issue 9 Pages T95-T98
Published: September 05, 1984
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSStrontium in silicate rocks was determined by the following procedure. A rock powder sample prepared to pass through a 100-mesh size sieve (0.10.5 g) was taken in a Teflon beaker, and 6 ml of 46 % hydrofluoric acid and 1 ml of 70 % perchloric acid were added. After being allowed to stand for over one day, the mixture in the beaker was concentrated by heating on a hot plate until white fumes of the perchloric acid appeared. The content in the beaker was transferred to a glass beaker with 2 ml of 61 % nitric acid and 0.5 ml of the perchloric acid, and concentrated until white fumes appeared. Further, 2 ml of 20 % hydrochloric acid was added and warmed. After cooling, the rock solution was made up to 100 ml with water. To a 50-ml stoppered centrifugal tube, a 10-ml portion of the rock solution was transferred, and 1 ml of 2 % 8-quinolinol solution was added. Then the solution was adjusted to pH 5 with both saturated sodium acetate solution and hydrochloric acid, and made up to 15 ml. The decomposed rock sample solution with 20 ml of chloroform was shaken for 5 min. The decomposed rock sample solution was shaken with 20 ml of chloroform for 5 min, and then centrifuged at 2500 rpm for 5 min to separate an aqueous phase from an organic one. After adding 1 ml of 2 % lanthanum solution into a 10 ml portion of the aqueous phase, strontium was determined by atomic absorption spectrometry at 460.7 nm. This method was applied to the rock reference materials, JB-1 and JG-1, issued from the Geological Survey of Japan. Analytical values of strontium in the rocks were almost consistent with their certified and recommended values.View full abstractDownload PDF (495K) -
Toshiyuki OSAKAI, Tadaaki KAKUTANI, Mitsugi SENDA1984 Volume 33 Issue 9 Pages E371-E377
Published: September 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe transfer of tetramethylammonium and picrate ions at the poly(vinyl chloride)-nitrobenzene gel/water and agar-water gel/ nitrobenzene interfaces was studied by means of cyclic voltammetry. Well-defined cyclic voltammograms of ion transfer were obtained for both ions with these polymer gel electrodes. The results indicate that the polymer gel electrode is promising for use in electrochemical analysis of ions.View full abstractDownload PDF (694K) -
Sachiko SAKURA, Hideo IMAI1984 Volume 33 Issue 9 Pages E379-E382
Published: September 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA flow cell voltammetry with twin working electrodes was applied to the trace determination of reducible organic substances in the presence of dissolved oxygen. Carbazilquinone, one of quinone drugs, which is not oxidized by itself, was chosen as a sample. The first electrode was set at the reduction potential of carbazilquinone, and the second electrode at the oxidation potential of the reductant (hydroquinone). The cathodic current at the first electrode composed of reduction currents of dissolved oxygen andthe sample, while the anodic current at the second electrode depends solely on the reduced sample flowing toward the second electrode. The results of the determination based on the anodic current measurement were as follows; 1) The linear calibration plot was obtained from 0.3 nmole to 1.9 nmole of carbazilquinone. 2) The value of R.S.D. was less than 1%.View full abstractDownload PDF (505K) -
APPLICATION OF XANTHENE DERIVATIVES FOR ANALYTICAL CHEMISTRY. Part 43Yoshikazu FUJITA, Itsuo MORI, Shoko KITANO1984 Volume 33 Issue 9 Pages E383-E388
Published: September 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple and sensitive spectrophotometric method for the determination of sulpyrine utilizing the decrease in the absorbance of ο-hydroxyhydroquinonephthalein-cerium(IV) complex was established. The method could be used in the concentration range of 2 - 20 μg/10 ml of sulpyrine; where the effective molar "desorptivity" at 570 nm was 1.2 × 105 dm3 mol-1 cm-1 The other pyrazolone derivatives(antipyrine, aminopyrine and phenylbutazone) could be also determined in the same way. The proposed method was successfully applied to the determination of sulpyrine in commercial injections.View full abstractDownload PDF (710K) -
Indirect atomic absorption spectrophotometric method for the determination of anions with thiourea-copper(I) complex and its related compound(III)Takahiko MATSUEDA1984 Volume 33 Issue 9 Pages E389-E392
Published: September 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA new indirect atomic absorption spectrophotometric method for the determination of thiocyanate ion in water is proposed. The method is based on the extraction of the ion-pairs formed between thiocyanate ion and thiourea-copper(I) complex with methyl isobutyl ketone. Under the optimum conditions established, thiocyanate ion ranging from 0.04 μg/ml to 2 μg/ml in water could be determined. The method was applied to the determination of thiocyanate ion in human saliva.View full abstractDownload PDF (434K) -
Atsushi HINO, Sunao YAMADA, Toshihiko NAGAMURA, Teiichiro OGAWA1984 Volume 33 Issue 9 Pages E393-E396
Published: September 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA system has been developed to measure sensitively photocurrents from laser two-photon photoionization and to detect aromatic hydrocarbons in reversed-phase high performance liquid chromatography. The limit of detection for pyrene in acetonitrile was 18 ng/ml.View full abstractDownload PDF (444K) -
Norio TERAMAE, Shigeyuki TANAKA1984 Volume 33 Issue 9 Pages E397-E400
Published: September 05, 1984
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe effect of heat generated at the rear surface of film samples on spectral features in Fourier transform infrared photoacoustic spectroscopy(FTIR-PAS) was examined experimentally. It was found that careful positioning of samples in a PA cell was required for obtaining reasonable FTIR-PA spectra of films corresponding to absorption spectra.View full abstractDownload PDF (445K)
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