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Volume 46, Issue 11
Displaying 1-12 of 12 articles from this issue
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Teiji TANIZAKI, Kenzo BABA, Kiwao KADOKAMI, Ryota SHINOHARA1997 Volume 46 Issue 11 Pages 849-855
Published: November 05, 1997
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe authors have developed an analytical method for arsenic, selenium and antimony in water by using hydride generation (HG) coupled with ICP-MS. The method provides simultaneous analysis with high sensitivity and precision. After samples had been decomposed with perchloric acid and nitric acid, the target metals were pre-reduced with HCl and potassium iodide, , and then introduced into HG/ICP-MS. Interference of 40Ar35Cl caused by HCl with measurement of 75As was negligible. 72Ge is a useful internal standard for HG/ICP-MS, because it can correct any drift of the sensitivity of ICP-MS. The instrumental detection limits of the method were as low as 10 ng/l; these values are one-one hundredth as those of HG/ICP-AES. The overall recoveries of sea-water and waste water samples to which the metals were spiked to make 1 μg/l of each were more than 80%; the relative stadard deviations were less than 10%. Applying the method to seawater, the authors found the three metals to have the same concentration levels as those published.View full abstractDownload PDF (1326K) -
Osamu FUJINO, Kunita HARA, Satoru IKEJIMA, Shiro GODA1997 Volume 46 Issue 11 Pages 857-862
Published: November 05, 1997
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSInductively coupled plasma-mass spectrometry (ICP-MS) was applied to determine the tellurium in lake water. Although ICP-MS is highly sensitive (ppb) to tellurium, the direct analysis of lake water is very difficult because of the extremely low concentration (ppt). Further, the intensity of tellurium was changed due to coexisting barium. It was therefore necessary to concentrate tellrium and to separate it from barium. After the tellurium in lake water was concentrated and separated from barium by coprecipitation with ferric hydroxide, the precipitate was dissolved in hydrochloric acid. The ferric ion was removed by a solvent-extraction method with HPMTFP-butyl ether system, and the aqueous phase was directly injected into the ICP-MS apparatus. Tellurium in Lake Biwa was found to be 0.0360.043 ppb.View full abstractDownload PDF (1205K) -
Kouichi TSUJI, Kazuaki WAGATSUMA, Hideyuki MATSUTA1997 Volume 46 Issue 11 Pages 863-867
Published: November 05, 1997
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA maximum high voltage of 5 kV was applied to a Grimm glow-discharge lamp using helium gas. The characteristic X-rays and continuous X-rays were measured from an X-ray window attached to the lamp, indicating the existence of fast electrons which could excite X-rays. The electrons emitted from the cathode surface by ion impact are accelerated by the cathode fall region, then pass right through both the negative glow and the hollow anode, resulting in bombardment to the X-ray window. The fast electrons were utilized as an excitation source in X-ray elemental analysis. It was demonstrated that quantitative analyses of Fe-Si alloys are possible by this electron-excited X-ray emission method.View full abstractDownload PDF (1112K) -
Akira MACHINO, Ikuno UCHIDA, Kunitoshi MATSUNOBU, Takanori YOSHIMORI1997 Volume 46 Issue 11 Pages 869-874
Published: November 05, 1997
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe odorant blend of tertiary butylmercaptan (TBM) and dimethylsulfide (DMS) is generally used as an odorant in city gas based on liquefied natural gas. The concentrations of both TBM and DMS in city gas are about 2 volppm. To control the quality of city gas, a simple method is required to determine the odorant concentration at the end of gas pipelines. This paper reports on the development of a gas detector tube which can measure the DMS concentration in city gas. The principle of coloration is the oxidation of DMS by KMnO4. The DMS concentration in city gas is determined by a newly developed gas detector tube conected to a TBM gas detector tube. The determination range at 293 K was 0.8-8.2 volppm when the test gas volume was 100 ml. The repeatability of measurements was within ± 10% as a relative standard deviation.View full abstractDownload PDF (1145K) -
Hideji TANAKA, Akiko MITANI, Kensaku OKAMOTO, Hideyoshi MORITA, Shiger ...1997 Volume 46 Issue 11 Pages 875-880
Published: November 05, 1997
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSGraphite atomizer tubes were treated with tantalum (Ta) in order to coat the surface of the tubes with tantalum carbide (TaC), and were used for the determination of gallium by AAS. The measurement conditions were optimized and the effects of diverse coexisting substances (metal cations, anions and organic compounds) were examined. By this treatment, the sensitivity increased by a factor over 5 along with an improvement in the repeatability. The calibration curve of Ga obtained by using a TaC-coated tube and a matrix modifier (250 mg dm-3 Al + 500 mg dm-3 Ni + l mol dm-3 HNO3) was linear over the range of 0 300 μg dm-3, and the detection limit (3σ0) was 10 μg dm-3 (0.10 ng). The present method, was applied to analyses of rock standard materials.View full abstractDownload PDF (1339K) -
Hitomi KOBARA, Koji TAKEUCHI, Takashi IBUSUKI1997 Volume 46 Issue 11 Pages 881-886
Published: November 05, 1997
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA diffusion scrubber system equipped with an ion chromatograph (IC) was used for the collection and determination of gaseous NH3 and HNO3 at 100200 ppb levels. Purified water was used as the absorbing solution of the scrubber. The gaseous HNO3 concentration was measured by the impinger trap-IC method and/or the reduction (to NOx)-chemiluminescence method. The gaseous NH3 concentration was measured by the impinger trap (boric acid solution)-IC method. The determined collection efficiencies were more than 97.4% for HNO3 and more than 92.3% for NH3 under a relative humidity of 070%. The relative standard deviations were less than 1.1% (n = 5) for successive collection and analysis. It was confirmed that this system can determine gaseous HNO3 and NH3 correctly even in the presence of ammonium nitrate particles.View full abstractDownload PDF (1338K) -
Takayuki ABE, Junko TAKAYANAGI, Chikakiyo NAGATA1997 Volume 46 Issue 11 Pages 887-889
Published: November 05, 1997
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSCarbon-13, silicon-29 and tin-119 chemical shifts were measured for chloro and bromo-substituted compounds [(CH3)nMX4-n; M=C, Si, Sn;n=0-4], and the behavior of the chemical shifts for carbon, silicon and tin atoms in those compounds were investigated. The 13C, 29Si and 119Sn chemical shifts of monochloro-substituted compounds were shifted to a lower field by 30-172 ppm in the order of 29Si, 13C and 119Sn, which could. be explained by an inductive effect. The 13C chemical shifts for chloro-substituted compounds were shifted to a lower field in order of mono, di, tri and tetrachloro substituents, however, the 119Sn chemical shifts in those compounds were shifted to higher fields with increasing number of chlorine atoms in a molecule. This is considered to be due to the effect of a steric compression between the substituted chlorine atoms. The 13C, 29Si and 119Sn chemical shifts of monobromo-substituted compounds were also shifted to a lower field by 27135 ppm in the same order as that of monochloro-substituted compounds. The 13C, 29Si and 119Sn chemical shifts for bromo-substituted compounds shifted largely toward a higher field with increasing number of bromine atoms in a molecule, which probably could be attributed to the heavy atom effect.View full abstractDownload PDF (485K) -
Akihiko SUZUKI, Fumio NAKADAI, Masayuki ITAGAKI, Kunihiro WATANABE1997 Volume 46 Issue 11 Pages 891-894
Published: November 05, 1997
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSCatalytic analysis of trace manganese using Stilbazo has been investigated in the presence of ethylenediamine and hydrogen peroxide. Stilbazo was decomposed by the hydroxy radical formed with hydrogen peroxide in the presence of trace Mn(II). The reaction rate was enhanced by ethylenediamine, which acts as an activator in addition to a masking agent. The concentration of Mn(II) was estimated by measuring the decrease in the absorbance of Stilbazo(S). The absorbances of Stilbazo were measured at the start and then t minutes after the reaction-start, respectively. The relation between [S]t and [Mn2+] is ln[S]t= -k [Mn2+]t, +ln[S]0. Here, [S]0 and [S]t denote the concentrations of Stilbazo at the initial state and, then t minutes after reaction-start. In the above, k is the apparent reaction rate constant. This reaction was considered to be pseudo-first order regarding S. A calibration curve showed linearity over the range 01.2 ppb at t=5. The detection limit of Mn(II) by the proposed method was 10 ppt. This method was applied to tap-water samples. The results showed good agreement with the values obtained from flameless atomic-absorption spectrophotometry. Diverse ions (Ca(II), Co(II), Cr(III), Cu(II), Ni(II), Ti(IV) and V(V)) did not interfere with the determination of Mn(II) at 0.8 ppb. On the other hand, Fe(III), Zn(II) and Al(III) interfered with the determination of Mn(II) in the presence of more than 50-fold the Mn(II) concentration.View full abstractDownload PDF (836K) -
Kimitoshi SATO, Motoyuki SUZUKI, Takashi GOTO1997 Volume 46 Issue 11 Pages 895-897
Published: November 05, 1997
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe separation and preconcentration of trace vanadium from an aqueous solution for a graphite furnace atomic-absorption spectrometric (GF-AAS) determination was studied using silica gel loaded with trioctylmethylammonium cloride (Capriquat). A sample solution containing V was adjusted to pH 6.0. The solution was then passed through 1.0g of Capriquat loaded in a silica gel column at a flow rate of 10 ml min-1. The V collected on the Capriquat-loaded silica gel on the column was eluted with 10 ml of 0.5 M perchloric acid, and then determined by GF-AAS. In this method, over 99% of the V was adsorbed at about pH 6.0. The calibration curve was linear from 0.05 to 2.5 μg/l of V. The proposed method has been applied to the determination of V in river water and seawater samples.View full abstractDownload PDF (527K) -
Yoshimi ITOH, Katsushi SUGAWARA, Itsuo YOSHIZAWA1997 Volume 46 Issue 11 Pages 899-903
Published: November 05, 1997
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn efficient synthetic method of 6-oxoestradiol was established by modifying the previous method by Garza and Rao. The present method is characterized by the quantitative extraction of 6-oxoestradiol produced during an oxidation reaction using Girard's reagent P (GP). The procedure is as follows: (1) reaction of estradiol-3, 17-diacetate with 5-dimethylpyrazole/chromium trioxide complex in dichloromethane; (2) column chromatography (SiO2) of the reaction mixture to obtain steroidal fraction by dichloromethane as an eluent, followed by saponification of the eluate; (3) reaction of the product with GP in methanol; (4) removal of the nonketonic steroid from an aq. layer, where the hydrazone of 6-oxoestradiol is remained; (5) formation of 6-oxoestradiol by acidification of the aq. layer. The overall yield of the 6-oxoestradiol from estradiol was greater than 45 percent.View full abstractDownload PDF (1018K) -
Shinichi YAMAGUCHI, Shuichi ETO, Yukuo EGUCHI, Kozo KIDO, Yoshiharu HI ...1997 Volume 46 Issue 11 Pages 905-914
Published: November 05, 1997
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple and rapid screening analysis for multiple pesticide residues in agricultural products was developed. It is an especially effective mean for detection in analyzing food with much interference because the reliability confirmation of substances is greatly improved over the SIM method. A sample is extracted with acetone and reextracted with a non-polar solvent by salting out. We used 50 % ethyl acetate/hexane as a non-polar solvent. The extract was cleaned up by GPC with ethyl acetate: cyclohexane (1: 1) as eluent. We used Bio Beads S-X3 (200-400 mesh) as a GPC gel. Measurements of GC/MS were performed in the scanning mode. We could confirm substances with mass spectra at high background levels, such as food, and perform with only one injection to the instrument without grouping pesticides, as in the case of the GC/MS-SIM method. Due to these merits, we could increase the reliability and decrease the time consumption. We could analyze as a screening analysis 102 kinds of pesticides. The detection limits in the samples were from 0.004 to 0.05 μg/g.View full abstractDownload PDF (1904K) -
Satoshi ITO1997 Volume 46 Issue 11 Pages 915-916
Published: November 05, 1997
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (485K)
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