All issues
Volume 20, Issue 3
Displaying 1-25 of 25 articles from this issue
- |<
- <
- 1
- >
- >|
-
Masaro SHIMIZU, Keiichiro HOZUMI1971 Volume 20 Issue 3 Pages 267-274
Published: March 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA rapid and automatic oxygen analyzer based upon the Unterzaucher's conversion of organic oxygen to iodine and successive measurement of the vapor phase iodine by optical integration in a long gas cell kept at 120°C has been examined with special reference to the reactivity between carbon granules and organic oxygen by varying amounts of carbon filling, temperature of conversion and flow rate of carrier gas. It has been found that the conversion of organic oxygen to carbon monoxide was quantitative with the carbon filling of 16 cm (4.8 g), the reaction temperature of 10501100°C and the argon flow rate of 20ml/min. Aromatic carboxylic acid such as benzoic acid and phthalic acid exhibited low reactivities compared with the other types of organic compounds, hence resulting in the above mentioned limiting operative conditions. It has been also concluded that the platinized carbon reacted quantitatively with organic oxygen under a temperature of 850900°C at the beginning, but itgradually reduced its reactivity during the use in routine analysis so that the quantitative reaction required temperature higher than 950°C for safety.View full abstractDownload PDF (1243K) -
Keiichi TANIKAWA, Kiichi ARAKAWA1971 Volume 20 Issue 3 Pages 274-277
Published: March 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThin layer chromatographic separation of Ce(tfa)4, Ce(tfa)3, La(tfa)3, Pr(tfa)3, Sm(tfa)3, Dy(tfa)3, Ho(tfa)3 and Er(tfa)3 was carried out by using Eastman chromatogram cellulose sheet.
The separation of Ce(tfa)4 and Ce(tfa)3 was possible by a single developer as benzene, toluene, cyclohexane and petroleum benzine. By using mixed solvents, the separation of Ce(tfa)4>Er(tfa)3>Dy(tfa)3 was done with petroleum benzine-acetylacetone (40 : 1) and the separation of Al(III) or Cr(III) and Cu(II) as well as that of rare earths was done with cyclohexaneacetylacetone (20 : 1). The Rf values were in the order, Al(tfa)3>Ho(tfa)3>Cu(tfa)2. The separation of La(tfa)3>Sm(tfa)3>Nd(tfa)3 was done by development with toluene-cyclohexane-acetic acid (30 : 20 : 1).View full abstractDownload PDF (590K) -
Keiichi TANIKAWA, Kiichi ARAKAWA1971 Volume 20 Issue 3 Pages 278-281
Published: March 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDerivatives of ferrocene were separated by thin-layer chromatography by using Merck TLC plates silica gel F254. The separation of monosubstitutes and disubstitutes were done by the development with petroleum benzine-ethanol (30 : 1), petroleum benzine-methanol (30 : 1) petroleum benzine-acetone (30 : 4) or toluenepetroleum benzine-acetone (30 : 2 : 2), whereby the Rf values of monosubstitutes were generally greater. The raw materials and intermediates in the synthesis of ferrocene derivatives were also separated. Rf values of various compounds obtained during the course of synthesis of 1, 1'-di(α-hydroxymethyl) ferrocene by the development with mixed solvents were in the order : ferrocene>1-methyl-1'-ferrocene carboxylic acid>1, 1'-diacetyl ferrocene >1, 1'-di(a-hydroxy-methyl)ferrocene.View full abstractDownload PDF (565K) -
Itsuo MORI1971 Volume 20 Issue 3 Pages 282-287
Published: March 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe colour development of a water soluble reddish violet complex between gallein and zirconium(IV) was enhanced by the catalytic action of fluorine, particularly in the coexistence of excessive cethylpyridinium chloride(CPC) which decreased the reagent blank of gallein and increased the absorbance of the complex. Its absorption maximum was at around 600 mμ against the reagent blank, and the absorbance was constant over the pH range from 3.84.8 in the coexistence of 1.0×10-3M CPC. The calibration curve was linear for 0 to 20μg of zirconium(IV), and 0.5 to 3.8 μg of F-. The recommended analytical procedure is as follow.
To the solution of zirconium(IV) were added each 1.5ml of 1.0×10-2M CPC, 4.0×10-3 M sodium fluoride solution and 1.5×10-3M methanolic gallein solution, and 2.0 ml of sodium acetate-acetic acid buffer of pH 4.6. To the solution of F- were added each 0.5 ml of 5.0×10-4 M zirconium(IV), and 1.5×10-3 M methanolic gallein solution, 2.0 ml of the buffer of pH 4.6. It was then diluted to 10 ml with water and, after 30 minutes, the absorbance was measured at 600 mμ for zirconium(IV), and 610 mμ for F-against the reagent. Many ions interfere with the determination.View full abstractDownload PDF (791K) -
Isao MATSUMOTO, Masao OKAMOTO, Masao KANDA1971 Volume 20 Issue 3 Pages 287-291
Published: March 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSRapid atomic absorption analysis of trace amounts of lead in bismuth oxychloride without separation of bismuth has been developed, in which the correction for the effect of excess bismuth on the analytical 2833Å line for lead is done precisely by referring to the non-absorbing 2802Å line.
The solution is prepared by dissolving 25 g of sample in 20ml of 6N HCl and diluting to 100 ml with 0.5N HCl.
The time required for an analysis is approximately 30 minuts, and coefficients of variation are 1.7% for 20 ppm of Pb and 4.5% for 5 ppm of Pb.View full abstractDownload PDF (786K) -
Analytical studies on thiopyrazolone derivatives. VTomoo TANAKA, Hiroshi KATAGIHARA, Nobuhiko IRITANI1971 Volume 20 Issue 3 Pages 291-296
Published: March 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThiopyrine(1-phenyl-2, 3-dimethyl-3-pyrazolin-5-thione) and its derivatives react quantitatively with Se(IV) in a strongly acidic solution to form water-soluble 1 : 4 (Se : thiopyrine) complexes. This reaction was applied to the spectrophotometric determination of selenium. The minimum acid concentration required for the determination was: sulfuric acid 14 N, hydrochloric acid 5 N or perchloric acid 6 N. Determination of less than 10μg/ml of selenium in concentrated sulfuric acid or in concentrated hydrochloric acid was possible.View full abstractDownload PDF (884K) -
Yoshio SHIJO, Tsugio TAKEUCHI1971 Volume 20 Issue 3 Pages 297-302
Published: March 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSChromazurol S(CAS) reacts sensitively with uranium(VI) to form a blue complex in a micelle solution of trimethylcetyl-ammonium chloride. The absorption maximum of this complex was at about 615 mμ, and the pH dependence of the absorbance became small at pH 45.5. The calibration line at 615 mμ was slightly curved but that at 625mμ was quite linear with apparent molar absorptivity 1.0×105. The continuous variation measurement indicated that the composition of the complex was U:CAS=1: 2. The acid dissociation of CAS in a micelle solution of trimethylcetyl ammonium chloride was remarkably enhanced in the acid solution but it seemed to be suppressed in the alkaline side.View full abstractDownload PDF (937K) -
Iwaji IWASAKI, Minoru YOSHIDA, Seiko YOSHIDA1971 Volume 20 Issue 3 Pages 302-307
Published: March 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSSample is decomposed with hydrofluoric-sulfuric acid in a platinum crucible. The content is evaporated to fumes, and then dissolved in hot water. To it are added p-nitrophenol as an indicator and then 0.2N sodium hydroxide solution dropwise until the color changes. The precipitate formed is filtered through a filter paper (The Toyo Filter Paper, No. 5A), and the filtrate is diluted to 50 ml.
To a 25ml volumetric flask is transferred 2 or 5 ml aliquot of the sample solution containing not more than 40 μg of calcium. Then 2 ml of buffer solution (pH 12.8), 1 ml of GHA-ethanol solution (0.25%) and 15 ml of ethanol-1-butanol mixed solvent (1 : 1) are added in that order. It is made up to the mark with water, and, after mixing, the volumetric flask is kept at 30°C for 30 minutes. The absorbancy is measured by using a 517 mμ filter against distilled water.
The absorbancy is affected seriously by pH of the solution, reagent concentration, amount of the solvent added and the standing time. Therefore, the conditions for the determination stated above must be controlled carefully.
Various substances commonly present in rocks do not interfere with the photometric procedure with the exception of Fe3+, Ti4+ and PO43-, which are easily eliminated by the precipitation procedure.View full abstractDownload PDF (747K) -
Chemical shift of characteristic X-ray and its applications.IIKatsumi OHNO1971 Volume 20 Issue 3 Pages 308-313
Published: March 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple X-ray technique and statistical data analysis are described for the study on AlKβ line shift as measure of state of chemical combination of the aluminum atom, using commercially available equipment.
The peak position in the spectra is statistically estimated with orthogonal polynomials.
It is estimated that the AlKβ' line shift due to chemical combination are proportional to the group number squared of bonded element with aluminum, and the AlKβ1 line shifts are proportional to the difference squared the group number of aluminum and the bonded element with aluminum.
It seems that so called “AlKβ line” on metallic aluminum is doublet, which consist with the Kβ1 and the Kβ', line.View full abstractDownload PDF (963K) -
Masahiro TSUBOUCHI1971 Volume 20 Issue 3 Pages 314-317
Published: March 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA spectrophotometric method is proposed for the determination of eserine. The method is based on the formation of an addition-compound between eserine and the tetrabromophenolphthalein ethyl ester (TBPE). The recommended procedure is as follows.
Pipette 210 ml of an eserine solution (2.5 × 10-5M), 5 ml of borate (0.1M)-phosphate (0.3M) buffer solution (pH 8) and 2 ml of a TBPE solution (5 × 10-3M in alcohol) into a 100-ml separatory funnel. Dilute the mixture to 25 ml with water and shake the solution for 2 min with 10 ml of 1, 2-dichloroethane. After the separation of the two layers, run off the extract into a glass tube through a filter paper to remove any droplets of water. Measure the absorbance of the extract at 576mμ against a reagent blank as a reference.
Optimum pH range for the extraction is 7.58.5 The absorbance of the extract showed a linear relationship to the concentration of eserine in the aqueous solution over the range of 2 × 10-61 × 10-5 M.View full abstractDownload PDF (623K) -
Masakazu DEGUCHI, Mikio YASHIKI1971 Volume 20 Issue 3 Pages 317-321
Published: March 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method for the spectrophotometric determination of copper in serum was studied in which thiothenoyltrifluoroacetone(STTA) was used as an extractant and a photometric reagent.
Copper(II) (up to 8 μg) was extracted quantitatively with exactly 5 ml of 6.3 × 10-5M STTA in carbon tetrachloride from an aqueous solution at pH3.55.5 by shaking for 2 minutes. The complex had an absorption maximum at 394mμ. The calibration curve followed Beer's law over the range of 0 to 8 μg/5ml of copper(II). The molar extinction coefficient was 2.8 × 104. The precisions in coefficient of variation were 1.7 and 1.3%, respectively, for 3 and 5 μg of copper(II).
An analytical procedure for copper in serum was as follows. Two milliliters of serum samples was taken into a centrifuge tube and proteins were precipitated with 1 ml of 1 N hydrochloric acid and 1 ml of 20 g/dl trichloroacetic acid solution. After centrifuging, 2 ml of the supernatant liquid was taken into a test tube. One milliliter of 30 g/dl sodium acetate solution was added, and the solution was made up to 10 ml with water. Five milliliters of 6.3 × 10-5M STTA in carbon tetrachloride was added to it, and the solution was shaken vigorously for 2 minutes. The absorbance of the extract was measured at 394 mμ against the reagent blank. The proposed method was simple and the recovery of copper added on serum samples was very satisfactory.View full abstractDownload PDF (795K) -
Shigeru TERASHIMA1971 Volume 20 Issue 3 Pages 321-326
Published: March 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method was proposed for the rapid determination of cobalt, copper, lithium, nickel, lead, strontium and zinc in various silicates by atomic absorption spectrophotometry.
The sample was decomposed with a mixture of HF and HClO4. After having been converted to the chlorides by HCl, the molecular absorption interference with determination of cobalt, nickel, lead and zinc from aluminum, calcium, iron etc. was eliminated by adding calcium to the standards. Strontium was determined by adding lanthanum to the samples and the standards. Copper and lithium were determined directly from the sample solution.
The results on seven elements in nine silicate samples agreed well with those by other methods. A complete procedure required about 6 hours.View full abstractDownload PDF (948K) -
Kiyoshi TAKIURA, Hidetaka YUKI, Yoko TASHIMA, Sachi INAZUMI1971 Volume 20 Issue 3 Pages 327-330
Published: March 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe reaction mixture of chloranil and aniline gives absorption maxima at 390 mμ and 540 mμ in the visible region. The former had been ascribed to the absorption of 2, 5-dianilino-3, 6-dichloro-p-benzoquinone(I) and the latter to the charge transfer complex compound of aniline and chloranil. The authors isolated 2-anilino-3, 5, 6-trichloro-1, 4-benzoquinone(II) from the reaction mixture of chloranil and aniline as purple crystals, which was identified by comparison of its melting point, visible and infrared absorption spectra with those of an authentic sample which was synthesized according to the literature. II had an absorption maximum at 550 mμ, and it was suggested that the absorption maximum at 540 mμ of the reaction mixture was due at least partly to II. The resolution of the absorption curve of the reaction mixture by a curve resolver showed the presense of II and another component which had weak and wide absorption band (λmax 520 mμ), and this component was supposed to be the charge transfer complex compound. The compound I also gave a very slight absorption near this region. Accordingly, it was concluded that the absorption at 540 mμ of the reaction mixture of chloranil and aniline was due mainly to II and partly to the charge transfer compound together with very slight contribution of I.View full abstractDownload PDF (599K) -
Tokunosuke NAKAJIMA, Yoshihiko OUCHI, Kaneharu KATO1971 Volume 20 Issue 3 Pages 330-335
Published: March 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe analytical conditions for the fluorescent X-ray determination of small amounts of Hf, Co, Cu and W in zirconium and zircaloy were established. X-ray tube with platinum target was used as the primary excitation source. Counting system of the single channel X-ray fluorescence spectrometer (GE-XRD-5 spectrometer) was replaced with solid-state signal processing electronics ( JAERI nuclear instrument module system) which eliminate difficulties of noise and drift at the linear amplifiers and pulse height analyzer, contributing to increase the detectabilities of minor elements.
In order to eliminate the interference from contaminated copper spectra, occuring at copper analysis, cobalt filter was inserted between the primary X-ray tube and the sample. Copper filter was all the same effective for the determination of tungsten in order to reduce the interference from the primary PtLα1 line.
The limits of detection of Hf, Cu, Co and W were estimated to be ca.40, 10.4, 8.2 and 15 ppm, respectively. Reproducibilities obtained were 6.9% for Hf, 2.7% for Cu, 3.1% for Co and 6.4% for W.View full abstractDownload PDF (975K) -
Studies on the hydroxyl derivatives of chromone as analytical reagents. IXTakushi ITO, Akira MURATA1971 Volume 20 Issue 3 Pages 335-340
Published: March 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSBeryllium reacts with 2-ethyl-3-methyl-5-hydroxy-chromone to form a fluorescent complex, which is soluble in various organic solvents. The complex extracted into carbon tetrachloride from a solution of pH 6.510 shows the strongest fluorescence with constant intensity. The excitation and emission spectra of fluorescence have maxima at 403 mμ and 483 mμ. An analytical procedure is as follows : To a beryllium solution are added 2.5 ml of 4×10-3 M methanol solution of reagent and 2.5 ml of buffer solution (pH ca. 8.08.5, boric acid-sodium hydroxide), and the mixture is diluted to 25 ml with water. After 1 hour, the solution is shaken for 30 seconds with 10 ml of carbon tetrachloride. The organic phase is:separated and dried over sodium sulfate. Its fluorescence intensity is measured, using a secondary filter passing above ca. 420 mμ, with an excitation wavelength of 405 mμ. An aqueous solution of fluorescein sodium (1 μg/ml) is used as a reference standard. The complex is stable at least for 5 hours. An analytical curve is linear in the range of 0.010.25 μg of beryllium. The effect of diverse ions was examined.View full abstractDownload PDF (922K) -
Studies on technical analytical methods by differential scanning calorimetry, differential thermal analysis and thermogravimetry. IIIGenzo HASHIZUME, Kayoko AMITA1971 Volume 20 Issue 3 Pages 340-346
Published: March 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSTwo series of OH- and ONa-terminated Graham's salt (G-OH and G-ONa) of various average chain lengths were prepared by heating NaH2PO4 or a mixture of NaH2PO4 and Na4P2O7 at 800°C for a given time. The chain length was determined by end point titration, and X-ray diffractometry and thin layer chromatography were used for identifying each peak on DTA curve.
The relative amount of products at a desired temperature during heating run was also determined by X-ray diffractometry and X-ray emission spectrometry.
Thermal changes on DTA curve involve (1) glass transition(G), (2) exothermic peak(C) corresponding to crystallization into (NaPO3)3I from Graham's salt, (3) endothermic peak(H) corresponding to condensed dehydration at G-OH, (4) several endothermic peaks between (C) and (F) corresponding to transition of by-products or eutectic fusion among them and (5) endothermic peak (F) due to melting of the salt.
The area under the peak (C) increased in proportion to the chain length. A linear relation existed between the chain length and the weight loss corresponding to dehydration. The maximum temperature of (F) of G-OH was 624°C which was the melting point of (NaPO3)3I while that of G-ONa rose rapidly depending on the chain length and approached to that melting point of (NaPO3)3I. Bueche's rule hold between the chain length and the temperature of (G) as already known.
The chain length of Graham's salt as well as the kind of terminal group and the ratio of G-OH and G-ONa were estimated conveniently by the methods of DSC, DTA and TG.View full abstractDownload PDF (1105K) -
Yuroku YAMAMOTO, Takahiro KUMAMARU, Yasuhisa HAYASHI, Makoto KANKE1971 Volume 20 Issue 3 Pages 347-354
Published: March 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method for the determination of ppb amounts of cadmium, zinc, lead and copper in water has been developed by combining atomic absorption spectrophotometry with solvent extraction with a volume ratio of aqueous phase/solvent as large as 5001000 ml/25ml. The following three procedures of extraction were compared.
(A) To a sample water in a separatory funnel were added sodium-potassium tartrate (20%, 5 ml) and hydroxylamine hydrochloride (10%, 2 ml). This mixture was neutralized with ammonia using Thymol Blue indicator, and the buffer solution (NH4Cl-NH3, pH 10) was added to adjust the pH. It was extracted twice by shaking with dithizone-carbon tetrachloride solution (0.03%, 10 ml). The extract was washed with water and then shaken with hydrochloric acid (1N, 10 ml). This hydrochloric acid solution was aspirated in an atomic absorption spectrophotometer to determine cadmium, lead and zinc (For the determination of copper, 6N hydrochloric acid should be used to strip the element from the carbon tetrachloride extract).
(B) To the dithizone-carbon tetrachloride extract in (A) was added methyl-isobutyl ketone (10 ml), and the mixture was aspirated.
(C) To the sample water whose acidity was preliminarily adjusted to pH 45 was added ammonium pyrrolidine dithiocarbamate solution (1%, 5 ml). The mixture was shaken with methyl-isobutyl ketone (25 ml) and the extract was subjected to the measurement.
All the three methods were applied satisfactorily to the determination of the four elements in various types of water samples. The method (C) showed the highest sensitivity because of the decreased volume of the extract due to an appreciable solubility (ca. 2%) of methyl-isobutyl ketone in water and also of the “solvent effect”, but the apparent solubility of the solvent was a little different in sea water and in pure water. The standard addition method gave good results in this case.View full abstractDownload PDF (1424K) -
Hiroshi NISHIDA1971 Volume 20 Issue 3 Pages 355-356
Published: March 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSOxine and cupric ion formed a yellow colored complex soluble in 40% pyridine solution. At its maximum absorption, 390 mμ, the sensitivity for 0.001 of the absorbance was 0.0125 μg/cm2. The analytical procedure was simpler and obtained values were more accurate and precise than that by the extraction method. Diverse ions such as zinc and lead interfered, and copper must be determined after the separation of copper oxinate by precipitation from zinc and lead ions at pH 2.72.8. The copper oxinate was dissolved in 1M hydrochloric acid and diluted with water. An aliquot of this solution was subjected to the spectrophotometric procedure by treatment with oxine and pyridine. The absorbance obeyed Beer's law for 0.312 ppm of copper. Copper in its alloys was determined with 0.1% standard deviation.View full abstractDownload PDF (297K) -
Analytical studies on thiopyrazolone derivatives. VITomoo TANAKA1971 Volume 20 Issue 3 Pages 357-358
Published: March 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThiopyrine (1-phenyl-2, 3-dimethyl-3-pyrazolin-5-thione) reduces Fe(III) to Fe(II) in an acidic solution and forms 5, 5'-dithiobis(1-phenyl-2, 3-dimethylpyrazolium) ion. This reaction was applied to the reduction of Fe(III) in the photometric determination of iron with 1, 10-phenanthroline. This compound was stable in air and did not produce substances disturbing the color development of Fe(II)-1, 10-phenanthroline. The method was comparable to the conventional hydroxylamine hydrochloride reduction.View full abstractDownload PDF (328K) -
Analytical studies on thiopyrazolone derivatives. VIITomoo TANAKA1971 Volume 20 Issue 3 Pages 359-360
Published: March 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThiopyrine (1-phenyl-2, 3-dimethyl-3-pyrazolin-5-thione) reacts quantitatively with iodine by mole ratio 1:2 in NaHCO3-alkaline solution and forms 1-phenyl-2, 3-dimethyl-5-sulfinopyrazolium hydroxide anhydride inner salt. This reaction was applied to the standardization of iodine solution by visual titration with starch as an indicator. This method was comparable to the conventional arsenic trioxide standardization at 1035°C in both accuracy and precision, and the procedure is very simple. The gram equivalent of the reagent was 51.075 g.View full abstractDownload PDF (345K) -
Hitoshi YOSHIDA, Mitsuhiko TAGA, Seiichiro HIKIME1971 Volume 20 Issue 3 Pages 361-363
Published: March 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA new method for the differential and continuous measurement of two components by direct injection enthalpimetry was proposed. A sample solution containing two components A and B was passed alternately with water through a series of two reaction cells with a constant flow rate. In the first cell was added a reagent for A and in the second cell was added a reagent for B both by definite and stoichiometrically excessive amounts. The difference of temperature of the two cells was recorded continuously by a bridge with two thermistors. The time lag of the signal based on the intermittence of the sample and the distance between the two thermistors gave well-defined waves useful for differentiating two components.View full abstractDownload PDF (447K) -
Kazuyuki HIRANO, Shunsuke KAGEHIRA, Tomoko MIZUNO, Satoshi KAWAI, Take ...1971 Volume 20 Issue 3 Pages 364-365
Published: March 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple and rapid procedure for gas chromatography of γ-BHC in milk has been presented. Six milliliters of water were added to 1 ml of milk. The first 25 ml of its steam-distillate was shaken with 10 ml of n-hexane and then an aliquot of the extract was applied to gas chromatography. Conditions of gas chromatographic separation are shown in Fig. 1.View full abstractDownload PDF (315K) -
Tomihito KAMBARA, Tomoe KIBA, Koichi SAITOH, Masayuki OHSHIMA1971 Volume 20 Issue 3 Pages 365-366
Published: March 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe end point detection of the precipitation titration of sodium dodecylbenzenesulfonate with Zephiramine (tetradecyl-dimethyl-benzyl-ammonium chloride) was achieved by the stalagmometric measurement of the interfacial tension between mercury and the solution being titrated, in which the drop time of mercury in the solution, measured by a stop watch, was considered as the indication of the interfacial tension. A Shimadzu dropping mercury electrode, DME-type, was used in open circuit, and all the experiments was carried out at room temperature under the atmospheric conditions. By setting h=50 cm, m was 0.8394 mg sec-1 and t was 17.07, sec in pure water at 21.6°C.
The drop time values were plotted against the volume of the titrant, and the point which gives the maximal drop time was taken as the end point.View full abstractDownload PDF (254K) -
[in Japanese], [in Japanese]1971 Volume 20 Issue 3 Pages 367-376
Published: March 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDownload PDF (1906K) -
[in Japanese], [in Japanese], [in Japanese], [in Japanese], [in Japane ...1971 Volume 20 Issue 3 Pages 377-391
Published: March 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (2524K)
- |<
- <
- 1
- >
- >|