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Volume 38, Issue 1
Displaying 1-14 of 14 articles from this issue
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Kunishige HIGASHI, Akinori KAWAHARA, Shinichi WAKIDA, Masataka YAMANE, ...1989 Volume 38 Issue 1 Pages 1-5
Published: January 05, 1989
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSSeparation characteristics of several types of compounds were studied by high performance gel chromatography to establish a speedy and sensitive method for evaluating molecular weight distribution of organic compounds in water. A column of 7.6 mm in internal diameter and 50 cm in length packed with Asahipak GS-220 was used as a stationary phase. This gel was made from polyvinylalcohol copolymer and has an exclusion limit of molecular weight of 3000. Distilled water was used as the mobile phase at a flow rate of 0.5 ml/min at room temperature, and the chromatogram was obtained with a refractive index detector. The separation characteristics depended on the chemical structures of the organic compounds. In the case of polyethyleneglycol series composed from several unit structures, those are hydrophilic in nature, the elution volume decreased with increasing molecular weight. On the other hand, in the case of aliphatic alcohol series, the elution volume increased with increasing molecular weight, and the adsorption effect on the gel was predominant on the separation. Hydrophobicity of the gel used in this study was larger than Sephdex gel G-15. The proposed method was speedy and had high sensitivity and reproducibility.View full abstractDownload PDF (763K) -
Noriko YAMAMOTO, Naoko KABEYA, Nahoko YAMAGISHI, Tsuneo SHIRAI1989 Volume 38 Issue 1 Pages 6-9
Published: January 05, 1989
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA new solvent extraction/spectrophotometric method for determining trace amounts of ammonia in the atmosphere is described. The procedure is based on the formation of indophenol by the reaction of phenol, hypochlorite and ammonia using a coupling agent. Indophenol solution was concentrated by solvent extraction by forming an ion-associate form indophenol and trioctylmethylammonium chloride (TOMA+ ) using cyclohexane as solvent. The procedure is as follows : Take 20 ml of indophenol solution fromed from an aliquot of ammonia sample solution as mentioned above. Add 2 ml of TOMA+-cyclohexane solution and shake for 1.52 min. After centrifuging, measure the absorbance of the organic phase at 630 nm. Calibration curve is linear over the range 01μl NH3 in 20 ml of indophenol solution (the apparent molar absorptivity is 2.3×104 1 mol-1 cm-1) and the relative standard deviation is 3.8% for the concentration of 0.2μl NH3 in 20 ml of indophenol solution. This represents a 10 fold concentration for indophenol solution. Ammonia above 0.6 ppb for 360l of air sampling volume could be determined by this method.View full abstractDownload PDF (534K) -
Tatsuya KITADE, Keisuke KITAMURA, Keiichiro HOZUMI1989 Volume 38 Issue 1 Pages 10-15
Published: January 05, 1989
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe ammonia electrode accurately develops a Nernstian potential relative to ammonia concentration in aqueous solution. However, it is susceptible to interference by various coexisting volatile amines. In order to overcome this disadvantage, an attempt was made to prepare a new separation medium composed of a porous polymer membrane on which a thin polymer layer was deposited by plasma polymerization technique. A typical hydrophobic plasma polymer made from tetrafluoroethylene and a hydrophilic one from propargyl alcohol were coated as mono or double layers on different types of porous polymer films. The result showed that Nuclepore membrane having a pore size of 150 Å was superior to other membranes tested in reducing the interfering effect of alkyl amine when the membrane was coated by the plasma-polymerized tetrafluoroethylene. Since quick response requires a thinner layer of the plasma-polymerized tetrafluoroethylene, the Nuclepore membrane was first coated with relatively gas permeable plasma-polymerized propargyl alcohol that closed the micropores of the membrane, and then was successively plasma-coated by tetrafluoroethylene for a thickness of 150 Å. The membrane thus prepared was further sandwiched by two sheets of Fluoropore-010 membranes for mechanical protection. The electrode mounted with the multilayer membrane effectively eliminated the interference by various volatile organic amines.View full abstractDownload PDF (930K) -
Yozo KABASAWA, Hiroyuki NAKAZAWA, Masatoshi YAMAMOTO, Takenori TANIMUR ...1989 Volume 38 Issue 1 Pages 16-20
Published: January 05, 1989
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe purification of barbaloin(BA) from aloin was examined by counter alternative current chromatography (CACC), which uses the different partition between two immiscible liquids for chromatographic purification of various substances. It is most distinctive feature of CACC that send alternately upper phase and lower phase as mobile phase to the column. Consequentry, separation is progressed by going and returning of solutes in the column. The commercially reagent grade Aloin has more than ten spots on silicagel TLC plate and contains ca. 17% of BA as biologically active compounds. The effect of the numbers for switchover of mobile phase and the amount of sample on separation of BA and iso-barbaloin(IB), and on purification of BA were investigated. The phase system used for purification is composed of chloroform : mathanol : 1-propanol : water (9 : 12 : 1 : 8). The separation of BA and IB was made by three time switchovers of mobile phase, and pure BA could be separated from aloin by twenty-five switchovers. The present method is applicable with the high efficiency to the preparative purification of natural products, particularly polar compounds, using the liquid two phase system.View full abstractDownload PDF (745K) -
Toru NOZAKI, Hiroshi YAMASHITA, Ryoji MISE, Katsushi KANDA, Hiroyuki T ...1989 Volume 38 Issue 1 Pages 21-24
Published: January 05, 1989
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIon flotation of Cu(II), Hg(II), Ag(I), Zn(II) and Cd(II) in sodium thiosulfate solutions with cetylpyridinium chloride (CPC) was investigated. A 20 ml aliquot of (0.15.0)×10-2M sodium thiosulfate solution (pH 4.15.5) containing (3.854.22)×10-4M of an abovementioned metal ion and (1.673.34)×10-3M of CPC. was subjected to flotation in a 2.7 cm i.d.×20 cm cell for about 10 min with nitrogen bubbles. The metals were floated from the respective metal solutions in 96100% yield. Separation of Cu(II) from Co(II) and Ni(II) were achieved fairly well in 1.0×10-2M thiosulfate solutions with 2.5×10-3M CPC. The analysis of the relations between the mean number of the ligand S2O32- per each metal and the concentration of thiosulfate by means of the molar ratio method suggested the existence of species such as M(S2O3)22-, M(S2O3)34- and M(S2O3)46- for Cu(II) and Hg(II), MS2O3-, M(S2O3)23- and M(S2O3)25- for Ag(I) in (0.16.0) ×10-2 M thiosulfate solutions (pH 5.5). This flotation method was successfully applied during pretreatment to the determination of Ag(I) and Cd(II) in a photo-processing waste solution by using 100 ml of the solution diluted 12.5 times, and of Zn(II) in the guaranteed reagent of magnesium nitrate by using 500 ml of the solution containing 5 g of the sample, and 4.0×10-3 M of thiosulfate in a cell (6.6 cm i.d. ×40 cm), respectively.View full abstractDownload PDF (645K) -
Shigehiko YAMAGUCHI, Jiro HIRANO, Yoshihiro ISODA1989 Volume 38 Issue 1 Pages 25-28
Published: January 05, 1989
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method for the compositional analysis of acrylic acid (AA)-ethyl acrylate (EA)-ethyl methacrylate (EMA) terpolymers by pyrolysis gas chromatography (PyGC) is described. Twelve samples, in which the contents of the AA unit are less than 20 mol %, are used for the experiments. Pyrolysis is performed at 590°C using a Curie point pyrolyzer. The EA/EMA ratio of samples can be determined by the previously proposed method {this journal, 33, 153 (1984)}. But when the AA monomer peak can not be detected clearly in the pyrogram, then another method not using the AA monomer peak is required for the compositional analysis. The EA/EMA ratios and EA monomer/dimer ratios in the pyrogram vary with the contents of monomer units, P1 (AA), P1(EA) and P1(EMA) in the samples, respectively. Thus the value of P1 (AA), P1 (EA) and P1(EMA) can be obtained by multiple regression analysis from the EA/EMA ratios and EA monomer/dimer ratios in the pyrogram. By the application of this proposed method, the composition of the AA-EA-EMA terporymers can be determined easily.View full abstractDownload PDF (547K) -
Tsuyoshi NOMURA, Genkichi NAKAGAWA1989 Volume 38 Issue 1 Pages 29-33
Published: January 05, 1989
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn alkali-free magnesium phosphate glass membrane containing silver oxide can be applied to the sensor for ammonia liberated from the enzyme reaction with L-aminoacid oxidase. This membrane responded to the large majority of monovalent anions and ammonia but not to acetate and hydroxide ions. The procedure for the immobilization of enzyme was accomplished by covalent bonding on the nylon net with L-aminoacid oxidase-bovine serum albumin-glutaraldehyde system. The probe was carefully made by overlapping the immobilized enzyme membrane on the glass sensing membrane. The potential response of the probe for some L-aminoacids shows a linear relationship between 10-2 and 5×10-4 M at a pH of about 910 at 40°C. It can be used repeatedly for about a hundred runs, and is stable for at least two months. The determination of various L-aminoacids, such as L-cysteine, L-arginine, L-lysine and L-histidine, was established as follows: 10 ml each of 0.05 M K2SO4 and 0.01 M KOH in a 100 ml beaker with suitable amounts of L-aminoacid sample added were diluted to 100 ml, and then heated at 40°C. When the probe was immersed in the solution, a stable equilibrium potential was attained after about one minute. The relative standard deviation for five determinations of 10-4 M L-histidine was within 3 %.View full abstractDownload PDF (779K) -
Toshiaki SATO, Tsuneo OKUYAMA, Tetsurou OGAWA, Masatomi EBIHARA1989 Volume 38 Issue 1 Pages 34-39
Published: January 05, 1989
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAs the packing material for HPLC, ceramic fluoroapatite beads were prepared from the micro crystalline through heat sintering procedure. Fluoroapatite has been known to be mechanically stronger and chemically more stable than hydroxyapatite, but chromatographic properties have not been known. In the present paper, basic properties of ceramic fluoroapatite beads are described. The beads appeared to be spherical and porous, and the distribution of particle size was in the normal distribution with logarithmic scale. The stability of the fluoride moiety of the fluoroapatite in chromatography was tested by X-ray analysis and IR-spectroscopy. The fluoride was stable in fairly acidic codition, and could be used for the chromatography of acidic proteins. The elution behavior of proteins on ceramic fluoroapatite column seemed to be very similar with ceramic hydroxyapatite beads column.View full abstractDownload PDF (2978K) -
Yoko YOKOUCHI, Yoshinari AMBE1989 Volume 38 Issue 1 Pages 40-45
Published: January 05, 1989
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAn automated analytical system for atmospheric volatile halogenated hydrocarbons is described. Dichloromethane, CFC113, chloroform, 1, 1, 1-trichloroethane, carbon tetrachloride, trichloroethylene, tetrachloroethylene and p-dichlorobenzene were analyzed using a system based on cryogenic concentration and capillary GC (FID). The deterction limit for trichloroethylene was estimated to be 20 pg (20 ppt in 200 ml of sample air), and the precision was ±3% at the ppb level. The method has been successfully used to determine hourly variations of 1, 1, 1-trichloroethane, trichloroethylene and tetrachloroethylene in the atmosphere at the Tsukuba area over two weeks in July.View full abstractDownload PDF (708K) -
Takeshi YAMANE, Mikito KAMIJYO1989 Volume 38 Issue 1 Pages 46-48
Published: January 05, 1989
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA FIA-reaction rate method has been proposed for simple and rapid measurement of hypophosphite concentration in chemical nickel plating bath. The rate of reaction between hypophosphite and iodate in a continuous flow system was measured by monitoring the absorbance change at 460 nm due to reaction product. The sample solution taken from the plating bath was diluted 5 times with distilled water and a 70 μl portion was injected into the carrier stream in the flow system. The system is suitable for measuring hypophosphite ranging 1.9 × 10-2 5.7 × 10-2 M in the final diluted solution with the sample throughput of ca. 15 per hour. The relative standard deviation was 2.1% (n=5) for 4.7 × 10-2 M hypophosphite. No separation of the major constituent, nickel and other usual additives in the plating bath was needed.View full abstractDownload PDF (467K) -
Norishige YAMAGUCHI, Taeko NISHIDA, Hiroshi NISHIDA1989 Volume 38 Issue 1 Pages 48-51
Published: January 05, 1989
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSBeryllium formed a red complex (absorption maximum : 530 nm) with Eriochrome Cyanine R (ECR) in the presence of hexadecylpyridinium chloride(HP) at pH 10, and the developed complex was applied to the spectrophotometric determination of beryllium. The optimum conditions for the determination of beryllium were as follows: [Be(II)] = (0.041.6) × 10-5 mol dm-3, [ECR] = 2.4 × 10-4 mol dm-3, [HP] = 1.4 × 10-3 mol dm-3, [EDTA] = 4 × 10-3 mol dm-3, pH = 10. The apparent molar absorptivity was 5.36 × 104 dm3 mol-1 cm-1. The sensitivity of the method was nearly equal to that of the Zephiramine-Chromazurol S method at pH 10. Less than 10 mg of Mg(II), Ca(II), 5 mg of Mn(II), Cd(II), Zn(II), As(V), 1 mg of Al(III), 0.5 mg of Fe(III), 0.8 g of chloride, 1 g of sulfate and 0.02 g of fluoride did not interfere. The anion effect in this method was smaller than that in the Zephiramine-Chromazurol S method at pH 10. This was because the absorbance at 530 nm of HP-ECR solution at pH 10 was not influenced by the anions within the range of concentrations described above. Therefore the difference in anion concentration between the sample and the reagent blank did not affect the absorbance of the complex. After separation by acetylacetone-benzene extraction, 1.6 ppb of beryllium in hot spring water was determined by the standard addition method (the relative standard deviation : ± 5%).View full abstractDownload PDF (689K) -
Junko YOSHITOMI, Hitoshi NAGANUMA, Hiroshi OGURO1989 Volume 38 Issue 1 Pages T1-T4
Published: January 05, 1989
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSXRF analysis using the fundamental parameter (FP) method was studied on a composite oxide material comprised of barium, zinc and tantalum oxides (BZT). In preparing the glass beads, lithium borate as the flux and potassium bromide as the releasing agent were found most suitable agents. No particular segregation of the elements was observed in the glass beads with the dilution ratio (sample : flux) ranging from 1 : 2 to 1 : 10. By using these glass beads, the calibration curves were derived based on both the calibration and FP methods. A better linearity with less beviations was obtained for FP method. The accuracy of the calibration curves obtained by the calibration method and the FP method were compared by using the glass beads having the dilution ratios of 1:2 and 1 : 10, and it was found that higher accuracy was obtained by FP method for both dilution ratios. Furthermore, the accuracy for the glass bead of dilution ratio of 1 : 2 was found higher than that of 1 : 10 ratio. This proposed method showed good repeatability and reproducibility, and the relative standard deviations for each component were less than 0.05%.View full abstractDownload PDF (489K) -
Eiichi ISHIKURO1989 Volume 38 Issue 1 Pages T5-T8
Published: January 05, 1989
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method for the determination of sulfaquinoxaline (SQ) in feed by HPLC has been developed. The ion pair chromatography method was suitable for the separarion of SQ from the ingredients. SQ was extracted from feed with 100 ml of dimethylformamide (DMF) and the extract was placed in a boiling water bath, with intermittent stirring, for 30 min. The supernatant was applied to an alumina column (E. Merck 1076, 10 g), then washed with ether, chloroform-methanol (3+1) and eluted with methanol. The effluent was injected onto a HPLC column. The recovery of SQ added to feeds at 60 μg/g of feed was 97.3%, and the detection limit was 0.5 μg/g. The recovery of SQ from feeds, as reported by 6 collaborators, was 101.9%, with a relative standard deviation of 4.1%. The proposed method can be applied to the determination of SQ in pellet feed and is recommended as an official method of feed analysis in Japan.View full abstractDownload PDF (563K) -
Katsushige TAKAMI, Kunio ODA1989 Volume 38 Issue 1 Pages T9-T14
Published: January 05, 1989
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe effects of nitrification on 5-day BOD, the DO measurement done by the membrane electrode (ME) method, and the azide modification of the iodometric (W) method were evaluated by the results of the round robin tests. The domestic wastewater and their effluent from activated sludge treatment were used as samples for the round robin tests and distributed to 23 laboratories. Five day-BOD test was performed by the JIS method and allylthio urea (ATU) was used as a nitrification inhibitor. The results were compared statistically using mean values, relative standard deviation and accuracy. For the domestic wastewater, on which nitrification had little effect, a satisfactory result was obtained with 13.1% (n=23) relative standard deviation (R.S.D.). However, the BOD data from the effluent, wherein nitrification was confirmed to take effect, were highly dispersed with 27.637.5% (n= 21) R.S.D., and the results of BOD were correlated to the dilution factor used by the laboratories with 0.7500.853 (n=21) correlation coefficient. These results suggested that the reproducibility of BOD test depended upon nitrification in samples and differences on the series of dilution used. The results of DO and BOD determined by W method were in good agreement with that obtained by ME method, but the similarity decreased by the addition of ATU in the diluted samples to inhibit nitrification. It is most likely that the determination of DO with W method was interfered by ATU added into the diluted samples.View full abstractDownload PDF (1100K)
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