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Volume 37, Issue 5
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Isao IKEUCHI, Tameyuki AMANO1988 Volume 37 Issue 5 Pages 211-215
Published: May 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSBoron-10 enriched sodium mercaptoundecahydrododecaborate(I), Na210B12H11SH, is one of the most useful agents for boron neutron-capture therapy of brain tumors. To monitor the quality of I, a simple spectrophotometric method has been developed for measuring its disulfide, sodium dithio(undecahydrododecaborate) (II), which presents as a main contaminant in I. The aqueous soultion containing II showed blue color by the addition of nucleophilic solvents such as acetone, acetonitrile, dimethylformamide and pyridine, based on bis (undecahydrododecaboranyl) disulfide radical produced from II. The absorption spectra of blue colored solutions showed the maxima at about 630 nm. The color intensities were affected by the contents of organic solvent in the mixed solutions. Among organic solvents added to an aqueous solution of II, pyridine was the most intensive for the color development. An aqueous solution of II mixed with an equal portion of pyridine showed a maximal absorbance at 634 nm. The color system obeyed Beer's law in the concentration range of II from 8 to 50×10-6 mol dm-3 in an aqueous solution. The detection limit was 5 ×10-6 mol dm-3.View full abstractDownload PDF (874K) -
Sunao YAMADA, Naoshi ADACHI, Hirofumi KAWAZUMI, Teiichiro OGAWA1988 Volume 37 Issue 5 Pages 216-220
Published: May 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSVarious aromatic molecules have been detected simply and conveniently by measuring the photocurrent signal induced by resonance enhanced two-photon ionization. Volatile benzene derivatives were measured in the ppmppb range by mixing the vapor of the analyte from a diffusion tube with nitrogen gas. Calibration curves were straight in the ppbsub ppm range. Detection limits (S/N=3) of eight benzene. derivatives were as low as ppb levels; the lowest detection limit was 0.8 ppb for aniline. The molecules with large molar absorptivities in isooctane gave the lower detection limits. Less volatile aromatic molecules were measured by the thermal vaporization technique; the solid sample was heated at a constant heating rate and the photocurrent signal was measured as a function of the temperature. Calibration curves were straight, and the lowest detection limit was 90 pg for triphenyl-amine. Some selective detections of mixtutes were possible within 10 min. This method may be useful for rapid identification and quantitation of organic adsorbates without any pretreatment.View full abstractDownload PDF (767K) -
Akiko OKAYAMA, Yoshimi KITADA, Yoshinari AOKI, Seiichi UMESAKO, Hiromi ...1988 Volume 37 Issue 5 Pages 221-224
Published: May 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA rapid, simple and accurate method for the determination of streptomycin (SM) in meat by HPLC was developed. The method includes extraction with perchloric acid solution and clean-up using a C8 pretreatment column. A 18 ml of the mixture of a edible tissue extract and the buffer solution including ion pair reagent was poured into a pretreatment column, and the column was washed with 5 ml each of water and 30% methanol solution successively. Streptomycin was eluted from the column with 3 ml of methanol. The eluate was concentrated to 0.1 ml under nitrogen stream, and adjusted to 1.0 ml with 5 mM sodium 1-octanesulfonate solution (pH 3.3). Then a 10 μl aliquot of the solution was injected into the HPLC system. The HPLC condition was as follows : column, Nucleosil 5C18 (5 μm, 250 mm×4.6 mm i.d.); mobile phase, water-acetonitrile (86 : 14) containing 20 mM disodium 1, 2-ethanedisulfonate, 5 mM sodium 1-octanesulfonate and 5 mM ninhydrin (pH 3.3); flow rate, 1.2 ml/min; column temp., 60 °C; detection, fluorescence Ex. 400 nm, Em. 495 nm; reaction coil, stainless steel tube (10 m × 0.5 mm i.d.); reaction solution, 0.3 M sodium hydroxide solution; flow rate, 0.3 ml/min; reaction temp., 80°C. A linear regression analysis of the calibration curve obtained from the standard solution (0.050.5 μg) yielded the equation Y=0.64X+0.26, r=0.9970. The recovery of SM added to chicken meat at the level of 2 μg/g was 66.7%. The detection limit of SM was 0.5 μg/g.View full abstractDownload PDF (669K) -
Masaru KIMURA, Junko KOMADA, Etsuko KAWABATA1988 Volume 37 Issue 5 Pages 225-229
Published: May 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe adsorption properties of Au(III), Mo(VI) and V(V) ions on surface of the Japanese green-tea (powder tea) particles were examined by measurements of the adsorption percentage and by plotting the adsorption isotherm curves in aqueous solutions of pH 16. The powder tea was treated with formaline in a dilute sulfuric acid. A 100 ml sample solution containing Au, Moand/or V was mixed with the treated tea (0.1 or 0.5 g for usual use) under stirring for 30 min. The solution was then centrifuged and the concentrations of Au(III), Mo(VI) and V(V) ions in the supernatant solution were determined with the atomic absorption spectrometer. Au and Mo at pH 16, and V at pH 36 were adsorbed over 80% on the tea. The maximum adsorption amounts under the conditions were determined by the isotherm and Langmuir plots to be 23, 12 and 3.5 mg g-1 for Au, Mo and V, respectively. It was found that 50 μg Au, 200μg Mo, and 150 μg V in a 100 ml solution containing 10 or 30 g Zn(NO3)2.6H2O were quantitatively adsorbed on 0.1 g of the tea. Effect of NaCl, Na2SO4, Na2C2O4, 8-quinolinol, 1, 10-phenanthroline and EDTA (Na2[H2edta]) on the adsorbability of Au, Mo and V was examined. The adsorption percentage of Au did not change at all by addition of anyone of them. On the other hand, adsorption of Mo and V was seriously inhibited by addition of EDTA, and that of Mo was remarkably inhibited by addition of 1, 10-phenanthroline.View full abstractDownload PDF (773K) -
Takao IIDA, Kazumi FUKAMACHI, Shigeyuki TAKENAKA, Reiko NAKAGAWA, Kats ...1988 Volume 37 Issue 5 Pages 230-235
Published: May 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSLevel and composition of polychlorinated quaterphenyls (PCQs) in blood are important for understanding of the etiology of Yusho, therefore, a highly sensitive and accurate determination has been examined. Six skeletal types of PCQ congener are theoretically formed by dimerization of polychlorinated biphenyls (PCBs). After perchlorination of the PCQ congeners to give six corresponding types of octadecachloroquaterphenyls (ODCQs), separation was carried out by GC equipped with a capillary column and electron capture detector. The column used was a fused silica methyl 50% phenylsilicone capillary column (25 m × 0.32 mm i.d., 0.25μm film thickness). GC conditions were as follows : The sample was injected splitlessly and trapped on the top of the capillary column at 80 °C. The column temperature was rapidly increased from 80 °C to 280 °C, and then the column temperature programmed from 280 °C to 315 °C at 1 °C/min with the final temperature being held for 120 min. In this method, the detection limit of each isomer of ODCQ was 3 pg, that was defined as the weight of each skeletal congener of PCQ giving a signal equal to 3 times the amplitude of the baseline noise. Six skeletal types of PCQ congener were detected in the thermotransfer medium used in the factory, in the blood and adipose tissue of Yusho patients, and in those normal persons.View full abstractDownload PDF (1062K) -
Toshio YAO, Yoshihiro MATSUMOTO, Tamotsu WASA1988 Volume 37 Issue 5 Pages 236-241
Published: May 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA bio-FIA system is proposed for the estimation of fish freshness. Alkaline phosphatase immobilized reactor (5 mm long, 4 mm i.d.) and purine nucleoside phosphorylase/xanthine oxidase co-immobilized reactor (12 mm long, 4 mm i.d.) were incorporated at fixed positions in a FIA system. The system was based on the splitting of the flow after the sample injection and subsequent confluence before reaching the glassy carbon electrode. Because each channel has a different residence time, two peaks were obtained. The peak current of the first and second peaks were linearly related to the total concentration of inosine and hypoxanthine in the range 0.012 mM and to the total concentration of inosine-5'-monophosphate, inosine and hypoxanthine in the range 0.011mM. The detection limits were 0.5 × 10-6 M for the first peak and 2 × 10-6 M for the second peak when a 10-μl sample was injected. An indication of fish freshness, K', is estimated by
K' =(s2/s1) (i1/i2) × 100
where s1 and s2 are the sensitivity (nA mM-1) and i1 and i2 are the peak current (nA) of the first and second peaks, respectively. The determining rate of fish freshness by the proposed system was 15 samples h-1with satisfactory precision (0.51.2% R.S.D.). In conclusion, the proposed FIA system was found to be useful as a new, simple, rapid and selective method for the estimation of fish freshness.View full abstractDownload PDF (923K) -
Yasuo INOKUMA, Jyo ENDO1988 Volume 37 Issue 5 Pages 242-247
Published: May 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA spectrophotometric method based on extraction of the hexafluorotantalate-Victoria Blue B ion association complex was examined for the determination of accurate values of the 10-4% level of Ta in steels and nickel base alloys. Samples (0.5 g) were dissolved in 15 ml of aqua regia and 3 ml of hydrofluoric acid by heating. Hydrochloric, nitric and hydrofluoric acids were eliminated by white-fume treatment with 10 ml of sulfuric acid (1+1) and 4 ml of phosphoric acid (1+1). After cooling and diluting to 50 ml with 4 ml of hydrofluoric acid (38+62), 15 ml of Victoria Blue B (VB-B) solution (1.2 g/l) and water, the sample solution was shaked vigorously for 30 s with 20 ml of benzene to extract the ion association complex. The Organic phase was washed twice by shaking with 25 ml of a washing solution (1.8 M, 0.6 M, 0.8 M and 7 × 10-4 M sulfuric, phosphoric and hydrofluoric acids and VB-B respectively) to remove the interference of Nb. Absorbance of the ion association complex in organic solvent was measured quickly at 630 nm with a 10 mm quartz cell against a reagent blank after washing the cell 3 to 4 times with the organic extract. Boron interference can be eliminated by adding 40 ml of methanol and carrying out white-fume treatment of sulfuric acid. The relative standard deviations were 5 to 3% for 0.003% to 0.022% of Ta content. The limit of determination minimum of this method was 0.0002%.View full abstractDownload PDF (945K) -
Toshio DEGUCHI, Ryoichi TAKESHITA, Akira TANAKA, Isao SANEMASA1988 Volume 37 Issue 5 Pages 248-252
Published: May 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSStilbazo, 4, 4'-bis(3, 4-dihydroxyphenylazo) stilbene-2, 2'-disulfonic acid diammonium salt, is oxidized in the presence of hydrogen peroxide, where cobalt(II) acted as catalyst and accelerated the oxidation reaction.The decoloration of stilbazo measured at 503 nm was found to be proportional to the hydrogen peroxide concentration over its low concentration range. A 90 μM stilbazo solution containing 0.5 ppm Co(II) and a buffer solution (pH 11.9, NaOH+Na2CO3) were delivered each into the FIA system at a flow rate of 1.0 ml/min. The resulting mixture was then converged with the water stream flowing at a rate of 2.0 ml/min, that served as a sample carrier. The sample solution of hydrogen peroxide (390μl) was injected into the sample carrier, and was sent to a reaction tube (3.5 m × 1 mm i.d.) thermostated at 30 °C. The absorbance change in stilbazo was measured at 503 nm. The following experimental conditions were examined: sample volume injected, reaction tube length, reagent solution flow rate, reaction temperature, concentration of stilbazo and Co(II), and the interference of diverse ions. Ascorbic acid seriously interfered, while glucose, fructose, urea, NaCl, KBrO3, and some other inorganic electrolytes did not. Heavy metals (Cu, Zn, Ni) were effectively removed by an ion-exchange column (25 cm × 2 mm i.d.) installed just after the sample injection section. The determination range of hydrogen peroxide was from 0.1 to 10 ppm. The sampling rates were ca. 30 samples/h with the ion exchange column and 75 samples/h without the column.View full abstractDownload PDF (801K) -
Yasuhiko OSAKI, Takahiko MATSUEDA1988 Volume 37 Issue 5 Pages 253-258
Published: May 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method for the simultaneous analysis of trace amounts of ο-, m- and p-aminophenols in water by electron capture GC of their pentafluorobenzoyl (PFB) derivatives conveniently prepared after acetate derivatization has been developed. The procedure for the determination of ο-, m- and p-aminophenols from environmental and waste water samples was as follows; 500 ml of water sample was taken in a 1 l separatory funnel and acidified with 0.5 ml of hydrogen chloride. To this aqueous solution, 1 ml of acetic anhydride was added. The mixture was shaken for 40 min at room temperature. This solution was adjusted to pH 7.7 by addition of 20 g of sodium hydrogen carbonate with occational mixing. After addition of 100 μl of pentafluorobenzoyl chloride, the reaction mixture was shaken for 10 min at room temperature. This solution was extracted twice with each of 100 ml of ethyl acetate with vigorous shaking. The combined ethyl acetate solution was concentrated to 1 ml using a Kuderna-Danish (KD) concentrator at 60 °C. The residual ethyl acetate solution was washed with 1 ml of 2.5% phosphoric acid. The organic solvent layer was rinsed into a Florisil column with 0.5 ml of ethyl acetate. After the solvent on Florisil column almost moved down, the contamination were removed by passing through the column 100 ml of 5% (v/v) diethyl ether in hexane and then hydroxyacetoanilide (HAA)-PFB derivatives were eluted with 200 ml of 30% (v/v) ethanol, 30% (v/v) ethyl acetate in benzene. The eluate was concentrated to 1 ml using KD concentrator. Aliquots of 25 μl cleaned-up sample were analyzed by ECD-GC. The amounts of aminophenols were calculated by multiplying the amounts of HAA obtained from calibration curves by the molecular-weight ratio of aminophenol to HAA. Recoveries of aminophenols from water samples employing this method were 6382% for ο-aminophenol, 6070% for m-aminophenol and 6376% for p-aminophenol, respectively. Detection limits by use of ECD-GC equipped with the packed column (OV 225+ SP 2401) were 0.2 μg/l for ο-aminophenol, 0.4μg/l for m-aminophenol and 0.4μg/l for p-aminophenol, respectively.View full abstractDownload PDF (925K) -
Yukio MINAMI, Toshiyuki MITSUI, Yoshikazu FUJIMURA1988 Volume 37 Issue 5 Pages 259-262
Published: May 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe determination of procaine hydrochloride was studied by means of curie point pyrolysis GC using an induction heating pyrolyser. The procedure for the determination was as follows : Procaine hydrochloride in water (150 μg) was applied onto 30 mg of mixed powder {Ni KI (NH4)2 SO4= 10 : 3 : 2} placed on pyrofoil by use of a microlitre syringe. After heating on a hot plate for 5 min at 100 °C to evaporate water, the pyrofoil was placed in the pyrolyser and pyrolysed for 4 s at 590 °C. The procaine hydrochloride reacts with potassium iodide and ammonium sulfate to form ethyl iodide. The peak area of ethyl iodide was used for the determination of procaine hydrochloride. No detectable interference was observed in determination of procaine hydrochloride by such compounds that sodium chloride, starch, glucose, lactose, fresh blood and putrid blood. The calibration curve for procaine hydrochloride constructed by using the peak area method were linear over the concentration range of 150μg. The relative standard deviation (n=10) was 1.95% for 24.5μg of procaine hydrochloride.View full abstractDownload PDF (661K) -
Yuji UENO, Nobuaki SASAOKA, Kiyotoshi MORISHIGE, Tsunenobu SHIGEMATSU, ...1988 Volume 37 Issue 5 Pages 263-268
Published: May 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSamarium (III) and europium (III) ions in the solution of mineral acids showed specific fluorescence. This fluorescence displayed apparent energy splitting which was different from the thenoyltrifluoroacetone-trioctylphosphineoxide complex. This communication reports the optimum condition for the fluorometric determination of Sm (III) and Eu (III) in hydrochloric acid solution {Sm (III) : Ex. 402 nm, Em. 597 nm, φf: 1.4 × 10-4, F.S.I. (fluorescence sensitivity index) : 1.41 × 10 -8μm; Eu (III) : Ex. 395 nm, Em. 597 nm, φf: 1.9 × 10 -3, F.S.I.: 7.67 × 10 -7μm}. Sm in xenotime and Eu in phosphor [YVO4 : Eu] were analyzed.The procedure for the analysis of Sm (III) and Eu (III) was established as follows : The rare earth mineral sample (xenotime) was treated with hot conc. H2SO4. The phosphor was fused with KHSO4 and the resulting cake was dissolved in 2 mol dm-3 hydrochloric acid. The rare earth were precipitated with oxalic acid from the digested sample solution. Then, the precipitates were filtered off and ignited to give the rare earth oxides. Appropriate amount of each was dissolved in conc. HCl and the solutions were diluted with water to give 2 mol dm-3 hydrochloric acid solution. Sm in, xenotime was analyzed by narrow base line method. The fluorescence intensities of the sample solutions were measured at exciting wavelengths 402, 399 and 405 nm with fixed emission wavelength of 597 nm. Xenotime (A) contained 0.63% of Sm2O3 and xenotime (B) contained 0.62% of Sm2O3. The fluorescence intensity of the sample solution was monitored at 591 nm with excitation wavelength at 395 nm for Eu in phosphor. The content of Eu2O3 was 3.79%. The relative standard deviation of the measurements were less than 5% for Sm (III) and Eu (III).View full abstractDownload PDF (1031K) -
Atsushi CHIBA, Masami NAWA, Tadahiko OGAWA1988 Volume 37 Issue 5 Pages 269-271
Published: May 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA chelating resin for the detector was prepared by mixing Pyrogallol Violet solution and 1.0 g of Dowex 2X8 or Dowex SAR anion exchange resin. After stirring for 30 min with magnetic stirrer, the resin was filtered off from the solution and dried at 50 °C in air to retain about 25% and 10% of the original water contentin Dowex 2X8 and SAR, respectively. A 200 or 300 mg portion of the resin was packed in a glass tube of 2.55 mmφ × 100 mm, both ends of resin were plugged with cotton wool. During determination, 0.5 cm3/3 min at 1525 °C (2X8) and 4 cm3/2 min at 90 °C (SAR) of sample solution (pH 3.5) was sucked into the column and the length of colored layer appearing in the column was measured. By placing a column containing cation exchanger in front of the detection tube, diverse cations could be preliminarily removed. Determinable concentration range of Mo (VI) ion was 0.272.7 (SAR) and 27665 (2X8) μg/cm3 with an error of ± 10%.View full abstractDownload PDF (465K) -
Takeshi YAMADA, Etsu YAMADA, Masanori SATO1988 Volume 37 Issue 5 Pages T61-T65
Published: May 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe direct potentiometric determination of fluoride ion in complicated environmental samples such as wastewaters from the university's organic waste incinerator by a fluoride ion selective electrode(ISE) without preliminary distillation was investigated. It was found that Al(III), Fe(III), Ca(II), Mg(II) and boric acid interfered with the direct potentiometric determination of fluoride ion based on calibration procedures with standard solutions. However, these interferences were removed by a total ionic strength adjustment buffer (TISAB) containing sodium citrate or CyDTA together with the use of known addition potentiometry or Gran's plot potentiometry. For the masking of Al(III), CyDTA was more effective than sodium citrate. Measurements of fluoride concentration between 0.1 100 mg/l were straightforward, with a relative standard deviation of about 2%. The results of wastewater samples obtained by the present method were in good agreement with the results by spectrophotometric and ISE methods with distillation which are recommended for the determination of fluoride ion in wastewater.View full abstractDownload PDF (867K)
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