BUNSEKI KAGAKU
Print ISSN : 0525-1931
Volume 27, Issue 11
Displaying 1-20 of 20 articles from this issue
  • Setsu KOBAYASHI
    1978 Volume 27 Issue 11 Pages 675-680
    Published: November 05, 1978
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A study was made on the metallographic effect on spectrographic analysis of cast iron for silicon and an analytical method without the influence was found out. A cylindrical rod of chilled casting which was solidified in unidirection from the chilled side was devided into two parts vertically. It was found by means of a microscope that the metallurgical structure of the cross section of the sample varied successively with distance from the chilled side. Then, silicon in the sample was determined at the positions on the cross section 10, 20, 30, 40 and 55 mm form the chilled side as follow; the sample was excited by high voltage spark discharge with a graphite electrode and an analytical line pair, Si I 2516.123Å/Fe II 2714.142 Å was used. When discharged in air, spectral line intensity ratio was stronger to a certain extent as apart from the chilled side, although silicon content was uniform in the sample. On the other hand, when discharged in argon, there was the intensity ratio in the same level at every position and its reproducibility was desirable. From these results, it was expected for metallic matrix to have no influence on the intensity ratio, if sparked in argon. Actually, for the chilled casting sample, gray cast and ductyle iron having indistinct metallurgical history, spectrographic results calibrated by the use of NBS standard samples were in good agreement with chemical results.
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  • Yoshifumi AKAMA, Hideaki NAKA, Toshio NAKAI, Fumikazu KAWAMURA
    1978 Volume 27 Issue 11 Pages 680-683
    Published: November 05, 1978
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    4-Capryl-3-methyl-1-phenyl-5-pyrazolone (CMPP) forms extractable chelates with many metals and is very stable in acid or ammoniacal solution compared with other similar reagents. A method is described for the determination of a micro amount of lead, using atomic absorption spectrophotometry in conjunction with solvent extraction technique. The effect of pH, amount of CMPP, diverse ions in the aqueous phase and shaking time on the extraction of lead were examined. Less than 250 μg of lead was quantitatively extracted into 5 ml of 0.3% (w/v) CMPP-MIBK solution from an aqueous solution at pH 10, by shaking for 5 min, and then the absorbance was measured with an atomic absorption spectrophotometer. More than 10 μg of Fe3+ caused a negative error, but 10 mg of Cd2+, Ni2+, 0.3 g of Zn2+, 1 g of Cu2+ did not interfere. The present method was applied to the determination of a micro amount of lead in high-purity zinc and copper. Copper {(1020)g} and zinc {(46)g} samples were dissolved in HNO3 and HCl by heating. When extracting lead, the sample solution was adjusted to pH 10 with ammonium hydroxide, because these matrices could be masked as copper or zinc ammine complex. The analytical results by the proposed method almost agreed with the values obtained by emission spectrophotometric method or spectrophotometric method.
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  • Masao SUGAWARA, Goro HANAGATA, Tomihito KAMBARA
    1978 Volume 27 Issue 11 Pages 683-687
    Published: November 05, 1978
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Cadmium (II) reacts with 8-quinolinol-5-sulfonic acid (H2qs) in weakly alkaline media and forms a chelate anion, which is extracted into xylene as an ion-pair with a cation of trioctylmethylammonium iodide (QI). The ternary complex has an absorption maximum at 405nm and the absorbance is constant in the pH range from 8.9 to 9.2. The composition of the complex is estimated to be [Cd2+(qs2-)2(Hqs-)-(Q+)3]0.The recommended procedure is as follows. To a cadmium (II) amount of (5.645.0)μg is added 5 ml of 1 M potassium iodide solution. The solution is diluted to 50 ml with water and shaken with 10 ml of 1% QI-xylene solution. The organic layer is washed twice with water and is transferred into a beaker containing anhydrous sodium sulfate to dehydrate. Then, a 5-ml portion of the extract is taken into another separatory funnel. After addition of 2 ml of 0.01 M NaHqs solution and 10 ml of borax-KH2PO4 buffer solution (pH 9.1), the mixture is shaken for 5 min and allowed to stand for 5 min. The organic layer is dehydrated as above and subjected to optical measurements after 30 min. Beer's law holds for cadmium (II) in (0.524.19)μg per ml of the extract with the molar absorption coefficient of (1.04±0.08)×104 cm-1 mol-1 dm3. Lead(II) and bismuth(III) interfere with the determination.
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  • Fumio KUSANO, Hitoshi KAWASAKI, Katsuhiko ITADANI, Kazuyoshi HAGIWARA
    1978 Volume 27 Issue 11 Pages 687-692
    Published: November 05, 1978
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Pure gum and filler-loaded compounds were prepared. One gram of its vulcanizates was extracted with acetone for 8 h. To the extract were added methanol (10 cm3), pyridine (2.5 cm3), [2M aqueous ammonia+2M ammonium chloride] (5 cm3), and acetone to make a solution of final 25 cm3. The ac polarographic peak potential for MBI was about -1.2V vs. S.C.E. in the region of (0.53)×10-4M. The peak height of the wave was proportional to the concentration of MBI in the same region. By this method, the recovery variation coefficient of MBI was 2.2% for 7 determinations. The determination was not interfered by dibenzothiazyle disulfide (I) or tetramethylthiuram monosulfide (II) compounded in vulcanized rubber. The variation coefficient was 3.7% of I and 2.6% of II, respectively, when (0.13)μg of each ingredient were added. In the case of vulcanized rubbers, the data of MBI in comparison with the MBI compounded were (4060)%. Its values were influenced by fillers.
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  • Toshio KUBOTA, Toshio UEDA
    1978 Volume 27 Issue 11 Pages 692-696
    Published: November 05, 1978
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    An atomic absorption spectrophotometric method for sensitive and precice determination of antimony has been studied-being reduced to antimony-hydride (stibine) by sodium borohydride solution. The apparatus used for stibine generation consists of the reaction flask, magnetic stirrer, gas-reservoir and U-shaped drying tube. Stibine in the gas-reservoir is subsequently introduced into an argon supported hydrogen flame and determined by atomic absorption spectrophotometry. A flexible bag (TEDLAR bag) with two mouths for the gas-reservoir results in good reproducibility of stibine generation. Some suppressive effects by diverse ions are found to. be almost entirely eliminated, when the prereduction procedure using hydrazine sulfate was combined with sodium borohydride reduction. With the prereduction procedure are not found interferenes, up to 500-fold excess of Mn (VII), Cr(VI), Fe(III). A calibration curve obtained shows linear up to 1μg-Sb. The detection limit is 0.02μg-Sb and coefficient of variation in the determination of 1μg-Sb is 2.3 in 20 runs. This method was applied to the analysis of N. B. S. Standard Reference Material (SRM-1575) and water samples with satisfactory results.
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  • Chozo YOSHIMURA, Kiyoshige MIYAMOTO
    1978 Volume 27 Issue 11 Pages 697-701
    Published: November 05, 1978
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Oxidimetric determination of the terpenes (citral, citronellol, geraniol, nerol and perillartine) with manganic salt and bromine in DMF was investigated. The solution of {Mn (III) salt +phosphoric acid} in DMF and those of bromine in DMF were found to be stable. Citral was treated with manganic salt dissolved in DMF containing 45% of anhydrous phosphoric acid at 25°C for 40 min. Perillartine was treated in DMF containing 25% of the same acid at 45°C for 20 min. Determination of citral and perillartine was carried out with manganic salt by using the above conditions. Citronellol, geraniol and nerol were determined with bromine in DMF. A reactive ratio of terpenes and manganic salt was observed at 1:2, and inflection points at 2:1, 1:1 and 1:2 were obtained by using bromine as a standard solution. The addition of magnesium chloride was effective to simplify and clarify the inflection points.
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  • Tadashi KIKUCHI, Shigeharu FUJI, Keiichi FURUYA, Masahiko TSUCHIYA
    1978 Volume 27 Issue 11 Pages 701-706
    Published: November 05, 1978
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    In the conventional methods for mass analysis of a mixture of nitrogen and carbon monoxide, it is usually required to solve simultaneous equations owing to the effect of multiplication of N+ and CO2+ ions at m/e=14, otherwise, a high mass resolution mass analyser to be used. In the present study, simultaneous measurement of nitrogen and carbon monoxide extracted from metals was developed with a combination of a vacuum fusion furnace and a conventional low resolution (mm= 56 at m/e= 28) quadrupole mass analyser without any modifications in the ionization chamber such as an additional repeller electrode. The behavior of mass spectra of nitrogen and carbon monoxide was investigated under various ion accelerating voltages. Only ions which have excess kinetic energy were detected at 0 V of ion accelerating voltage, hence an interference of CO2+ for N+ at m/e=14 was eliminated when carbon monoxide less than 3.6×10-2 ml (STP) was introduced. The relationships between peak intensities of N+, C+, and O+ and the concentration of nitrogen and carbon monoxide were linear over the range of 0.1×10-2 to 3.0×10-2 (STP). By measuring gas extraction curves with programmed temperature {(1020) °C/min}, N+, C+ and O+ ion peaks showed characteristic behavior which gave informations on the states of nitrogen and oxygen in the samples, respectively. The gas extraction curves of metallic chromium and one of the constituents, chromium nitride (Cr2N), were demonstrated.
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  • Tadao HATTORI, Yukio WASHIO, Masahide INOUE
    1978 Volume 27 Issue 11 Pages 707-711
    Published: November 05, 1978
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    A spectrophotometric method for the determination of chlorpheniramine maleate (MCP) by solvent extraction with zincon has been established. MCP is extracted as a 1 : 1 ion association complex with zincon in the organic phase, and determined by measuring absorbance of the extract at 530 nm. The absorbance of the extract showed to be linear over the concentration range of (1.0×10-51.0×10-4) M MCP in aqueous solution. Assay method is as follows: One ml of a sample solution containing (1.05.0)×10-4 M MCP is taken in a test tube and 5 ml of acetate (0.1 M) buffer (pH 4.6), 1 ml of zincon solution (1.0×10-3 M) and 3 ml of water are added. This solution is shaken with 5 ml of dichloromethane for 3 min. The extract is filtered through a dry filter paper to remove water. The absorbance is measured at 530 nm against either a reagent blank or water. The method proposed has high sensitivity and is applicable to the determination of MCP in drug preparations.
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  • Kenjiro HAYASHI, Yoshiaki SASAKI, Shoji TAGASHIRA, Eriko YAMATE
    1978 Volume 27 Issue 11 Pages 712-716
    Published: November 05, 1978
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Manganese (II) ion could be extracted with methyl isobutyl ketone (MIBK) in the presence of a large excess of potassium ethylxanthate (potassium O-ethyl dithiocarbonate, Ketx). The distribution ratio of manganese, D, was affected by the factors of pH, the concentration of etx-, and the kinds and/or concentrations of coexisting cations in the aqueous phase. Manganese (II) was extracted quantitavely under the following conditions: pH of (8.09.2), [Ketx] of 0.6 mol dm-3 or above. The relationship between log [etx-] and log D, gave a straight line with the slope equal to 3. Consequently, the extracted species contains manganese (II) and etx- in the mole ratio of 1:3. The solid yellow Mn-etx complex was synthesized by the addition of a 3 mol dm-3 solution of manganese sulfate into a 4 mol dm-3 solution of Ketx at the temperature below 5°C. The crystal of this complex, which was recrystallized with a mixed solvent of ethanol and diethylether (1:1) had the composition of K [Mn (etx)3], being modelately soluble in water and very soluble in MIBK. The solid complex was unstable in air. The visible absorption spectra of the MIBK solution of the synthesized complex coincided with that of the MIBK extract from the aqueous solution. From these results, the extracted species with MIBK is expected to be K [Mn (etx)3].
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  • Junko SHINOHARA, Ryota SHINOHARA, Shuichi ETO, Teiji HORI
    1978 Volume 27 Issue 11 Pages 716-722
    Published: November 05, 1978
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Micro determination of 2-mercaptobenzothiazole (2-MBT) in water and sediment samples was studied. After 11 of a water sample was adjusted to pH 34 with 1 M hydrochloric acid, 2-MBT was extracted with 50 ml each of dichloromethane twice. In case of sediment samples, 200 ml of distilled water was added to a sample, and the pH of the solution was adjusted to 1011 with 1 M sodium hydroxide. The mixture was filtered after vigorous shaking for 10 min. The filtrate was washed with 50 ml of dichloromethane to remove neutral and basic organic substances. 2-MBT was extracted twice with 50 ml each of dichloromethane after the pH of the aqueous layer being adjusted to 34 with 1 M hydrochloric acid. The extract was dried through an anhydrous sodium sulfate column and concentrated to 1 ml with a KD evaporator under atmospheric pressure. The concentrated sample was further reduced to 0.1 ml with nitrogen gas stream. 2-MBT was methylated with dimethyl-formamide diacetal for 15 min at 60°C to 2-methyl-mercaptobenzothiazole (2-MMBT) and 2-MMBT was determined by gas chromatography with a flame photometric detector. Recoveries of 2-MBT for a water sample were 75% and 40% at 100μg and 1 μg added to samples, respectively. For determination of 2-MMBT, dibenzothiophene was used as an internal standard. Detection limits of 2-MBT in a water sample (11) and sediment sample (20 g) were 0.04 ppb, and 2 ppb, respectively. This method was applied to some environmental samples. 2-MBT was detected in the range of (4.644)ppb in river sediment samples, but not detected for the water samples and marine sediment samples examined.
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  • Chozo YOSHIMURA, Hiroshi ANDO
    1978 Volume 27 Issue 11 Pages 722-725
    Published: November 05, 1978
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    The suppressive effect on the polarographic maxima was observed by dispersing carbon black in the sample solutions of antimony (V) chloride, tin (IV) chloride and thallium (I) chloride in dimethylformamide. Carbon blacks {Excellsior (20 nm), # 600 (14nm) and Corax-L (23 nm)} was dispersed by a ultrasonic irradiation method. Optimum dispersion range of carbon black was (0.150.8)%. It was observed from the polarograms of the investigated metal ions that the suppressive effect of maxima was not affected by the kind of supporting electrolyte. The reduction waves of the surface functional group and the other metal ions on carbon black were not observed in blank test.
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  • Hiroshi ONISHI, Hideko KOSHIMA
    1978 Volume 27 Issue 11 Pages 726-729
    Published: November 05, 1978
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Re-examination of conditions for the photometric determination of chromium (VI) with diphenylcarbazide gave the following results: a suitable sulfuric acid concentration, 0.02 to 1.0 N; a suitable volume of 0.25% diphenylcarbazide solution, 0.5 to 2.0 ml per 25 ml of final solution. The acetone solution of diphenylcarbazide was more stable than the ethanol solution. Five diphenylcarbazide reagents commercially available were tested. They could be divided into two groups-one giving a molar absorptivity of 4.3 × 104l mol-1 cm-1 at 542 nm and the other giving 3.5 × 104. The result of the elemental analysis indicated that the latter group reagents were an approximately equimolar mixture of diphenylcarbazide and phenylsemicarbazide. In the determination of 1 to 10μg of chromium in 0.2 or 0.5 N sulfuric acid solution, 0.1 mg of iron (III) did not interfere if an Eastman diphenylcarbazide was used. However, an appreciable error was observed if a Tokyo Kasei Kogyo reagent was used. When either of the reagents was used, 0.1 mg of vanadium (V) did not interfere with the determination of 1 to 10 μg of chromium in 0.2 or 0.5 N sulfuric acid solution.
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  • Yoshimi SASAKI
    1978 Volume 27 Issue 11 Pages 729-731
    Published: November 05, 1978
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    In the investigation of the extraction system of metals with 2, 4, 6-tris (2'-pyridyl) -s-triazine (TPTZ), it is often necessary to determine the amounts of the participating TPTZ in both aqueous and organic phases. A selective determination of TPTZ was established by the following procedure : Transfer a sample solution containing TPTZ {(0.21.2)mg} in a 50 cm3 measuring flask. Add 2 cm3 of 0.01 mol dm-3 Mohr's salt solution and 1 cm3 of 10% hydroxylamine hydrochloride solution. Adjust the pH to 45 with acetate buffer solution, dilute to the mark with water, and measure the absorbance at 595 nm against, the reagent blank. In the ordinary extraction system involving TPTZ, the two phases were separated from each other and then the amounts of TPTZ in the aqueous phase was first determined as above. On the other hand, the organic phase was shaken with 6 mol dm-3 hydrochloric acid to strip TPTZ. The amounts of TPTZ in the hydrochloric acid solution was determined. From the above two determinations, the percentage extraction of TPTZ was obtained with various organic solvents as a function pH of the aqueous phase. The pH1/2 of TPTZ was found to be 0.38 with phenylcarbinol, 1.20 with chloroform, 1.72 with 1-butanol, 1.93 with nitrobenzene, 2.16 with dichloroethane, 2.28 with 1-pentanol, and 2.50 with trichloroethane.
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  • Yoshimi SASAKI
    1978 Volume 27 Issue 11 Pages 732-734
    Published: November 05, 1978
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    The determination of silver in silver alloys was performed. The procedure is as follows : A sample was dissolved in nitric acid and the solution was diluted to 500 cm3 with water; an aliquot, containing (220)mg of silver, of the solution was transferred. into a conical beaker; 2 cm3of saturated sodium chloride solution was added; silver chloride formed was filtered off through a Toyo No. 5C filter paper. Copper, zinc and cadmium in the filtrate were determined by the titration with 0.01 mol dm-3EDTA solution. The precipitate remaining on the filter paper was dissolved in aqueous ammonia. The solution was diluted to about 100cm3 with water; pH was adjusted to 10 with sulfuric acid; 15 cm3 of 0.02 mol dm-3 diethyldithiocarbamate (NaDDTC)solution was added. After adding one drop of Bromothymol Blue indicator solution, the excess of NaDDTC was titrated with 0.01mol dm-3 standard cadmium sulfate solution till the color turns from blue to red. This method was applicable to the determination of (860)% silver in silver coin or silver brazing filler metals.
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  • Toshiyasu KIBA, Kikuo TERADA, Chie NAKAGAWA
    1978 Volume 27 Issue 11 Pages 734-736
    Published: November 05, 1978
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    An oxidizing reagent consisting of the mixture of 2.5 g of potassium dichromate, 10 g of silver sulfate, 600 ml of sulfuric acid and 400 ml of phosphoric acid was recommended to use for the simple and rapid determination of COD of various waste waters. A 10-ml portion of sample water was put into a 50-ml Kjeldahl flask with 0.3 g of mercury (II) sulfate and several pieces of boiling stone, and 25 ml of the reagent-mixture was added. The solution was boiled at 160°C for 30 min, setting a cooling finger inside the neck of the flask. The contents of the flask was transferred into a 50-ml measuring flask and was diluted with water to the mark. The absorbance of the solution was measured at the wavelength of 630nm with a 50-mm glass cell. Beer's law was obeyed over the range of 01000 ppm COD. The calibration curves using glycine, glucose, ethanol and starch, as the reference, gave their slope of 7.05 × 10-4 as the mean. Therefore, the COD value can be calculated from the following equation : COD =absorbance/ 7.05 × 10-4. An appropriate volume ratio of sulfuric acid to phosphoric acid for the decomposition of glycine was found to be 3 : 2. The reaction time could be reduced to about one fourth of JIS (CODcr) method. The analytical results obtained for several kinds of industrial waste water are in good agreement with those obtained by JIS (CODcr) method.
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  • Masao SUGAWARA, Keiko ISAZAWA, Tomihito KAMBARA
    1978 Volume 27 Issue 11 Pages 737-738
    Published: November 05, 1978
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    A stalagmometric back titration of chromium(III) with copper (II) was successfully performed in the presence of calcium myristate as a surface-active indicator. The end point indicated by the remarkable increase in the surface tension was in good agreement with that obtained by the visual method with manganese (II) standard solution using BT indicator, in which the chromium (III) solution was previously five times diluted, the blue-violet coloration of the chelate being weakened. The measurement of the surface tension was carried out with a Shimadzu du Nouy surface tensiometer equipped with a platinum ring (0.610 mm in thickness, 19.568 mm in mean diameter). To a portion of 0.05 M chromium(III) nitrate standard solution in a beaker are added 10.0 ml of 0.05 M EDTA·2Na standard solution and 10 ml of 1 M CH3COONH4-HCl buffer solution of pH 3.3. After boiling the solution for 15 min, followed by cooling to room temperature, the pH of the solution is adjusted to 9.7 with ammonia water. As the indicator, 0.005 g of calcium myristate is added and the solution is diluted to about 60 ml with water. After addition of a small increment of the 0.05 M copper (II) standard solution the mixture is mixed well with a magnetic stirrer and subjected to the surface-tension measurements. The sudden increase in the surface tension at the end point is ascribed to the formation of slightly soluble calcium myristate.
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  • Jun'ichi TAKAHASHI, Kiyoshi TANABE, Hiroki HARAGUCHI, Keiichiro FUWA
    1978 Volume 27 Issue 11 Pages 738-740
    Published: November 05, 1978
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Atomic absorption spectrometry of mercury utilizing the Hg I 184.9 nm atomic line which is in the vacuum UV region has been investigated, and compared with that utilizing the atomic line at 253.7 nm. The atomic line at 184.9 nm is a resonance line, and has a larger oscillator strength (about 45 times) than that of the atomic line at 253.7 nm. Therefore, it can be expected that better sensitivity is obtained by utilizing the atomic line at 184.9 nm than at 253.7 nm. In order to realize the measurement of mercury atomic absorption at 184.9 nm, a conventional absorption-cell system was constructed. The cell is fixed inside a large Pyrex glass tube which includes an electrode-less discharge lamp of mercury, two quartz lenses and nitrogen gas inlets. The absorption-cell system was positioned in front of the entrance slit of a monochromator. The monochromator was purged with argon gas. A cold vapor generation method using a tin(II) chloride (3%) solution was used for the atomization of mercury from the sample solution. By using the conventional system mentioned above, the sensitivity (1% absorption) of mercury atomic absorption at 184.9 nm was 0.23 ng (or 0.23 ng/ml), while that at 253.7 nm was 1.2 ng (or 1.2 ng/ml). The relative standard deviation for 8 measurements at 184.9 nm was about 4%, when a 10 ng/ml Hg solution was used.
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  • Michiko NAMIKI, Jin KIMURA
    1978 Volume 27 Issue 11 Pages T39-T43
    Published: November 05, 1978
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Several methods for the determination of alloying elements at the major and minor concentration levels were described. The determination of copper was based on the copper-aquo complex formation in nitric acid media. This method was successfully applied to copper-zinc alloys with the coefficient of variation of less than 0.2%. The spectrophotometric determination of phosphorus in iron-phosphorus and nickel-phosphorus alloys was carried out by the phosphovanadomolybdate method. Antimony { (0.116) %} in antimony-iron alloys was determined as follows. Samples were dissolved with nitric and sulfuric acids. Antimony was allowed to form iodide complex in 3 N sulfuric acid by the addition of potassium iodide and sodium hypophosphite. The absorbance was measured at 425 nm. When the sample contained bismuth, the antimony was extracted into benzene. After the back extraction with sulfuric acid (1 + 20), the antimony was determined as described above.
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  • Tetsuo UCHIDA, Isao KOJIMA, Chuzo IIDA
    1978 Volume 27 Issue 11 Pages T44-T48
    Published: November 05, 1978
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    The use of a small sample volume in flame atomic absorption spectrometry is tested. A drop of sample solution taken into Teflon cup with micro-pipet is nebulized through ordinary capillary tube. A minimum sample volume giving the same sensitivity as that obtained by the conventional procedure can be estimated. from the sample flow rate, peak height, and overall response time of apparatus including pen-speed of recorder. The measurement with the estimated minimum volume or more can be carried out with excellent reproducibility and linearity of calibration curve. Even with the volume less than the minimum estimated, elements can be determined with the fairly good results. The detection limits (S/N=2) obtained with 100 μl sample solution are given for 11 elements in concentration and absolute amount. The present method was applied to the determination of 6 elements in NBS-SRM 1577 Bovine Liver after decomposition with a mixture of nitric and perchloric acids in a sealed Teflon vessel. Analytical results obtained agree well with the data reported. The one-drop method gives the advantages of use of commercially available apparatus without any modification, reduction in sample size, simple sample preparation, time-saving, good accuracy, and high precision.
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  • Toshiyuki HIOKI, Yukiko DOKIYA, Kenji NOTSU, Keiichiro FUWA
    1978 Volume 27 Issue 11 Pages T48-T51
    Published: November 05, 1978
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    In order to determine trace elements in silicates by atomic absorption spectrometry, the interference of major elements in the digested solution can not be neglected. Practically, the addition of one major element, such as Ca, to a series of standard solutions (proposed by TERASHIMA) is effectively adopted for the compensation of this interference. In this study, detailed observation of this effect was performed by changing the flame conditions and utilizing the response-surface plot method. Copper and Zn were found to give accurate results at a comparatively wide range of flame condition, while Ni was at a strict flame condition. According to our investigation, the analytical condition, especially that of flame, should be carefully considered, when solutions which contain large amount of other elements are measured by atomic absorption spectrometry.
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