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Volume 26, Issue 12
Displaying 1-16 of 16 articles from this issue
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Akemi YASUI, Chuichi TSUTSUMI1977 Volume 26 Issue 12 Pages 809-814
Published: December 05, 1977
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA simple and rapid wet decomposition method with nitric, sulfuric, and perchloric acids was adapted to various food samples. The procedure is as follows: (0.252.5)g (dry weight) of food and 10ml of concentrated nitric acid are taken into a 100ml bolosilicate glass beaker (arsenic free) and mixed thoroughly. The mixture is heated gently on hot plate-sand bath at (170220)°C covered with a bolosilicate glass watch dish (arsenic free). After subsidence of the sample foaming, the pre-decomposed mixture is cooled and 3ml of concentrated nitric acid, 2.5ml of concentrated sulfuric acid and 5ml of perchloric acid (60%) are added. The mixture is heated strongly on hot platesand bath at (300380)°C to steady boiling. If slight charring occurs, analysis loss can be prevented by immediate addition of a small amount of concentrated nitric acid. Perchloric acid is boiled off and residual sulfuric acid is concentrated to less than 1ml. The residue is washed into a 25 or 50ml volumetric flask with 3N hydrochloric acid after cooling. Arsenic is then determined by arsine generation-atomic absorption spectrophotometry. It takes (1.52.0) hrs to accomplish the decomposition. Recoveries of inorganic arsenic (arsenic trioxide) or organic (p-arsanilic acid) added to various foods were (93105) %. It was suggested that recovery of arsenic was independent of matrix of food, form of arsenic and presence of large amount of sodium chloride. Precision was (58) % R.S.D. at 0.1μg arsenic trioxide and (14)% at 0.4μg. Analysis of NBS standard reference material (orchard leaves) for arsenic by this method showed a good agreement with certified value. This decomposition method would be adaptable to the determination of arsenic in almost all kinds of foods.View full abstractDownload PDF (1328K) -
Shigeki OHNISHI, Yasushi NISHIJIMA, Keiji KIJIMA, Shizuo KANO1977 Volume 26 Issue 12 Pages 814-818
Published: December 05, 1977
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSFat soluble tar dyes for cosmetic products (C.I. No.12120, 26100, 12085, 12075, 12315, 26105, 12140, 12100, 11680, 11380, 11390 and 47000) were separated on a LiChrosorb SI 100 (5μ, irregularly shaped porous silica gel) column by the isocratic elution technique. The experiment was carried out using a model 635 liquid chromatograph (Hitachi Ltd.) equipped with wavelength tunable effluent monitor. The high speed liquid chromatographic condition was as follows; column size: 4mm i.d.× 250mm, detector: VIS spectrophotometer {(420500) nm}, flow rate: 1.5ml/min. Eight tar dyes except C.I. No. 12140, 12100, 12075 and 12315 were separated with chloroform and n-hexane mixtures as eluent. C.I. No. 12140 and 12100 were separated with diethylether/n-hexane=4/96 mixture and C.I. No. 12075 and 12315 were separated with acetone/n-hexane =9/91 mixture as eluents, respectively. These methods were suitable for the quantitative analysis. The plots of peak height vs. amount of tar dyes were linear with the injection volume of 5 microliters or less without a lowering of column efficiency. The recoveries from wax base of lip sticks ranged from 91.9% to 97.0%. Permanent orange was only detected from commercial lip sticks and its contents were (0.0841.69)%.View full abstractDownload PDF (831K) -
Fumio YAMAGATA, Hisataka KASAI, Tsuneo OKUYAMA1977 Volume 26 Issue 12 Pages 819-824
Published: December 05, 1977
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSWe tried to develop an estimation method for γ-carboxyglutamic acid in a protein. A proposed analytical method is as follow. Hydrolysis of a peptide or a protein {(0.51.0)mg} was performed with 0.1ml of 2.5 N NaOH at 110°C for four to twenty four hrs. The hydrolyzate is neutralized to pH 3.25 with 0.26ml of 1 N HCl and lyophilized. The lyophylized sample was dissolved in 1.5ml of 0.1 N Na-citrate buffer (pH 3.25). 0.5ml of the sample solution was analyzed by an automatic amino acid analyzer (with acidneutral column). γ-Carboxylglutamic acid was eluted at the interval of (20±0.5)min after the introduction of the sample, where aspartic acid was eluted at 46min site. The color value was 0.39 of that of glutamic acid. The overall recovery was (98±3)%. The method was tested with several γ-carboxyglutamic acid containing peptides. It is known that there are γ-carboxylglutamic acid in prothrombin and all of them are localized in the N-terminal part of the protein and none are in the C-terminal part (thrombin). From the application results of the present method, about ten residues of γ-carboxyglutamic acid was found in prothrombin as well as in N-terminal peptides, prepared by two different procedures and none were found in thrombin and also in serum albumin, which was used as a control substance.View full abstractDownload PDF (1052K) -
Yoshimasa TANAKA, Yutaka SAITO, Kazutaka NISHIMURA, Mariko NAKASHIMA1977 Volume 26 Issue 12 Pages 824-828
Published: December 05, 1977
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe zirconium complex (APR-Zr) of 1-(4-arsonophenylazo)-2-naphthol-3, 6-disulfonic acid (APR) reacts with fluoride ion in an acid solution to give a coloration corresponding to the amount of fluoride. The coloration was caused by the liberation of APR from insoluble APR-Zr. By using this reaction, a new spectrophotometric method for the determination of fluoride ion has been investigated. Five milliliter of a sample solution containing less than 25μg of a fluoride ion was taken in a test tube with glass stopper and 2ml of 1 N hydrochloric acid and 5mg of reagent powder (APR-Zr 0.1g +lactose 1.1g) were added. The mixture was shaken for 10 minutes and was filtered. The absorbance of the filtrate was measured at 482nm against the reagent blank. The colored solution containing APR was very stable within 24 hours. Beer's law holds for (225)μg of fluoride ion per 5ml. The presence of iron (III), aluminum, chromium(III), thiosulfate, phosphate and sulfide causes an error. The composition of APR-Zr was investigated by the gravimetric analysis of zirconium content of zirconium complexes of APR and related compounds. APR-Zr is the polymer which contains chlorine and the molar ratio of APR, zirconium and chlorine was 4 : 5 : 4.View full abstractDownload PDF (687K) -
Study of solvent synergism for the selective extraction. ITaitiro FUJINAGA, Toshitaka HORI, Yoshihiro KANADA1977 Volume 26 Issue 12 Pages 829-833
Published: December 05, 1977
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSTwo phase separation behaviour was investigated with such three component systems as n-butanol-water-cyclohexane and methyl isobutyl ketone-water-cyclohexane, and the results are discussed by using phase diagrams. In these solvent systems, cyclohexane acts as an auxiliary solvent against n-butanol or methyl isobutyl ketone of the executive solvent and improves noticeably the phase separation between the aqueous and organic phases : for instance n-butanol and 5N hydrochloric acid are miscible in all proportion in the absence of cyclohexane, but the executive solvent, n-butanol, is easily separated from the aqueous phase by the addition of a little amount of the auxiliary solvent cyclohexane (Fig.4). The auxiliary solvent thus functions not only to decrease solubility of the executive solvent into aqueous phase, recovering enough volume as the organic phase, but also to increase selectivity in solvent extractions. For example, by the aid of cyclohexane, phosphomolybdic acid can be separated purely from silicomolybdic acid and molybdic acid. These synergistic effects of the auxiliary solvent should. always be considered in practical separation and concentration of trace components by solvent extraction. In such a case, also use was made of the phase diagram which manifests the actualy separating volume of two phases composed of three component solvents.View full abstractDownload PDF (835K) -
Satoru KUROSAWA1977 Volume 26 Issue 12 Pages 833-839
Published: December 05, 1977
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSTo improve the reliability of the analytical results of garnet epitaxial films by electron probe microanalysis (EPMA), the analytical conditions and sample preparing methods for plasma emission spectroscopy are discussed, and the deviation of analytical values between plasma emission spectroscopy and EPMA is compared. The chemical etching and sputtering methods are useful to separate the garnet epitaxial film from the gadolinium gallium garnet (GGG) substrate, and the epitaxial film with 1 1/4, inches diameter and 5 μm thickness can be analyzed by plasma emission spectroscopy. The coefficient of variation was 5%. The correction methods of EPMA analytical values are discussed. The optimal standard for gallium was GGG. The maximum deviation of the analytical values between plasma emission spectroscopy and EPMA was 3 wt.%.View full abstractDownload PDF (1066K) -
Tadaaki MIZOGUCHI, Hajime ISHII1977 Volume 26 Issue 12 Pages 839-843
Published: December 05, 1977
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe effects of solvents and chelating agents on the determination of cobalt and nickel by the titled method were investigated systematically. Cobalt (260 ng) was extracted quantitatively into 5 ml of chloroform in the pH ranges: 2.66.3 (DDTC), >3.0 (1-nitroso-2-naphthol) and >4.6(PAN), whereas nickel (500 ng) was extracted in the pH ranges: 3.56.3 (DDTC), 6.77.7 (oxine), 6.18.7 (oxine-pyridine), >6.5 (1-nitroso-2-naphthol), >5.5 (1-nitroso-2-naphthol-pyridine) and >3.8 (PAN). When chloroform was used as an extracting solvent, the relative atomic absorbance values were as follows: APDC 103, 1-nitroso-2-naphthol 102, PAN 100 and DDTC 89 for cobalt, and 1-nitroso-2-naphthol 124, 1-nitroso-2-naphthol-pyridine 113, oxine-pyridine 110, APDC 106, PAN 100 and DDTC 79 for nickel. The ashing time required for obtaining a maximum absorption signal was as follows: oxine 45, APDC 50, PAN 50, DDTC 70 and 1-nitroso-2-naphthol 100 s at about 400°C. The atomic absorbance was changed also with organic solvents used. An extraction system of PAN-chloroform was recommended for the simultaneous determination of cobalt and nickel. The coefficients of variation of this method for cobalt and nickel were 3.4 and 3.8%. respectively. This method was not interfered with 1 mg each of Ag(I), Al(III), Ca(II), Cd(II), Cr(III), Fe(III), Mg(II), Mn(II), Mo(VI), Pb(II), V(V) and W(VI), or 100 μg of Cu(II), Hg(II) and Zn(II). The method was applied to the analysis of commercial reagents, steel and ores.View full abstractDownload PDF (895K) -
Kunihiro WATANABE, Akio FUJIWARA, Mitsumasa SAKAI, Kyozo KAWAGAKI1977 Volume 26 Issue 12 Pages 844-848
Published: December 05, 1977
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe solvent extraction-spectrophotometric determination of cobalt with salicylideneamino-2-thiophenol (SATP) was studied. Under the optimum conditions Beer's law was obeyed up to 65μg cobalt in 10ml of chloroform. The molar extinction coefficient was 1.7×104 1 mol-1, cm-1 (325nm). When the pH of the aqueous phase was in the range of 6.37.0, a constant absorbance was obtained, and the extractability was greater than 99%. Since many elements interfered with the determination of cobalt, a procedure for the removal of the interfering ions was developed. Copper was masked with thiourea, and vanadium masked with triethanolamine, respectively. Nickel was separated by back-extraction with dilute hydrochloric acid. The standard procedure is as follows: Take (1030)ml of a sample solution containing less than 65μg of cobalt. Add 1ml of buffer solution (1 M acetic acid and 1 M sodium acetate) and adjust the pH to 6.5. Then add 1ml of 0.1% SATP (ethanol solution) and dilute to about 50ml with water. Extract the cobalt chelate with 10ml of chloroform by shaking for 3min. Measure the absorbance of chloroform phase at 450nm (the molar extinction coefficient, 9.4×10 1 mol-1 cm-1). The modified method was applied to the determination of cobalt in high speed steel. A large amount of the iron was removed by MIBK extraction before the cobalt determination. Relative errors were as low as 1% to 3%.View full abstractDownload PDF (789K) -
Thin-layer chromatography and liquid chromatography. IITamotsu OKUMURA1977 Volume 26 Issue 12 Pages 848-855
Published: December 05, 1977
Released on J-STAGE: January 19, 2010
JOURNAL FREE ACCESSLiquid chromatographic separation was investigated by reversed phase partition chromatography of eight kinds of cephalosporin compounds, 7-aminodesacetoxycephalosporanic acid (7-ADCA), Cephalexin (CEX), 7-aminocephalosporanic acid (7-ACA), Cephalothin (CET), Cephaloglycine (CEG), Desacetylcephalothin (DACET), Ethoxycarbonyl desacetylcephalothin (ECDACET), Cephaloridine (CER). Prior to reversed phase liquid chromatography (LC) with dimethylsilanised silica gel columns packed by balanced density slurry method, reversed phase thin-layer chromatography (TLC) with the same stationary phase was performed to obtain suitable liquid chromatographic conditions for separation of these compounds. Five solvent systems and five kinds of LC packings were tested: methanol-water, acetonitrile-water, acetone-water, dioxane-water and tetrahydrofuran-water; aminopropyl-, cyanopropyl-, dimethyl-, octyl-and octadecyl-silanised silica gels. Among these, a combination of methanol-water and dimethylsilanised silica gel column was found to effect satisfactory separation in liquid chromatography when used in the solvent ratio (1 : 4). The use of ion-pair chromatographic method was effective for the sharp separation of CET from 7-ACA in LC. Correlation of mobility between TLC (Rf) and LC(R) was obtained {R_??_1.05Rf(n=7), correlation analysis:y=1.0275x+0.0513, γ=0.9153**, n=7}, and direct transfer of chromatographic systems from TLC to LC for separation of cephalosporin compounds was confirmed.View full abstractDownload PDF (1147K) -
Ryota SHINOHARA, Minoru KOGA, Junko SHINOHARA, Teiji HORI1977 Volume 26 Issue 12 Pages 856-861
Published: December 05, 1977
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSFor the analysis of water for trace organics procedure of sample treatment to extract and concentrate the organics with XAD-2 resin was studied. At the levels of 10 ppb and 20 ppt the extraction and the concentration method were tested for 60 organic compounds including polycyclic aromatics, n-alkanes, phthalates, chlorinated benzenes, phenols, fatty acids, fatty acid methylesters, and steroids possibly found in surface waters. To 5 1 purified distilled water, 50 μg or 100 ng of each compound was added. After mixing the solution was passed through the XAD-2 resin column. The absorbed. organics were eluted from the resin with 100 ml diethylether and then the eluate was concentrated to 1 ml in a Kuderna-Danish evaporator. In ppb levels the organics were determined by GC-FID method and their average recovery was 83%. In ppt levels the analysis was performed by mass fragmentography and average recovery was 86%. By this method polycyclic aromatics (acenaphthene, fluorene, phenanthrene, and chrysene) and n-alkanes (C15C24) were determined in tap water. In these determinations polycyclic aromatics were found in the range of 1 ppt to 10 ppt and n-alkanes in 3 ppt to 30 ppt.View full abstractDownload PDF (932K) -
Yasuhiko FUJITA, Ken-ichi NARA, Akiyoshi ITO, Osamu MANABE1977 Volume 26 Issue 12 Pages 862-867
Published: December 05, 1977
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe determination of a mixture of azoxybenzene, azobenzene, hydrazobenzene and their 2, 2'-dichloro derivatives was studied by high-speed liquid chromatography. The column was packed with Permaphase ODS or Zorbax Sil and eluted with (5060)% aqueous methanol solution or n-hexane. The flow rate was adjusted to (0.360.42)ml/min and eluents were monitored at 240nm and 254nm. Under these conditions, all compounds were thoroughly separated. On the quantitative analysis with the ODS column, the calibration curves gave straight lines. The coefficient of variation was below 2% and the recovery of mixed sample was better than 98%. Both trans and cis isomers of azobenzene and its 2, 2'-dichloro derivatives were also separated and determined. The equilibrium ratio of trans isomer/cis isomer of 2, 2'-dichlorobenzene in methanol solution by visible ray irradiation was 52/48.View full abstractDownload PDF (788K) -
Takayoshi YOSHIMORI, Norio KATOH, Takashi SHIOTA, Toshibumi HOSHINO1977 Volume 26 Issue 12 Pages 868-870
Published: December 05, 1977
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSMicroamounts of carbon compounds in argon, nitrogen, oxygen and standard gases of carbon monoxide (SRMs from NBS) were determined by a combustion-nonaqueous titrimetric method. The sample gas was oxidized with copper (II) oxide at 700°C. Then, carbon dioxide produced was absorbed with N, N-dimethylformamide containing 5% of monoethanolamine. The absorbent was titrated with the standard benzene-methanol solution of tetra-n-butylammonium hydroxide {(0.0030.001)M} using thymolphthalein as an indicator. The standard solution was standardized against benzoic acid. Carbon compounds of as low as (0.21) ppm (molar fraction) could be determined in argon and nitrogen. Much carbon compounds could be found in oxygen. One sample contained 6 ppm of carbon dioxide and 11 ppm of other carbonaceous materials. The results of the analysis of the standard gases from NBS were coincided excellently with its certified value for the sample of 47 ppm of carbon monoxide. The results for the sample of 9.7 ppm, however, were 0.7 ppm higher than its certificated value. Two reasons may be considered for this discrepancy. First, the gases were prepared on Nov. 1973, and analyzed here 2 years after its certified date. Secondly, because total amount of carbon compounds can be determined by this method, there may be the influence of carbon compounds in the nitrogen used as the diluent of the standard gas.View full abstractDownload PDF (555K) -
Hiroki OHURA, Sumio YAMASAKI1977 Volume 26 Issue 12 Pages 870-872
Published: December 05, 1977
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA method for the determination of selenocyanate ion by square-wave polarography was studied. Selenocyanate ion in neutral sodium nitrate medium produced three peaks on the square-wave polarogram. It was convenient to use the first anodic peak at-0.07 V vs. Hg pool for the determination of selenocyanate over the range of (1 × 10-46× 10-4)M. The recommended procedure was as follows: to a sample solution containing up to 6 × 10-4M of selenocyanate ion in 50 ml measuring flask, 25 ml of 4 M sodium nitrate and 5 ml of 0.05% gelatin were added, and the pH of mixture was adjusted with 0.01 M sodium hydroxide or 0.01 M perchloric acid to the range 5.58.5. Polarographic measurement was carried out by using the solution after bubbling nitrogen gas for (1015) min at 25°C. The peak height at-0.07 V was approximately constant in sodium nitrate concentration between 1.5 and 2.8 M. The coexistence of some anions and organic compounds except for thiosulfate and nide did not interfere. The interference from cyancyaide ion could be avoided by addition of formaldehyde.At concentrations of the selenocyanate ion higher than 7 × 10-4 M, two anodic peaks are observed at more positive potential than-0.07 V.View full abstractDownload PDF (427K) -
Masahiro UCHIYAMA, Michiko YAMAGUCHI1977 Volume 26 Issue 12 Pages 872-874
Published: December 05, 1977
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA fluorophotometric determination of phenols in waste water was developed. Sample water was distilled and the total phenols in the distillate was measured spectrofluorophotometrically at exitation, 278nm, and emission, 299nm. Various inorganic salts did not interfere, but some organic compounds, such as formaldehyde and aniline, interfered with the determination. This method was compared with an official 4-aminoantipyrine method. The good agreements were obtained. This method is useful for the research of environmental pollution because of it's accuracy and easiness.View full abstractDownload PDF (431K) -
Teruaki ISHII, Rieko OHNISHI1977 Volume 26 Issue 12 Pages 874-877
Published: December 05, 1977
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSFor determination of zinc and nickel in coal and coke by atomic absorption spectrophotometry the three following decomposition methods were applied; the high temperature ash method by electric furnace, the low temperature ash method by plazma asher, and the wet dissolution method with hydrofluoric acid, nitric acid and perchloric acid. Comparison of the three methods was made in terms of volatility losses. It was found that the amount of zinc observed was smaller by the high temperature ash method or the low temperature ash method than the amount by the wet dissolution method, while the amounts of nickel observed by each method were almost the same. The experimental results indicated that zinc had significant losses during the incineration process but nickel had not. This was confirmed by the absorption of the generated gas on the incineration process. It is concluded that the wet dissolution method is the most suitable among the three for the determination.View full abstractDownload PDF (617K) -
Problems in determination of zinc at sub-pico gram by carbon rod atomic absorption spectrophotometryTomoko HARADA, Kitao FUJIWARA, Keiichiro FUWA1977 Volume 26 Issue 12 Pages 877-880
Published: December 05, 1977
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSAlthough atomic absorption spectrometry of zinc is highly sensitive, its precision and accuracy are decreased on account of the zinc contamination from the environment or the strong interferences of concomitant acids when carbon rod is applied as the atomization tool. The authors, therefore, checked the contamination of zinc in the distilled or deionized water which is used as the media diluting the sample, and examined the acid interference in zinc atomic absorption at ppb level. In the present study, atomic absorption spectrophotometer, with a D2 lamp background compensation circuit, and a carbon rod atomizer were employed. Analytical line for zinc atomic absorption was 213.9nm, and spectral slit width was 1.1nm. Among the hydrochloric, sulfuric, and nitric acid, the hydrochloric acid most suppresses the atomic absorption peak of 0.05ng zinc. Under the coexistences of these acids, the peak height of zinc atomic absorption is complicatedly varied against the change in the ashing temperature of carbon rod. The distilled or deionized water obtained by the ordinary methods contain (0.21) ppb zinc as the contaminant. Conversely, the sub-oiled water obtained from the sub-boiling distiller by (Daiken Quartz Co., Ltd.) contain zinc below 0.02 ppb, and is suitable for the trace analysis of zinc. The sub-boiled water stocked over two weeks in the polyethylene container which was beforehand soaked in 1:1 nitric acid is free from the zinc contamination. During the sixty times of repetitions of zinc measurements in 5μl sub-boiled water, the high atomic absorption peaks ascribed to the zinc contamination sometimes appeared, which corresponded with the zinc content over 0.05 ppb. This can be interpreted as the zinc contamination in the carbon rod or the pipet used in mounting the sample. The present result suggests that the zinc determination at sub-ppb level includes unexpectable error over 100%.View full abstractDownload PDF (556K)
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