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Volume 40, Issue 3
Displaying 1-13 of 13 articles from this issue
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Hiroshi UMEDA, Isamu INAMOTO, Koichi CHIBA1991 Volume 40 Issue 3 Pages 109-114
Published: March 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSIsotope dilution/inductively coupled plasma mass spectrometry (ID/ICPMS) was applied to the determination of ng g-1 levels of antimony in high purity copper. Mass discrimination effects of two main components, copper as a matrix and lanthanum for coprecipitation, on the measurement of isotope ratio(123Sb/121Sb) were not significant.It was found that there is isobaric interference of 123Te in the measurement of the isotope ratio. But this effect could be corrected by subtracting the spectral intensity of 123Te from that of m/z=123; the intensity of 123Te can be obtained by measuring the intensity of 125Te and the relative intensity of 123Te and 125Te. The analytical results for NIST SRMs obtained by ID/ICPMS agreed well with the certified values. After concentrating antimony by the coprecipitation method, ID/ICPMS can determine 4.4 ng g-1 of antimony in copper sample with 10% RSD.View full abstractDownload PDF (661K) -
Sahori TAKASUKA, Akinori KAWAHARA, Shin-ichi WAKIDA, Masataka YAMANE, ...1991 Volume 40 Issue 3 Pages 115-118
Published: March 05, 1991
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSTrace thiamine in environmental water was oxidized to fluorescent thiochrome by potassium ferricyanide in an alkaline solution (pH 13). The resulting thiochrom was enriched on a reversed-phase HPLC column (Asahipak ODP-50, 6 mm i.d.×150mm), eluted with methanol-water {1:1(v/v)}, and determined by fluorometry at 430nm (excitation wavelength 375nm). Under the optimum conditions, linear calibration curves were obtained for 010ppt and 0100ppt of thiamine when either 10ml or 20ml sample solution was used. Relative standard deviation obtained in each of 6 measurments at 10ppt and 100ppt was 3.9% and 1.4%, respectively. The detection limit of thiamine was 0.8ppt (S/N=2) and the determination period was approximately one hour. The present method was applied to the determination of dissolved thiamine in lake, pond, river and treated sewage water.View full abstractDownload PDF (419K) -
Satoshi OHRUI, Hiroyuki KATAOKA, Yoshiaki MIYAMOTO, Kimiyo OHTSUKA (ne ...1991 Volume 40 Issue 3 Pages 119-123
Published: March 05, 1991
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA selective and sensitive method for the determination of primary amines by GC is described. After benzenesulfonylation of amines by Hinsberg reaction, primary amines were completely separated from secondary amines by extraction with hexane in 50% potassium hydroxide-22.5% methanol solution. Benzenesulfonyl derivatives of primary amines in acidic aqueous layer were extracted by diethyl ether, and analyzed by GC with flame photometric detection (FPD-GC) using a DB-1 capillary column. Derivatization yield of butylamine was 96.7±4.0% (n=3). By FPD-GC, the calibration curves of amines were linear in the range of 201000 ng for the derivatives and the detection limits were about 10100pg as injection amounts, which were above 20 times more sensitive than that obtained by GC with flame ionization detection.View full abstractDownload PDF (486K) -
High performance liquid chromatographic determination of glucose using an immobilized enzyme reactorKazuo MURAKAMI, Michiko KAKEMOTO, Toshikatu HARADA, Yosehu YAMADA1991 Volume 40 Issue 3 Pages 125-129
Published: March 05, 1991
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSGlucose was determined by using a high performance liquid chromatographic system comprised of an immobilized glucose oxidase reactor followed by amperometric detection of hydrogen peroxide. Glucose oxidase immobilized on pellicular particles of silica was packed into a short stainless steel column. The immobilized enzyme reactor incorporated with a C18-bonded column. The sensitivity of this system was the same as that of chemiluminescence detection and about 5×103-fold greater than when using differential refractive index detection. The least amount of glucose detected was 2ng (S/N=3). The uses of specific enzymatic reaction and the electrochemical detector made sample pretreatments extremely simple. This system was successfully used to determine glucose in carbonated water, sake, wine and soy sauce.View full abstractDownload PDF (524K) -
Tuneaki MAEDA, Hitoshi SHINOHARA, Eigo KOBAYASHI, Toshiyuki HOBO1991 Volume 40 Issue 3 Pages 131-135
Published: March 05, 1991
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA commercially available portable dust meter was modified for use as a light scattering detector (LSD) for supercritical fluid chromatography (SFC). The sample introduction port of the meter was replaced by a specially designed interface which was connected to the supercritical fluid chromatograph. This connector consisted of a nebulizer tube of a fused silica capillary tube (i. d. 50μm) and a heater tube over the nebulizer. It was connected to a packed column (ODS, 5μm, i. d. 4.6mm×250mm) and was operated at inlet pressure of 180kg/cm2 and temperature of 50°C. The temperature of the heater tube was set at 50°C. The samples evaluated were choresterol, butter and margarine extracts. After examining the optimal conditions using cholesterol as the sample, chromatograms of the extracts were obtained together with those using UV detector. Addition of a modifier to the mobile carbon dioxide phase did not give any interference. Though the LSD has some problem with spike noise and repeatability yet, it proved to be an universal detector for SFC.View full abstractDownload PDF (399K) -
Hidenobu OHMORI, Hiroshi OHMAE, Chihiro UEDA1991 Volume 40 Issue 3 Pages 137-141
Published: March 05, 1991
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA composite plane electrode has been fabricated by compressing a micro-electrode (MiE; 25μmφ) between two macro-electrodes (MaE: area, ca. 0.08cm2×2) placed in close proximity to each other. Voltammetry of ferrocyanide ion in aqueous solution at the composite electrode indicated that the environment of the MiE can be controlled by a potential applied to the MaE. Thus, when the MaE was kept at a potential well anodic to the oxidation of Fe(II), the voltammetric current observed by sweeping the potential of the MiE from -0.20V (vs. Ag/AgCl) to anodic direction was primarily composed of the reduction of Fe(III) instead of the oxidation of Fe(II). One application of the composite electrode was the analysis of dopamine (>0.5 mM) in aqueous solution containing ascorbic acid (10mM). By keeping the potential of the MaE at an appropriate value, the ascorbic acid was selectively removed from the surface of the MiE and the dopamine was determined at the latter electrode by differential pulse voltammetry.View full abstractDownload PDF (652K) -
Hiromu IMAI, Zenichi ARAI1991 Volume 40 Issue 3 Pages 143-147
Published: March 05, 1991
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe determination of malondialdehyde (MDA) which is an end product of the hydrolysis of 1, 1, 3, 3-tetramethoxypropane (TMP) was investigated spectrophotometrically. TMP in aqueous solution, adjusted pH to 1, was completely hydrolyzed, after 5h at 25°C. The rate constant of hydrolysis was 2.78×10-4s-1. The determination of MDA is carried out as follows: take 1ml of a sample solution, which contain less than 6.5×10-6M of MDA, add 12ml of a solution, which has 6.9×10-2M thiobarbituric acid dissolved in 5×10-2M sodium hydroxide; after adjusting pH to 1 with hydrochloric acid, dilute this solution with water to a 15ml; put the sample in boiling water for 15min and after cooling for 2h at room temperature, read the absorbance value. The calibration curve was prepared from MDA obtained by the hydrolysis of TMP. The linear relationship between the concentration of MDA and the absorbance was in the range of 0.5×10-6M to 6.5×10-6M. The molar extinction coefficient was 1.4×105l mol-1cm-1 at the wavelength of 532nm. This procedure can be applied to the determination of hydroxy radical.View full abstractDownload PDF (455K) -
Michie KOYAMA, Syokichi CHAKI, Manabu YAMAMOTO, Takahiro KUMAMARU1991 Volume 40 Issue 3 Pages 149-152
Published: March 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSCollecting conditions using various absorbing solutions were investigated for the determination of arsine in the working environment of semiconductor plants. Recommended procedure is as follows: the sample gas is collected by passing the gas through an impinger containing 20cm3 of 2.0w/v% potassium permanganate-0.6v/v% sulfuric acid solution at the flow rate of 1000cm3 min-1 for 30min. The impinger comprises a bent-type gas dispersion tube sintered with a porous glass plate (20mm diameter, pore size 40100μm). Following the sampling, 10cm3 of 2.5w/v% hydrogcn peroxide-0.6v/v% sulfuric acid solution is added to the absorbing solution in order to prevent the precipitation of manganese dioxide or to dissolve the precipitate already formed. Arsenic in the solution is then determined by flow injection/hydride generation-atomic absorption spectrometry according to the literature. The collection efficiency for arsine with 10 replicate determinations was 95±1% at the level of 31μgm-3. Arsine in the working environment inthe range of 8.7420 μgm-3 can be determined with 30 dm3 of the sample gas using this procedure.View full abstractDownload PDF (575K) -
Shizuko HIRATA, Kazuo MIYAZI, Takahiro KUMAMARU1991 Volume 40 Issue 3 Pages T47-T51
Published: March 05, 1991
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSICP-AES of biological standard reference materials was investigated. Direct graphite cup insertion technique with microliter volume of the samples was used. The sample solution (20μl) was inserted into a graphite cup, which was placed into a modified plasma torch in the dry-ashing position. After dry-ashing for 20s, the graphite cup was transferred to the atomizing position, which was 2mm above the load coil. Emission signals of Cu at the wavelength of 324.754nm readings were taken every 20ms. Detection limits and precision of this method were 0.87ng ml-1 (3σ) and 2.9% (n=10) for 10ng ml-1 of Cu standard solution, respectively. Analytical results for Cu in the biological standard reference materials (NIES No.1, No.6 and NBS SRM 1571) with standard addition methods were in good agreement with the certified values for these materials.View full abstractDownload PDF (500K) -
Junichi MATSUSHITA, Yutaka TSUCHIHASHI, Yoshihiko OKAMOTO, Tsutomu YAS ...1991 Volume 40 Issue 3 Pages T53-T57
Published: March 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSIn order to reduce labor-intensive tasks and to increase productivity in the quality control testing of pharmaceutical products by HPLC, an automated HPLC system with the function of self-diagnosis was developed. This system can change and adjust instrumental conditions automatically according to specific parameters for the method preprogrammed in the data processor (C-R4A). Additionally, it can also perform the validation of system suitability, and judge "Pass/Fail" results. Therefore, this system has the capability of multiple sample analysis automatically and sequentially without any operator's intervention.View full abstractDownload PDF (527K) -
Fumio HIROSE, Kei YAMADA, Haruno OKOCHI, Morimasa SAITO1991 Volume 40 Issue 3 Pages T59-T63
Published: March 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe simultaneous determination of hafnium, tin and nickel in zircaloys was investigated by the isotope dilution method using enriched 179Hf, 117Sn and 60Ni, combined with the spark source mass spectrometry. The sample of 0.2g of zircaloy was dissolved in nitric acid (1+1) and hydrofluoric acid after the spike solutions were added. The dissolved solution was evaporated to dryness and the salt residue was mixed with high purity graphite powder, and then formed into electrodes. The proposed method was applied for the determination of hafnium, tin and nickel in zircaloys standard reference materials JAERI CRM Z11, Z12, Z13 and Z14. The results of analysis were in good agreements with the certified values. Hf, Sn and Ni can be determined with the detection limits of 10ppm, 5ppm and 10ppm, respectively. The relative standard deviation of the measurements for Hf, Sn and Ni were within 3%, 6.5% and 9.1%, respectively.View full abstractDownload PDF (603K) -
Hirohito KUROSAKI, Hiromi YOKOYAMA, Kunio OZAKI1991 Volume 40 Issue 3 Pages T65-T69
Published: March 05, 1991
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSFive different extraction methods for gas chromatographic determination of tributyltin (TBT) and triphenyltin (TPT) compounds in fish tissue were compared. Analytical results of TBT in the sea bass tissue by 5 different methods varied from 0.013 to 0.098μg g-1 and that of TPT varied from 0.18 to 0.78μg g-1. No interfering peaks were found in the gas chromatograms. The method in which alkaline hydrolysis and extraction with hexane/ethyl acetate/ (1:1, v/v) mixture was used, gave the best analytical results.View full abstractDownload PDF (690K) -
Katsumi IGARASHI, Ryozo NAKASHIMA, Toshiharu NAYA1991 Volume 40 Issue 3 Pages T71-T75
Published: March 05, 1991
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA microwave digestion technique for trace element analysis of coals was examined. Each 0.25g of twelve coals and cork containing fixed carbon ranging from 43.0 to 88.8% was digested in a microwave oven using a borosilicate vessel with two type mixtures of nitric-sulfuric acids or nitric-perchloric acids. The complete digestion times were compared by referring to the fixed carbon contents. The digest was transferred to a 50ml of PTFE vessel and evaporated until white fume appeared. After hydrofluoric acid treatment, boric acid was added and the solution was diluted to 25ml. Matrix matching was made by adding corresponding amounts of major elements. Chromium, copper, manganese, nickel, lead and zinc were determined by AAS. The analytical data for the digests of Black Water and Smoky River coals showed satisfactory agreement with those obtained by a sealed PTFE bomb method. However, the recovery for chromium in NIST SRM 1632a and Smoky River coal was low.View full abstractDownload PDF (607K)
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