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Volume 17, Issue 7
Displaying 1-18 of 18 articles from this issue
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Toshiaki KUROHA, Seiji SHIBUYA1968 Volume 17 Issue 7 Pages 801-805
Published: July 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA fluorescent X-ray method for trace metals involving their concentration by solvent extraction and fixation on a myler film with an addition of polystyerne was developed.
An amount of diethyldithiocarbamate solution was added to a sample solution, and the metals were extracted into carbon tetrachloride from pH 5.9 medium. A definite amount of polystyrene was added to the extract, and it was dried up by an infrared lamp illumination to fix the complex on a myler film. The fluorescent X-ray intensity was measured, and the amounts of the components were calculated referring to the calibration curves.
The analyses were done on 15 elements including Co, Cu, Fe and Ni, and the limits of detection were 3 × 10-8 1.5×10-6 g. The lower limits of determination were 3×10-85×10-7 g for Co, Cu, Fe, Ni, Mn and Zn. The coefficient of variation was 35% with selenium as an inner standard, and the calibration lines were sufficiently linear for 025μg of metals.View full abstractDownload PDF (2891K) -
Koichiro OIWA, Taeko KIMURA, Hideo MAKINO, Late Yahei KINOSHITA1968 Volume 17 Issue 7 Pages 805-809
Published: July 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA new catalytic reaction of iodide ion was applied to the spectrophotometric determination of micro amounts of iodine with Pyrocatechol Violet as the reagent. Pyrocatechol Violet was discolored by hydrogen peroxide in dilute HCl-HNO3 solution, and this reaction was greatly enhanced by the catalytic action of trace iodide. Iodine in the range of 0.010.1 ppm was determined successfully by measuring absorbances at 550 mμ after an hour. As much as 10 times of Fe(II) and (III), Cu(II) and Zn(II), and 1000 times of Al(III), Ba(II), Co(II), Cl-, ClO3-, Ca(II), F-, SO42-, H2PO4-, Li(I), Mg(II), Pb(II) and Sr(II) scarcely interfered. Br- and ClO4- interfered seriously.View full abstractDownload PDF (685K) -
Koichiro OIWA, Taeko KIMURA, Hideo MAKINO, Mitsuo OKUDA1968 Volume 17 Issue 7 Pages 810-815
Published: July 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSConditions for the atomic absorption spectrometric determination of zinc in blood serum and red cells were examined. Both serum and cell samples must be preliminarily deproteinized since those by simple dilution gave unstable flame. The recoverises of zinc by this procedure were 99% for serum and 96% for cells. Distributions of zinc concentration in serum and red cells of 50 patients were: 81100 μg/100 ml for serum and 12011400 μg/100 ml for red cells. The limiting concentration fot the determination was 0.02 ppm as giving 0.1% absorptivity.View full abstractDownload PDF (931K) -
Samuro MIWA, Akira TATEMATSU1968 Volume 17 Issue 7 Pages 816-819
Published: July 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn quantitative gas chromatographic analysis, it is necessary to know the relative molar responses of compounds, a lot of them having been reported by many workers. On three α-olefins from ethylene (C2) to butene-1 (C4), they have been measured by Messner et al. in 1959, using a thermal conductivity cell and helium as carrier gas. They discussed about the relation between the relative molar response (R) and the molecular weight (M), and offered a general equation for C2 to C4 as follows:
R=13.0+1.20 M
Now in this work, higher α-olefins from C6 to C14 were examined with the same condition as mentioned above.
On the relative molar response and molecular weight, propene-1 (C3) to octene-1 (C8) were plotted on astraight line, while ethylene was deviated a little from it. This deviation of the first member seems to be general in other homologous series. On the other hand, octene-1 (C8) to tetradecene-1 (C14) made up a curve. Generalequations for the relative molar response of α-olefins were
R=9.5+ 1.28 M (C3 to C8)
R=40.37+ 1.187 M-0.00147 M2 (C8 to C14) which were a little different from the Messner's formula.View full abstractDownload PDF (608K) -
Tomoo MIWA, Syuichiro OKI, Atsushi MIZUIKE1968 Volume 17 Issue 7 Pages 819-823
Published: July 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA glassy carbon electrode has been applied to the determination of microgram or submicrogram quantities of silver in high purity lead using the general technique of anodic stripping voltammetry. A lead sample (0.11.0 g) is dissolved in nitric acid, the solution evaporated to dryness twice, and the residue dissolved in 20 ml of 0.5 M potassium nitrate. Silver in, the resulting solution is electrodeposited on the polished electrode (surface area: 0.2 cm2) at -0.1 volt vs. S. C. E. for 30 min. with stirring; then the anodic stripping wave in the same solution is recorded by linearly varying the potential over a range of 0.0 to +0.8 volt vs. S. C. E. at a rate of 0.2 volt per min: Two hundredth to 6 ppm of silver in high purity lead can be determined by this method with an accuracy of approximately 10%. The time required for a determination is approximately 90 min.View full abstractDownload PDF (868K) -
Yoshizo HORIUCHI, Hiroshi NISHIDA1968 Volume 17 Issue 7 Pages 824-829
Published: July 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA small amount of cerium was determined spectrophotometrically with Chromazurol S(CAS).
Two milliliters of 0.25% CAS solution was added to 1015 ml of the acidic solution containing cerium, and pH was adjusted to 6.40 with 7% hexamine solution. After a dilution to 25 ml with water and allowing to stand for 10 min., the absorbance was measured at 510 mμ against the reagent blank. The absorbance obeyed Beer's law over 5120 μg Ce/25 ml, and the apparent molar absorptivity was 1.83×104.
By a separation of cerium as fluoride from di-, tri- and tetra-valent cations with sulfuric acid and hydrofluoric acid, interfering cations were removed except for lanthanum and yttrium, which were colored intensely at pH 9.60 with CAS where cerium was colored very slightly.
Then 10200 μg of cerium, 7142 μg of lanthanum and up to 60 μg of yttrium were determined simultaneously by measuring the absorbances at 510 mμ (pH 6.4), 610 mμ and 560 mμ (pH 9.6), respectively.View full abstractDownload PDF (1000K) -
Hiroshi ASAOKA1968 Volume 17 Issue 7 Pages 829-835
Published: July 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSFor the determination of 0.010.2% silicon in steels, a 0.25 g sample was decomposed with 12 ml of (1+6) sulfuric acid and 5 ml of 15% hydrogen peroxide, and then boiled to destroy the excess of the peroxide. After an addition of 5 g of ammonium sulfate, the solution was transfered into a 100 ml volumetric flask, and filled to the mark with water. The pH of the final solution should have been 1.1 ± 0.1. A 20 ml aliquot was transfered into a separatory funnel, and 4 ml of 10% ammonium molybdate solution was added. After 4 minutes' standing, 12 ml of 9 N sulfuric acid was added and the silicomolybdic acid formed was extracted immediately with 10 ml of iso-butanol. The extract washed 4 times with 5 ml of 2 N sulfuric acid was transfered into a 25 ml volumetric flask, and filled up to the mark with 8 ml of ethanol and water. The polarogram was then recorded in the usual way, the double waves of silicomolybdic acid being at -0.3 V and -0.5 V vs. the S. C. E. Germanium(IV) took the same behavior under the condition. The values by this method agreed well with the certificated values of the standard steels.
Another method involving the measurement of the maximum wave produced in a perchloric acid-hydrogen peroxide-iso-butanol mixture, was also investigated for determining minute amounts of silicon and germanium.View full abstractDownload PDF (1292K) -
Determination of trace elements in cement. V.Hisahiko EINAGA, Hajime ISHII1968 Volume 17 Issue 7 Pages 836-842
Published: July 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSTraces of vanadium in portland cement was determined by spectrophotometric method after extraction of vanadium into benzene with N-benzoylphenylhydroxylamine (BPA).
A sample is dissolved in perchloric acid, and silica, being made insoluble, is filtered off. Vanadium in the filtrate is converted completely into the vanadium(V) state with potassium permanganate, the excess of which is then disintegrated with hydrochloric acid. Vanadium(V) in the aqueous solution adjusted to about 3.4 N as hydrochloric acid is extracted into benzene with BPA, and the absorbance of the benzene phase is measured at 530 mμ.
The extracted vanadium(V)-BPA complex has a composition of 1 to 2 (metal to ligand), and shows an absorption maximum at 530 mμ. There exists a linear relationship between the amount of vanadium extracted and the absorbance. The molar extinction coefficient at 530 mμ is 4, 500. The diverse ions usually found in cements do not interfere with the determination except titanium(IV) and chromium(VI) in large amounts. The modified procedures are also given for these cases.
As little as 0.001% vanadium in cement was determined with satisfactory results, and about 0.0010.005% of vanadium was found in commercial products.View full abstractDownload PDF (1168K) -
Kaoru OHASHI, Masaaki MATSUO, Atsuko KAWASAKI, Hisashi KOIKE1968 Volume 17 Issue 7 Pages 843-846
Published: July 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA number of spectrophotometric methods have been given for the determination of chlorpheniramine, an antihistaminate, but there have been no specific reagents.
Plasmocorinth B as a metal reagent reacts with chlorpheniramine in an acidic medium to form a stable complex extractable into chloroform. The extract shows an absorption maximum at 567 mμ, and a linear relation holds between the absorbance and the chlorpheniramine concentration over 0.50.3 mg/ml. The reagent has been therefore applied to the determination. There are only few interfering substances, and the procedure is comparatively simple and seems practically useful.View full abstractDownload PDF (528K) -
Shun ARAKI, Shigetaka SUZUKI, Toshiyuki HOBO, Tsuguchika YOSHIDA, Kimi ...1968 Volume 17 Issue 7 Pages 847-854
Published: July 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDetermination of ultra-micro amounts of alkali and alkaline earth metals by hydrogen flame ionization method had been reported previously by the authors {This Journal, 15, 27 (1966)}. This ionization method has high sensitivity, but lacks selectivity.
For determining individual metal ion in a solution, further improvement of the detector and combination of this method with ion exchange chromatography werenecessary.
A modified detector with a sample holder of ringformed platinum wire (Fig. 2) was constructed. A small volume of sample solution (generally 1 μl or less) was loaded on the holder, and was evaporated to dryness in the drying chamber. After drying, the sample was inserted into hydrogen flame, and the response from the collector electrode was recorded. The procedure was suitable for successive analysis, since the holder has eight seats for samples.
For chromatographic separation of these metal ions, zirconium phosphate was chosen as an ion exchanger. Using ammonium chloride and hydrochloric acid solutions as eluates, the separation was carried out as shown in Fig. 9.
Sodium and potassium in human serum (Table II), hot spring water (Table III) and reagent grade barium hydroxide (Table IV) were determined. The results by this method agreed well with those by the flamephotometry.View full abstractDownload PDF (3069K) -
Hitoshi KOHARA, Nobuhiko ISHIBASHI, Saburo FUJITA1968 Volume 17 Issue 7 Pages 854-863
Published: July 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSChloro-substituted acetic acids were extracted from their dilute aqueous solutions into organic solvents containing tri-n-octylamine, by amounts considerably greater than those expected by sto ichiometry. Generally, 3 moles of the acids were extracted by one mole of tri-n-octylamine. Various factors on the formation of an ion pair and of complexes with excess acids were also examined. Extractions of acetic acid, propionic acid and butyric acid, however, were dependent largely on the number of alkyl carbons and hence partly on their solubilities in the solvent.
The NMR and IR spectra in carbon tetrachloride indicated that tri-n-octylammonium ion and dichloroacetate anion formed an ion pair in the range R< 1, and, in higher acid concentrations, hydrogen bond complexes were formed between these ion pairs and acid molecules, which would result in a weakening of the ion pair bond. The number of acid molecules in the complexes did not exceed three, since further interactions seemed to be very weak.View full abstractDownload PDF (1644K) -
Haruo TSUJI, Yuzuru KUSAKA1968 Volume 17 Issue 7 Pages 864-870
Published: July 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA rapid and nondestructive activation analysis of silicon and aluminum in silicate was proposed, by means of 28Si(n, p)28Al and 27Al(n, p)27Mg reactions caused by 14 MeV neutron irradiation.
A sample(3 g) in a polyethylene rabbit and a quartz neutron monitor were irradiated simultaneously for 3 min. with 14 MeV neutrons produced by T-d reaction in a Cockcroft-Walton neutron generator, and then the induced radioactivities were measured by a well type scintillation detector. A multichannel analyzer or two single-channel pulse height analyzers were used for counting the 28Al and the 27Mg photopeaks. One minute's counting after 3.5 min. cooling was adopted for silicon, and 3 or 4 min. counting after 25 min. cooling for aluminum. The radioactivities were normalized with the activity induced in the monitor, and then silicon and aluminum were determined, referring to the calibration curve.
The determination of aluminum was interfered from 56Mn introduced by (n, p) reaction of iron as a sample constituent, and the result should be corrected for this by counting 56Mn at 1 hr. after the 27Mg counting.
The analytical errors by this method were 2% for silicon and 4% for aluminum, under the neutron flux 1× 107 n/cm2/sec.View full abstractDownload PDF (1139K) -
[in Japanese]1968 Volume 17 Issue 7 Pages 871-878
Published: July 05, 1968
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1968 Volume 17 Issue 7 Pages 878-888
Published: July 05, 1968
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese], [in Japanese], [in Japanese], [in Japane ...1968 Volume 17 Issue 7 Pages 888-897
Published: July 05, 1968
Released on J-STAGE: June 30, 2009
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[in Japanese]1968 Volume 17 Issue 7 Pages 897-907
Published: July 05, 1968
Released on J-STAGE: June 30, 2009
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[in Japanese]1968 Volume 17 Issue 7 Pages 908-915
Published: July 05, 1968
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1968 Volume 17 Issue 7 Pages 916-923
Published: July 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (1473K)
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