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Volume 35, Issue 4
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Takeshi MURATA1986 Volume 35 Issue 4 Pages 339-343
Published: April 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe principle of the jet separators used in gas chromatography mass spectrometry (GC/MS) combined system requires that helium should be used as a carrier gas because it has a small mass number. With helium as a carrier gas, a GC/MS system ensures its highest performance, but helium has the drawbacks that it is costly and hardly available in some countries. A series of investigations has been carried out to see if nitrogen can be used as a substitute for helium. Though the higher molecular weight(large molecular radius) of nitrogen than that of helium caused some problems, practically satisfactory results could be obtained if suitable operational parameters were selected. The GC was directly connected to the MS by using a fused silica capillary column. The system was equipped with an EI/CI dual ion source of a differential evacuation type. The electron impact energy was a set to 200 eV so that detecting sensitivity might not lower even if nitrogen was used as the carrier gas. The sample was a methyl caprate solution, which was introduced via the SPL-G9 splitless sample injector. The column inlet pressure, measured with the pressure gauge of the SPL-G9, was raised from 0.5 kg/cm2 to 2.3 kg/cm2 in step, and the pressure of ion source and the total ion intensities in these steps were investigated. When helium was used, pressure of ion source was found to change from 0.5 × 10-5 Torr to 2.5 × 10-5 Torr, while in the case of nitrogen, it changed from 6 × 10-5 Torr to 14 × 10-5 Torr. This low vacuum resulting in a low sensitivity could be enhanced, however, by 34 times by raising electron impact energy from 70 eV to 200 eV. In short, the sensitivity for nitrogen carrier gas could be raised to 1/34/4 times than ensured for helium carrier gas, by a suitable selection of MS parameters. When nitrogen was used as the carrier gas, a high flow rate could not be allowed ; otherwise it would result in longer retention time, low resolution, and/or asymmetry of peaks. Putting these data together, the GC/MS with nitrogen carrier gas provided a sensitivity 1/71/10 lower than ensured for helium carrier gas.This sensitivity is satisfactory enough except when minor components are to be determined.View full abstractDownload PDF (783K) -
Kyoji TÔEI, Shoji MOTOMIZU, Mitsuko OSHIMA, Minoru ONODA1986 Volume 35 Issue 4 Pages 344-348
Published: April 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSpectrophotometric determination of boron existing as boric acid in water was examined with H-resorcinol {1-(2, 4-dihydroxy-1-phenylazo)-8-hydroxynaphthalene-3, 6-disulfonic acid} by flow injection analysis. Carrier solution (deionized water) and reagent solution were propelled by double plunger pump (flow rate : 0.6 ml/min), and sample solution (320 μl) was injected into a carrier stream. The reagent solution was prepared by dissolving 0.096 g of H-resorcinol in 1 1 of ammonium acetate buffer solution (50 g/l, pH 5.5) containing 3.72 g of EDTA. The two streams were mixed in 16 m long Teflon tubing (0.5 mm i.d.), and the mixture was flowed through a flow cell (36 μl; 1.5 mm i.d. × 20 mm), at which the absorbance of boron-H-resorcinol complex was detected (λ=510 nm). The linear relationship between the peak height and concentration of boron was obtained in the range of 0 to 1 ppm. The detection limit was 5 ppb (S/N=2). The sampling rate was 30 samples per hour. Generally ions co-existing in river and sea waters did not interfere with the determination of boron by adding EDTA solution.View full abstractDownload PDF (706K) -
Hiroki OHURA, Toshihiko IMATO, Sumio YAMASAKI, Nobuhiko ISHIBASHI1986 Volume 35 Issue 4 Pages 349-355
Published: April 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA rapid and highly sensitive method for the determination of bromate ion has been developed by applying to potentiometric detection of the flow injection technique (FIA). The method was based on the transient change of the potential in the redox-reaction of bromate ion with the iron(III)-iron(II) potential buffer solution containing bromide ion and sulfuric acid. The sample solution (140 mm3) injected into a carrier water stream is, at a confluence point, merged with the stream of the buffer solution containing sulfuric acid (1.2 mol dm-3), sodium bromide (0.4 mol dm-3) and the iron(III)-iron (II) (0.01 mol dm-3). The reaction takes place during flowing of the sample zone through the reaction tube to the flow-through type ORP electrode detector. The potential change is observed as a peak-shaped signal. A linear relationship between the peak height and concentration of bromate ion was observed in the range of 1 × 10-6 to 5 × 10-6 mol dm-3. At the sampling rate of ca. 40 samples per hour, the relative standard deviation was 0.98% (n=9) for the determination of 3 × 10-6 mol dm-3 bromate ion. Chloride, sulfate, nitrate and phosphate ions in 1000 times excess to bromate did not interfere with the determination of bromate ion.View full abstractDownload PDF (1306K) -
Kiyoshi SAITO, Shoji ICHIDA1986 Volume 35 Issue 4 Pages 356-360
Published: April 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe improved Liebig method developed by the authors is as follows : a sample is pyrolyzed under passing helium and the evolved volatile matter is oxidized by heated copper dioxide. Then the residues of the sample are burned and the reduced copper is oxidized by passing oxygen. Thus the increase in weights of magnesium perchlorate and caustic soda as absorber for water and carbon dioxide are measured. In this method, the passing of dried oxygen to the absorber after combustion procedure was necessary to get a constant weight. But if the oxygen contained minute amounts of moisture, magnesium perchlorate and caustic soda were activated, making it difficult to get a constant weight. The activation also occurred from the vapor of phosphoric acid. The procedure for the sequential analysis of moisture, carbon and hydrogen in low rank coal and the analysis of volatile liquid fuel were established. The relative standard deviation was 0.2% for carbon. The time required for each analysis was 20 min.View full abstractDownload PDF (919K) -
Kitao FUJIWARA, Toshiki MORIKAWA, Keiichiro FUWA1986 Volume 35 Issue 4 Pages 361-367
Published: April 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSCoprecipitation with metal chelate complex formation has been studied for determining molybdenum and vanadium in seawater. As coprecipitation carriers, several pairs of metal ion and chelating agent were applied : Co(II)-ammonium pyrrolydinedithiocarbamate (APDC), Cu(II)-APDC, Cr (VI)-APDC, Co (II) -sodium diethyldithiocarbamate, AI ( I I I) -8-quinolinol, Cu(II)-cupferron, and Ni(II)-dimethylglyoxime. The procedure was as follows : A 100 ml molybdate {Mo(VI)} and metavanadate {V(V)} sample solution was taken to which were added acetate buffer solution. After addition of the carrier metal ion, the pH of the solution was adjusted and the chelating agent was then added. After stood for 1 h, the precipitate was collected by a membrane filter(pore size 0.2μm), and dissolved in 5 ml of nitric acid(1 mol/1). It was then analyzed by graphite furnace atomic absorption spectrometer. The coprecipitation done with Co (II) APDC surpassed the others in recoveries of molybdenum and vanadium ; which were 94±3 and 96±3%, respectively. The minimum detectable amounts in the initial solution were found to be 0.05μg/l for molybdenum and 0.1μg/l for vanadium. Molybdenum and vanadium were determined in seawater sampled at the Japan Trench in the North Pacific Ocean.View full abstractDownload PDF (1054K) -
Hiroshi NISHIDA1986 Volume 35 Issue 4 Pages 368-372
Published: April 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn the spectrophotometric determination of beryllium with Chromazurol S (CAS, H4L) in the presence of cationic surfactant at pH 10.2, an increase in CAS concentration was required along with an increase in cationic surfactant concentration in order to obtain maximam and stable absorbance. From these results, the apparent equilibrium constant at pH 10.2 (Kapp) of the 1: 2 beryllium-CAS complex formation was investigated by varying the concentrations of cationic surfactant. The Kapp value decreased with an increase in cationic surfactant concentration. It was considered that possibly this was due to the effect of micellar volume on the partition of CAS between the water phase and the micellar pseudo phase. Partition ratio (DL) of CAS (HL3-) and the complex formation constant at pH 10.2 (k) could be determined from the Kapp value in the various concentrations of cationic surfactant. The DL value increased in the order of hexadecyltrimethylammonium chloride(HT)>hexadecyldimethyl-benzylammonium chloride(HD)>tetradecyldimethyl-benzylammonium chloride (TD)>hexadecylpyridinium chloride(HP)>dodecyltrimethylammonium chloride (DT)>dodecylpyridinium chloride (DP), according to the sum of carbon number of long chain alkyl and methyl radicals in the cationic surfactant. The k value decreased in the order of HP_??_DP>TD_??_HD>DT_??_HT, according to the number of methyl radical in the cationic surfactant. Molar absorptivity of the complex had the maximum value in the presence of HD and/or TD, and was 5.86×104 dm3 mol-1 cm-1 at 525 nm.View full abstractDownload PDF (845K) -
Mikita ISHII, Masaaki YAMADA, Shigetaka SUZUKI1986 Volume 35 Issue 4 Pages 373-378
Published: April 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSMicellar enhanced chemiluminescence(CL) is used to determine copper(II) at sub-picogram level by using the 1, 10-phenanthroline-hydrogen peroxidesodium hydroxide-hexadecylethyldimethylammonium bromide micelle system. The CL mechanism is based on the following chemical reactions; the superoxide radical anion which is produced through the catalytic decomposition of hydrogen peroxide by the copper (II)-1, 10-phenanthroline complex, reacts with 1, 10-phenanthroline to form the excited 3, 3'-diformyl-2, 2'-dipyridyl via a 1, 2-dioxetane derivative intermediate. The system is composed of three flow lines, in which optimum conditions are specified. This method permits the determination of copper(II) much more selectively than any other CL methods with a limit of determination of 8.0×10-14g(20μlsample injection) or 1.6×10-13 M(continuous sample flow at the sample feed speed 5.0 ml/min). The linear dynamic range is 4 orders of magnitude, the sampling rate is 180/h, and the reproducibility is less than 1.7% in terms of coefficient of variation for 5×10-13 g copper(II) injection (n=10). Lead(II), the strongest enhancer after copper(II), provides signal 0.03% of that for copper (II). The method is successfully applied to the determination of copper(II) in the tap water.View full abstractDownload PDF (1070K) -
Application to rabbit lensMikita ISHII, Masaaki YAMADA, Shigetaka SUZUKI1986 Volume 35 Issue 4 Pages 379-383
Published: April 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe micellar enhanced chemiluminescence of 1, 10-phenanthroline-flow injection method was applied to determine trace amounts of copper(II) in rabbit lens; the distribution of copper(II) in the lens was first reported. The lens was dissolved with conc. HCl by heating, and the sample volume was adjusted to 2.5 ml by adding distilled and deionized water. The copper (II) contents in the lenses were measured through the standard addition method and the calibration curve method. The values agreed well between both methods; the average content was 3.3 μg per 1 g of the lens. It was first confirmed by the proposed method that copper(II) distributed homogeneously in the lens. The measurement can be performed with only 4μg of the lens in 2.5 ml sample solution. The limits of determination and detection for copper(II) in the lens, were 0.11 and 0.012 pg (20μl injection), respectively. The linear dynamic range for the copper(II) was about 104. The selectivity was very high; lead(II) and zinc (II), the strongest enhancers after copper(II), provided signals 0.01% of that for copper(II). Analysis time required was very short; less than 10s. The relative standard deviation was less than 1.9% for 10 repeated tests by 6.5×10-10 M copper(II) injection. For the cross-check between atomic absorption spectrophotometry and the present method, the correlation coefficient 0.94 (n=8) was obtained.View full abstractDownload PDF (820K) -
Ayako NAKAJIMA, Taro USHIJIMA, Junji MIGITA1986 Volume 35 Issue 4 Pages 384-388
Published: April 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA rapid and sensitive method for the determination of 3, 5-dimethyl-4, 6-diphenyl-tetrahydro-2H-1, 3, 5-thiadiazin-2-thion (NIP-200) in rat peripheral serum was developed by using high performance liquid chromatography, with post column derivatization with NaCIO and o-phthal aldehyde (OPA) followed by detection with fluorometer. The NIP-200 was separated by the reversed phase on Zorbax ODS(5μm4.6 mmφ×150mm). In the first reaction coil, NIP-200 was decomposed to methylamine, then, in the second reaction coil, the methylamine was made to react with OPA. The OPA derivative was detected fluorometrically(Ex 335 nm/Em 450 nm). The optimum concentration of OPA was in the range from 0.01% to 0.02%. A sample of 0.5 ml of rat serum was transferred to a 10 ml conical centrifuge tube. Then 5 ml of chloroform was added and the two phases were mixed thoroughly. The mixed solution added 1 ml of water was mixed softly, and centrifuged at 3000 rpm for 10 min. After 4 ml of the organic phase transferred was evaporated at 40°C, 50 μl of methanol was added, and 10μl of the final solution was injected into a chromatograph. The determination was made by measurement of the peak height of the NIP-200 derivative. The practical lower limit of the determination was 2.5 ng/ml serum (S/N=3).The relative standard deviations for 2.5 ng/ml and 5.0 ng/ml NIP-200 were6.97% and 5.02%, respectively. The calibration curve was linear in the range from 0.2 ng to 10 ng of NIP-200.View full abstractDownload PDF (721K) -
Hiroyuki KATAOKA, Kazuyuki OHISHI, Noriko INOUE, Masami MAKITA1986 Volume 35 Issue 4 Pages 389-393
Published: April 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method for the determination of cysteic acid in animal tissues by gas chromatography is described. After extraction of tissue sample with dilute sulfuric acid containing sodium tungstate, cysteic acid in the tissue extract was converted into its stable volatile derivative, methyl β-dibutylsulfamoyl-α-(isobutyloxy-carbonylamino)propionate by the procedure reported previously {J. Chromatogr., 354, 482 (1986)} prior to gas chromatography. In the derivatization process, the interfering substances such as cysteinesulfinic acid could be conveniently removed as their N-isoBOC derivatives by the extraction with isopropanol-diethylether (1 : 9). Separation and determination of the cysteic acid derivative was performed on a 1.0% 0V-17+0.2% FFAP column (1.5m×3mm i.d.). Recoveries of cysteic acid added to several tissue extracts were above 93% and relative standard deviations were below 5%. Taurine could be simultaneously determined by this method. Analytical results of tissues of four different animals are presented.View full abstractDownload PDF (811K) -
Hiroaki TSUCHIAI, Tsugikatsu ODASHIMA, Hajime ISHII1986 Volume 35 Issue 4 Pages 394-399
Published: April 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSquare-wave anodic stripping voltammetry with a mercury thin-film electrode (MTFE) was investigated for the determination of traces of cadmium in high concentrations of zinc. When cadmium is electrodeposited on the MTFE at -1.0 V vs. SCE in 0.5 M ammonia-ammonium chloride buffer solution (pH 9) and then stripped in the same solution by scanning the potential in the positive direction at the rate of 30 mV/s, the sharp stripping peak appears at -0.78 V vs. SCE, even in high concentrations of zinc. On this basis, a simple, sensitive and selective method for the determination of traces of cadmium in zinc was proposed. The stripping peak current of cadmium was proportional to the concentration in the range of 9 × 10199 × 10-8 M and also to the deposition time between 5 and 30 min. The relative standard deviation for 11 runs at 5.8 × 10-8 M Cd(II) was 4.3%. The proposed method was successfully applied to the determination of cadmium in zinc and its salts of guaranteedreagent grade.View full abstractDownload PDF (901K) -
Masaru KIMURA, Hiromi YAMASHITA, Junko KOMADA1986 Volume 35 Issue 4 Pages 400-405
Published: April 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method was described to collect the several metal ions in water with the Japanese green tea (powder tea). The tea powder was treated with formalin in a dilute sulfuric acid. A 100 ml solution containing Ag+, Cd2+, Co2+, Cu2+, Fe3+, Mn2+, Ni2+, Pb2+ and Zn2+ was mixed with 0.5 g of the tea under stirring for 30 min. The solution was then centrifuged or filtered through and the concentrations of metal ions in the filtrate were determined with a flameless atomic absorption spec trometer. The 8 metals but Fe3+ (0.4 11 ppm in total concentrations) are collected over 90% from the solution of 0.01 mol dm-3 sodium acetate at pH 6. The tea can be reused over several times as the ad sorbent, after the metals are washed away with 0.1 mol dm-3 HCl. Addition of 8-quinolinol or 1, 10-phenanthroline leads to the collection over 90% for all the ions including Fe3+. The effect of ethylenediaminetetraacetate, trans-1, 2-cyclohexanediaminetetraacetate, chloride, sulfate, oxalate, and L-ascorbate anions on the collection efficiency is also examined. Metal adsorbabilities are compared as well between green tea and activated carbon.View full abstractDownload PDF (1180K) -
Motonori ETO1986 Volume 35 Issue 4 Pages 406-408
Published: April 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDetermination of palladium in the presence of chloride ion was studied by the potentiometric titration method. A gold-plated platinum electrode was used as the indicator electrode. The recommended procedure is as follows : Place the sample solution into a 200 ml beaker. Evaporate it to dryness on a water bath. Add 1 ml of hydrochloric acid (1+4) and water, and then dissolve it on a water bath. After cooling, dilute it to about 150 ml with water and titrate it with 0.02 M potassium iodide solution. This method was applied. to the determination of palladium in the sodium tetrachloropalladate solution and the palladium carbon as catalyst. The results are in good agreement with the values obtained by the gravimetric method using potassium iodide, and the relative standard deviation is less than 0.5%.View full abstractDownload PDF (562K) -
Itsuo MORI, Yoshikazu FUJITA, Kinuko FUJITA, Hiroshi KAWABE, YOZO KOSH ...1986 Volume 35 Issue 4 Pages 408-410
Published: April 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSImproved spectrophotometric method for determination of gallium with Zincon in the presence of Tween 20(polyoxyethylene sorbitanmonolaurate, LT-20), as a nonionic surfactant, in a weakly acidic solution has been proposed. The absorption maximum of the Zincon-gallium complex in the presence of 0.2% Tween 20 is at 640 nm against water. The absorbances of the gallium complex and Zincon are stable and constant in the pH range of 3.4 to 4.1. The Beer's law is obeyed up to 35 μg of gallium in final volume of 10 ml at 640 nm. The apparent molar absorptivity is 2.44 × 104 dm3 mol-1 cm-1 with Sandell sensitivity of 0.0029 μg/cm2. The relative standard deviation is 1.1 % for 17.5 μg of gallium(n=6). Aluminum, zinc, calcium, thiosulfate ions did not interfere. The molar ratio of Zincon to gallium is estimated to be 1.5 : 1 in the presence of Tween 20 by continuous variation, mole ratio, and equilibrium concentration methods.View full abstractDownload PDF (511K) -
I. Application to stopped-flow spectrophotometric determination of glucoseJun-ichi TOEI, Nobuyuki BABA1986 Volume 35 Issue 4 Pages 411-413
Published: April 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA new type valve for a stopped-flow flow injection analysis (FIA) was developed. The valve has two characteristic functions. The first is that a sample solution is injected in a “plug flow” into a flow of eluant, and the second is passage change-over of the eluant flow.At the load position, the eluant is recycled from tank to tank and the sample loop is filled with sample solution when the flow in reaction tubing is stopped. At the injection position a sample solution is injected into the flow of the eluant and is sent into reaction tubing. By rotating the valve from a injection position to a load position the reaction flow is stopped in a reaction tubing and the reaction will proceed. Stopped-flow FIA using the new type valve was one of the useful method for determination of glucose.View full abstractDownload PDF (513K) -
Kenjiro HAYASHI, Yoshiaki SASAKI, Shoji TAGASHIRA, Nobuyuki MITO1986 Volume 35 Issue 4 Pages 413-415
Published: April 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSSodium salts of octyl- (OCX), decyl- (DEX), dodecyl- (DOX) and hexadecyl-xanthate (HDX) were newly synthesized from higher alcohols, metallic sodium and carbon disulfide in hexane. Both DOX and DEX form the micelles above the critical micellar concentrations. The colored complexes of some metal ions with these reagents were soluble in aqueous solutions. Nickel(II) and cobalt(II) were spectrophotometrically determined as metal-DOX complexes. In the presence of 5.0 × 10-4 mol dm-3 DOX at pH 7.0, Beer's low holds between concentrations 2.3 × 10-6 and 9.7 × 10-5 mol dm-3for nickel(II), or 2.5 × 10-6 and 1.0 × 10-4 mol dm-3 for cobalt(II). The apparent molar absorptivities for nickel(II) and cobalt (II) complexes were 4.39 × 103 dm3 mol-1 cm-1 at 509 nm and 1.48 × 104 dm3 mol-1 cm-1354 nm, respectively.View full abstractDownload PDF (564K) -
Kazufusa SHINOMIYA, Hiroyuki OCHIAI, Hiromasa SUZUKI, Ichiro KOSHIISHI ...1986 Volume 35 Issue 4 Pages T29-T32
Published: April 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple method was developed for the determination of total rnucopolysaccharides (MPS) commonly found in human urine. It is based on the separation of urinary MPS with cellulose column and the determination of the carboxyl group of MPS by colorimetry. MPS were separated from human urine as follows : To 20 ml of human urine, 4 ml of aqueous 0.1% (w/v) cetylpyridiniumchloride solution was added, and the mixture was charged onto a cellulose column (8 mm I.D. × 35 mm). After washing with 20 ml of distilled water and 30 ml of ethanol saturated with sodium chloride, urinary MPS were eluated with 9 ml of distilled water. MPS were determined by colorimetry based on the reaction of carboxyl group with o-nitro phenylhydrazine (ONPH) in the presence of 1-ethyl3- (3-dimethylaminopropyl)carbodiimide. Recovery of chondroitin-4-sulfate added to human urine by the present pretreatment was 92.5%. The determination method of MPS using a reaction with ONPH was correlated to the carbazole method.View full abstractDownload PDF (561K) -
Shinji ITOH, Koichi SATO, Kunikazu IDE, Haruno OKOCHI1986 Volume 35 Issue 4 Pages T33-T37
Published: April 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe study of the X-ray fluorescence analysis of main component and alloying elements in nickel-based heat-resisting alloys has been performed. The calibration curves were made by using NBS SRM's, JAERI and home-made nickel-based standard samples and the correction was made for the matrix effects using theoretical alpha coefficients. Accuracies (ad) for respective element obtained from those curves with correction were improved, especially for chromium and iron, in comparison with uncorrected ones. The relative standard deviation for each element was in the range of 0.251.27% with the exception of aluminum (0.26 Al%;r.s.d. 3.01%). The analytical ranges were as follows; Cr(12.7526.49%), Mo(1.09 9.18%), W(0.0194.57%), Co(0.398.90%), Ti(0.353.44%), Al(0.156.68%), Nb(0.885.38%), Fe(0.1223.2%), Mn(0.010.65%). The analytical values of nickel-based heat-resisting alloys such as Inconel 713LC, Mar-M247 and so on, showed good agreement with those determined by chemical analysis.View full abstractDownload PDF (882K)
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