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Volume 27, Issue 5
Displaying 1-16 of 16 articles from this issue
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Itsuo MORI, Yoshikazu FUJITA, Yoshiyuki KAMATA, Takehisa ENOKI1978 Volume 27 Issue 5 Pages 259-263
Published: May 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSο-Hydroxyhydroquinonephthalein (Qn. Ph.)-molybdenum (VI) {Mo(VI)} complex in the presence of nonionic surface-active reagent (LT-221) can be used for the spectrophotometric and fluorometric determination of a minute amount of Mo (VI). A maximum absorption wavelength of the complex is 520 nm in a strongly acidic medium, where the apparent molar absorption coefficient is 130000. The sensitivity is 0.0007μg/cm2 Mo (VI) for an absorbance of 0.001. This method is applicable to the analyses of iron and steel for Mo(VI). The mole ratio of Mo (VI) and Qn. Ph. in the complex was estimated to be 1 : 3 by the continuous variation and mole-ratio methods. The recommended procedure for Mo(VI) is as follows. Spectrophotometry-To a 10 ml measuring flask an aliquot portion of the sample solution containing less than 9.2μg of Mo(VI), 2.0 ml of 3.5% LT-221, and 1.0 ml of 1.0 × 10-3 M Qn. Ph. are added, and the pH of the mixture is adjusted to 1.8 by the Walpole buffer solution. After diluting the solution exactly to 10 ml with water, the absorbance is measured at 520 nm against the reagent blank. Fluorometry-To a 10 ml measuring flask, an aliquot portion of the sample containing less than 2.1μg of Mo(VI), 1.0 ml of 3.5% LT-221 and 0.5 ml of 1.0 × 10-3 M Qn. Ph. are added, and the pH of the mixture is adjusted to 1.8 by the Walpole buffer solution. After diluting the solution exactly to 10 ml with water, the fluorescence intensity of Qn. Ph.-Mo(VI) solution is measured at 520 nm.View full abstractDownload PDF (806K) -
Takashi GOTO, Nobuyuki UNOHARA1978 Volume 27 Issue 5 Pages 264-268
Published: May 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSNickel thiocyanate-complex is formed when thio-cyanate ion is added to a sample solution containing trace amounts of nickel. The complex can be extracted with a solution of trioctylmethylammonium chloride (capriquot) in isopropyl acetate. The resulting organic phase can be used for atomic absorption analysis. To a sample solution containing up to 50μg of nickel, ammonium thiocyanate was added and the concentration of thiocyanate was adjusted to 1 M. The solution was adjusted to pH 4 with 5 ml of sodium acetate-acetic acid buffer solution. The total volume was made up to 50 ml with water. The thiocyanate-complex was extracted with 10 ml of 7 vol.% solution of capriquat in isopropyl acetate. The absorbance of the organic phase in air-acetylene flame was measured at 2320.0Å. A calibration curve obtained was straight up to 50μg of nickel. The standard deviation obtained from 10 runs was 2.13% for the determination of 30 μg of nickel. The presence of more than 1000μg of Cd(II), Co(II), Bi(III) and Fe(III) gave negative errors, but other ions did not interfere with the determination. By using isopropyl acetate as a diluent, it was possible to determine nickel in waste water with high sensitivity and precision.View full abstractDownload PDF (775K) -
Shohei ODA, Tsuguo SAWADA, Hitoshi KAMADA1978 Volume 27 Issue 5 Pages 269-273
Published: May 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDetermination of MnO4-in aqueous solution was attempted by a laser-induced photo-acoustic detection technique to the aimes of practical trace analysis. In photo-acoustic measurement of MnO4-, periodically chopped argon ion laser beam (514.5 nm) was directed into the sample cell. The piezoelectric ceramic (PZT-5H) was used for the detection of a photo-acoustic signal. This piezoelectric ceramic acts simultaneously as a sample cell and as a photo-acoustic detector. A linear relationship exsisted between a photo-acoustic intensity and MnO4- concentration up to 1.5 × 10-5 M, in the case that the laser power used was 400 mW. This is satisfactory for analytical use. In order to determine the optimum conditions, the effects of the laser power and chopping frequency on a photo-acoustic intensity were examined. The detection limit of MnO4-(defined as a 2 : 1 photoacoustic signal to noise ratio) was down to 5×10-8 M (6 ppb). This value is approximately 60 times lower than that obtained from the conventional-colorimetric analysis. It is obvious that the photo-acoustic detection method has an analytical utility as a new technique for the determination of trace amounts of materials in liquid.View full abstractDownload PDF (864K) -
Yasuyuki HOSHIKA, Giichi MUTO1978 Volume 27 Issue 5 Pages 273-278
Published: May 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe gas chromatographic determination of the ppb level concentration of 11 phenols, i.e., phenol, ο-, m-and p-cresol, 2, 3-, 2, 5-, 2, 6-, 3, 4-and 3, 5-xylenol, ο-and p-ethylphenol in air succeeded by the use of Tenax-GC precolumn (60/80 mesh, 18 cm ×4 mm i. d. glass), or Tenax-GC plus alkaline precolumn (2% KOH on glass beads, 30/60 mesh, 3 cm × 8 mm i. d. glass). The identification and determination of the 11 phenols were carried out based on the difference in chromatograms obtained by Tenax-GC or Tenax-GC plus alkaline precolumns. The chromatographic conditions are as follows : main analytical column packing, 0.1% SP-1000 on Carbopack C (80/100 mesh) ; column size, 1.75 m × 3 mm i. d. glass; column temperature, 220°C; carrier gas, nitrogen; flow rate, 37 ml/min. The eleven phenols were separated completely within 18 min. without tailing, except the overlapping of 2, 3-and 3, 5-xylenol peaks. The conditions of Tenax-GC and alkaline precolumn were as follows : operating temperature for the trapping, room temperature (about 25°C) ; operating temperature for the injection of the trapping samples into the gas chromatograph equipped with a flame ionization detector (FID), increased from the room temperature to 250°C in 35 s. In the case of the Tenax-GC precolumn injection method, repeatabilities of the retention times and the peak area (obtained from the counts of a digital integrator) of (9450)ng of 11 phenols were less than 1.0% and 10.3%, respectively, expressed as the coefficient of variation. The FID response showed a linear relationship with the peak area of the 11 phenols in the range of (22000) ng. Minimum detectable quantities of the 11 phenols were as low as 1 ng. The present method was ap-plied to determine phenols in ambient air of a phenol resin factory, and phenols in urban air (Nagoya area).View full abstractDownload PDF (994K) -
Satori UTSUMI, Yoshiyuki OINUMA, Akinori ISOZAKI1978 Volume 27 Issue 5 Pages 278-282
Published: May 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDimethylsulfonazo III reacts with barium ion to form a stable complex with change of color from wine red to blue, and has been used as a reagent for the titration of sulfate ion. The present work was undertaken to propose a spectrophotometric method for the indirect determination of micro amounts of sulfate ion based on this complex. The procedure is as follows. Five milliliters of the sample solution, 1 ml of 0.1 M acetic acid and 5 ml of ethanol are added to a 20 ml glass tube with a glass stopper, and the mixture is shaken. One milliliter of 3.0 ×10-4 M barium chloride is added to it, and the solution is allowed to stand for 30 min in order to form the barium sulfate. Then, 1 ml of 6.0 × 10-4M dimethylsulfonazo III is added to the solution. The absorbance is measured within five min at 660 nm against a reagent blank containing no barium ion. The concentration range of (0.25.0) × 10-5 M of sulfate ion could be determined. Many cations, especially the alkaline earth metals, interferred with the determination of sulfate ion. The application of a strongly acidic cation exchange resin eliminated the interference of metals. The coefficient of variation of the determination was found to be 1.7% from 10 repeated measurements with 35.3 × 10-5 M of sulfate ion in a river water.View full abstractDownload PDF (893K) -
Kazuo HIIRO, Akinori KAWAHARA, Takashi TANAKA1978 Volume 27 Issue 5 Pages 283-287
Published: May 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSTotal amount of nitrate and nitrite nitrogens was determined by measuring absorbances at 223 nm (A223) and 232 nm (A232) and calculating the difference between both absorbances (A223-A232). Absorption spectra of artificial sea waters containing various amounts of nitrate or nitrite nitrogen were measured and calibration curves at various wavelengths were constructed. Absorbances for each 1.0 mg/l of nitrate and nitrite nitrogens were plotted against wavelength. From these cruves, A219, A219-A241 and A223-A232 were adopted as suitable parameters for the determination of total amount of nitrate and nitrite nitrogens. From the result of determinations of nitrate and nitrite nitrogens in water samples by the sulfanilic acid-α-naphthylamine method, A223-A232 was found to be superior than A219-A241 and from the result of interference studies of inorganic and organic coexisting substances, A223-A232 was better than A219. Total amount of nitrate and nitrite nitrogens in 14 samples of sea waters and 18 samples of river waters was determined by the sulfanilic acid-α-naphthyl- amine method and A223-A232 of these water samples was also measured. Correlation coefficients between the nitrogen amounts and the A223-A232 were calculated to be 0.81 and 0.94, respectively.View full abstractDownload PDF (797K) -
Yoshifumi AKAMA, Toshio NAKAI, Fumikazu KAWAMURA1978 Volume 27 Issue 5 Pages 287-291
Published: May 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESS4-Capryl-3-methyl-1-phenyl-5-pyrazolone (CMPP) was used as the colorimetric reagent for the determination of iron(III). As iron(III) reacts with CMPP giving a red complex insoluble in water but soluble in organic solvent, small amount of iron was extracted from aqueous solution of pH 3.55.0 into 1-butanol as CMPP complexes and was determined spectrophotometrically. The complex exhibits its maximam absorption in 1-butanol at 450 nm with the molar absorptivity of 5×103. Formation of a 3: 1 complex of CMPP with iron was confirmed by the continuous variation method. Tin (IV), vanadium (V), aluminum (III) and phosphate interfered with the determination. The proposed procedure for the determination of iron is as follows : Take a sample solution containing less than 100 μg of iron, adjust the pH to 3.5 with sodium acetate and dilute to 40 ml with distilled water, and then extract the iron with a 10 ml portion of 0.3% (w/v) CMPP-1-butanol solution. Centrifuge the organic layer for 5 min and measure the absorbance at 450 nm against the reagent blank prepared in the same way. The method has been successfully applied to the determination of iron in zinc sample.View full abstractDownload PDF (782K) -
Kenyu KINA, Katsuhiko SHIRAISHI, Nobuhiko ISHIBASHI1978 Volume 27 Issue 5 Pages 291-295
Published: May 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSMacrocyclic compounds such as dibenzo-18-crown-6 (DB18C6) and naturally occurring polynactin react with alkali metal ions especially potassium ion. Thus forming cationic complexes can be extracted into 1, 2-dichloroethane as an ion-pair with anilino-naphthalene sulfonate. Anilinonaphthalene sulfonate has its maximum emission at 468 nm with an excitation at 377 nm in 1, 2-dichloroethane phase. The concentration of ppm level of potassium was able to be easily determined by the extraction-fluorometric measurement. The overall extraction equilibrium constant (Kex) and dissociation constant of the ion-pair in 1, 2-dichloroethane (Kd) was estimated by successive approximation method. DB18C6 has an inherent fluorescence based on the aromatic ring in the ultraviolet region (λex=277 nm, λem=306 nm). The complex formation constant in aqueous phase (Ks) and partition coefficient of uncomplexed DB18C6 (Pe) were deter-mined by means of the direct measurements of DB18C6 fluorescence under the extraction equilibria. The partition coefficient of the complex (Pc) was evaluated by substituting the values in the following relationship: Pc=Kex·Pe/Ks. The obtained values are as follows : log Kex=5.24, log Kd=-5.2, log Ks=1.4, logPc=8.8, log Pe=4.00. Monovalent cations, strontium (II), barium(II) and lead (II) interfere seriously with the determination of potassium with DB18C6. However, the interference of alkaline earth metals and lead (II) ion can be completely reduced by the use of polynactin.View full abstractDownload PDF (845K) -
Kazuo ISE1978 Volume 27 Issue 5 Pages 295-298
Published: May 05, 1978
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSMolybdenum was determined by atomic absorption spectrophotometry in 0.05 N ammoniacal solution after the decomposition of the concentrate with aqua regia. Negros ore from Philippines was used as a flotation feed, which contained chalcopyrites and calcium-magnesium minerals. Among the metals tested copper, iron and the alkaline earths interfered. Less than 50 ppm of copper yielded lower results for molybdenum. Higher results came out with more than 50 ppm of copper. In the presence of iron and citric acid (0.4 g/100 ml) which is a suppressor for hydroxide formation, a lower estimation resulted for molybdenum. Calcium interfered, lower results by 2 and >10% being obtained with respective 2.5 and 20 ppm of calcium. More than 20 ppm of magnesium behaved similarly. Sodium sulfate (0.5 g/100 ml) served as the suppressor for copper, iron and citric acid; 100 ppm each of copper and iron did not interfere in this way. Interferences due to calcium and magnesium (less than 60ppm) was able to be masked by the addition of sodium silicate (200 ppm as silica). The analysis of flotation products and synthetic samples consisting of molybdenite, chalcopyrite, calcium chloride and magnesium sulfate revealed that the atomic absorption method can be applied to the analysis of the concentrates for molybdenum with an error of about 2%.View full abstractDownload PDF (568K) -
Toshihiro HOSHIDA, Kunio MURASE, Kazunobu KODAMA1978 Volume 27 Issue 5 Pages 299-302
Published: May 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA new method is presented for the gravimetric determination of fluoride by precipitation as calcium fluorophosphate. The precipitation is formed by dropwise addition of a fluoride solution to a solution containing excess of calcium and phosphate ions, which is buffered with formic acid-ammonium formate at pH 3.70. The precipitate is crystalline, and confirmed to be fluoroapatite, Ca5F(PO4)3, by X-ray diffraction. It is readily filtered on a G4 sintered glass crucible and washed with the 0.1 M buffer solution and water, and then dried at 130°C to a constant weight. The gravimetric factor is 0.03768, and the determinable range is (28) mg F with the relative standard deviation of 2.4%. Sodium ion less than 100 mg dose not interfere. This method has the advantage of no interference from phosphate ion and ready filtration and washing.View full abstractDownload PDF (583K) -
Atsuo MIYAGAWA, Tsuneo OKUYAMA1978 Volume 27 Issue 5 Pages 302-309
Published: May 05, 1978
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSRecently, covalent chromatography has been developed for the purification of various thiol compounds. The method is based on the sulfhydryl-disulfide exchange reaction on the matrix beads. The so-called "activated thiol gel" used in previous studies was mainly 2-pyridyl-glutathione disulfide derivative of Sepharose 4B, but the reaction rate of sulfhydryl-disulfide exchange reaction of this gel had to be increased for the more effective use of covalent chromatography. In the present paper, we prepared seven different kinds of activated thiol Sepharose 4B, and sulfhydryl-disulfide exchange reaction of those gel was estimated directly on the matrix beads. The direct spectrophotometric suspension method uses the practically stable suspension of matrix beads in the solution of 0.05% agarose. The estimation of immobilized ligand was performed colorimetrically at the wavelength of absorption maximum. The reaction was performed with glutathione or BSA either at pH 7.5 or 9.5. 2-Pyridyl-N-oxide, 4-pyridyl, 3-carboxy 4-nitrophenyl, and 2-benzothiazole derivatives on activated thiol Sepharose 4B showed much higher reaction rate than 2-pyridyl-glutathione disulfide-Sepharose 4B. Covalent chromatography may be performed more easily and effectively with these higher reactive "activated thiol gel".View full abstractDownload PDF (1054K) -
Chozo YOSHIMURA, Kiyoshige MIYAMOTO, Kunihiko TAMURA1978 Volume 27 Issue 5 Pages 310-312
Published: May 05, 1978
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDetermination of small quantities of water in organic solvents (acetone, benzene, chloroform, diethylether, methanol and carbon tetrachloride) with the dimethylsulfoxide (DMSO) solution of lithium hydride was studied by conductimetry. The standard solution was prepared by dissolving lithium hydride in DMSO at about (6070)°C. The reaction proceeds as follows;
LiH + CH3-S→O-CH3→(CH3-S→O-CH2-·Li+) + H2↑
The procedure is simple and the solution is stable unless moisture is present. DMSO-Li reacts quantitatively with water in organic solvents and a sharp inflection point in the conductimetric titration curve indicates the end point. Influence due to the side reaction between DMSO-Li and organic solvents was also investigated.View full abstractDownload PDF (517K) -
Takahiko MATSUEDA, Masahiro MORIMOTO1978 Volume 27 Issue 5 Pages 312-314
Published: May 05, 1978
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAdsorption behavior of some metal ions by an activated carbon treated with 8-hydroxyquinoline (HOx-AC) was studied for the preconcentration of trace metals. The HOx-AC was prepared as follows : 20 g of pre-dried activated carbon was added into a conical flask containing 500 ml of 8-hydroxyquinoline solution (20 g/l ethanol solution) and the mixture was stirred for 24 h at 20°C. The activated carbon was separated by suction filtration and air-dried. It was washed two times with 500 ml portions of 0.2 M acetate buffer solution (pH : 4), and then washed four times with 500 ml portions of distilled water and air-dried again. Finally it was dried at 40°C for 60 min. The adsorbed amount of 8-hydroxyquinoline was 154 mg on 1 g of activated carbon. The HOx-AC can be used in the pH range from 5 to 10 for the adsorber. The adsorption capacity of Cu (II), Zn(II), Cd(II), Ni(II), Mn(II), Ca(II) and Mg(II) was determined. Effect of pH on the recovery of metal ions was also studied. The recovery of 25μg each of Cu(II), Zn(II), Cd(II) and Mn(II) in 500 ml of 0.5 M sodium chloride solution was more than 95%. The adsorption rate was rapid. The HOx-AC proved to be useful for the enrichment of trace metals.View full abstractDownload PDF (486K) -
Hitoshi HOSHINO, Takao YOTSUYANAGI, Kazuo AOMURA1978 Volume 27 Issue 5 Pages 315-316
Published: May 05, 1978
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA novel method for the separation of metal ions by reverse phase ion-pair partition chromatography is developed based on the ion-pair formation of anionic metal-4-(2-pyridylazo)resorcinolato (PAR, H2L) complexes with quaternary ammonium cation. The quantitative separation of cobalt (III)-, iron(III)-, and nickel(II)-PAR complexes was accomplished within 20 min on a 3.9 mm ×300 mm μ-Bondapak C18 column (Waters Associates), where 56.2% (v/v) methanol-water mixture containing 0.014 mol dm-3 of tetrabutylammonium bromide was used as a mobile phase in a flow rate of 0.91 cm3 min-1. These metal ions of (10-610-5)mol dm-3 level can be determined with the peak height calibration curves obtained at 254 nm using 0.04 absorbance unit full-scale. The order of the peak positions of the singly charged anions such as [CoL2]- [FeL2]- and HL- were well correlated to that of their ion-pair extraction constants.View full abstractDownload PDF (344K) -
Makoto MUNEMORI, Yuroku YAMAMOTO, Shigeru SHIMOMURA, Kazuo HIIRO, Taka ...1978 Volume 27 Issue 5 Pages T15-T19
Published: May 05, 1978
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA joint committee on analysis of mine drainage, organized in the Osaka Mine Safety and Inspection Department, planned a study on the spectrophotometric determination of selenium with 3, 3'-diaminobenzidine. According to our cooperative investigation the procedure prescribed by JIS K 0102-1972 is recommended to be modified in part as follows : (1) Ferric hydroxide, instead of basic ferric acetate, is used for the coprecipitation of selenium with Thymol Blue as an indicator for pH adjustment. (2) Two ml, instead of 1 ml, of warm hydrochloric acid (1+1) is used for dissolving coprecipitated selenium. (3) Hydrochloric acid, instead of formic acid, and ammonia are used for the adjustment of pH to 1.5 to 2.0 when selenium is allowed to react with 3, 3'-diaminobenzidine. The mixture is heated in a water bath for 5 to 10 min, instead of being allowed to stand for 40 min at room temperature. Eleven analytical laboratories of mining works participated in the round robin tests. In each laboratory, two parallel determinations a day were conducted on the same sample for three days, thus resulting in six determinations. The results are illustrated as χ-R charts for water sample C containing 0.225 ppm selenium alone and for water sample D containing 0.247 ppm selenium and foreign ions. Averages obtained for selenium were 0.221 ppm for sample C and 0.242 ppm for sample D. Based on the analysis of variance, the standard deviations among laboratories were found to be 0.008 ppm for sample C and 0.010 ppm for sample D.View full abstractDownload PDF (946K) -
Makoto MUNEMORI, Yuroku YAMAMOTO, Kazuo HIIRO, Takashi TANAKA, Takahir ...1978 Volume 27 Issue 5 Pages T19-T23
Published: May 05, 1978
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA joint committee on analysis of mine drainage, organized in the Osaka Mine Safety and Inspection Department, planned a round robin test concerning a spectrophotometric method for the determination of arsenic with silver diethyldithiocarbamate. This is one of the methods prescribed by JIS for the determination of arsenic. Twelve laboratories of mining works participated and in each laboratory two parallel determinations a day were made for three days on the same control sample. The results are summarized as χ-R charts for the sample A containing 0.0220 ppm arsenic alone and for the water sample B containing 0.0250 ppm arsenic and various foreign ions. Averages of arsenic found were 0.0222 ppm for the sample A and 0.0255 ppm for the sample B. The results of analysis of variance revealed that the standard deviations among laboratories were 0.14×10-2 ppm for the sample A and 0.06×10-2 ppm for the sample B.View full abstractDownload PDF (860K)
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