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Volume 16, Issue 5
Displaying 1-29 of 29 articles from this issue
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Shuji ABE, Akira HONGO, Eiji SHIRAKAWA1967 Volume 16 Issue 5 Pages 399-405
Published: May 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe investigation was carried out in an attempt to select the most suitable column packings for complete and rapid separation of chlorobenzenes in mixtures by gas chromatography.
Chromatograms were measured with use of six kinds of column packings; (1) Bentone-34, (2) P. E. G.-6000, (3) P. E. G.-6000+Bentone-34 (series column method), (4) D. I. D. P.+Bentone-34 (blended liquid phase method), (5) 7, 8-benzoquinoline and (6) T. T. P.
Results indicate that both (3) and (4) are more useful for gas chromatographic analysis of the chlorobenzenes in mixtures than the other four. The following measurement conditions give high peak resolutions (1.60 or more) and short retention times (within about 20 minutes) for all components; column (3) : P. E. G.-6000 25 w/w% 75 cm+Bentone-34 10w/w% 225 cm in series, 140°C, N2 40 ml/min, 0.1 μl, column (4): D. I. D. P. 5w/w%+Bentone-34 5w/w%, blended liquid phase, 225 cm, 120°C, N2 30 ml/min, 0.1 μl.
It is also recognized that ο-dichlorobenzene is eluted later than 1, 2, 4-trichlorobenzene from the Bentone-34 column, quite contrary as to have been referred to.View full abstractDownload PDF (976K) -
Isamu TSUBAKI1967 Volume 16 Issue 5 Pages 405-409
Published: May 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe oxidation of a compound of low-valence state is an increase of its valence, and it means a transition of a substance from basic to acidic. It is then obvious from the law of chemical equilibrium that the reaction proceeds in the presence of a base which removes acid from the system. It is nowadays understood as one of well-known chemical rules.
The reversed rule, the reduction in the presence of acid, which may be naturally expected is, however, scarcely recognized, and only few examples have been known.
The author has shown in his experiments the reduction of Mn(VII), Mn(IV), Cr(VI), V(V), Mo(VI), W(VI) and U(VI) in the presence of H2SO4, H3PO4, H3BO3 or SiO2, and asserts the presence of the above rule. In addition, he reduced V(V) by H3PO4 and oxidimetrically titrated it and discussed the propriety of representing monazite by CePO4 and rhodonite by MnSiO3.View full abstractDownload PDF (894K) -
Microdetermination of herbicides by loose-layer chromatography and azodye formation reaction. IShinko GOTO1967 Volume 16 Issue 5 Pages 409-413
Published: May 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA spectrophotometric method for determination of herbicides with chloroaniline group was devised employing loose-layer chromatographic separation followed by diazo-coupling reaction. A test sample containing 550 μg of herbicide was extracted with methylene chloride and washed with 1 N hydrochloric acid. After the evaporation of the solvent the residue obtained was dissolved in ethanol and hydrolyzed by refluxing in basic or acidic medium. The resulting chloroaniline was partitioned into ether from basic aqueous solution. One ml of n-hexane was added to the ether solution and concentrated to about 1 ml. The condensed solution was applied to a loose-layer plate with 1 mm thickness of alumina powder containing 10% of 3 N ammonia. The plate was developed using n-hexane-ethylacetate (9:1) as a solvent. After drying for 10 minutes the band of chloroaniline was scraped from the plate, collected into a centrifuge tube and eluted with 15 ml of ethanol-glacial acetic acid-3 N hydrochloric acid (1:2:3). After centrifuge, 10 ml of the supernatant was pipeted into a test tube. The chloroaniline solution was diazotized with sodium nitrite, and the excess of nitrite was decomposed with ammonium sulfamate.
The diazonium compound formed was coupled with N-(1-naphthyl)ethylenediamine dihydrochloride, and resulting magenta color was subjected to the spectrophotometric determination. The hydrolysis of some herbicides and loose-layer chromatographic behavior of chloroanilines were also investigated.View full abstractDownload PDF (897K) -
Analytical studies on the polymers. IIIKoichi KONDO, Masatake HORI, Masatoshi HATTORI1967 Volume 16 Issue 5 Pages 414-418
Published: May 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA colorimetric gel permeation chromatography of polyetherpolyols (PEP) was performed by the use of auto analyzer. The crosslinked polystyrene was packed to a chromatographic column after swelling with 1, 2-dichloroethane (EDC). PEP dissolved in EDC was subjected to the column and eluted by the same solvent. PEP contents in the effluent from the column was determined colorimetrically by means of cobalt-thiocyanate complex. The good linearity was observed between effluent volume of the peak obtained from each PEP and the logarithm of the average molecular weight of the each corresponding PEP. The advantages of this method are in, (i) selectivity to PEP, (ii) sensitivity (only 2.5 mg of the sample), (iii) rapidity (only two hours), and (iv) good reproducibility.View full abstractDownload PDF (685K) -
Analytical studies on the polymers. IVKoichi KONDO, Mitsuyo MIYAZAKI, Masatake HORI, Masatoshi HATTORI1967 Volume 16 Issue 5 Pages 419-422
Published: May 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe method for the separatory analysis of polyetherpolyols (PEP) was investigated by thin-layer chromatography (TLC) and dry-column chromatography (DCC). The PEP obtained by ring-opening polymerization of propyleneoxide was separated into their functionality by the use of silica gel as thin-layer or column, and a mixture of n-hexane/diisopropyl ether/ethanol/water (5 : 10 : 5 : 3) as the solvent. The spots or peaks of separated PEP were determined colorimetrically by means of cobalt-thiocyanate complex.
The coefficients of variation of these methods were 4.04 for TLC, and 1.84 for DCC.
Some considerations on the principle of this mechanism of chromatographic separation were attempted, additionally, referring to the variation of the ratio of components in the effluent.View full abstractDownload PDF (639K) -
Shizuya MAEKAWA, Kiyotoshi KATO1967 Volume 16 Issue 5 Pages 422-427
Published: May 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA photometric determination of 0.002 to about 0.1% of magnesium in iron and steel with methylthymol blue (MTB) has been investigated. The magnesium-MTB complex is formed in a methyl alcohol-water medium at the pH range from 9.3 to 10.4, and Beer's law was obeyed up to 100 μg of magnesium when 5 ml of MTB solution (0.15%, w/v) was used.
The established procedure is as follows: 0.2 to 1 g of sample is decomposed in 5 to 20 ml of a mixture of perchloric acid and nitric acid, and it is evaporated to vigorous fumes of perchloric acid.
The graphite and silicate are removed by filtration. Interfering metals may be removed by electrolysis on a mercury cathode in diluted perchloric acid solution followed by precipitation as hydroxides by ammonia water (1+1) in the presence of 3 ml of hydrochloric acid.
Two ml of sodium cyanide solution (10%, w/v) is added, and the mixture is diluted exactly to 100 ml with water. One tenth aliquot is taken and to it is added 5 ml of buffer solution (pH 10.8) and 5.0 ml of MTB solution (0.15%, w/v).
Then it is diluted exactly to 100 ml with methyl alcohol. The absorbance is measured at 610 mμ against reagent blank as the reference.
The time required for an analysis was about 80 minutes.View full abstractDownload PDF (807K) -
Hiroshi ASAOKA1967 Volume 16 Issue 5 Pages 427-434
Published: May 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA system of water and isobutyl alcohol giving two phases can be homogenized to a single phase by adding a much less amount of perchloric acid than sulfuric acid. Molybdate ion and phosphomolybdate complex both provide the same maximum wave at about + 0.2 V vs. S. C. E. in a supporting electrolyte composed of 0.5 M perchloric acid-ca. 0.2 M hydrogen peroxide-ca. 0.8 M isobutyl alcohol. The height of the maximum is proportional to the concentration of molybdenum less than 2 × 10-5 M, and phosphate ion can be determined after the extraction of the complex by isobutyl alcohol. The lower limit of detection or determination is about 3 × 10-7 M phosphorus. For steels containing less than 0.03% phosphorus, 0.1 g of the sample is taken and dissolved with nitric acid. The phosphorus is oxidized to orthophosphate with potassium permanganate and arsenic is eliminated with sulfuric acid and potassium bromide. The solution is diluted to exactly 200 ml in which the final concentration of sulfuric acid should be about 0.75 N. A 10m l aliquot of this solution is transferred into a separatory funnel and after adding 1 m l of ammonium molybdate solution (ca. 5%) the phosphomolybdate complex is extracted with 10m l of isobutyl alcohol. A 2m l aliquot of the extract washed four times with 5m l of 0.5 N sulfuric acid is taken exactly into a 25 ml volumetric flask and filled up to the mark with 1.4m l of perchloric acid (60%), 5 ml of hydrogen peroxide solution (ca. 3%) and water. The polarogram is recorded using this solution and the height of maximum wave is measured. Small amounts of vanadium (V) and tungsten (VI) do not interfere.View full abstractDownload PDF (1197K) -
Toshio OZAWA1967 Volume 16 Issue 5 Pages 435-440
Published: May 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSTitanium reacts with 4-(2-pyridylazo)resorcinol (PAR) to form a water-soluble red complex. The complex has an absorption maximum at 527 mμ with a constant absorbance at pH 3.23.8.
The molar absorptivity of the complex is ca. 21, 000.The mole ratio of Ti and PAR is 1 : 2.
On the other hand, titanium reacts with PAR to form another complex which is also water-soluble and red in the presence of hydrogen peroxide. It has an absorption maximum at 510 mμ with a constant absorbance at pH 3.13.9. In the other pH range, however, the absorbance is dependent largely on pH, its maximum being obtained at pH about 8. The molar absorptivity of the complex is ca. 14, 000 and 51, 000 at pH 3.5 and 7.9 respectively. The mole ratio of Ti, H2O2 and PAR is 1 : 3 : 3.
Cu, Fe, Co, V, Ni, Bi, Sn, and Zr interfere with the determination, but vanadium not does in the presence of hydrogen peroxide.
The Beer's law is obeyed in the range 0.241.2 μg Ti/ml, in case of Ti-PAR complex, or 0.241.2 μg Ti/ml, 0.120.96μg Ti/ml at pH 3.5 and 7.9 in case of Ti-H2O2-PAR complex.View full abstractDownload PDF (709K) -
Yoko SHIBUYA, Eisuke NISHIYAMA, Kenjiro YANAGASE1967 Volume 16 Issue 5 Pages 440-444
Published: May 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe determination of sulfur in heavy oils by vacuum type X-ray fluorescence analysis was investigated. The problems involved in this method relate of conditions of sample in vacuum, such as influence of bubbles in sample on X-ray intensity, variation in X-ray intensity with time and strength of Mylar foil.
The results showed that the vacuum type X-ray fluorescence analysis was a useful method for a determination of sulfur in heavy oils. For the range of 2.10 to 4.15% sulfur in heavy oil, a linear relationship was obtained in terms of sulfur content against intensity ratio SKα/WLα. The results of determination of sulfur in heavy oil referring to this calibration curve gave standard deviation of 0.028% against 3.72% of the value by conventional chemical analysis.View full abstractDownload PDF (692K) -
Sanae IKEDA, Sôichirô MUSHA1967 Volume 16 Issue 5 Pages 445-450
Published: May 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSShort-circuit amperometric titrations of halides with silver nitrate solution in the presence of cyanide and cyanate have been investigated using a rotating platinum wire electrode (1000 rpm) and a saturated calomel electrode.
Cyanide can be readily masked with formaldehyde solution to give formaldehyde-cyanohydrin in a neutralweakly basic solution, and excess formaldehyde and cyanate decomposed by adding dilute nitric acid to make the pH of the solution below 3. Since formaldehyde-cyanohydrin did not interfere with an argentometry on chloride, bromide or iodide ions, they were successfully determined after adding excess formaldehyde solution and then nitric acid to make the pH of the solution below 3.
A chloride solution involving 0.02% gelatin was titrated by this method in the presence of one thousand fold amounts of cyanide and cyanate informal concentrations without any disturbance.
The relative percentage errors were about ±0.1% for 0.01F, ±1% for 0.001F, and ±4% for 0.0001F halides solutions, respectively.
The whole procedure can be carried out within 15 minutes.View full abstractDownload PDF (822K) -
Keisuke SUZUKI, Sinko GOTO, Fujio ITO1967 Volume 16 Issue 5 Pages 450-454
Published: May 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method was described for the ultraviolet spectrophotometric determination of 2, 6-dichlorothiobenzamide (DCBN) in wettable powders and technical products. One milliliter of acetone solution of the sample containing 30 mg of DCBN was applied to a thin layer plate of alumina powder with 2 mm thickness at a line 4 cm from the end. The plate was developed ascendingly with a mixture of ether and n-hexane (6+4), until the solvent front arrived at 10 cm line. The adsorbing band of DCBN was detected under the light of a short-wave UV lamp (250 mμ). The value of RF for DCBN in this system was about 0.4. After air-drying for 1 hour, the adsorbent of marked spot was scraped from the plate into a glass-filter (3G-4). DCBN was extracted with ether into a 50 ml volumetric flask. After making up to the mark, its 1 ml aliquot was diluted to 50 ml with methanol. The reagent blank was prepared on the same amount of the support carried through the whole procedure without the sample solution. The absorbances of the test solution and the reagent blank at 277.5 mμ were measured against methanol as the reference. The amount of DCBN was obtained from the difference between these values referring to a calibration curve.
The results of recovery tests were tabulated in Table V.View full abstractDownload PDF (813K) -
Shizuya MAEKAWA, Yoshio YONEYAMA, Hiroshi MORINAGA1967 Volume 16 Issue 5 Pages 455-460
Published: May 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSTwo grams of sample are decomposed with 25 ml of perchloric acid. After filtration, a bulk of iron and other heavy metals are removed by mercury cathode electrolysis. Then, the solution is drained and evaporated until the perchloric acid is given off completely. Five milliliters of hydrochloric acid are added to dissolve the residue. After dilution, remaining metals such as iron, aluminum, titanium etc. are precipitated in the form of hydroxide by adding ammonia water. After filtration, the filtrate is made up to 100 ml. Two fifths of the solution is titrated photometrically to determine the sum of calcium and magnesium by using M/500 EDTA and EBT indicator at pH 10±0.2. Another two fifths aliquot is titrated to determine the amount of calcium with M/500 EDTA and NN indicator at pH 12.513. The blank test through the whole procedure is required for the calibration of results. The accuracy of determination of the trace amount of calcium was increased successfully by prescribing on pH range, amounts of coexisting magnesium, indicator blank, standing time after the addition of sodium hydroxide, etc. Trace amounts of calcium and magnesium contained in steel as little as 0.0010.02% were determined within the deviation 0.001%.View full abstractDownload PDF (1052K) -
Hajime ISHII1967 Volume 16 Issue 5 Pages 460-463
Published: May 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA study was carried out on the determination of iron using the formation of an iron(III)-diantipyrylmethane complex and a new spectrophotometric procedure was proposed, which was applied to the determination of iron in cements as an example.
An iron(III)-diantipyrylmethane complex is formed in a slightly or weakly acidic medium (the optimum acidity: pH 2.03.5) and has an absorption maximum at 450 mμ. The complex formation is instantaneous at room temperature and the color is very stable. A linear relationship was maintained between the concentration of iron and the absorbance. The molar extinction coefficient and the sensitivity for log(I0/I) = 0.001 under the recommended conditions were 5400 and 1.0 × 10-2 μgFe/cm2, respectively. Several ions including molybdenum, tungsten, lead, perchlorate, phosphate, etc. interfered with the determination. Satisfactory results were obtained in the determination of iron in cements.View full abstractDownload PDF (653K) -
Masakichi NISHIMURA, Syu NAKAYA1967 Volume 16 Issue 5 Pages 463-467
Published: May 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSeveral metal-indicators for complexometry have been applied by other workers to spectrophotomteric determination of magnesium by measuring the absorbance of chelate in aqueous solutions.
It was found, in this experiment, that magnesium-EBT chelate as well as EBT itself are extracted well into n-amyl alcohol. The red color of EBT in n-amyl alcohol changes to blue with an absorption peak at 678 mμ, when it is shaken with a solution of pH 11.5. The magnesium-EBT chelate in n-amyl alcohol has its absorption maximum at 565 mμ.
A sample solution containing magnesium less than 0.8 μg is made to pH 11.5 with piperidine-hydrochloric acid buffer, and shaken with 10.0 ml of n-amyl alcohol containing 0.005% EBT. The difference of absorbances at 677.5 mμ between the blank and the sample gives the magnesium concentration. The n-amyl alcohol solutions of EBT and of magnesium-EBT are stable. This extraction method is several times more sensitive than the spectrophotometry of magnesium-EBT in aqueous solution. Calcium interferes.View full abstractDownload PDF (780K) -
Tsunenobu SHIGEMATSU, Katsuya UESUGI1967 Volume 16 Issue 5 Pages 467-469
Published: May 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA new spectrophotometric method for the determination of scandium was studied, using Pontacyl Violet 4BSN (Color index 16580) as a reagent. Scandium reacts with Pontacyl Violet 4BSN at pH 6.47.2 to form a colored complex with an absorption maximum at 630 mμ, which can be used for the determination of scandium. Beer's law was followed up to 1.2 ppm of scandium, and molar absorption coefficient was 13, 700 at 630 mμ. Aluminum, iron(III), copper(II), nickel, chromium(III), beryllium and phosphate interfere with the determination of scandium. The mole ratio of scandium to the reagent was 1:2 at pH 6.8.View full abstractDownload PDF (401K) -
Hitoshi KOHARA, Nobuhiko ISHIBASHI1967 Volume 16 Issue 5 Pages 470-475
Published: May 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe solvent extraction of iron(III) with 3-hydroxyflavone and the effects of pH upon the complex-forming ability of chelatogenic groups of two kinds have been investigated for the determination of small amounts of iron(III). Iron(III) can form the complex with either3, 4- or 4, 5- derivatives of flavone, but hydroxyl and carbonyl groups on 3, 4-positions react with iron(III) more easily than those on 4, 5-positions. Brownish-red iron(III) complex of 3-hydroxyflavone is extracted with several organic solvents. The extract in benzene shows absorption maxima at 407 mμ and 470480 mμ with constant absorbances at pH 3.59. The molar ratio of iron(III) to 3-hydroxyflavone in the complex is estimated to be 1 to 3. For the absorbance of complex in analytical condition, Beer's law is obeyed at least up to an iron(III) concentration of 4×10-5 M in benzene. The molar extinction coefficient of the complex in benzene is 1.4×104 at 475 mμ. Co(II), Ni(II), Zn(II), Cu(II), Al(III), Ti(IV), Zr(IV), Th(IV), V(V), U(VI), Mo(VI), W(VI), etc. scarcely interfere with the determination.View full abstractDownload PDF (1011K) -
Microdetermination of herbicides by loose-layer chromatography and azodye formation reaction. IIShinko GOTO1967 Volume 16 Issue 5 Pages 476-478
Published: May 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA spectrophotometric method for determination of 2, 4-dichlorophenyl-4'-nitrophenyl ether (NIP) and 2, 4, 6-trichlorophenyl-4'-nitrophenyl ether (CNP) was investigated and the recommended procedure for the analysis of soil sample was presented. A test sample containing 10100 μg of NIP or CNP was extracted with methylene chloride by batch procedure. One ml of n-hexane was added to the extract and the solution was concentrated to 1 ml on a water bath at about 50°C. The condensed solution was applied to a loose-layer plate with 1 mm thickness of alumina powder. The plate was developed using n-hexane-acetone (9 : 1) as a solvent. After drying for 15 minutes the band of NIP or CNP was scraped out, collected into a glass filter and eluted with ether. After evaporation of ether, NIP or CNP obtained was dissolved in acidic ethanol and reduced with zinc dust by refluxing for 10 minutes. The resulting amino compound was diazotized with sodium nitrite solution containing potassium bromide, and the excess of nitrite was decomposed with ammonium sulfamate. The diazonium compound formed. was coupled with N-(1-naphthyl) ethylenediamine dihydrochloride and the resulting magenta color was subjected to the spectrophotometric determination. The results of recovery test were shown in Tables IIIIV.View full abstractDownload PDF (605K) -
Hiroshi HASHITANI, Kazuo KATSUYAMA, Kenji MOTOJIMA1967 Volume 16 Issue 5 Pages 478-482
Published: May 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSFor the accurate determination of 1.20 to 1.70% tin in Zircaloy, the method of Eberle and Lerner [Anal. Chem., 34, 627 ('62)] has been modified. The operation became easier by widening pH ranges for the extraction. An excess of the associated 8-quinolinol and other metals which might cause errors, were removed. by washing the first extract. As a result of these modifications, the accuracy and the precision have been much improved, when compared favorably with the standard volumetric method.
A recommended procedure is as follows: A 0.1 g of Zircaloy is dissolved in 10 ml of sulfuric acid and 5 mlof 50% ammonium sulfate solution. An aliquot containing 200 to 400 μg tin is taken, and to this 5 ml of 20% ammonium chloride solution and 20 ml of 5% 8-quinolinol (HOx) solution are added. The pH of the solution is then adjusted at 0.8 to 1.5. The resulting solution is transferred to a 200-ml separatory funnel and the Sn(Ox)2Cl2 formed is extracted with exactly 20 ml of chloroform by shaking for 1 minute. The extract is then shaken with 50 ml of an ammonium chloride-hydrochloric acid solution (pH 0.85±0.1) for 10 to 30 seconds in another separatory funnel. Tin is determined by measuring the absorbance of the washed solution against chloroform at 385mμ.View full abstractDownload PDF (933K) -
Shizuya MAEKAWA, Kiyotoshi KATO1967 Volume 16 Issue 5 Pages 482-485
Published: May 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA preliminary separation procedure of a small amount of iron, ranging from 0.001 to 0.5%, in nickel, copper, cobalt, titanium and aluminum metals and alloys, prior to the colorimetric determination with 2, 4, 6-tris (2-pyridyl)-s-triazine method, has been investigated.
In nickel, copper, cobalt, titanium metals, iron was separated from on 7 N hydrochloric acid solution by the extraction with methyl-isobutyl ketone. As for aluminum and its alloys, after being decomposed with sodium hydroxide, iron was precipitated and separated as a form of hydroxide, together with the calcium added as a coprecipitant.
In coloration ascorbic acid was used for the reduction of Fe3+ to Fe2+, and it was found that the time required for the reduction was much faster.View full abstractDownload PDF (684K) -
Shizuya MAEKAWA, Kiyotoshi KATO1967 Volume 16 Issue 5 Pages 485-488
Published: May 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA photometric determination of phosphorus in niobium steel with molybdenum blue has been studied. The established procedure is as follows: 0.5 to 1 g of sample is decomposed with 10 ml of aqua regia, to this is added 10 to 15 ml of perchloric acid and it is evaporated until nitric acid is removed fuming perchloric acid vigorously.
After cooling, the solution is diluted to approximately 50 ml with hot water, to this 10 ml of hydrofluoric acid (1+4) is added. It is then heated, and 4 g of boric acid is added and mixed.
After masking interfering niobium, Fe3+ is reduced. by sodium bisulfite, and subsequently, a mixture of hydrazin sulfate and ammonium molybdate is added to the solution and finally it is colored by heating on either a water bath or a hot plate.
The absorbance is measured at 825 mμ. The time required for the analysis is about 40 minutes.View full abstractDownload PDF (800K) -
Shizuya MAEKAWA, Yoshio YONEYAMA, Kazuo CHIBA1967 Volume 16 Issue 5 Pages 488-490
Published: May 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDetermination methods of small amounts of lead and bismuth, contained in molybdenum trioxide briquette which is charged into the steelmaking furnace as a substitute for the ferromolybdenum, have been studied. Crashed and powdered sample are dissolved in aqua regia and organic matters present are decomposed completely by the addition of perchloric acid. After being cooled, the molybdenum acid anhydride deposited is dissolved either with ammonia water in the presence of tartric acid or with sodium hydroxide. Lead is extracted with dithizone-tetrachloride solution in advance from the solution of pH 10, containing tartarate and cyanide, and then, separated from bismuth by shaking with 0.05 N nitric acid. Finally, lead is extracted and measured as dithizonate in dithizone-benzene solution. Bismuth is extracted and determined photometrically as diethyldithio carbamate in the carbon tetrachloride solution, after being separated and concentrated according to the ferric hydroxide coprecipitation procedure. In the use of the spectrographic detection, conbined with the dithizonate extraction, it is confirmed that the samples do not contain any amount of thallium, which is interfered with the determination of lead and bismuth. Analytical results some commercial briquettes and ferromolybdenums are shown in Tables I and II.View full abstractDownload PDF (550K) -
Takayasu SHIRASAKI, Ken-ichi MUKAIDA1967 Volume 16 Issue 5 Pages 491-492
Published: May 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSolid acidity of powdered Silica Alumina catalyst was measured by the gas phase neutralization method which employs a fluidized bed consisting of sample catalyst as fluidized powder and fluid flow purified air.
When catalyst particles were colored in red (acidic color) with dimethyl yellow as an indicator, the fluid air was flowed at nearly a minimum fluidization velocity and ammonia gas was added continuously to fluid air.
The solid acidity of the samples was determined rapidly(about 20 min.) by the observation of the color change from red to yellow. The acidities measured by this method agreed reasonable well with the Tamele's acidities.View full abstractDownload PDF (319K) -
Taitiro FUJINAGA, Yoshinori OGINO, Shigeo MURAI1967 Volume 16 Issue 5 Pages 492-493
Published: May 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn the gas chromatographic analysis kiesel-gel has widely been used as a support material, but it has a defect of showing a tailing phenomenon on chromatograms for polar compounds, such as water, alcohols or amines.
In the present paper, use of a glassy carbon as a support material is suggested.
Peak of methanol is almost symmetrical and well defined using the column of glassy carbon coated with 1% DOP, and also a mixture of alcohols was separated using the column of glassy carbon coated with 1% PEG.
In summary, a glassy carbon has shown the following advantages, (1) it is effective for polar substances, (2) it is applicable to both the light loaded (<1%) and the heavy loaded (510%) columns, (3) it is packed easily in the column, and (4) it is available at high temperatureView full abstractDownload PDF (287K) -
[in Japanese]1967 Volume 16 Issue 5 Pages 494-498
Published: May 05, 1967
Released on J-STAGE: February 15, 2010
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[in Japanese], [in Japanese], [in Japanese]1967 Volume 16 Issue 5 Pages 499-510
Published: May 05, 1967
Released on J-STAGE: June 30, 2009
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[in Japanese]1967 Volume 16 Issue 5 Pages 511-512
Published: May 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (312K) -
[in Japanese]1967 Volume 16 Issue 5 Pages 512-513
Published: May 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (302K) -
1967 Volume 16 Issue 5 Pages 514-516
Published: May 05, 1967
Released on J-STAGE: June 30, 2009
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1967 Volume 16 Issue 5 Pages 517-518
Published: May 05, 1967
Released on J-STAGE: June 30, 2009
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