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Volume 39, Issue 12
Displaying 1-13 of 13 articles from this issue
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Hiroyasu YOSHIKAWA, Hideo IWATA, Takanori AKIYOSHI, Fukuchu TUTUMI1990 Volume 39 Issue 12 Pages 801-804
Published: December 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA rapid determination of free calcium oxide in basic oxygen furnace slag was investigated by measuring the conductivity of the solution after ethyleneglycol extraction. Oxides of iron and manganese (FeO and MnO), which were contained as solid solutions with the calcium oxide, were also extracted by ethyleneglycol. Because conductivity of the calcium was influenced by the presence of these co-extracted metals, a method of correcting the conductivity was investigated. This method consisted of measurement of the absorbance at 490 nm for the determination of co-extracted metals. The analytical values obtained by the present method were in agreement with those obtained by atomic absorption. Analytical precision was 2.53.3% R.S.D.View full abstractDownload PDF (713K) -
Hiroshi NISHIDA1990 Volume 39 Issue 12 Pages 805-809
Published: December 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSIn the spectrophotometric determination of beryllium with Chromazurol S (CAS, H4L) in the presence of Zephiramine (ZCl) at pH 5.5, the absorbance of a sample solution against a reference solution was measured by exact matching pH and anion concentration between the two solutions. Therefore, beryllium was successfully determined by utilizing the reference solution prepared by adding acetylacetone as the masking agent of beryllium to the sample solution in order to cancel the influence of anions. The optimum conditions for the preparation of the sample solution were as follows; [Be]: (0.26.7)×10-6 mol dm-3, [NH4Cl]: 0.2 mol dm-3, [EDTA]: (0.44)×10-3 mol dm-3, [CAS]: 9.4×10-5mol dm-3, [Zephiramine]: 4×10-3 mol dm-3, pH: 5.5, standing time : 20 min, wavelength : 615 nm. The reference solution was prepared in the same manner as the sample solution but with the exception of adding 0.078 mol dm-3 of acetylacetone before the addition of CAS. The absorbance of the sample solution was measured at 615 nm against the reference solution. The relation between the absorbance (A) and the beryllium concentration(xμg/25 cm3) was given by A=0.010+0.539x. The apparent molar absorptivity at 615 nm was 1.21×105 dm3 mol-1 cm-1. When 4×10-4 mol dm-3 of EDTA was added, less than about 2.7×10-4mol dm-3 of the other cations such as Al(III), Fe(III) and Cu(II) etc. and less than 2×10-6 mol dm-3 of U(VI) did not interfere. By this method, 12.4 ppm of beryllium in Coal Fly Ash (NBS SRM 1633a) was determined by the standard addition method without separation of the other cations (the relative standard deviation: ±3%). The species of beryllium-CAS complex formed in micelles was also investigated. In the presence of chloride ion, Z4Be(HL)2(ZCl)4 was formed.View full abstractDownload PDF (984K) -
Futoshi SUGIMOTO, Hiroki IWAYA, Yoshimichi MAEDA, Takatugu AZUMI1990 Volume 39 Issue 12 Pages 811-816
Published: December 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSSpectrophotometric determination of hypophosphite ions in electroless plating solution was studied using Molybdenum Blue method. Ten milliliters of 500 mg/1 Fe(III) solution was added to 300 ml of a sample solution containing phosphite and hypophosphite ions, and pH of the solution was adjusted to 5. The precipitate including Fe(III) phosphite was removed by filtration. Hypophosphite remaining in the filtrate was oxidized to phosphate ions by the addition of 25 ml of 0.2% potassium permanganate solution. The phosphate was then precipitated with 5 mg of Fe(III). The precipitate collected on a membrans dissolved with 20ml of (lt20) H2 SO4 and 2 ml of 0.3% hydrogen peroxide solution. The phosphate in the solution was determined by the Molybdenum Blue method (JIS K 0101). The proposed method was not influenced by the coexistence of phosphite(<100 μg), phosphate(<750μg), nickel(<50mg), cobalt(<5 mg), tartrate(<5 mg) and citrate(<2mg) ions, and can be used for the determination of hypophosphite ions in plating solution.View full abstractDownload PDF (791K) -
Yukio YOKOYAMA, Hiroaki KAKINUMA, Masahiko TSUCHIYA1990 Volume 39 Issue 12 Pages 817-822
Published: December 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSLiquid ionization (LI) mass spectrometry was applied to analysis of organic acids in urines of newborns suffering inborn errors of metabolism. Addition of nitric acid to a sample urine was found to be a useful and effective pretreatment for detecting organic acids due to disorders. In the case of methylmalonic acidemia, the MH+ peak at m/z 119 in LI mass spectrum of the acidified urine was about ten times more intense than that of the nontreated urine. Nitric acid is a proton doner for organic acids and also increases ion abundances in aqueous solution. The MH+ peaks of lactic acid (m/z91) in congenital lactic acidemia, of 3-hydroxybutanoic acid (m/z 105) in glycerol kinase deficiency, and of phenylacetic acid (m/z 137) in phenylketonuria (PKU) were clearly observed as characteristic peaks. The MH+ ions of amino acids such as phenylalanine were also observed as intense peaks. The method is simple and rapid, and is useful for screening and/or diagnosis of inborn errors of metabolism.View full abstractDownload PDF (1030K) -
Koji MATSUSAKI1990 Volume 39 Issue 12 Pages 823-827
Published: December 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA method for removal of interference by chlorides in the determination of indium by graphite furnace AAS was investigated. The mixture of ammonium salt of EDTA, nickel nitrate and aluminium nitrate was suitable as a matrix modifier. Since the analyte and the other cations were masked by EDTA, the formation of indium chloride in drying step was prevented and the volatile ammonium chloride formed could be easily removed from the furnace in pre-atomization steps. On the other hand, EDTA complexes of nickel and aluminium act as sensitivity enhancement agent for the atomic absorption of indium. In the presence of 5×10-2M diammonium-EDTA, 0.3M ammonia, 4×10-3 M nickel nitrate and 1×10-3 M aluminium nitrate, the tolerance concentration of coexisting metallic chlorides were about 4001000 times larger than that resulted in the absence of EDTA. Furthermore, the sensitivity of indium in the atomic absorption was increased by a factor of about 20 compared to that resulted in the absence of the matrix modifier.View full abstractDownload PDF (730K) -
Hiroyasu YOSHIKAWA, Youichi ISHIBASHI, Naoki GUNJI, Takeshi MISUMI1990 Volume 39 Issue 12 Pages 829-833
Published: December 05, 1990
Released on J-STAGE: January 19, 2010
JOURNAL FREE ACCESSTrace metals (Fe, Ni, Mn, Cu, Co, Mg, Sn and Cr) in high-purity titanium were determined by ICP-AES after coprecipitation separation with a mixture of bismuth hydroxide and indium hydroxide. A sample (500 mg) was dissolved with 20cm3 of 6 M hydrochloric acid and 0.5cm3 hydrofluoric acid. Before the coprecipitation procedure, the resulting titanium ions were masked with hydrogen peroxide to form its peroxocomplex. At least 4cm3 of hydrogen peroxide was required for masking the titanium ions. Sn and Cr did not show quantitative recovery, due to the formation of their oxocompounds. Although the recovery of Ni and Co was constant, the recovery of Fe, Mn and Cu decreased with increase of added hydrogen peroxide or pH. Fe, Ni, Cu and Co at pH 9.5 and Mg at pH 11.5 were recovered quantitatively. Analytical results for Fe, Ni, Cu, Co and Mg obtained by the present method showed satisfactory precision and accuracy.View full abstractDownload PDF (863K) -
Kyohko KOBAYASHI, Hajime FUJISHITA, Yoshiyuki SATOH, Toshimasa NAKAYAM ...1990 Volume 39 Issue 12 Pages 835-839
Published: December 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA sensitive and rapid determination of Na and Fe in an ethoxy ethyl acetate (EEA) solution of positive type photoresist has been investigated using ICP-MS for routine analysis of factory products. A sample of the photoresist, OFPR800, was diluted 7 to 20 times with EEA and directly introduced into an ICP-MS nebulizer. A deposition of carbon on the sampling cone front of the mass spectrometer could be eliminated by the addition of oxygen (70 ml/min) into carrier gas. An optimum condition to reduce the intensity of ArO at m/z 56 was as follows : rf power 1.3 kW, cooling gas flow rate 18 1/min, plasma gas flow rate 1.2 1/min, sampling depth 12 mm. Under these conitions, the regression coefficients of the working curve were almost the same among 7 to 20 times diluted solutions, showing that the variation of viscosity and polymer content of the products has no significant effect on the determination of Na and Fe. The detection limits (3σ) were 1.2 ppb for Na and 1.0 ppb for Fe in a diluted solution of the photoresist.View full abstractDownload PDF (770K) -
Sadayuki MATSUDA1990 Volume 39 Issue 12 Pages 841-843
Published: December 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSAddition of aqueous protamine solution to Methyl Orange solution caused color change from bright orange to pale yellow at pH 6.80. A significant decrease in absorbance at 465 nm (λmax) and increase at 365 nm with increasing protamine concentration was observed with isosbestic point at 383 nm. This metachromasy was inhibited by the presence of ethanol. This phenomenon was used to determine ethanol content. The calibration curve was not a straight line. The applicable maximum range was 13( v/v %) of ethanol.View full abstractDownload PDF (367K) -
Eiko NAKAMURA, Kumiko ISHIWATA, Hiroshi NAMIKI1990 Volume 39 Issue 12 Pages 845-847
Published: December 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSAfter removal of anionic surfactants by an ion-exchange technique, cationic surfactants were extracted as their chlorides into chloroform. Ion pairs of the cationic surfactants and Disulphine Blue formed in the chloroform phase were measured spectrophotometrically as follows : A 50 ml of a sample solution containing cationic surfactants (above 1 μg as Zephiramine) is passed through an anion-exchange column (Amberlite IRA-401, 15 ml) at a rate of 1 ml/min and the column is washed with 50 ml of 50% methanol. Five milliliters of sodium chloride solution (10%) and 10 ml of chloroform are added to the eluate. The mixture is then shaken for 1 min to extract cationic surfactants into chloroform. The chloroform phase is shaken for 1 min with a mixture of 10 ml of citrate buffer solution (0.1 M, pH 5), 5 ml of sodium sulfate solution (0.4 M) and 1.5 ml of Disulphine Blue solution (1.17×10-4 M). The absorbance of the chloroform phase is measured at 628 nm. Cationic surfactants in water above 20 μg/1 could be determined by the proposed method.View full abstractDownload PDF (355K) -
1990 Volume 39 Issue 12 Pages e1
Published: 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSDownload PDF (106K) -
Yoshinori MIYAKI, Hiroe YOSHIOKA, Kunihiko HASEGAWA1990 Volume 39 Issue 12 Pages T163-T167
Published: December 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSMicro scale batch method was used for the isolation of 125mTe from the system of the penta valent antimony-125 {125Sb(V)} and tellulium-125 m (125mTe) system in radioactive equiliblium state. In preliminary experiments, the effects of the volume of bromine water, and the time of adsorption on the adsorption ratio were examined using the best conditions. The effects of acid concentration and the time of elution on the elution ratio were examined using 125mTe as tracer. A hundred microliters (ca. 0.03 g) of anion exchange resin(Cl- form) treated with concentrated HCl was placed in a polypropylene micro-tube (1.5 ml) equipped with a stopper. A hundred microliters of the sample solution [(125mSb(V)-215mTe)/ in 9 M HCl solution including bromine water of 5 vol % ] was mixed with the resin and shaken for 10 min, in order to adsorb metal ions. After the resin was precipitated by centrifugation, the supernatant solution including 125mTe(VI) was pipetted off, 9 M HCl solution including bromine water of 5 vol% was added and then analyzed for 125mTe(VI). The aliquots were ajusted to the HCl concentration of 1 M by adding of 1.0 ml of dil.HCl or deionized water. The samples were again shaken for 10 min and centrifuged. The supernatant solution including 125mTe(IV) was pipetted off. The radioactivities of the supernatant solutions were measured using scintillation counter of NaI (T1) well-type. The yields of 125mTe(IV) by this method were 75, 97 and ca. 100% respectively for one, two and three time elutions. The elution ratio (contamination ratio) of 125Sb(V) was 0.51 %. This method was compared with ordinary macro-scale column method. It was found that this method gave higher concentrations of radioactivity and that less amount of radioactive wastes because this method required less volume of the eluting solution and resin.View full abstractDownload PDF (740K) -
Tadashi MOCHIZUKI, Akiko SAKASHITA, Yoichi ISHIBASHI, Naoki GUNJI, Hid ...1990 Volume 39 Issue 12 Pages T169-T174
Published: December 05, 1990
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSAn ICP-MS has been developed for the rapid determination of trace elements in silicate rocks. Rock sample solutions were prepared by fusion with a mixture of lithium carbonate and boric acid and the subsequent dissolution of the melt with 1.4 M nitric acid. The resulting solutions containing 0.05% (m/v) solids were analyzed using ICP-MS without making any further treatment. The use of Rh as an internal standard was effective to minimize the signal suppression caused by high concentration of the borate flux used. This procedure has been applied to the determination of trace elements in standard silicate rocks of the Geological Survey of Japan. Accuracy and precisions were satisfactory for the analytes such as V, Cr, Sr, Y, Zr, Ba; and rare-earth, Hf, Ta, Bi, Th and U. However, Si polyatomic ions interfered in the Sc determination and the loss on fusion lowered the values for Rb.View full abstractDownload PDF (808K) -
Shinichiro NORIKI, Masayuki MINAKAWA, Masami FUKUSHIMA, Shizuo TSUNOGA ...1990 Volume 39 Issue 12 Pages T175-T178
Published: December 05, 1990
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA practical method is proposed for the determination of manganese at ppbppt level in seawater. Manganese in 250 ml of seawater is extracted at pH 9.09.3 into 10 ml of chloroform with oxine (8-quinolinol) chelate, which is subsequently extracted into 4 ml of 7 M-HNO3. Manganese in the HNO3 solution is determined by graphite furnace AAS. The recovery of manganese is determined by spiking 54Mn to the seawater. The relative standard deviations were 6% at the 0.07 ppb level and 7% at the 0.5 ppb level of manganese in seawater.View full abstractDownload PDF (490K)
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