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Volume 29, Issue 4
Displaying 1-16 of 16 articles from this issue
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Masamitsu KATAOKA, Yukihiro KONDOH, Tomihito KAMBARA1980 Volume 29 Issue 4 Pages 225-228
Published: April 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe surface tension titration methods of potassium ion and some quaternary onium cations with tetraphenylborate anion {B(C6H5)-4, TPB-} were described. TPB is widely used as a precipitant of potassium and some monovalent metal ions and is known as an anionic surfactant. Surface tension was measured by the Shimadzu surface tensometer ST-1, which is based on the Wilhelmy method. Some quaternary ammonium cations which have strong surface activity were titrated directly with standard TPB solution. Potassium ion and some quaternary onium cations having small surface activity were back titrated as follows. To the sample solution was added an excess constant amount of TPB solution, the precipitate was removed by filtration, and then the excess TPB was titrated with a standard zephiramine (benzyldimethyltetradecylammonium chloride) solution. The end point showed good agreement with the color change of the titanium yellow adsorption indicator. This method is compared with argentimetric titration of the chloride ion in the quaternary onium salts. The F- and t-tests showed that there are no significant differences between the variances and means of the present and argentimetric titration methods.View full abstractDownload PDF (865K) -
Koichi TANINO, Kunika SUGAWARA1980 Volume 29 Issue 4 Pages 229-233
Published: April 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSFor the gravimetric determination of boron by using barium borotartrate precipitate, two methods have been presented. In drying-weighing method(I) boron is precipitated as borotartrate, and weighed as 4BaC4H4O6·Ba(BO2)2· 4H2O after drying at 110°C, while the precipitate, in ignition-weighing method(II), is converted to borate by ignition {(700800)°C} and weighed as Ba2BO6. Our experiments dealt with the method(II) and led to several results; (a) the above empirical formula as a weighing form (Ba2BO6) should be corrected to the formula containing about 2.5% of carbonate carbon, (b) a part of the pre-cipitate was dissolved when the precipitate was washed even with water at (510)°C, (c) the Ba/B ratio of 2:1 in the weighing form should be corrected to the ratio of 5:2, and (d) from X-ray powder diffraction data of a product ignited at (700800)°C, it was considered to be a product containing barium carbonate and barium borates. The formula of the ignition product obtained was thus determined as Ba5B2C2O14 (mainly composed of Ba4B2O7 and BaCO3). We recommend therefore the use of the calibration curves prepared under the present experimental conditions for the determination of boron by the method(II).View full abstractDownload PDF (974K) -
Kunihiro WATANABE, Hideyuki YOSHIZAWA, Kyozo KAWAGAKI1980 Volume 29 Issue 4 Pages 233-238
Published: April 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe solvent extraction of iron (II) with bismuthiol II was conducted in the presence of 1, 10-phenanthroline (phen). Iron (II) was quantitatively extracted as ion-pair into the chloroform phase over the pH range 3.59.5. The logarithm of partition constant (P) of the ion-pair was logP=3.87. The composition of the extracted ternary species was confirmed to be [Fe2+ (phen)3 (bismuthiol II-)2]. The logarithm of the stability constant (β2) for the ion-pair was found to be logβ2= 6.4. In the method of continuous variation, the differences in the absorbance between the theoretical values calculated with the constants obtained in this study and the observed values were discussed. The absorption maxima of the iron (II) ion-pair in the chloroform phase were found to appear at 360 nm and at 515nm with molar extinction coefficients of 2.53×104lmol-1 cm-1 and 1.15×104 lmol-1 cm-1, respectively. Under optimum conditions, absorbance follows Beer's law up to 25μg iron in 10 ml chloroform. The possible range of the determination is from 2 to 25μg. As many elements interfere with the determination of iron, a masking method for the interfering ions was studied. The proposed method was applied to the determination of iron in tap water. Good agreement was observed between results obtained by the proposed method and those by the conventional colorimetric method with phen.View full abstractDownload PDF (1120K) -
Hisaaki ITOH, Yoshio SHINBORI1980 Volume 29 Issue 4 Pages 239-243
Published: April 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIon chromatographic analysis of sea water for anions was studied. In sea water, Cl-, SO2-4 as the components of high concentration and F-, Br-, NO-3, etc. as those of low concentration are contained. One can easily and simultaneously determine these anions by I C method without any tedious pretreatments. The procedure is as follows: the sample (about 2cm3) previously diluted with distilled water is inserted into the micro-loop (100mm3) with a syringe, which has been washed with the eluent (2.5mM Na2CO3/3.0mM NaHCO3), then, the micro-loop is introduced into the analytical systems. The components of sample are passed through the separating column, the stripper column in which all anions are converted into acids, and are introduced into the conductivity cell and recorded. The determination of five anions (F-, Cl-, Br-, NO-3, SO2-4) was made by comparing the peak areas (peak height x half width) of sample solution with those of the artificial sea water prepared by dissolving each corresponding sodium salt. The relative standard deviations of five anions in five replicate measurements were as follows: F-: 4.2%, Cl-: 0.4%, Br-: 2.6%, NO-3: 7.6%, SO2-4: 0.7%.View full abstractDownload PDF (778K) -
Masato AIHARA, Mitsuo KIBOKU1980 Volume 29 Issue 4 Pages 243-247
Published: April 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe complexes of bismuth(III) or thallium(I) with potassium xanthates (KRX) such as ethylxanthate (KEtX), propylxanthate (KPrX), butylxanthate (KBtX), pentylxanthate (XPeX) and benzylxanthate (KBzX), can be extracted from aqueous solution into methyl isobutyl ketone (MIBK). The extracting conditions, the interferences of co-existing ions and the precision of the determination were investigated. The recommended procedure is as follows : To a portion of a test solution (prepared from a sample, e. g., human organ) is added 10ml of 10% ammonium citrate buffer solution for bismuth or 10% ammonium tartrate buffer solution for thallium respectively. The pH is adjusted to 8 with either diluted hydrochloric acid or potassium hydroxide, and then 10ml of a 5% solution of KRX is added. The extraction is performed with 10.0ml of MIBK by shaking for 3 min, and the extract is directly subjected to atomic absorption spectrophotometry at 223.1nm for bismuth and 276.8nm for thallium. The optimum pH regions of extraction are from 6.0 to 10.0 for bismuth-xanthate and from 7.0 to 12.0 for thallium-xanthate. The coefficient of variation of this method ranged from 0.12% to 0.90% for 25.0μg to 50.0μg of bismuth and from 0.31% to 0.91% for 20.0μg to 80.0μg of thallium. From sensitivity and accuracy, this method is comparable to the conventional methods with sodium diethyldithiocarbamate or ammonium pyrrolidinedithiocarbamate. Bismuth in human organs could be determined successfully by this method.View full abstractDownload PDF (930K) -
Yoshiharu TADA, Tadashi YONEMOTO, Aiko IWASA, Kiyoshi NAKAGAWA1980 Volume 29 Issue 4 Pages 248-253
Published: April 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple and rapid method for the determination of selenium in blood without prior chemical treatment is developed. This method is based on the enhancement effect of rhodium on selenium absorption, which is found in the present work. Among 35 metals investigated, rhodium showed the largest effect in enhancing, and also in preventing matrix interference on the selenium absorption. Addition of rhodium to selenium standard solutions resulted in an increase in 2.5 times as much selenium absorbance as that of unspiked solutions. When the standard solutions contained mineral acid, selenium absorbance descreased: it reduced to 1/2 or less in case that the standards were 0.1M hydrochloric acid or 1M nitric acid solutions. In the presence of rhodium, however, selenium sensitivity remaind unchanged up to the above mentioned acid concentrations. Calibration curve for the selenium standard solutions containing 100ng of rhodium and hydrochloric acid (0.12M) was linear up to 1ng of selenium. The detection limit for S/N=2 is 0.25ng, although 1% absorption (absorbance=0.0044) corresponds to 0.005ng of selenium. The procedure of the blood analysis is as follows. Place 4ml of diluent (0.01M nitric acid solution of rhodium nitrate, 100μg Rh/ml) in a 5ml measuring flask, and fill it to the mark with the blood sample. Ten μl of the diluted sample is placed in the graphite tube furnace. Optimum operating conditions are: drying at ca. 270°C for 300s, charring at ca. 1150°C for 60s, atomization at ca. 3000°C for 5s, and argon flow rate of 21/min. Background correction by simultaneous subtraction of molecular absorption was done with a continuous light source and two optical path system. Standard additions method was used. The results of our analysis of five human blood samples are that the average selenium content is 125 ng/ml (110ng/ml in the minimum case, and the maximum is 140ng/ml), and the c. v. value for each sample (10 measurements for each sample) is 5% or less.View full abstractDownload PDF (978K) -
Katsumi YAMAMOTO, Masuzi OZAKI, Kousaburo OHASHI1980 Volume 29 Issue 4 Pages 253-258
Published: April 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSolvent extraction of iron (III) with quercetin-6'-sulfonic acid was investigated spectrophotometrically. Iron (III) is extracted with quercetin-6'-sulfonic acid in the presence of antipyrine into 1, 2-dichloroethane as a Fe (III) -quercetin-6'-sulfonic acid-antipyrine which shows an absorption maximum at 430nm. The extracted complex is very stable in 1, 2-dichloroethane for a long standing. The optimal pH range for the extraction is from 3.0 to 4.0. The Fe (III): quercetin-6'-sulfonic acid : antipyrine ratio is 1:2:3. Fe (III) quercetin-6'-sulfonic acid complex may be extracted with antipyrine as an ionic-pair form, [Fe(QS)2-(H2O)2]3-·(HA+)3. Beer's law is obeyed from 0.10 to 0.70μg/ml of iron (III) in the organic phase. The molar extinction coefficient is 38000cm-1mol-1l at 430nm.View full abstractDownload PDF (1003K) -
II. Analysis of wineRyuzo TSUJINO, Yoshiharu TADA, Taketoshi NAKAHARA, Soichiro MUSHA1980 Volume 29 Issue 4 Pages 259-263
Published: April 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn the previous paper (Part I), it was found that chemical and physical interference from ethanol and glucose was almost corrected automatically with two channel atomic absorption spectrophotometer utilizing internal standard method. This technique was applied to the analysis of wine which contained mainly ethanol, saccharides and organic acids. Iron, copper, manganese and zinc in wine were determined by internal standard method by gold at various kinds of dilution ratios with water, which resulted in good agreement between the values obtained by internal standard method and those by standard addition method at every dilution ratio, while calibration curve method gave different values at every dilution ratio due to dilution effect. For chromium, lead and cadmium which were not found in wine, the internal standard method was successful as well. Internal standard method also gave good long-term reproducibility and corrected the effect of temperature of the sample solution on manganese determination. It can be concluded that trace elements in every wine could be determined with internal standard method which requires smaller sample volume and shorter time for pretreatment of the sample compared with standard addition method. This technique would be applied to the analysis of other actual samples, for example, those in the fields of food and organic chemical industories.View full abstractDownload PDF (881K) -
Akio SAKURAGAWA, Toshio HARADA, Tadao OKUTANI, Satori UTSUMI1980 Volume 29 Issue 4 Pages 264-266
Published: April 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAlthough iodine does not react with sodium azide, the following reaction is catalytically promoted in the presence of micro amounts of sulfur compounds.
2 NaN3+I2→2NaI+3N2
This catalytic reaction is applied to the photometric determination of a trace amount of sulfide ion. The sample solution (10.0ml) is placed in a 15ml glass centrifuge tube containing a precipitate of basic zinc carbonate formed by mixing 0.50ml of zinc nitrate solution {3g Zn(NO3)2·6H2O/100ml} with 0.50ml of sodium carbonate solution (1.5g Na2CO3/100ml) and 0.50ml of formaldehyde solution (37%). After shaking, the precipitate containing zinc sulfide is separated by centrifugation. Then 5.0ml of water is added to the precipitate, and the content is shaken vigorously. Three milliliters of the sodium azide solution (20g/100ml) and 2.0ml of the triiodide solution, which is prepared by mixing a mixed reagent solution (1×10-3N in KIO3 and 1N in KI) with an equal volume of 1N acetic acid, are added into the centrifuge tube. The absorbance is measured at 350 nm against water at 5 min after the addition of the triiodide solution. By this method, sulfide ion in the concentration range of (225)ppb can be determined. An interference of sulfite ion is removed by the addition of formaldehyde solution.View full abstractDownload PDF (489K) -
Shinichiro OKAWA, Bunshiro KOMINAMI, Akira KAWASE1980 Volume 29 Issue 4 Pages 267-269
Published: April 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS1-(2-Pyridylazo)-2-naphthol (PAN) reacts with Cu2+ over the wide pH range. Al:1 (metal-toligand ratio) chelate with an absorption maximum at 555nm is formed in acidic solution, and a 1:2 chelate (abs. max. 558nm) in alkaline solution. Both chelates are insoluble in water, but can be solubilized in the presence of non-ionic surfactants. EDTA titrations of metals with PAN and Cu-PAN indicators are therefore facilitated with them. The optimum conditions for such titrations, and especially the rate of color change in the course of the titration of Cu2+ with PAN, were studied. The rate (obtained with the assumption of a pseudo-first order law) is increased by the surfactants such as Triton X-100 and Brij 35 all over the course of titration, and the addition of dioxane is effective only near the end point. In the presence of Triton X-100 surfactant, Pb2+ can be titrated with Cu-PAN indicator at pH 3.44.3twice as quickly as in the absence, Ni2+ can be titrated at pH3.5 with a very sharp end point in the presence of Brij 35 at 80°C, where Triton X-100 was ineffective because of its low cloud point.View full abstractDownload PDF (432K) -
Naobumi OI, Osamu HIROAKI, Hiroo SHIMADA, Masao HORIBA, Hajimu KITAHAR ...1980 Volume 29 Issue 4 Pages 270-272
Published: April 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAlthough s-triazine derivatives of amino acid esters, dipeptide esters and tripeptide esters are very valuable as the thermostable optically active stationary phases for the gas chromatographic separation of amino acid. enantiomers, their resolving power is rather unsatisfactory. To improve such property, a new s-triazine derivative of the amino acid amide, N, N', N"-[2, 4, 6-(1, 3, 5-triazine) triyl] tris (Nα -lauroyl-L-lysine-t-butyl-amide) (I) was synthesized. Several N-TFA-DL-amino acid isopropyl esters were resolved with good sepa-ration factors on a glass capillary column (0.25mm i. d.×40m) coated with the compound (I). In relation to the separation of amino acid enantiomers, this new compound (I) has more excellent property than the typical s-triazine derivatives of amino acid ester, dipeptide ester and tripeptide ester such as N, N', N"-[2, 4, 6-(1, 3, 5-triazine) triyl] tris (L-valine isopropyl ester) (II), N, N'-[2, 4- (6-ethoxy-1, 3, 5-triazine) diy1] bis (L-valyl-L-valine isopropyl ester) (III) and N, N'- [2, 4- (6-ethoxy-1, 3, 5-triazine) diy1] bis (L-valyl-L-valyl-L-valine isopropyl ester) (IV), which were already reported by the authors. For example, the separation factors for N-TFA-DL-valine isopropyl ester are 1.114 on (I), 1.047 on (II), and 1.055 on (III) at 110°C, and for N-TFA-DL-methionine isopropyl ester are 1.105 on (I), 1.000 on (II), 1.029 on (III) and 1.089 on (IV) at 150°C. The high separation factors on (I) allow the separation of some amino acid enantiomers with a packed column [10%coated on Shimalite W {(170200) mesh}, 0.5mmi. d.×2.8 m]. This compound (I) shows rather high thermal stability, and its maximum permissible operational temperature is about 150°C. Moreover, due to its relative low melting point { (9395)°C}, the column is effective over a wide range of temperature. It is concluded that this new compound (I) is very available as an optically active stationary phase for gas chromatographic separation of amino acid enantiomers.View full abstractDownload PDF (557K) -
Shigeki OHNISHI, Takashi SATO, Toru YONEYA1980 Volume 29 Issue 4 Pages 272-275
Published: April 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSHigh speed liquid chromatographic analysis of isopropylmethylphenol (3-methyl-4-isopropylphenol) on Nucleosil 5NH2 (5μm, Macherey-Nagel) was studied. The condition was as follows; column size: 4mm i.d.×250mm, detector: fluorescence spectrophotometer (exciting wavelength: 280nm and fluorescence wavelength: 305nm), eluent: 10% ethanol- hexane, flow rate: 1.16ml/min. column temperature: 40°C.Determination was carried out successfully by using thymol or estradiol as an internal standard. The plots of peak height ratio vs. amount ratio (isopropylmethylphenol-thymol or estradiol) were linear between 2.5ppm to 12.5ppm. The experimentally prepared hair tonic and cream were diluted (1:100) with ethanol and dehydrated with anhydrous sodium sulfate. Thymol (5ng/μl) or estradiol (20ng/μl) was incorporated into this mixture as an internal standard. The averaged recoveries from hair tonic and cream ranged 100.5% to 100.6% and c. v. (%) were 1.25 to 1.02, respectively. This method is very simple, accurate and selective, therefore it is applicable to determine isopropylmethylphenol in cosmetic products at routin analyses.View full abstractDownload PDF (641K) -
Determination of copperHajime ISHII, Katsuhiko SATOH, Hidemasa KOH1980 Volume 29 Issue 4 Pages 276-277
Published: April 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIt has been found that the water-soluble porphyrins such as α, β, γ, δ-tetrakis (4-sulfophenyl) porphine [T(4SP)P] or α, β, γ, δ-tetrakis(1-methylpyridinium-3-yl) porphine [T (3-MPy) P] and their metal complexes can be extracted quantitatively into organic solvent in the presence of suitable counter ions, and that only the complexes can be extracted selectively under a suitable condition. On the basis of this finding, highly sensitive extraction-spectrophotometric methods for the determination of ultramicro amounts of copper, zinc, lead, cobalt, manganese and palladium have been developed. As an example, two determination methods for copper are described here. In one of them, a copper (II)-T (4-SP)P complex is extracted into benzene in the presence of trioctylmethylammonium chloride (Capriquat), and in another, a copper (II)-T (3-MPy)P complex is extracted into 2 nitropropane in the presence of perchlorate ions. In either method, a straight-line calibration curve was obtained. The sensitivity for 0.001 absorbance was 0.138ng Cu/cm2 in the T (4-SP)P method and 0.159 ng Cu/cm2 in the T (3-MPy)P method.View full abstractDownload PDF (425K) -
Tsutomu FUKASAWA, Takeshi YAMANE, Shoji KOBAYASHI, Ryoji KIKUCHI1980 Volume 29 Issue 4 Pages T21-T24
Published: April 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDifferences in adsorption property were studied among the same kind of strongly basic anion exchange resins, i.e., Diaion SA 100, Dowex 1 and Amberlite CG 400, using some trace elements. Adsorptivities of chloride and iodide ions, as strongly adsorbed elements, on those resins were examined in strongly alkaline solutions, and vanadium ion as an weakly adsorbed element in a H2SO4-H2O2 medium. Significant differences were observed among Dv, values of those elements obtained by use of the resins of different manufacturers. A considerable difference was also observed between elution curves of vanadium by use of different lots of resin from the same manufacturer. It is shown that sufficient care must be taken in the use of ion exchange resin for analytical separation and/or concentration of elements.View full abstractDownload PDF (729K) -
Taitiro FUJINAGA, Satoshi OKAZAKI, Ikko SAKAMOTO, Kaoru MASUDA, Heung ...1980 Volume 29 Issue 4 Pages T24-T28
Published: April 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe purification method of acetylacetone (H-AA) has been developed for use as a solvent in electro chemical studies. The commercial H-AA, which contains water, acetone and acetic acid in the range of (0.030.05)v/v%as determined by gas chromatography, was purified by shaking with calcium hydride, followed by distillation under reduced pressure (at ca. 25mmHg and ca. 50°C) in the nitrogen gas atmosphere. The electrolytic conductivity, dielectric constant and viscosity of the purified H-AA were 1×10-8S cm-1, 27.20 and 0.694cP at 25°C, respectively. The water content of the purified H-AA was. ca. 0.01v/v %, but acetone and acetic acid were not detected. Perchlorates of lithium, sodium, and tetrabutyl ammonium (TBAP), and bromide of tetrabutyl ammonium are soluble in H-AA to the extent of more than 1M. The useful potential range in 0.1M TBAP-H-AA is (-0.2-2.25)V at the dropping mercury electrode, and (+0.9-2.35)V at the stationary Pt microelectrode, vs. Ag/0.1M AgClO4 (H-AA). From the conductivity measurements, it is found that alkali metal ions are not strongly solvated in H-AA as in the case of acetone and 2, 2, 2 trifluoroethanol (TFE), and that their salts form contact ion-pairs. On the other hand, small anions such as Cl- and Br- are solvated to a great extent due to the effect of the enol form of H-AA, and, thus, the ion-pairs of tetrabutylammonium halides in H-AA are found to be solvent-separated like those in TFE. Thus, the solvation of H-AA towards cations and anions is very similar to that of TFE which is nearly isodielectric to H-AA and known to solvate anions very effectively through hydrogen bonding.View full abstractDownload PDF (902K) -
Akira ONUMA1980 Volume 29 Issue 4 Pages T29-T30
Published: April 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe methylene blue can be formed by the reaction of hydrogen sulfide with p-aminodimethylaniline and extracted into nitrobenzene from the aqueous solution acidified with sulfuric acid. Using these facts, micro amounts of sulfur in iron and steel can be determined by the following analytical procedure: Dissolve the sample (S<5μg) in nitric acid and hydrochloric acid mixture. Add purified perchloric acid and evaporate to fume. Cool and add hydrochloric acid and then evaporate to dryness. Dissolve the residue in hydrochloric acid. Reduce the sulfate in the solution by using hydroiodic acid and hypophosphorous acid mixture. Collect the hydrogen sulfide evolved in zinc acetate solution. Add p-aminodimethylaniline and ferric ammonium sulfate to the solution, and extract the methylene blue formed with nitrobenzene. Filter the organic layer with a dry filter paper, and measure the absorbance at 665nm.View full abstractDownload PDF (322K)
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