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Robert C. BRASTED
1986 Volume 2 Issue 2 Pages
103-107
Published: 1986
Released on J-STAGE: July 27, 2007
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Sadao MORI
1986 Volume 2 Issue 2 Pages
108
Published: 1986
Released on J-STAGE: July 27, 2007
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Masao S. HASHIMOTO, Hideo YAMADA, Kohnosuke OHISHI, Kazuo YASUDA
1986 Volume 2 Issue 2 Pages
109-112
Published: 1986
Released on J-STAGE: June 23, 2006
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A method of extending the dynamic range in flameless ZAAS (Zeeman atomic absorption spectroscopy) was proposed. The calibration curve in this method was made as follows: Slice the absorbance-time profile at a height
Awt, which is higher than (1/20)
A0 and lower than (1/2)
Ap
0, where
A0 is the peak height and
Wt is the width resulted from this slicing procedure. The slicing was done so as to give a constant
Wt for all the aliquot of the solutions. It was shown that the dynamic range can be extended more than 10 times compared to the usual peak height method.
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Akinori UEJIMA, Fumio ITOGA, Yoshinori SUGITANI
1986 Volume 2 Issue 2 Pages
113-117
Published: 1986
Released on J-STAGE: June 23, 2006
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A new method of correlation photoacoustic imaging for the non-destructive depth-resolved analysis of a solid material has been developed. This method is made up of the two independently developed methods, thermal wave imaging and correlation photoacoustic spectroscopy. The new method has been applied to a layer-structured model sample where the separation of component layers is 15μm and found to be clearly resolved. As for color reversal films the depth resolution was about several μm for levels near the surface and somewhat less for the deeper levels.
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Atsuko TSUNODA, Keiichiro FUWA, Kazuko MATSUMOTO
1986 Volume 2 Issue 2 Pages
119-123
Published: 1986
Released on J-STAGE: June 23, 2006
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Effect of absorption-tube shape in flame-in-tube atomic absorption spectrometry of selenium was investigated. About ten quartz tubes with various hydrogen and air introduction systems were designed and compared for selenium sensitivity. From the examination of the tube size ranging 6 to 50cm in length and 1 to 7mm in id., the following conclusion was found. At relatively large i.d. (-7mm), no sensitivity increase is observed by tube elongation. However, at i.d. of 1mm, elongation of the tube length from 30 to 50cm increases the sensitivity in proportion to the tube length. At i.d.′s between 1 and 7mm, sensitivity increase is certainly observed for tube elongation, but the increase is not so much as expected if it would be in proportion to the tube length. This would be due to the difference of the atomic population in a tube in this medium i.d. range. The best sensitivity and detection limit obtained with a tube of 50cm long and 1mm id. were 0.021ng (1% absorption) and 0.047ng, respectively. The method was successfully applied to the analyses of NBS SRM′s.
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Hajime ISHII, Michiyo AOKI, Takeshi AITA, Tsugikatsu ODASHIMA
1986 Volume 2 Issue 2 Pages
125-129
Published: 1986
Released on J-STAGE: June 23, 2006
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A selective flow injection analysis (FIA) system has been proposed for the spectrophotometric determination of trace amounts of iron based on the 1:2 (metal:ligand) complex formation between iron(II) and 2-pyridyl-3′-sulfophenylmethanone 2-pyrimidylhydrazone(PSPmH). The system permits high throughput of 70 solutions per hour. The lower limit of determination is 10ppb of iron. The procedure has been applied successfully to the determination of iron in water samples. Possibility of further enhancement in the sensitivity in FIA by introducing analogue-derivative spectrophotometric monitoring is also suggested.
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Katsuo OHSHIMA, Hiroto WATANABE, Kensaku HARAGUCHI
1986 Volume 2 Issue 2 Pages
131-135
Published: 1986
Released on J-STAGE: June 23, 2006
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Ethylenediaminetriacetate-bonded silica gel (ED3A-SG) was used for preconcentration of heavy metal ions prior to their determination by inductively coupled plasma-atomic emission spectrometry (ICP-AES). ED3A-SG was prepared by reacting silica gel with N-(trimethoxysilylpropyl)ethylenediaminetriacetate. Coastal seawater up to 2dm
3, buffered at pH 5.0, were passed through a column filled with 250mg of ED3A-SG. Then the metal ions adsorbed were eluted with 10cm
3 of 0.5mol dm
-3 hydrochloric acid. The concentrate thus obtained was analyzed by ICP-AES.
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Tatsuya SEKINE, Takashi KURIHARA
1986 Volume 2 Issue 2 Pages
137-140
Published: 1986
Released on J-STAGE: June 23, 2006
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Rate of stripping of beryllium(II) extracted into carbon tetrachloride from aqueous solution as benzoylacetonate chelate by perchloric and nitric acid was enhanced when 4-methyl-2-pentanone was added to this solvent. This was explained in terms of a change in the reaction route. When the organic phase was carbon tetrachloride, the chelate in the organic phase was partially washed into the aqueous phase and underwent dissociation into the metal ion and this reaction in the aqueous phase controlled the stripping of the chelate. However, when 4-methyl-2-pentanone was added, part of the acid in the aqueous phase was extracted and the dissociation of the chelate also took place in the organic phase. This reaction in the organic phase enhanced the rate of stripping.
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Hisatake NARASAKI
1986 Volume 2 Issue 2 Pages
141-144
Published: 1986
Released on J-STAGE: June 23, 2006
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Trace arsenic and selenium in copper or nickel powder were determined, after separation with Chelex 100 resin, by hydride-generation atomic absorption spectrometry in the presence of masking agents. When recoveries of arsenic or selenium were checked in the presence of copper or nickel ion in solution, they were quantitative. On the contrary, the recoveries of arsenic or selenium added to copper powder were not quantitative without masking agents, which may be due to partial elution of copper from the resin. Accuracies tested with an NBS Standard Reference Material were within the certified values.
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Kazuo HIIRO, Takashi TANAKA, Akinori KAWAHARA, Shin-ichi WAKIDA
1986 Volume 2 Issue 2 Pages
145-148
Published: 1986
Released on J-STAGE: June 23, 2006
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Urushi, a kind of natural oriental lacquer, has excellent durability and mechanical strength. Therefore, its use as a membrane matrix for tetrafluoroborate ion selective electrode was examined. A linear potential-concentration curve was obtained within the concentration range 10
-1-10
-5mol dm
-3 tetrafluoroborate. The slope of the linear part of the curve was 55mV per decade change of the concentration with the electrode prepared from 50 wt% of tri-n-octylmethylammonium tetrafluoroborate and 50wt% of raw Urushi latex. This electrode exhibited a constant potential within the pH range 2-6. The static response time of the electrode was about 1min and the dynamic response time was about 10s. Utilization of other kinds of ion-exchanger and Urushi latex as electrode membranes was also examined. The selectivity coefficient for each electrode was measured. Two types of flow-through electrodes were prepared. They showed similar potential-concentration curves to that for the usual type electrode. The electrode was applied to the measurement of the formation rate of tetrafluoroborate from boric and hydrofluoric acids. The electrode could be used for more than 5 months.
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Shigeroku YAMAGUCHI, Katsuya UESUGI
1986 Volume 2 Issue 2 Pages
149-152
Published: 1986
Released on J-STAGE: June 23, 2006
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Extractive spectrophotometric determination of copper(II) with 5-nitrosalicylaldehyde-4-phenyl-3-thiosemicarbazone (NSPS) is described. The method is based on the formation of an insoluble copper(II)-NSPS complex, which is extractable into chloroform from an aqueous solution in the pH range 2.3 to 6.2 by shaking for 3min. The absorbance is measured at 390nm and the molar absorptivity is 2.5×10
4 l mol
-1 cm
-1. The complex system conforms to Beer′s law for up to 2.5μg ml
-1 of copper(II ). The method is simple in that a single extraction suffices; common ions, except palladium(II), silver(I), gold(III) and mercury(II), do not interfere in the determination. The method has been applied successfully to the analysis of aluminum and magnesium alloys.
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A. WASEY, B. K. PURI, Mohan KATYAL, M. C. MEHRA
1986 Volume 2 Issue 2 Pages
153-156
Published: 1986
Released on J-STAGE: June 23, 2006
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A spectrophotometric method has been developed for the microdetermination of osmium(VIII) as its 9, 10-phenanthrenequinone monoximate after coprecipitation on to microcrystalline naphthalene. The optimum pH range for the coprecipitation is 6.8-10.5. Naphthalene and the metal complex is separated by filtration and dissolved in chloroform. The absorbance is measured at 475nm against a reagent blank. Beer′s law is obeyed in the concentration range 5.0-99.0μg of osmium in 10ml of chloroform solution. The molar absorptivity and sensitivity are 1.695×10
4 l mol
-1 cm
-1 and 0.00112μg/cm
2, respectively. Ten replicate determinations of a sample containing 57.0μg of osmium give a mean absorbance of 0.508 with a standard deviation of 0.0049 and relative standard deviation of 0.96%. The accuracy of the method is checked by the determination of osmium in synthetic mixtures corresponding to its occurring in native and alloys.
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Takeshi HASHIZUME, Wataru TANIGUCHI, Tamiji SUGIYAMA
1986 Volume 2 Issue 2 Pages
157-159
Published: 1986
Released on J-STAGE: June 23, 2006
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Mass spectrometric determination of the biologically important
N6-isopentenyladenosine and
N6-isopentenyladenine from human urine has been carried out on the basis of stable isotope dilution and selected ion monitoring. Both compounds were detected in human urine; their levels in the urine of a young human were estimated to be 0.153ng/ml(S.D. 0.009) and 3.680ng/ml(S.D. 0.270), respectively.
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Takeji CHIKAMOTO, Takeshi MAITANI
1986 Volume 2 Issue 2 Pages
161-164
Published: 1986
Released on J-STAGE: June 23, 2006
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A new gas chromatographic method was developed for the determination of thiocyanate ion in biological fluids. Fluid sample solutions deproteinized with acetone or methanol were centrifuged. After evaporation of the organic solvent of the supernatant by a rotary evaporator, thiocyanate ion was ethylated with ethyl iodide in an immiscible aqueous phase-organic phase system by using an immobilized phase-transfer catalyst. The resulting ethyl thiocyanate was determined by gas chromatography on a 20% polyethylene glycol 20M column. Either a flame ionization detector (FID) or a flame thermionic detector (FTD) was used. Thee method was capable of detemining thiocyanate ion concentrations in the range of 5 to 40μg/ml with the FID and 0.05 to 20μg/ml with the FTD. The detection limits were 1μg/ml with the FID and 0.01μg/ml with the FTD. The recoveries of thiocyanate ion added to cow′s milk, human saliva, and human urine samples were over 92% with good repeatability.
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Keiko OHSAWA, Yoshihiro YOSHIMURA, Shuji WATANABE, Hiroshi TANAKA, Kaz ...
1986 Volume 2 Issue 2 Pages
165-168
Published: 1986
Released on J-STAGE: June 23, 2006
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Pulsed amperometric detection with an ion chromatograph was used for the determination of xylitol in the human serum and saliva. Xylitol in serum and saliva was determined by using 0.15M sodium hydroxide as an eluent and D-mannitol as an internal standard. Xylitol and D-mannitol could be separated completely with retention times of 1.98min and 2.47min, respectively. Linearity of peak heights was 0.025 to 1.0μg/ml xylitol.The detection limit was 0.01μg/ml with an
S/N=2. Mean recovery of xylitol ranged from 99.5 to 101.4%.Maximum concentrations of xylitol in serum and saliva were observed approximately 30min and 150min, respectively, after oral administration.
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Takeo KATAMI, Tomokuni HAYAKAWA, Masamichi FURUKAWA, Shozo SHIBATA, Ta ...
1986 Volume 2 Issue 2 Pages
169-174
Published: 1986
Released on J-STAGE: June 23, 2006
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2-[2-(3, 5-Dibromopyridyl)azo]-5-dimethylaminobenzoic acid(3, 5-diBr-PAMB) and 2-(2-benzothiazolylazo)-5-dimethylaminobenzoic acid(BTAMB) give sensitive color change by the reaction with a few metal ions. The metal complexes are extracted into organic solvents from aqueous solutions and the reagents have been used for the determination of trace amounts of those metals. To study analytical properties of these reagents, the acid dissociation constants and the stability constants of metal complexes in 40% (v/v) dioxane solution were determined spectrophotometrically. The optimum analytical condition for the formation of a metal complex in aqueous dioxane solution and for the extraction of a metal complex into organic solvent was determined. The composition of a metal complex was measured by the continuous variation method. The apparent molar absorptivities and stability constants of 3, 5-diBr-PAMB metal complexes were larger than those of BTAMB. But, the selectivity of BTAMB was good comparison with 3, 5-diBr-PAMB. The copper(II) and palladium(ll) cationic complexes can be extracted into organic solvent to form an ion-pair compound with singly charged anion.
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Junichi GOTO, Toshiyuki CHIKAI, Toshio NAMBARA
1986 Volume 2 Issue 2 Pages
175-178
Published: 1986
Released on J-STAGE: June 23, 2006
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A method for the separation and characterization of bile acid 7- and 12-sulfates without prior deconjugation by means of high performance liquid chromatography (HPLC) is described. Bile acid 7- and 12-sulfates were derivatized quantitatively into the fluorescent compounds through the hydroxyl group at C-3 by treatment with 1-anthroyl nitrile in the presence of quinuclidine in acetonitrile. Subsequent resolution into each individual sulfate was attaind by HPLC on a Cosmosil 5C
18 column using 0.3% potassium phosphate buffer (pH 4.0)-methanol (1:3) as a mobile phase. The 3-(1-anthroyl) derivatives of 7- and 12-sulfates were monitored by fluorescence detection (excitation wavelength 370nm; emission wavelength 470nm), the limit of detection being 30 fmol.
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Hajime OHTANI, Tadashi KIMURA, Shin TSUGE
1986 Volume 2 Issue 2 Pages
179-182
Published: 1986
Released on J-STAGE: June 23, 2006
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Thermal degradation of a series of terephthalate polyesters has been studied by high-resolution pyrolysis-gas chromatography. A wide range of the degradation products can be separated by using a fused silica capillary column. Sharp peaks of the polar compounds which are characteristic of the polymer structures are observed even in the fragments of the degradation products which carry acid end groups. The degradation mechanisms of the terephthalate polyesters are discussed on the basis of the observed pyrograms.
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Masako MAEDA, Akio TSUJI
1986 Volume 2 Issue 2 Pages
183-186
Published: 1986
Released on J-STAGE: June 23, 2006
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Chemiluminescence reactions of lucigenin with various biological compounds were examined by a flow injection method. It was found that chemiluminescence from reducing sugars and related compounds was enhanced 100-times when incubated with sodium periodate prior to the reaction with lucigenin. The standard curve of glucose was linear over the range 50pmol-700pmol. Detection limits of glucose with and without treatment of sodium periodate were 50pmol and 50nmol, respectively. Corticosteroids and other compounds having an α-hydroxycarbonyl group in their molecule gave intensive chemiluminescence without treatment of sodium periodate. It was estimated that the α-hydroxycarbonyl group which converts to 1, 2-enediol was essential for the chemiluminescence reaction with lucigenin.
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Yukiko DOKIYA, Shinichi BESSHO
1986 Volume 2 Issue 2 Pages
187-190
Published: 1986
Released on J-STAGE: June 23, 2006
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Ion chromatographic determination of ammonium ion using a non-suppressor-type ion chromatographic apparatus was applied to the rain and snow samples. Analytical conditions, including the concentration of eluent and the pH of the sample solutions, were examined to achieve the maximum sensitivity. The recovery of the amount added to the actual rain sample was found to be 95-105%. Comparison with the spectrophotometric determination using indophenol was also done with sufficient reliability for a field method. Each event rain sample at Tsukuba Science City, Japan, during 1984 was used for this determination. The seasonal variation of the concentration of ammonium ion was obtained. Vertical differences of the concentration of ammonium ion in the deposition sample of 1985 were also studied using the Meteorological Observation Tower (213m).
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Takeshi YAMANE
1986 Volume 2 Issue 2 Pages
191-195
Published: 1986
Released on J-STAGE: June 23, 2006
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A catalytic method is presented for the simple, sensitive and selective determination of manganese at trace levels in natural waters. The on-line cation-exchange separation in tartrate media was directly coupled with catalytic detection, based on the oxidation of protocatechuic acid by hydrogen peroxide in alkaline media, in a continuous flow system. The increase in the absorbance at 480nm, owing to the manganese catalyzed oxidation of protocatechuic acid, was monitored and recorded. The limit of detection of the proposed method is 0.2ng ml
-1, when a 906μl sample is injected. The relative standard deviations less than 2.5% were evaluated in the analysis of river and lake waters for 1.4-11.2ng ml
-1 manganese.
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Akira TANAKA, Kouichi OBATA, Toshio DEGUCHI
1986 Volume 2 Issue 2 Pages
197-198
Published: 1986
Released on J-STAGE: July 27, 2007
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Sunao YAMADA, Teiichiro OGAWA
1986 Volume 2 Issue 2 Pages
199-200
Published: 1986
Released on J-STAGE: July 27, 2007
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Shizuo FUJIWARA, Nobuaki KONDO, Rokuro KURODA
1986 Volume 2 Issue 2 Pages
201
Published: 1986
Released on J-STAGE: June 23, 2006
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Hiroomi NAKAMURA, Yoshinori KIDANI, Akira KOSAKA
1986 Volume 2 Issue 2 Pages
203-204
Published: 1986
Released on J-STAGE: June 23, 2006
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