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Toru NOZAKI, Keiichi KATO, Misaki UCHIDA, Masashi DOI, Noriko MISE, Yo ...
1983 Volume 32 Issue 3 Pages
145-148
Published: March 05, 1983
Released on J-STAGE: June 19, 2009
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Ion flotation of fifteen kinds of metal ion was investigated in hydrobromic acid solutions with employing cationic surfactants, such as cetylpyridinium chloride (CPC), cetyltrimethylammonium chloride(CTMAC), and tetradecyldimethylbenzylammonium chloride (TDBAC). A 12ml of solution containing (25.596.6)μg/ml of metal and (0.702.2)×10
-3 M of a surfactant in (0.013.7)M hydrobromic acid was subjected to flotation in a cell of 2.7 (diameter) × 20cm for about 20min with nitrogen bubbles. Cd (II), Pb(II), Bi(III), Sb(III), and Sn(IV) were floated from the respective metal solution in (95100) % yield, while Ni(II), Co(II), Cu(II), Mn(II), Al(III), Ga(III), and Cr(III) were not floated in the above acid concentration range. Separation of Cd (II) and Pb(II) from a mixture of Sn(IV), Cd(II), and Pb(II), and that of Pb(II) from Cu(II), Ni(II), Co(II) and Pb(II) were fairly good in a acid concentration rangeof (0.330.46)M. The analysis of the relations between
n (the mean number of the ligand Br
- per each metal) and the concentration of bromide by means of the mole ratio method, suggested the exis tence of the species such as CdBr
3-, CdBr
42-, CdBr
53-, PbBr
3-, PbBr
42-, BiBr
4-, and BiBr
52- in hydrobromic acid solutions used for the flotation experiments.
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An improved program to benzenoid compounds
Yoshiaki ISHIDA, Tokio OOSHIMA, Keiji SAITO, Shin-ichi SASAKI
1983 Volume 32 Issue 3 Pages
148-154
Published: March 05, 1983
Released on J-STAGE: June 19, 2009
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Improvement of accuracy of the structure determination of organic compounds with benzene ring by the computer-assisted method, CHEMICS, has been made. The CHEMICS system provides a lot of the candidate structures for benzenoid compounds because of the ambiguous analyses of H-1 and C-13 NMR spectra of the samples. This ambiguity brings on the generation of the structures of acyclic polyene in addition to those of benzene ring system. CHEMICS-UBE, a modified system of the CHEMICS, has been endowed with an interactive function to input user'sconstraints into the structure generation step. For instance, a user may input the presence of aromatic rings by his discretion so that a number of candidate structures containing acyclic polyene system can be eliminated. The revised system of CHEMICS-UBE gave only one structure for 3-phenylpropionic acid or six isomers for protocatechualdehyde. This system has been applied to 41 derivatives of phenols and catechols and the compounds with very small number of isomeric structures have been generated.
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Kenji TATSUMI, Nobuaki OGAWA, Iwao WATANABE, Shigero IKEDA
1983 Volume 32 Issue 3 Pages
154-158
Published: March 05, 1983
Released on J-STAGE: January 18, 2010
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Chemical stripping chronopotentiometry was applied to determine cadmium(II) and copper(II) by using oxygen as an oxidant. The calibration curve for cadmium(II) was linear within a range of (10
-610
-4) mol dm
-3, while the calibration curve for copper(II) was distorted, since copper(II) ion in the sample solution also worked as an oxidant. The calibration curve for cadmium(II) in the presence of constant concentration of copper(II) ion was linear within the range of (10
-52×10
-4) mol dm
-3. In order to determine copper(II) in the presence of cadmium(II), it was necessary to electrodeposit only copper by re ducing at -0.5V
vs. SCE. The instrumentation used in this work was composed of only a simple voltage supply circuit, a stirrer, a
y-
t recorder and a pH-meter used as a high-impedance potentiometer.
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Kazuo IMAEDA, Keiko OHSAWA, Katsumi UCHIYAMA
1983 Volume 32 Issue 3 Pages
159-164
Published: March 05, 1983
Released on J-STAGE: January 18, 2010
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A photobacterial sensor immobilized on acrylamide gel was applied to the determination of trace amounts of oxygen in air and liquid. The apparatus of this study was assembled by ourselves. The immobilized photobacterial sensor and 20ml of 5% NaCl were transferred into a cell having a volume of 32 ml andargon was bubbled through the solution. The photobacterial sensor emitted light by the luciferin-luciferase reaction according to the amount of oxygen. The light emitted was detected with a photomultiplier 931A and recorded by amplifying its output logarithmically. The acrylamide gel concentration of (78)% was found to be suitable for bacterial fixation in both of stability and luminous intensity. The concentration of NaCl solution had been adjusted to 5%, at which the luminous intensity was highest showing favorable stability. The luminous intensity of the sensor became stronger as the flow rate of argon was raised. However, a flow rate of 20ml/min was most suitable because the filling solution overflowed at high flow rates. A correlation was obtained between the lumirums intensity and the amount of oxygen in oxygencontents of 0.83μg to 8.30μg. The detection limit was 20ng at
S/N2. This sensor was stable for about 30h in continuous use and showed reproducibility of c. v.=5% when 50μl of air passed at 20°C. From the results, it can be concluded that this new sensor is applicable to the microdetermination of oxygen having advantages of easy procurement, simple procedure, and repeatability.
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Gui-wen ZHAO, Shou-xin WANG, Ming-yang ZHU, Kaoru SAKAI
1983 Volume 32 Issue 3 Pages
164-168
Published: March 05, 1983
Released on J-STAGE: May 07, 2010
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Trace amount of rare earth and other several elements was determined by graphite furnace atomic absorption spectrometry using the pyrolytic graphite coated tube, the three kinds of metal carbides (any of the tantalum, zirconium, and lanthanum carbide) coated tubes on the pyrolytic graphite coated tubes, and the tantalum foiled tube. The apparatus used was the Perkin-Elmer atomic absorption spectrometer (Model 460) equipped with the Perkin-Elmer graphite furnace atomizer (Model HGA-76). The highest en hancement factor in sensitivity was obtained by using the tantalum foiled tube within 100 times of mersur ments, but its sensitivity falls extremely when the number of measurements exceeds 100 times. The sensitivity using the three kinds of metal carbides coated tubes for rare earth elements was nearly equal, and their enhancement factors were 6 to 20 fold than that using the untreated tube, 1.5 to 3 fold than that using the pyrolitic graphite coated tube. The lifetime of the lantanum carbide coated tube was about 6 fold than that of the tantalum foiled tube, about 2 fold than that of the pyrolitic graphite coated tube, and about 3 fold than that of the untreated tube. This method may be considered to be useful for routine analysis of trace amount of rare earth and other several elements.
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Takashi YAMASHIGE, Hiromichi IDA, Manabu YAMAMOTO, Yasumasa SHIGETOMI, ...
1983 Volume 32 Issue 3 Pages
169-173
Published: March 05, 1983
Released on J-STAGE: January 18, 2010
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Various wet digestion methods were examined for the determination of metals in ambient particulates. The recommended procedure was as follows. A given amount of sample was gently heated in a mixture of 10ml of hydrofluoric acid, 20ml of nitric acid and 3ml of hydrogen peroxide and the solution was evaporated to dryness. The residue was dissolved in 10ml of 0.5M hydrochloric acid by heating gently. After filtering insoluble residue off, the filtrate was adjusted to 50ml with 0.5M hydrochloric acid. Metal concentrations were then determined directly on the solution by atomic absorption spectrometry with an air-acetylene flame. For metals of low concentration such as copper, lead, cadmium, and nickel, the metals were extracted with diethyldithiocarbamate in butyl acetate before the measurement. In this case, a large amount of iron present in the sample had to be eliminated beforehand. This was attained by extraction from 10M hydrochloric acid solution with isopentyl acetate. This solvent was found most suitable, because it was free from the formation of emulsion and could be separated quickly from aqueous phase. By the present method, the certified values for NBS SRM-1648 urban particulates matter were satisfactorily reproduced. When hydrofluoric acid was not used, about 22%, 10%, and 9% lower values were observed for iron, manganese, and nickel, respectively.
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Akio OZAWA, Eiko NAKAMURA, Hiroe JIMBO, Takao FUJITA, Aizan HIRAI, Tak ...
1983 Volume 32 Issue 3 Pages
174-178
Published: March 05, 1983
Released on J-STAGE: June 19, 2009
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It has been reported that polyunsaturated fatty acids and their metabolites play a major role in the regula tion of cell function. For the determination of poly unsaturated fatty acids in various lipids of human plasma, platelets, and erythrocyte membrane, we established an improved method using a thin layer chromatography (TLC) for the separation of lipids and a gas chromatography equipped with a glass capillary column. Lipids of plasma, sonicated platelet suspensions, and erythrocyte ghost were extracted with chloroform-methanol solution (2 : 1, v/v) in the presence of butylated hydroxytoluene (BHT) at room temperature for 60min. Their lipids were separated by TLC on silica-gel plates with a solvent system consisting of petroleum ether/ethyl ether/acetic acid (82 : 18 : 1, v/v/v). The areas corresponding to the lipids were detected with the spray of 8-anilino-naphthalene-sulphonic acid ammonium salt (ANS). Phospholipids were extracted from the silica-gel plates with methanol three times, while free fatty acids, triglycerides, and cholesterol esters were extracted with the solution of chloroform-methanol (9 : 1, v/v) three times. Recovery of fatty acid methyl esters from the silica-gel plates were 101.4% for 20 : 4 ω 6, 99.9% for 20.5 ω 3, and 93.1% for 22 : 6 ω 3, respectively. Methyl esters of fatty acids in various lipids were prepared with boron trifluoride and methanol. The fraction of the esters was analyzed by gas chromatograthy using a Shimadzu GC-7APTF gas chromatograph with a hydrogen flame ionization detector. C
23 : 0 was used as an internal standard. Operating condition was as described in a previous paper {A. OZAWA
et al.:
BUNSEKI KAGAKU, 31, 89 (1982)}. Methyl esters were identified using the authentic substances. Reproducibility (C. V. value) of the determination of 20 : 4 ω 6, 20 : 5 ω 3, and 22 : 6 ω 3 in plasma phospholipids of this method were 6.30%, 6.36%, and 5.86%, respectively. As a clinical application of this method, fatty acid distribution in phospholipid fractions of plasma, platelets, and erythrocyte membrane were determined in healthy male subjects who ingested a highly purified ethyl ester of 20 : 5 ω 3 for 4 weeks. A significant increase in 20 : 5 ω 3 was observed in phospholipid fractions of all samples. This newly developed method will be useful for the basic and clinical investigation for its high reliability.
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Hiroyuki NAKAZAWA, Eigo TAKABATAKE, Seiji HINO, Canutte Anthony MTEMA
1983 Volume 32 Issue 3 Pages
179-183
Published: March 05, 1983
Released on J-STAGE: January 18, 2010
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A simple and rapid method for the determination of five anticoccidials in the chicken tissue has been developed by means of high performance liquid chromatopraphy. The acetonitrile extract of sulfamonomethoxine, dinitolmide, ethopabate, sulfadimethoxine, and sulfaquinoxaline from the chicken tissues was concentrated and injected into Unisil QC18 column at 30°C (4.0mm i.d.×150mm). The sufficient resolution was obtained by an isocratic elution using acetonitrile/0.05M phosphate buffer, pH3.0 (20/80) as mobile phase (1.1ml/min). The quantitation was achieved by measuring the wavelength at 250nm and 270nm simultaneously using Hitachi 635M UV monitor. When the tissue was extracted simply by acetonitrile without using Hyflo Super-Cel and the cleanup process on Florisil column, the recovery for each drugs was in the range of 81.9% to 97.8%. By the extraction procedure with acetonitrile, the limits of detection of dinitolmide, ethopabate, sulfadimethoxine, and sulfaquinoxaline in chicken tissues were 0.08ppm, 0.09ppm, 0.14ppm, 0.23ppm, and 0.14ppm, respectively. Thus, the five anticoccidials in chicken tissues were determined simultaneously and rapidly by the proposed HPLC method.
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A new distinguish method between aromatic nuclei and isolated double bonds by infrared spectra
Yoshiaki ISHIDA, Tokio OOSHIMA, Shin-ichi SASAKI
1983 Volume 32 Issue 3 Pages
184-190
Published: March 05, 1983
Released on J-STAGE: January 18, 2010
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Hitherto, the presence of carbon-carbon double bond has been detected by the analysis of NMR spectrum in the computer-assisted systems developed by the present authors. However, it has not always been clearly informed whether the signals appeared in double bond region correspond to aromatic double bonds or isolated double bonds. Thus, a new method to discriminate between aromatic and isolated double bonds in the automated interpretation of IR has been developed. The method or a so-called identifier contained several simple functions and their parameters, and calculated from the observed IR spectrum a probability for the sample to contain aromatic or isolated double bonds. The parameters were empirically determined from the spectra of 247 known compounds. Spectra of 459 aromatic and 488 non-aromatic com pounds were tested using the identifier. Ninety percent of 459 aromatic samples were suggested correctly to contain aromatic rings, and only 17.6 percent of 488 non-aromatic samples were misconceived to be benzenoids. Most of the compounds misconceived contained amino groups. The identifier was applied. satisfactorily to the spectral interpretation of 33 derivatives of phenol and catechol, and 41 compounds with ordinary double bonds.
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Shoji MOTOMIZU
1983 Volume 32 Issue 3 Pages
191-196
Published: March 05, 1983
Released on J-STAGE: January 18, 2010
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The flow streams are propelled by gas pressure in the flow injection system, and 2-nitroso-5-dimethylaminophenol (nitroso-DMAP) is used as the color reagent for iron and cobalt. The signals were detected with a spectrophotometer equipped with a flow cell (18μl). For the determination of iron(II), the reagent and carrier stream solutions were the nitroso-DMAP solution (pH9.2) and 10
-3M sulfuric acid solution respectively, and were flowed at about 1ml/min, and the signals were detected at 750nm. The calibration curve was linear from 2×10
-7M to 5×10
-4M of iron.For the detection of cobalt, the reagent stream and carrier stream solutions were the solution of nitroso-DMAP dissolved in trisodium citrate solution and 10
-3Msulfuric acid solution, respectively. After mixing the reagent stream and carrier stream solutions in the reaction coil, the sulfuric acid solution (4M) was mixed in order to decrease the reagent blank and decompose other metal chelates such as iron, copper and nickel chelates, and the signals were detected at 530nm. The calibration curve was linear from 5× 10
-7M to 6×10
-6M of cobalt. By the proposed FIA system for cobalt, nickel at concentrations of 10
-3M, iron(III) at concentrations of 10
-4M, and iron (II) and copper at concentrations of 5×10
-5M did not interfere with the determination of cobalt, and 0.001% to 0.06% of cobalt in commercially available nickel salts were determined.
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Kunio TAKADA
1983 Volume 32 Issue 3 Pages
197-200
Published: March 05, 1983
Released on J-STAGE: January 18, 2010
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Copper (
xx×10ppm) and silver (0.0
xxppm) in a small amount of tin were determined. A small sample {(0.11) mg} was prepared through cutting of tin ingot with a pair of nippers. A particle of the sample was atomized with an electrothermal graphitecup cuvette in argon atmosphere (3dm
3, /min). Analytical condition for copper was at 2800°C for 45s and for silver at 2500°C for 45s. Under these conditions, tin samples of up to 0.4mg for copper and of up to 1mg for silver were atomized, and the area of absorption signal was measured. As the atomization temperature was high, an aerosol of matrix tin was evaporated. The background absorption (0.010.1 in absorbance) of the aerosol was automatically corrected by polarized Zeeman atomic absorption spectrometer. Calibration curve for copper was constructed with standard solution of copper and for silver with the standard solution of silver together with high purity tin, in which silver content was less than detection limit. The relative standard deviations for copper and silver were (628) %. The detection limits (correspond to twice of the standard deviation of noise) were 0.082 ng of copper and 0.011ng of silver. Those values correspond to copper content of 0.2 ppm (in sample 0.4 mg) and silver content of 0.01ppm (in sample 1mg). One graphite cuvette could be repeatedly employed for atomization procedures of (120200) times. Chemical treatments (dissolution, concentration etc.) for samples were not carried out, so the analytical period of one sample was around 5min.
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Akira KITO, Koji KOMATSU
1983 Volume 32 Issue 3 Pages
201-205
Published: March 05, 1983
Released on J-STAGE: January 18, 2010
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Gas-liquid chromatography of metal chelates was applied to the indirect determination of the cyanideion. The standard procedure was as follows. One ml of a sample solution containing (0.10.5) mg/ml {(100500)ppm} of the cyanide ion was taken into a 15-ml vial (73.5mm × 20.5mm o.d.). To the solution, 1.00ml of an aqueous copper (II) sulfate solution {1.2mg/ml as Cu(II) }, 3.00ml of a buffer solution of 1 M acetic acid-1M sodium acetate (pH6.0), and 1.00ml of a benzene solution containing 27.2mg of 1, 1, 1-trifluro-4-cyclopropy1-2, 4-butanedione {(TFCPBD)H} and 1.8mg of docosane as an internal standard were added. The mixture was shaken for 20min and then allowed to stand for 5min. The resulting Cu (TFCPBD)
2 extracted in benzene was analyzed by gas-liquid chromatography. The coefficient of variation of 2.88% was obtained in fifteen repeated determinations of the cyanide ion in a solution of 0.3mg/ml concentration. Interference of iodide-, sulfide-, and thiosulfate anions, and silver(I), nickel(II), and zinc (II) cations was significant but those of other ions negligible.
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Yukio MINAMI, Toshiyuki MITSUI, Yoshikazu FUJIMURA
1983 Volume 32 Issue 3 Pages
206-209
Published: March 05, 1983
Released on J-STAGE: January 18, 2010
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α-Amino acids were indirectly determined with good precision by atomic absorption spectrophotometry (A.A.S.). Reagent: To 40ml of 70.75mg of Na
3PO
4·12H
20/ml solution is added 20ml of 27.79mg of CuCl
2·2H
2O/ml solution with stirring and then centrifuged at 3000rpm. The supernatant is flowed out by decantation. To the precipitate 60ml of 19.04mg of Na
2B
4O
7·10H
2O/ml solution is added and centrifuged at 3000rpm. And the supernatant is flowed out by decantation. This procedure is repeated twice. To the precipitate 3.01g of NaCl is added and diluted to 100ml with 19.04mg of Na
2B
4O
7·10H
2O/ml solution. Procedure: The aqueous sample solution, containing (25500)μg of α-amino acids, is mixed with 1ml of reagent (diluted to ten times), and then brought to 10ml with water. The mixture is shaken for 30s and standed for 2min. After filtration, the copper content in the filtrate is measured by A.A.S. No detectable interference for determination of α-amino acids with any of the other compounds such as acetaldehyde, ethylamine, sodium acetate, glucose, urea, ammonium nitrate, and sodium phosphate, however, Fe
3+ interfered with the determination of α-amino acids.
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Motohisa FURUSAWA, Masaki TACHIBANA, Yohko HAIBARA, Hiromi AIKAWA
1983 Volume 32 Issue 3 Pages
209-212
Published: March 05, 1983
Released on J-STAGE: June 19, 2009
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It has been reported that the fluorescence intensity of carbazole can be selectively measured by the additions of sodium methoxide, potassium iodide, and methanol to dimethyl sulfoxide solution of the sample. The fluorescence intensities of interfering polynuclear aromatic compounds decreased because the intensities of the interfering substances are quenched by the potassium iodide and the fluorescence maximum of carbazole is shifted to longer wavelength by the ionization with sodium methoxide. In the present investigation, the applicability of this method to the determination of benzocarbazoles was studied. The results indicated that the fluorescence intensity of 5
H-benzo[
b]carbazole was stable and measured without interferences of 11
H-benzo[
a]carbazole and 7
H-benzo-[
c]carbazole. 5
H-Benzo[
b]carbazole could be determined by measuring the fluorescence intensity at 533nm with excitation at 470nm. This method could be applied for the determination of 5
H-benzo-[
b]carbazole in commercial carbazole. The limit of the determination was 0.01%.
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Yasuhisa HAYASHI, Yoshiko YABUTA, Toshiyuki TANAKA, Takayuki NOSE
1983 Volume 32 Issue 3 Pages
212-214
Published: March 05, 1983
Released on J-STAGE: January 19, 2010
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A simple and precise methods for the determination of trace amounts of Cu, Fe, and Zn in lymph were investigated by graphite furnace and "one-drop method" in flame-atomic absorption spectrophotometry (GF-AAS and OD-AAS). Lymph samples were collected from cutaneous leg lymphatic vessels of rabbits by cannulation, and diluted to appropriate concentration of each metal with 0.1N-HNO
3 prior to measurements. Aliquots of 20μl for Cu and 100 μl for Fe and Zn determination were then analyzed by GF-AAS (Cu) and OD-AAS (Fe and Zn). For example, the optimum operating conditions of GF-AAS were as follows: wavelength: 324.8 nm; drying: 150 °C, ramp time: 40s, hold time: 20s; ashing I: 500°C, ramp time: 20s, hold time: 20s; ashing II: 950°C, ramp time: 15s, hold time: 20s; atomization: 2500 °C, hold time: 6s; cleaning: 2600°C, ramp time: 1s, hold time: 3s. The calibration curves for Cu, Fe, and Zn were linear up to 60 ppb, 3.0 ppm, and 0.8 ppm respectively. The detection limit (
S/
N = 3) was 2 pg for Cu, 7 ng for Fe, and 3 ng for Zn. The recovery of Cu added to lymph samples averaged (98 ± 3) % with a relative standard deviation (
n =10) of 1.0 % for 1.0 ng of Cu. The both GF-AAS and OD-AAS methods were applied to the determination of Cu, Fe, and Zn in lymph samples. As the results, the average levels of lymph Cu, Fe, and Zn in 24 healthy rabbits were (0.16
6±0.09
9) (SD)ppm, (0.91
3±0.53
6) (SD) ppm, and (1.45±0.78
1) (SD) ppm, respectively.
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Takayoshi YOSHIMORI, Seiji HAYAMA
1983 Volume 32 Issue 3 Pages
214-217
Published: March 05, 1983
Released on J-STAGE: June 19, 2009
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Since the coulometric titration method of a microamount of water after conversion into ammonia with sodium amide can be used for the analysis of carbon dioxide and oxygen, various impurities in commercial argon were fractionally determined by this method. The apparatus included the furnace of copper and copper (II) oxide, phosphorous pentoxide and cold trap of about-70°C, and these devices were used under various combinations. Carbon dioxide in the samples was determined separately and directly by the non-aqueous microtitration method. Oxygen reacts with sodium amide and produces ammonia. The stoichiometric production ratio between oxygen and ammonia was 3 : 1 in the range of (10100)ppm of oxygen in argon, which was one half of the value shown in literature. Appreciable amounts of impurities could be determined in commercial argon by this method. They were (250940)ppm H
2O, (2036)ppm 0
2, (0.40.8)ppm CH
4, 00.5ppm CO
2, (0.20.4) ppm H
2.
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Tamotsu WASA, Hiroshi YAMAMOTO, Kengo AKIMOTO
1983 Volume 32 Issue 3 Pages
T21-T25
Published: March 05, 1983
Released on J-STAGE: January 18, 2010
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A system control program and automatic data processing for differential pulse anodic stripping voltammetry (DPASV) by using microcomputer-controlled electroanalytical system have been developed, and the performance and applicability of the system were evaluated by comparing the result of data processing by computer with that of manual treatment. The system control program coded by machine language was established by adding sub-program for electrodeposition to the program of differential pulse polarography. The data-processing programs for approximate and fitting methods were developed by using BASIC language in the same manner of differential pulse polarography. The results of the data processing for DPASV with a hanging mercury drop electrode were in good agreement with those of manual treatment. The overall precision of the system for the analysis of metal ions (Pb
2+, Cd
2+ and Zn
2+) in the range 10nM to 250nM was better than (42) % for peak current (
Ip), 1% for peak potential (
Ep), and 5% for half-peak width (
Wp). The data-processing times for approximate and fitting methods were (2030) s/peak and (12) min/peak, respectively.
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Yoshio NARUSAWA, Kunio NAKANO
1983 Volume 32 Issue 3 Pages
T25-T28
Published: March 05, 1983
Released on J-STAGE: June 19, 2009
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Correction for measuring flasks is one of the most essentials in volumetric method of analysis and the correction values were recalculated so as to match the present situation, because they were obtained from data of thermal expansion coefficient of soft glass and density of a balance weight of brass. With data of densities of water from 0°C to 30.5°C with increment of 0.5°, polynomial approximation method with least squares was performed and the polynomial equation for evaluating density of water at desired temperature above 0°C was determined from simultaneous linear eqations. In order to solve the matrix in the least squares method, Gaussian elimination method was applied. It was found that the fifth-order polynomial was sufficient to be used in the calculation. Using these parameters, correction values used in calibrating the volume of measuring flask were calculated, and the correction values for converting the volume at an arbitrary temperature to the volume at the standard temperature (20°C) were calculated for the sake of convenience to be used in preparing sample solutions at arbitrary temperatures.
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Yûetsu DANZAKI, Minoru HOSOYA, Masahiko SASE
1983 Volume 32 Issue 3 Pages
T28-T31
Published: March 05, 1983
Released on J-STAGE: June 19, 2009
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In the determination of phosphorus in tungsten-containing steels by molybdenum blue-spectrophotometry, low analytical values were often obtained when the interfering tungsten was removed by precipitation as tungstic acid. The XPS study indicated that phosphate was adsorbed on tungstic acid and lost on filtration. Phosphorus was satisfactorily determined after separating tungstate by co-precipitation with beryllium hydroxide.
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Masami SHIBUKAWA, Naoichi OHTA
1983 Volume 32 Issue 3 Pages
E53-E60
Published: March 05, 1983
Released on J-STAGE: June 19, 2009
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Sample concentration dependence of the elution behavior of various ions on Sephadex G-10 has been investigated on the basis of the ion partition mechanism presented for inorganic gel chromatography. When the sample ion has the same charge as that of the background eluant coion, sample concentration dependence of the elution behavior was found to be determined by the difference in the affinity for the gel phase between the sample ion and the coion regardless of the type of the counterion, this result being shown to be in good agreement with the prediction derived from the ion partition mechanism presented.
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Avadesh KUMAR, C.L. SETHI, Masatada SATAKE, B.K. PURI
1983 Volume 32 Issue 3 Pages
E61-E67
Published: March 05, 1983
Released on J-STAGE: June 19, 2009
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A new reliable method for the spectrophotometric determination of tellurium(IV) after extraction of its 1-pyrrolidinecarbodithioate into molten naphthalene is developed. Tellurium reacts with 1-pyrrolidinecarbodithioate to form a water-insoluble, thermally stable colored complex which can be quantitatively extracted into molten naphthalene in the pH range of 0.5-2.5. The extracted naphthalene crystals are dissolved in dimethylformamide. The absorbance of the solution is measured at 445 nm. Based on the thermal instability of selenium complex of this reagent, a method is suggested for the simultaneous determination of tellurium and selenium using this technique and the liquid-liquid extraction at room temperature.
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Shunji SAKAMOTO, Noriko SHIBAHARA, Keijiro SAMEJIMA
1983 Volume 32 Issue 3 Pages
E69-E76
Published: March 05, 1983
Released on J-STAGE: June 19, 2009
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An enzyme immunoassay for Δ
1-pyrroline after being converted to 2, 3-trimethylene-4-quinazolone (TQ) through a reaction with o-aminobenzaldehyde followed by chromic acid oxidation is described. The method for determination of TQ is based on chemiluminescence derived from luminol and hydrogen peroxide in the presence of horseradish peroxidase-labeled 6-(β-carboxypropionyl)amino-2, 3-trimethylene-4-quinazolone bound competitively to an immobilized anti-TQ antibody on Sepharose 4B. As little as 10 picomole of Δ
1-pyrroline was successfully determined by this method. The method is applicable to determine some compounds from which Δ
1-pyrroline is quantitatively liberated by a specific chemical or enzymatic reaction. An example of application is shown for determination of spermidine coupled with spermidine dehydrogenase from Serratia marcescens.
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Masashi HOJO, Yoshihiko IMAI
1983 Volume 32 Issue 3 Pages
E77-E80
Published: March 05, 1983
Released on J-STAGE: June 19, 2009
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The half-wave potential (E
1/2) of the anodic wave of acetate ion (AcO
-) shifted more positively in the presence of alkali metal cations (M
+) than in the presence of tetraalkylammonium cations. The difference of E
1/2 was caused by ion-pair formation between AcO
- and M
+. The ion-pair formation constants were roughly estimated by the ΔE
1/2 of anodic wave of AcO
-.
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Toshiyuki OSAKAI, Tadaaki KAKUTANI, Yoshinori NISHIWAKI, Mitsugi SENDA
1983 Volume 32 Issue 3 Pages
E81-E84
Published: March 05, 1983
Released on J-STAGE: June 19, 2009
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The standard Gibbs free energies of transfer of fifteen kinds of alkylammonium ions from nitrobenzene to water, ΔG
Θ, N→Wtr, j, were determined by means of cyclic voltammetry and potential-step chronoamperometry. The ΔG
Θ, N→Wtr, j of the alkylammonium ions has an additive-constitutive property.
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