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Volume 32, Issue 7
Displaying 1-19 of 19 articles from this issue
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Simultaneous determination of aluminum, iron, and titanium with 8-quinolinolYasuo IIDA, Kazuo GOTO, Masamichi FURUKAWA, Shozo SHIBATA1983 Volume 32 Issue 7 Pages 401-406
Published: July 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSData reduction and calibration methods in an overdetermined multicomponent analysis are discussed on the accuracy and precision of determination. In the data analysis, the matrix representation of the LambertBeer's law (AKC method) and their reversed form, expressing the concentration as the function of absorbance (CPA method) are compared. The CPA method is superior to the AKC method in the accuracy and precision when the number of the analytical wavelengths is equal to, or a few more than the number of component. But there is a problem in the calculation of the inverse matrix in the highly over-determined case with regard to the analytical wavelengths. On the.other hand, the AKC method has several advantages in the course of date analysis. In the AKC method, the data collected from many wavelengths can be dealt with; therefore, we can observe not only the individual spectrum of each component by calculating the absorptivity matrix after the calibration, but also the difference spectrum by subtracting the raw data spectrum from the calculated one after the analysis. From these spectra, validity of the Lambert-Beer's law, or the additivity of the spectrum of each component can be ascertained. In both methods, the accuracyand precision of determination are improved by adding the nonzero intercept term to the calibration model, and by the calibration with standard mixtures instead of a standard solution of single component. The present methods could be successfully applied to the simultaneous determination of aluminium, iron, and titanium in the standard reference materials: NBS 81a (glass sand) and BCS 314 (silica brick).View full abstractDownload PDF (1115K) -
Kazuo IMAEDA, Keiko OHSAWA, Takashi YOKOTA1983 Volume 32 Issue 7 Pages 406-410
Published: July 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe present investigation was undertaken to study the stability of squalene as precursor of steroids by examining the relation among the direct determination of oxygen, the oxygen uptake, peroxide value (POV), and infrared spectrum (IR). After enclosure squalene with gelatin capsule or addition of various antioxidants or pro-oxidants to squalene, we measured the quantity of oxygen which was taken up by the squalene. Vitamine A palmitate, calciferol, 7-dehydrocholesterol (V. D3), DL-α-tocopherol, linoleic acid, β-carotene, and lecithin were used as antioxidants, and ironnaphthenate (III), copper naphthenate (II), zinc naphthenate, iron plate, and copper plate were used as pro-oxidants. Those antioxidants and pro-oxidants were added to or contacted with squalene at various concentrations { (0.12.0) %} or surface areas. The oxygen uptake, oxygen direct determination, POV, and IR of a test sample was determined in an absorption cell under an oxygen atmosphere at 40°C or 50°C by 10-W ultraviolet light irradiation from a distance of 15cm. As the results, it was found that oxygen analysis was able to detect at an early stage of deterioration, and the volume of measurement had small standard deviation. Squalene enclosed with gelatin capsule was the most effective way on stabilization of squalene. It was found that V. D3 and DL-α-tocopherol were the useful antioxidants for squalene. Regarding pro-oxidants, squalene containing or contacted with copper showed the acceleration for oxygen uptake more marked than squalene containing or contacted with iron.View full abstractDownload PDF (1018K) -
Determination of optical constants of adsorbed layer for the state analysis of the electrode surfaceFumiyo KUSU, Satoshi INOUE, Atsuko MORI, Kiyoko TAKAMURA1983 Volume 32 Issue 7 Pages 410-416
Published: July 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSSpecular reflectivity measurement is applied to the determination of the optical constants, such as refractive index and extinction coefficient, for an adsorbed layer of organic compound formed on a gold electrode in 0.1M NaClO4. In the presence of barbital, adenine, 2'-deoxyadenine, thymine, benzene, naphthalene, and anthracene in the solution, marked decrease in reflectivity ascribed to the adsorption of them was found on the reflectivity-potential curves. The adsorption isotherms and the potential dependence of the adsorption were obtained and the adsorption film thickness was estimated. According to Mclntyre-Aspnes' theory, data of the reflectivity change caused by the adsorption were treated and the optical constants of adsorbed monolayer were calculated. The values of refractive index obtained at (400525) nm appear to be close to those of the compounds in crystalline states, and the valuesof extinction coefficient are essentially zero for most of the compounds. These facts suggest the usefulness of the specular reflectivity measurement as a tool in the study of the adsorbed state.View full abstractDownload PDF (1491K) -
Toshiyuki MITSUI, Yoshikazu FUJIMURA1983 Volume 32 Issue 7 Pages 416-419
Published: July 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSCartap {S, S'-2- (Dimethylamino) trimethylene bis (thiocarbamate) } reacts with benzylchloride to form benzyl derivative, which is extracted into dichloromethane at pH 1.813.78 in the presence of Tropaeoline OO forming an ion association complex. The concentration of Cartap can be measured by the absorbance at 543 nm. Calibration curve obeyed Beer's law over the range of (1.60×10-62.16×10-5) M. The procedure for the determination is as follows. Place 1ml of the sample solution containing less than 2.70 × 10-4 M of Cartap, 5ml of benzylchloride acetone solution containing 2.37 × 10-2 M, and 5ml of 3% sodium carbonate solution in a 30ml Erlenmeyer's flask. Warm it a water bath for 15min adding acetone, and for 10 min without adding acetone at (75±2) °C. After cooling, add 10ml of dichloromethane. Shake it for 30s and allow to stand for 3min. In a 15ml test tube, place 5ml of the dichloromethane phase, 1ml of a Tropaeoline OO solution containing 3.25±10-3M, and 2ml of a buffer solution (pH3.29). Shake the solution for 2min mechanically, and centrifuge for 2min at 3000rpm. Take 2ml of the dichloromethane, and 0.5ml of methanol solution of 10% hydrochloric acid and measure the absorbance at 543nm using 1cm glass cells. No detectable interference for the determination of Cartap have been observed with other compounds, such as Ca2+, Mg2+, Fe3+, Al3+, sodium acetate, phenol, acetaldehyde, and agricultural chemicals of carbamate derivatives. Interference of Ni2+, Cu2+, Zn2+, Co2+, and alkylbenzene sulfonate were eliminated by extraction of Cartap with dichloromethane under alkaline condition.View full abstractDownload PDF (742K) -
Isao SANEMASA, Takemi MIZOGUCHI, Junko OHTSUKA, Toshio DEGUCHI, Hideo ...1983 Volume 32 Issue 7 Pages 420-425
Published: July 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSMixed resins are prepared to make anion- and cation- separation columns for ion chromatography. The optimum conditions have been studied. Aminex®and Dowex® are mixed in the weight ratio of 1 : 2 in pure water with stirring. The mixed resins thus prepared are packed in Teflon® tubes (1mm i. d., 3mm o. d.) and are used as separation columns. For The separation of anions, Aminex A-27 (13.5μm) -Dowex 50W-X16 { (200400) mesh} is used. On a 20cm column, seven anions (F-, Cl-, NO2-, HPO42-, Br-, NO3-, and SO42-, in the mixture) can be separated in 60min with 1.0mM NaHCO3 - 2.0 mM Na2CO3 eluent at a flow rate of 1ml min-1. For the separation of cations, Aminex A-5 (13μm) -Dowex 1-X8 { (200400) mesh} is used. On a column of 13cm to 15cm, six monovalent cations (Li+, Na+, NH4+, K4+, Rb+, and Cs+, in mixture) can be separated in 100min with 5mM HCl eluent at a flow rate of 0.5ml min-1. A mixture of six monovalent (from Li+ to Cs+) and four divalent (Mg2+, Ca2+, Sr2+, and Ba2+) cationscan be separated with 1.25 mM m-phynylenediamine dihydrochloride-1.25 mM HCl eluent, that is, a single peak corresponding to monovalent cations followed by four peaks of divalent cations (on a 13cm column Ba2+ ions are eluted in 110min at a flow rate of 0.5ml min-1). The elution times are longer compared to those for the commercially available columns, but the separation profiles of both cations and anions are satisfactory.View full abstractDownload PDF (1146K) -
Ken ISOBE, Hideaki AKADA, Saburo YANAGISAWA, Hidenari INOUE, Tsuneo SH ...1983 Volume 32 Issue 7 Pages 425-429
Published: July 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe oxidation and absorption processes in the zinc reduction-naphthylethylenediamine method were examined and improved so as to make the method suitable for rapid and precise determination of nitrogen oxides in flue gases. The use of alkaline absorption solution containing 0.15% hydrogen peroxide could promote the oxidation and absorption of nitrogen oxides. In this process, nitrogen oxides absorbed by the solution are converted to nitrite and nitrate ions. After the oxidation and absorption were finished, excess amount of hydrogen peroxide was easily decomposed by the addition of 0.3% solution of potassium chlorate. The pH range of the sample solution was then adjusted to 5.75.9, followed by the reduction of nitrate ions using zinc powder. The total amounts of nitrogen oxides were determined from absorbance of the colored solution based on the diazo-coupling reaction. Nitrogen monoxide over the concentration range of 10ppm to 100ppm was successfully determined by the present method. The coefficient of variation was less than 3%.View full abstractDownload PDF (904K) -
Keiya KOTSUJI, Mayo KAWAKAMI, Kazumi WAKIYA, Shigehiko HAYASHI1983 Volume 32 Issue 7 Pages 429-434
Published: July 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA method for the determination of microgram amounts of copper, based on the extraction flotation of bathocuproine-copper (I) chelate cations, has been developed. The chelate cations in an aqueous solution (pH4.68.0) were floated with lauryl sulfate anions by bubbling nitrogen through the aqueous phase, and collected with yield of about 97% in a mixture of 4-methyl-2-pentanone and 1, 2-dichloroethane (4 : 1 in vol.) on the solution surface. The copper in the organic phase was determined by spectrophotometrically. The proposed method could be successfully applied to the determination of copper in a small quantity of serum sample. The recommended procedure is as follows. Place (0.30.5) ml of serum and 0.5ml of trichloroacetic acid (0.2g/ml) solution in a 10ml test tube. Heat the mixture for 15min at 90°C, cool to room temperature and centrifuge for 15min at 1800g. Remove the supernatant and wash the precipitated serum proteins two times with 1ml each of water. To the combined supernatant, add 1ml of ammonium citrate (0.2g/ml) solution and 2ml of hydroxylammonium sulfate (0.1g/ml) solution, adjust pH to 7.0±0.2 with 0.5M sodium hydroxide solution, then add 4.7ml of ethanol and 1ml of 0.01% bathocuproine ethanol solution. After standing for 15min, add 2 ml of 0.005% sodium lauryl sulfate solution to the solution and dilute to 20ml with water. In a flotation cell, place the solution and 1.2ml of the mixed solvent. Bubble nitrogen through the aqueous phase at a flow rate of 60ml min-1. After 7min of bubbling, remove the organic phase, make up to 1ml with ethanol and measure the absorbance at 476nm against the reagent blank with 1cm microcells. The analyzed values were in good agreement with those obtained by using the modified LandersZak's method.View full abstractDownload PDF (1172K) -
Shozaburo HIRAOKA, Daijiro YAMAMOTO1983 Volume 32 Issue 7 Pages 434-438
Published: July 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA new highly sensitive spectrophotometric method is proposed for the determination of copper (II). This method is based on the catalytic effect of copper (II) ion on the coloration of potassium trithiocarbonate (K2TTC). By this method, ultratrace amount of copper (II) can be determined. The recommended procedure is as follows: To a sample solution (4cm3), containing copper (II) less than 120ng, was added buffer solution of pH12 (containing 1.5 × 10-3M EDTA, 11cm3) and 2w/v% sodium citrate (1cm3). The mixed solution was cooled with ice, and then added 4cm3 of a precooled 0.4w/v% K2TTC solution. Color was developed for 1h at pH12 at 40°C in a dark room. The absorbance was measured at 395 nm against the reagent blank. This catalytic effect was facilitated with an increase in temperature, but the colored product decomposed extensively at above 45°C. Serious interferences from manganese (II), nickel (II), iron (II), iron (III) ions can be eliminated by the addition of EDTA and sodium citrate solutions. The coefficient of variation (n = 5) of determination for the standard reference material (NIES No.1 PEPPER-BUSH) was 1.5%. This method is highly sensitive with the apparent molar coefficient of 107dm3mol-1cm-1, and enables the facile determination of copper (II) at the ppb level.View full abstractDownload PDF (745K) -
Kazuhiko TANAKA1983 Volume 32 Issue 7 Pages 439-443
Published: July 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe ion-exclusion chromatography with a cation exchange resin (H+-form) using methanol-water mixture as an eluent was investigated for the determination of F- in several metal industry wastewaters. Fluoride ion eluted from the column was monitored with conductometric detector (COND) and flow coulometric detector (FCD) based on the electrochemical reaction of Hion from H+ with p-benzoquinone at a constant applied potential (+0.45V vs. Ag-AgI). The retention volume (VR) of F- increased with increasing the concentration of methanol in the eluent, and that of very weak acid anion (HCO3-) decreased. Furthermore, the VR of strong acid anion (Cl-) did not vary and corresponded to the column void volume. Thus, quantitative separation of F- from Cl- and HCO3- was accomplished by elution with 40% (v/v) methanol-water. The COND responses of Cl-, F-, and HCO3- remarkably decreased with increasing the concentration of methanol. The FCD responses of Cl-, F-, and HCO3- did not remarkably decrease in comparison with the results obtained with the COND under the same elution conditions. This is most striking characteristics of the FCD. The calibration graph for F- obtained with the COND showed a nonlinear because of low dissociation at higher concentrations. However, the good linear relationship was obtained under the concentration range (5400) ppm of F- with the FCD. Therefore, it is recommended to use the FCD in this method. The present method was applied to the determination of F- in several actual samples with satisfactory results.View full abstractDownload PDF (795K) -
Minoru HOSOYA, Hideyuki KONNO, Shurô TAKEYAMA1983 Volume 32 Issue 7 Pages 444-448
Published: July 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA hydride generation-spectrophotometric method for the determination of tin in steels was proposed. In order to generate SnH4 completely, the very weak acidity was required for the sample solution. Therefore, SnH4 was generated by adding a sodium borohydride solution containing NaOH (22%) into the acidic sample solution. The liberated hydride was absorbed with a KMnO4 solution containing buffersolution (pH1.6), then Sn in it was determined by phenylfluorone spectrophotometric method. By this method, micro-amounts of tin {(0.0010.005)%} could be easily determined with better reproducibility compared to iodide separation method.View full abstractDownload PDF (860K) -
Soei SATO, Hironobu OHSHIRO, Shigeyuki TANAKA1983 Volume 32 Issue 7 Pages 449-452
Published: July 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe conditions for separation of aromatic sulfonates were examined by ion-pair high-performance liquid chromatography using μ Bondapak NH2 as a polar stationary phase. Benzene monosulfonate, benzene 1, 3-disulfonate, α-and β-naphthalene monosulfonates, three isomers of naphthalene disulfonates, and naphthalene 1, 3, 5-trisulfonate were used in this study. The influences on the elution behavior of aromatic sulfonates were evaluated in terms of solvent composition, the type of counter ion, the concentration of counter ion for forming ion-pair complex and pH value in mobile phase. Furthermore, the results obtained were compared with that of non-polar stationary phase such as octadecyl silanized silica gel. It is shown that the retention volume of aromatic sulfonates increases with increasing of the water content in H2O-CH3OH and the length of alkyl chain of counter ions and with lowering of pH value in the mobile phase. On the contrary, the retention volume decreases with increasing of counter ion concentration in the mobile phase. Except for the effect of the concentration of counter ions, above results were similar to those of reversed-phase ion-pair chromatography using non-polar stationary phase. These aromatic sulfonates were separated satisfactorily with a mobile phase of water-methanol (80/20 v/v) containing 2.5×10-3 M PIC-A reagent at pH 7, when μ Bondapak NH2 was used as a stationary phase. It is found that this method is applicable to the separation of aromatic sulfonates in practical imported samples.View full abstractDownload PDF (789K) -
Sanae IKEDA, Hiromu SATAKE, Hiroshi NISHIOKA, Masaru HIRAIWA, Yoichi I ...1983 Volume 32 Issue 7 Pages T75-T78
Published: July 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA method for the determination of total sulfur in blast furnace slags by means of the tin (II)-strong phosphoric acid was investigated. Sulfur species in blast furnace slags were reduced to hydrogen sulfide by heating a test portion in tin (II)-strong phosphoric acid after oxidizing to sulfate by bromine-acetone solution. The evolved hydrogen sulfide was absorbed in a zinc acetate solution, and titrated iodometrically. The analytical values {(0.060.9)%} of total sulfur in various blast furnace slags and iron ores were obtained with a coefficient of variation of less than 3% and a relative error of less than 5%. The whole procedure could be carried out in ca. 40 minas follows. Blast furnace slag (0.1g, ca. 200mesh) was decomposed with 10ml of tin (II)-strong phosphoric acid at ca. 300°C for 20min to evolve hydrogen sulfide quantitatively, followed by the absorption in a zinc acetate solution. To the sulfide solution, 5ml of 5×10-3 M potassium iodate standard solution, 5ml of 50% potassium iodide solution and 5ml of 6M hydrochloric acid were added, and then excess amount of evolved iodine was titrated potentiometrically with 0.1M sodium thiosulfate solution.View full abstractDownload PDF (736K) -
Hidek KIMURA, Koichi OGUMA, Rokuro KURODA1983 Volume 32 Issue 7 Pages T79-T83
Published: July 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA flow-injection method was described for the atomic absorption spectrophotometric determination of calcium in various types of silicate rocks. An about 50mg of powdered rock sample was fused with a mixture of 150mg of anhydrous lithium carbonate and 150mg of boric acid. The fusion cake was dissolved in 1M HCl and the volume was made up to 100ml with the same acid. A 120μl of the resulting solution was injected into the flow system, which was combined with an atomic absorption spectrophotometer. The atomic absorption spectrophotometer was operated under the standard conditions. To remove the interferences such as aluminum, phosphate, silicate, and sulfate, 130μl of 2% lanthanum solution was added to the sample zone by a merging zone technique. The results obtained for fourteen USGS and two GSJ rock standards were in good agreement with the recommended or reported values. The precisions ranged from 0.3% to 2%. Thesampling rate is 180samples per hour on the solution basis.View full abstractDownload PDF (971K) -
Preparation of heat-stable, weakly polar columns by superposing two different packings and application to the separation of partially methylated alditol acetatesAkira OKAHIRA, Hiroshi KOBATAKE1983 Volume 32 Issue 7 Pages T83-T88
Published: July 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSWe prepared heat-stable support of appropriate polarity by superposing two packings (SE30 and Silar 10C) in one column. Relative retention times of 8 partially methylated alditol acetates from arabinose, 8 from xylose, 17 from glucose, 23 from galactose, and 16 from mannose, were measured at various preparations of bed lengths, and the results indicated suitability of these column for the separation and indentification of these partially methylated alditol acetates.View full abstractDownload PDF (959K) -
A. WASEY, R.K. BANSAL, Masatada SATAKE, B.K. PURI1983 Volume 32 Issue 7 Pages E211-E218
Published: July 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA selective spectrophotometric method has been developed for the determination of nickel(II) and cobalt(II) as their phenanthrenequinone monoximate into molten naphthalene. The naphthalene was allowed to solidify, separated by filtration, dried and dissolved in dimethylformamide. The solution was diluted to 10 ml and the absorbance measured at 460 nm for nickel and 470 nm for cobalt. In both cases, the solutions were stable for more than 18 h. Beer's law is obeyed over the concentration range of 1.2-10.6 μg of nickel and 0.6-7.8 μg of cobalt in 10 ml of dimethylformamide. The various factors such as pH, amounts of reagent and naphthalene, and shaking and standing times were studied. The interference of various ions has been examined in detail and the method were developed for the determination of nickel and cobalt in various alloys and also nickel in hydrogenated oils. Conditions were also developed for the simultaneous determination of nickel and cobalt in alloys.View full abstractDownload PDF (952K) -
Qiu Xing-chu, Zhang Yu-sheng, Zhu Ying-quan1983 Volume 32 Issue 7 Pages E219-E223
Published: July 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA more sensitive spectrophotometric method for phosphorus determination was developed. The effects due to acidity, time, reagent concentration, temperature and diverse ions are reported. The method is satisfactory for analysing water-soluble inorganic phosphorus in soils.View full abstractDownload PDF (460K) -
Hiroko WADA, Tomosuke ISHIZUKI, Genkichi NAKAGAWA1983 Volume 32 Issue 7 Pages E225-E230
Published: July 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSSome thiazolylazo- and pyridylazobenzoic acids were studied for the metallochromic indicator in EDTA titration of nickel:2-(2-thiazolylazo)-4-methyl-5-(sulfomethylamino)benzoic acid(TAMSMB), 2-(5-bromo-2-thiazolylazo)-4-methyl-5-(sulfomethylamino)benzoic acid (5-Br-TAMSMB), 2-(2-thiazolylazo)-5-(N-ethyl-N-sulfomethylamino)benzoic acid(N-Et-TASMB) and 2-(3, 5-dichloro-2-pyridylazo)-4-methyl-5-(sulfopropylamino)benzoic acid(3, 5-diCl-PAMSPB). The formation constants of the nickel chelates with these reagents and the rate of the substitution reaction of nickel-TAMSMB chelate with EDTA were determined. TAMSMB is an excellent indicator for nickel because of the good color contrast between indicator and the nickel chelate, the large rate of color change reaction at equivalence point and the easy preparation of the reagent.View full abstractDownload PDF (755K) -
Ryoji KIKUCHI, G.KAISER, G.TOLG1983 Volume 32 Issue 7 Pages E231-E238
Published: July 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSFor the determination of silicon traces in gallium arsenide the sample is decomposed in a mixture constisting of HF/HNO3/HClO4 in a PTFE vessel. Silicon is separated from the matrix as SiF4 which is collected in an absorbing solution consisting of boric acid, ammonium molybdate and amidosulfonic acid. By the addition of H2O2, As(III) is oxidised to As(V) thus avoiding co-volatilization of As(III) which interferes with the photometrical measurement. After addition of ascorbic acid the reduced silicomolybdic acid is determined at 830 nm using 2 cm cells. The detection limit was found to be 2 μg/g. The standard deviation at the 30 μg/g level was found to be 3.4 %.View full abstractDownload PDF (1174K) -
Ajay K.JAIN, Sushma S.GAUR(AGRAWAL), Raj P.SINGH1983 Volume 32 Issue 7 Pages E239-E242
Published: July 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSSorption of two ammine complex cations, i.e., Co(NH3)63+ and Co(en)33+ on the heteropolyacid salt exchangers, collidinium tungsto and molybdo arsenates, which do not show affinity for simple transition metal ions, is investigated and discussed according to their cationic size.On the basis of the studies carried out it is concluded that these exchangers may also be used for the sorption and separation of transition metal ions as ammine complex cations.View full abstractDownload PDF (503K)
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