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Yoshifumi HARADA, Natsuko KURATA, Yoshinori GOTO
1984 Volume 33 Issue 2 Pages
71-76
Published: February 05, 1984
Released on J-STAGE: February 16, 2010
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The separation of bismuth, antimony, and tin from lead by coprecipitation with iron(III) hydroxide has been investigated. The method for decomposition of lead metal, not requiring the redecomposition of antimony and tin precipitates after the coprecipitation, has also been investigated. The following procedure is recommended : Heat and decompose 10 g of lead with 50 ml of mixed acid (perchloric acid 2 : nitric acid 1 : water 2, v/v/v). Add 3 ml of iron(III) perchlorate solution (Fe : 5 mg/ml) and dilute to 100 ml with water. Add 3 M aqueous ammonia solution dropwise with stirring on magnetic stirrer until iron(III) hydroxide precipitates, then adjust pH to 4.04.5 with 0.7 M aqueous ammonia solution. Heat the solution to boil and filter it. Dissolve the precipitate on the filter paper by addition of 8 ml of 6 M hydrochloric acid and wash with about 15 ml of 0.2 M hydrochloric acid. Transfer the solution into a 25-ml volumetric flask, and dilute to the mark with water. And determine bismuth, antimony, and tin by atomic absorption spectrometry. The coefficients of variation for (210) ppm levels of bismuth and antimony, and (50130) ppm levels of tin were below 5%. The detection limits were 0.5 ppm for bismuth and antimony, and 5 ppm for tin. The proposed method is very simple, rapid, and precise, and suitable for the determination of (110) ppm levels of bismuth and antimony, and (10100) ppm levels of tin in lead metal.
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Nobuo SUZUKI, Hiromasa NOMURA, Koichi SAITOH
1984 Volume 33 Issue 2 Pages
76-80
Published: February 05, 1984
Released on J-STAGE: June 30, 2009
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This study has been intended to determine whether polyethylene has useful characters as a stationary phase substance for liquid chromatography. The capacity factors,
k', were determined for acetate esters and benzoate esters on spherical beads of high density polyethylene (diameter,
ca. 20 μm) with water-methanol binary mobile phases. The
k' value for each ester increased with an increase in the volume fraction, φ
w, of water in the mobile phase. Linear relationship was observed between log
k' and alkyl chain length,
nc, of a series of esters. The slope of this relationship was almost equal to that observed on a octadecyl-bonded silica, provided the mobile phase was same. It is concluded that polyethylene has similar character to a octadecyl-bonded silica with respect to the selectivity for at least a series of esters.
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Shurô TAKEYAMA, Minoru HOSOYA
1984 Volume 33 Issue 2 Pages
80-84
Published: February 05, 1984
Released on J-STAGE: February 16, 2010
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Volatility of silicon tetrafluoride compounds was utilized to separation of microgram amounts of silicon in high purity metals. In order to generate silicon tetrafluoride completely without heating, the presence of sulfuric acid about twice amounts of the sample solution was required before addition of hydrofluoric acid. The liberated silicon tetrafluoride was absorbed into a solution containing boric acid by oxygen carrier gas, then silicon in the absorbent was determined by molybdenum blue spectrophotometric method. By this method, microgram amounts of silicon (1 ppm) could be rapidly determined within (4045) min, and the coefficient of variation in determination of 0.0006 % silicon in pure iron was about 6.4 %. Furthermore, the procedure is applicable to silicon in Ga-As semiconductor, and in other metals.
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Masayuki KIUCHI, Masahiro HORI, Yositaka KOBAYASHI
1984 Volume 33 Issue 2 Pages
85-89
Published: February 05, 1984
Released on J-STAGE: February 16, 2010
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A spectrophotometric method for determination of nitrogen dioxide with chloroform was studied to solve the problem of the reaction factor in Saltzman method. A chloroform absorption solution contains 0.2% aniline, 10% acetic acid and 1 g/l 2-naphthylamine. Sample air was aspirated at the flow rate below 400 ml/min through the bubbler filled with 20 ml of the absorption solution. The bubbler is a glass vessel of 30 ml which has a sintered glass filter with a pore size of 0.1 mm to 0.12 mm. At the conclusion of the sampling the volume of the sample solution was made 20 ml by the addition of the absorption solution, and the absorbance was measured at 440 nm after it was allowed to stand for 20 min. The reaction factor was constantly 0.98 below 90 ppm of nitrogen dioxide, and its coefficient of variance was 3%. The determination limit of nitrogen dioxide was 0.02 ppm at a sample size of 20 l. The merit of this method is that the reaction factor is independent of concentration of nitrogen dioxide in a sample air and the absorbing conditions. The concentration of nitrogen dioxide in the urban air measured by the proposed method agreed with that done by Saltzman method of which the reaction factor was subsequently determinde with the standard gas close to the concentration of the sample air.
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Soichi OTSUKA, Takahiro YAMAMOTO, Kazuhiko SAKAMOTO, Issei IWAMOTO, Na ...
1984 Volume 33 Issue 2 Pages
90-94
Published: February 05, 1984
Released on J-STAGE: June 30, 2009
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Nitric oxide impurity in purified air and high purity nitrogen gases, which causes uncertain errors in setting zero level of a nitrogen oxides analyzer, was determined with a newly developed computer-controlled second derivative spectrometer. In the spectrometer the second derivative of UV and visible absorption spectra was measured according to wavelength modulation method using a calcium fluoride plate, and smoothed by third order polynomial approximation method. Nitric oxide was determined with a multi-reflection cell (50 cm) of flow type under following conditions : sample flow rate 1l/min, wavelength range (210220) nm, scanning step 0.1 nm, frequency of wavelength modulation 12 Hz, amplitude of wavelength modulation 0.8 nm, slit width 0.2 mm, optical path length 10 m, and number of data accumulation 5000. As a result, contents of nitric oxide were found to be (1.3±1.1) ppb at a 95% confidence level in purified air prepared as a zero gas through a zero gas generator, and (3.3 ± 1.0) ppb and (3.1 ± 1.0) ppb in commercially available two grades of high purity nitrogen gas. These are less than half of literature values, but can not be neglected in accurate measurements of nitric oxide at ppb level.
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Kazutoshi TANABE, Jiro HIRAISHI, Tadao TAMURA, Osamu YAMAMOTO, Masaru ...
1984 Volume 33 Issue 2 Pages
95-98
Published: February 05, 1984
Released on J-STAGE: June 30, 2009
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The efficiency of the combined search by IR,
13C-NMR, and MS spectral data was examined in comparison with that of the simple search by data of one kind of spectrum. The search file was created from peak data for 933 kinds of compounds, which were compiled in the SDBS data bank of NCLI. The search was tested by peak data of the strongest peak stored in the search file as the input data, and the results of 933 test searches were totaled. If a spectrum in the search file had a peak corresponding to the input peak within the allowance values of 10 cm
-1, 1 ppm, and 0
m/z for IR,
13C-NMR, and MS, respectively, the spectrum was judged as being accepted and its score as a measure of the coincidence of spectra between the input and the search file was computed by
S=
NfΣf
IsIf-(Σs
Is) (Σf
If)/[
NfΣs
Is2-(Σs
Is)
2]
1/2[
NfΣf
If2-(Σf
If)
2]
1/2 × 100
where
Nf is the number of peaks in the search file,
Is the intensity of the input peak,
If the intensity of the file peak, Σs the summation over the input peaks, and Σf the summation over the file peaks. Error answers showing scores higher than the score of the correct answer minus 10 points were judged as the search noises, and their rates were counted. The percentages of the search noises were averaged for 933 test searches. As a result, it was found that the combined search by all kinds of spectral data decreased the search noises one figure or more compared with the simple search by only one kind of spectral data.
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Katsurou YAMADA, Mamoru AOYAMA, Toshiyuki HOBO, Shigetaka SUZUKI
1984 Volume 33 Issue 2 Pages
99-103
Published: February 05, 1984
Released on J-STAGE: June 30, 2009
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An ion flotation-spectrophootometric method has been developed for the determination of trace amounts of iron ion in natural waters. Iron(III) ion in the sample (1000 ml) was reduced to iron(II) ion, which was then reacted at pH 46 with 1, 10-phenanthroline (phen) to give a chelate ion [Fe(phen)
3]
2+. The solution was poured into a foam separator where the chelete was floated by using sodium lauryl sulfate (SLS) as the counter ionic surfactant. Nitrogen bubbling gas flow rate was 147 ml min
-1, the flow rate of 1% SLS aqueous solution was 0.335 ml min
-1 and separation time 15 min. The foam coming out of the cell was subsided into a small foam collector which contained 2 ml of 1-propanol as the foam breaker. The collected solution was diluted to 10 ml and initial iron ion content was determined by measuring its absorbance at 510 nm. The calibration graph was linear in the iron ion concentration range of (3 × 10
-86 × 10
-7)M. After examined the effect of foreign ions, the proposed method was applied to the determination of iron ion in water samples.
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Tomiki TAKAHASHI, Sumio OHOKOSHI, Nariko SHINRIKI, Toshio SATO
1984 Volume 33 Issue 2 Pages
104-107
Published: February 05, 1984
Released on J-STAGE: June 30, 2009
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Gas chromatographic determination of hydrogen isotopes D
2 and HD has hitherto been carried out with a molecular sieve column kept at -195°C under the H
2 carrier gas. However, the amount of D
2 in hydrogen gas containing low HD concentration of less than 5 % can be practically neglected judging from the equilibrium constant of H
2-D
2exchange reaction. Therefore, there is no need to separate HD from D
2. As an improvement, in this paper, the gas chroma tographic determination of HD in low concentration (<5%) was carried out by maintaining the temperature of the molecular sieve 13X column at room temperature. Since HD passed freely through the column under this condition, rapid analysis became possible. Moreover, the use of ultra pure H
2 as a carrier gas enabled us to enhance the cell current of TCD drastically, hence gave rise to high sensitivity of HD detection. The limit of determination of the concentration of HD was 0.01%. In the case of the higher concentration (>5%) of HD in hydrogen gas, D
2 and HD have been separated and determined by the method described above, but this method takes more than ten minutes. Therefore, we designed a new gas chromatographic analysis of the HD-D
2 mixture with an activated alumina column at -195 °C under the H
2 carrier gas (330 ml/min). The advantages of this method are in (1) rapid analysis (in 1 min), (2) no need of the rigid activation temperature {(110250) °C}, (3) no change of the relative molar sensitivity of HD to D
2 at the various flow rates of H
2 carrier gas {(100300) ml/min}.
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Bunichi EZAKI, Mikihiko SAITO, Toshiaki IMAMURA, Kenyu KINA
1984 Volume 33 Issue 2 Pages
108-110
Published: February 05, 1984
Released on J-STAGE: February 16, 2010
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The negatively charged values of agar-agar for electrophoresis were determined by colloid titration. Anionic residues such as sulfate and carboxylate in agar-agar are responsible for electroendosmosis which causes poor resolution of migration pattern. Therefore, the measurement of negatively charged value is important for characterization of agar-agar for electrophoresis. Commercially available agar-agar is dried at 70 °C for 3 h in a vacuum. A 25 mg of the sample is accurately weighed and dissolved in hot water. To this solution, 10 ml of N/1600 polydiallyl dimethyl ammonium chloride are added and the solution is titrated with N/1600 potassium polyvinyl sulfate at 50°C in order to prevent the gellation of agar-agar. The end-point is indicated by a color change of toluidine blue from blue to red. Electroendosmosis was measured by comparison of the mobilities of BSA and starch.
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Takeshi YAMANE, Mikito KAMIJO
1984 Volume 33 Issue 2 Pages
110-112
Published: February 05, 1984
Released on J-STAGE: June 30, 2009
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A flow injection system is proposed for the rapid and simple determination of total water hardness with spectrophotometric detection. The method is based on the exchange reaction between calcium in the sample and the magnesium complex of EDTA at a medium of pH 10. Change in the absorbance of Hydroxynaphthol Blue (HNB), owing to the complex formation of HNB with magnesium, is measured spectrophotometrically at 645 nm for determining the sum of magnesium in the sample and magnesium liberated by this exchange reaction. A linear relationship was observed between the water hardness up to 103 mgCaCO
3/l and peak height. This system allows the analysis of
ca. 80 samples per hour with the relative standard deviation of (0.92.4)%. The results for analysis of tap and river waters agreed well with those obtained by standard EDTA titrations. Sample size injected is as little as 20μl for single analysis and no complicated manipulation is required.
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Shigeroku YAMAGUCHI, Katsuya UESUGI
1984 Volume 33 Issue 2 Pages
112-116
Published: February 05, 1984
Released on J-STAGE: June 30, 2009
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An extraction-spectrophotometric method for the determination of cobalt(II) using 2-hydroxy-1-naphthaldoxime(HNA) was studied. Cobalt(II) reacts with HNA to form a water insoluble complex in aqueous solution in the pH range of 8.39.2, which can be extracted quantitatively into ethylacetate and has an absorption maximum at 387 nm. The cobalt complex in ethylacetate was stable and showed molar absorption coefficient of 1.17 × 10
4 dm
3 mol
-1 cm
-1. Under the optimum conditions, the colored system obeyed Beer's law over the range of 050 μg of cobalt (II) in 10 ml of ethylacetate. The sensitivity was 5.1 × 10
-3 μg Co(II)/cm
2 for 0.001 absorbance, and the coefficient of variation was 0.93% in six determinations. The recommended procedure is as follows : take an aliquot of sample solution containing up to 50 μg of cobalt(II) to a 50 ml separatory funnel. Add 10 ml of borax buffer solution (pH 8.8), and dilute with water to about 30 ml. Then add 10 ml of 0.01 M HNA ethylacetate solution and shake vigorously for 10 min. Filter the organic phase through a dry filter paper and measure the absorbance at 387 nm against reagent blank. Copper (II), iron(III), and nickel(II) seriously interfere with the determination of cobalt(II).
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Shoji MOTOMIZU, Hiroshi MIKASA, Mitsukom OSHIMA, Kyoji TÔEI
1984 Volume 33 Issue 2 Pages
116-119
Published: February 05, 1984
Released on J-STAGE: June 30, 2009
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Continuous flow method was examined for the determination of phosphorus. The molybdophosphate formed between orthophosphate and molybdate in hydrochloric acid medium diminished the fluorescence of Rhodamine 6 G. Carrier solution (distilled water) and reagent solution were propelled by double plunger pump P
1 and P
2 (flow rate : 0.98 ml/min), and sample solution(160μl) was injected into the carrier stream. The two streams were mixed in 20 cm long Teflon tubing (1 mm i.d.), and the mixture was flowed through a flow cell(18μl), at which the fluoresence of Rhodamine 6 G was detected(λ
ex =350 nm, λ
em=580 nm). The reagent solution consists of 0.035 M molybdenum and 1 × 10
-5 M Rhodamine 6 G in 0.8 M hydrochloric acid. Co-existing ions generally existing in river and sea waters did not interfere the determination of phosphorus. The calibration curve was linear from 0 to 45 ppb of phosphorus. The method was applied to sea water. The sampling rate was 20 samples per hour.
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Ikuo SAWATANI, Mitsuko OSHIMA, Shoji MOTOMIZU, Kyoji TÔEI
1984 Volume 33 Issue 2 Pages
119-121
Published: February 05, 1984
Released on J-STAGE: June 30, 2009
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Cobalt was spectrophotometrically determined as an anionic metal complex of 2-nitroso-1-naphthol-4-sulfonic acid (nitroso-NW acid) on a reversed-phase high-performance liquid chromatograph. An ODS column(4.6 mm i.d. × 100 mm) was used, and the mobile phase consisted of 1.4 × 10
-2 M tetrabutylammonium bromide and phosphate buffer (pH 8, 5 × 10
-3 M) in a mixture of 52 vol% methanol and 48 vol% distilled water. To 7.5ml of sample solution, 1 ml of citrate buffer solution(2 M, pH 5.4) and 1 ml of nitroso-NW acid(4 × 10
-3 M) were added. After 10 min, 0.5 ml of 2 × 10
-3 M EDTA was further added, and the resultant solution was diluted to 10 ml with distilled water. One hundred μl of the solution was injected on to the column. Detection was made on a UV detector at 368 nm. The calibration curve was linear in the range of (125) × 10
-7 M of cobalt. By the proposed method, cobalt contents in four commercial nickel salts, Ni(NO
3)
2 · 6H
2O, NiSO
4 (NH
4)
2SO
4 · 6H
2O, NiSO
4·6H
2O, and NiCl
2·6H
2O, were determined to be (0.0030.06)% with relative standard deviation of 1.3% (seven determinations of the nitrate salt).
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Mitsuo IKEDA, Kenji SHIMADA, Ushiho MATSUMOTO
1984 Volume 33 Issue 2 Pages
122-123
Published: February 05, 1984
Released on J-STAGE: June 30, 2009
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A procedure for high-performance liquid chromatographic (HPLC) determination of picomole levels of arachidonic acid (AR) and eichosapentaenoic acid (EPA) has been developed by using 9-aminophenanthrene as a fluorescence prelabeling reagent. The correlation coefficients between the proposed method and a routine gas chromatographic and a UV labeling HPLC methods were determined. An adequate correlation was observed between the present method and the other two methods. The recovery test of AR and EPA added to a human plasma for the proposed method showed the satisfactory results for both fatty acids.
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Hisako SUZUKI, Hiroko MINAMI, Kimiko ABE, Hiromi HIRAIWA, Tetsuo UCHID ...
1984 Volume 33 Issue 2 Pages
T5-T9
Published: February 05, 1984
Released on J-STAGE: February 16, 2010
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Some methods of sample decomposition were applied and compared each other for the determination of eight elements in Chinese cabbage. After the mixing of frozen sample with water in a kitchen mixer, the representative aliquots of sample suspension were served for such pretreatments as dry ashing in an electric furnace, wet digestion with nitric acid and hydrogen peroxide, sealed Teflon vessel method (I and II) with nitric and perchloric acids, and leaching with hot and dilute hydrochloric acid. Sodium and potassium were measured by flame emission spectrometry. Magnesium, calcium, copper, iron, manganese, and zinc were measured by atomic absorption spectrometry by one-drop method. The leaching method with hydrochloric acid gave good analytical results in accuracy and reproducibility except for iron. The method can be recommended for a practical use because of its easy and simple operation and low cost.
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Ikuo HAYASHI, Hideo HARA, Yoichi GOSHI
1984 Volume 33 Issue 2 Pages
T9-T13
Published: February 05, 1984
Released on J-STAGE: February 16, 2010
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Rapid determination of gallium in silicon-germanium-gallium alloy was investigated by inductively coupled plasma emission spectroscopy (ICP-ES). Two methods, with and without germanium separation, were studied. A sample of (0.60.7)g was dissolved with 10 ml of hydrofluoric acid and 10 ml of nitric acid. After addition of 5 ml sulfuric acid (1+1), the sample solution was evaporated to fumes to expel excess hydrofluoric acid. Although precipitation of germanium dioxide was occurred then, the precipitate was dissolved by adding 4 g of oxalic acid and heating. The residual fluoride ion was masked with 0.5 g of boric acid. The solution was transferred into 100 ml volumetric flask and diluted to the mark with water and 294.4 nm emission was measured by ICP-ES. The coefficient of variation was better than 3.5 % for 0.5 % to 5 % of gallium in alloy. This method is more simple and rapid than the other method which needs complicated filtration of the precipitate of germanium dioxide.
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Yoshio KOSUGI, Hideyuki KONISHI
1984 Volume 33 Issue 2 Pages
E47-E53
Published: February 05, 1984
Released on J-STAGE: June 30, 2009
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13C NMR data of eleven sodium alkanesulfonates in deuterium oxide have been obtained. Simple equations for prediction of chemical shifts have been derived. Maximum deviation between observed and predicted values is ± 0.8 ppm. Substituent effect of sulfonate group on α-carbon is much larger than the degree predicted by linear relationship with electro-negativity of 1-substituted alkanes. On the other hand, β-effect is not much variable with kinds of substituents, but comparatively smaller effect is found for sulfonate group. Thus the difference between the effect on α- and β-carbon caused by sulfonate group is larger (about 36 ppm), which is contrasted with the effect of, for example, methyl group (0 ppm).
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Boron Chelates and Boron-Metal Chelates XIV
Eberhard HOHAUS
1984 Volume 33 Issue 2 Pages
E55-E60
Published: February 05, 1984
Released on J-STAGE: June 30, 2009
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The “reversed-phase” thin-layer chromatography (plates:silica gel 60 silanized, mobile phase:methanol/water, 80:20, v/v) is more suited for the separation of primary n-alkylamines after their derivatization into 3-alkyl-2, 2-diphenyl-1-oxa-3-azonia-2-boratanaphthalenes than the method using thin-layer plates of silica gel 60 and benzene/chloroform (80:20, v/v). The quantitative analysis of amine mixtures is achieved by in situ fluorimetry of the developed chromatogram. With a limit of detection of 30 ng/8 μl for n-hexylamine, this method allows the quantitative determination of, e.g., 162 ng in 8 μl sample volume with a standard deviation of ± 7 ng hexylamine. The separation and quantitative analysis of decylamine from river water, containing amines, is described here.
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Noriko NAKAMURA, Toshio KINOSHITA, Kazuyo MURAYAMA, Fumio IINUMA
1984 Volume 33 Issue 2 Pages
E61-E65
Published: February 05, 1984
Released on J-STAGE: June 30, 2009
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DNA and RNA were found to enhance the fluorescence of dansylprotamine. This finding was applied to microdetermination of nucleic acids. This method is valid for samples containing 0.1 - 5.0 μg/ml of nucleic acids. Nucleic acids and dansylprotamine were found to bind each other through both electrostatic and hydrophobic interaction.
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Bernd Wenclawiak, Friedrich Bickmann
1984 Volume 33 Issue 2 Pages
E67-E72
Published: February 05, 1984
Released on J-STAGE: June 30, 2009
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Reversed phase and normal phase LC-separation of all noble-metal-8-hydroxyquinolinates (oxinates) have been made. The chelates were derivatized using a pre-column technique with an under-water-melt procedure. With detection at 254 nm less than 5 ng and less than 20 ng in the VIS-range at 396 or 435 nm of each metal can be detected. For Ru-, Ir-, Rh-oxinates it is preferable to use a NP-Si 60 7μm analytical column eluted with CHCl
3:THF = 3:2, and for Pd-, Ru-, Os-oxinates a RP-C18 5-20 μm analytical column, with MeOH: Buffer (pH4.6) : CHCl
3 = 57.5 : 30 : 12.5 vol.% and 2.5×10
-4M oxine in the eluent. The elution order in NPLC is inverted for Rh- and Os-oxinate from that observed in RPLC.
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Satoshi KAWAI, Chie TSUTSUI
1984 Volume 33 Issue 2 Pages
E73-E76
Published: February 05, 1984
Released on J-STAGE: June 30, 2009
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A new method for the fluorometric determination of hydrogen peroxide is described. The method is based on the combination of catalase reaction and the Hantzsch Reaction. The fluorometric characters of the Hantzsch Reaction were investigated using three reagents, acetylacetone, ethyl acetoacetate and methyl acetoacetate. Then methyl acetoacetate was found to be the best of the three reagents.
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Kousaburo OHASHI, Katsumi YAMAMOTO
1984 Volume 33 Issue 2 Pages
E77-E80
Published: February 05, 1984
Released on J-STAGE: June 30, 2009
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Solvent extraction of molybdenum(V) with ethylxanthate and diphenylcarbazone (HDPCO) was investigated. When the perchloric acid concentration was above 0.2 mol dm
-3, a 1.32 × 10
-4 mol dm
-3 molybdenum(V) was completely extracted with 1.39 × 10
-2 mol dm
-3 ethylxanthate into chloroform. The extracted species contained molybdenum and ethylxanthate in a 1 : 2 molar ratio. Solid dark green complex formulated as Mo
2O
3(C
2H
5OCS
2)
4 was prepared. One molybdenum-oxygen-molybdenum bond in Mo
2O
42+was suggested to be cleaved on the coordination of ethylxanthate. The optimum pH for the extraction of molybdenum(V) with HDPCO was 2.2, 2.7 and 3.8 for chloroform, nitrobenzene and n-butylacetate, respectively. The complex extracted was formulated as Mo
2O
3(DPCO)
4. Two molybdenum (V) atoms are bridged with one oxo group.
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