All issues
Volume 37, Issue 9
Displaying 1-12 of 12 articles from this issue
- |<
- <
- 1
- >
- >|
-
Takako MANO, Shinji CHUSHI, Keiichiro HOZUMI1988 Volume 37 Issue 9 Pages 445-448
Published: September 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSOrganic samples containing inorganic ingradients have been plasma ashed currently in a glow discharge region of a plasma chamber equipped with an external electrode system. In spite of the so-called low-temperature ashing condition, ion chromatographic analysis of the residual ash indicated very low recovery for chloride or bromide in a sample containing known quantity of NaCl or NaBr and a part of the individual halogenide was converted to oxyhalogenide. The total recovery of the halogen species was low. This low recovery seems to be caused by a violent attack of kinetic electron and ion onto the ashed sample placed within the glow discharged oxygen. Therefore, a modified plasma chamber equipped with an internal parallel electrode system was constructed, in whcih a lower electrode served for a sample container on which a stainless steel mesh (ca. 30 mesh) was installed for electrostatic shielding of the glow discharge. Plasma ashing was thus carried out essentially with atomic oxygen. Although a small quantity of oxyhalogenide was found even with the new apparatus, quantitative recovery of the total halogen species was obtained from organic samples containing known quantity of halogenides.View full abstractDownload PDF (608K) -
Katsushige TAKAMI, Tameo OKUMURA, Hiroyasu YAMASAKI, Masao NAKAMOTO1988 Volume 37 Issue 9 Pages 449-455
Published: September 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSTriphenyltin and tributyltin compounds (TBT, TPT) in fish and shellfish were determined by a combination of clean-up with ion exhange resins and capillary GC equipped with a flame photometoric detector (FPD). A homogenized sample was extracted with 1 M hydrochloric acid-methanol/ethyl acetate (1:1, v/v) and the extract was filtered under reduced pressure. Organotin compounds (OTC) in the filtrate, which was mixed with 10% sodium chloride solution, were extracted with hexane/ethyl acetate (2 :3, v/v). The organic layer was dehydrated with anhydrous sodium sulfate, and then made up to 10 ml with ehtanol. The sample solution of 510 ml was passed through cartridge (A) packed with an anion exchange resin and cartridge (B) packed with a cation exchange resin. The OTC trapped in cartidge (B) were eluted with 1 M hydrochloric acid/methanol. The eluate was mixed with water and the OTC were extracted twice with 2.5 ml of hexane/cyclohexane (1 :1, v/v). The hydrogenenation of OTC was performed by mixing the organic extract with 2.5% sodium tetrahydroborate/ ethanol. The reactent was mixed with water and shaken for 2 min. Five μl of the organic layer was analyzed by GC. GC conditions were as follows: column; Ultra-1 (cross linked methyl silicone gum, 0.32 mm i.d. × 25 m, df=0.52 μm), column temp.; 80 °C (4 min)-8 °C/min-250 °C, nitrogen (2.5 ml/min), detector; FPD (Sn-filter). OTC in the fish samples were identified on the basis of retention time and determined by peak height method. Further confirmation was performed by GC/MS spectra. Recoveries of OTC from a fish sample were 83.390.8% and the relative standard deviation were 6.812.1%. The limits of determination were 0.01 μg/g for TBT and 0.02 μg/g for TPT, when 5 g of the sample was analyzed.View full abstractDownload PDF (984K) -
Hitoshi ZUMI, Yoshihito SUZUKI1988 Volume 37 Issue 9 Pages 456-459
Published: September 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA semi-micro HPLC of fatty acids coupled with a resonance Raman detection system is described. 4-Nitro-4'-N·methyl, N·β-hydroxy ethylaminoazobenzene (NHA) was synthesized as a labeling reagent for sensitive Raman detection. Fatty acids were activated with oxalyl chloride, followed by derivatizing with NHA reagent. Since these NHA esters in methanol exhibited their absorption maximum at 468 nm in visible region, resonance Raman effect could be obtained by 488.0 nm line of an Ar laser. HPLC separation of NHA esters of long chain fatty acids was accomplished on a μS-Finepak C18 (1.5φ×250 mm) and 95% acetonitrile in water as a mobile phase at a flow rate of 100 μl/min. Chromatograms were obtained by measuring the intensity of Raman scattering at 1343 cm-1 with 488.0 nm line of an Ar ion laser at 300 mW output. By this procedure, calibration curve (relative peak height for pentadecanoic acid as the internal standard) was linear in the concentration range of 5 ppm to 200 ppm for lauric acid. The relative standard deviation of relative peak height (n=5) was 4.4% at 20 ppm of lauric acid.View full abstractDownload PDF (581K) -
Masako MIZUNO, Yoshiaki OKAJIMA, Junkichi MIURA, Hiroyuki MIYAGI1988 Volume 37 Issue 9 Pages 460-465
Published: September 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSPerformances of 2 μm porous polymer packings, styrene-divinylbenzene co-polymer (S-DVB) and S-DVB with quaternary ammonium were presented. Correlation between chromatographic preformances and physical properties such as specific surface area and ion exchange capacity was studied. The column packed with 2 μm S-DVB showed 12 μm of height equivalent to a theoretical plate (HETP), which was 50 and 30% decrease as compared with 6 μm and 3 μm respectively. The column packed with S-DVB with quaternary ammonium of 2 μm or 3 μm showed 10 μm of HETP, which was 50% decrease as compared with 6 μm. By decreasing the particle diameter less than 3 μm, improvement of chromatographic efficiency was not clear. It was suggested that the minimum possible particle diameter of porous polymer packings was 23 μm for HPLC.View full abstractDownload PDF (968K) -
Shigeki ABE, Masatoshi ENDO1988 Volume 37 Issue 9 Pages 466-470
Published: September 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple spectrophotometric method that requires no computational kinetic data-fitting process is developed. For differential determination of Fe(II) and Fe(III) in aqueous samples, we utilize the fact that the aerial oxidation of Fe(II), which proceeds first order in acetate buffer media, is suppressed by decreasing the.pH; it requires about one day for complete Fe(II) oxidation at pH 4. In the present method, Fe(III) is measured spectrophotometrically as Fe(III)-Tiron complex. The recommended procedure is as follows: a mixture of 20 ml of 1 M acetate buffer(pH 4) and 5 ml of 5% Tiron is diluted to (50-x)ml with water. The reaction is started by addition of x ml of sample solution (x=225ml). The absorbance of Fe(III)-Tiron complex at 680 nm (isosbestic point) is measured immediately and after standing one day. The absorbance values at the beginning(A0) and at equilibrium(A0) correspond to Fe(III) and Fe(II + III) concentrations, respectively. The molar absorptivity of Fe(III)-Tiron complex is 2.01×103 1 mol-1cm-1 and it obeys Beer's law at 130 ppm of Fe. No precise pH preadjustment is required for the sample solutions. The method is applied to Fe-rich groundwaters. The problem of sample deterioration during storage is discussed; the behavior of Fe(II, III) in acidified solutions with sulfuric acid is shown.View full abstractDownload PDF (913K) -
Keiko OHSAWA, Yoshihiro YOSHIMURA, Katsumi UCHIYAMA, Rieko OHKI, Kazuo ...1988 Volume 37 Issue 9 Pages 471-475
Published: September 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSTributyltin chloride (TBTC) and dibutyltin dichloride (DBTC) in yellow tail, sea bream, salmon and sea tangle were simultaneously determined by GC equipped with an electron capture detector. Samples (10 g) were homogenized in saturated sodium chloride solution, and then 0.3 M hydrochloric acid was added in order to convert tributyltin and dibutyltin compounds into TBTC and DBTC. TBTC and DBTC in the homogenates were extracted with hexane/diethyl ether (3/1). The extract was poured absorbed on florisil(3 g), washed with acetone, then eluted with hexane/diethyl ether/acetic acid (75/25/1) and was concentrated by a rotary evaporator. The extract was dissolved with hexane to make up 5 ml. The optimun analytical conditions were as follows; column, Thermon-Hg (25m × 25 mm i.d.) fused silica column; columm temperature, 160 °C; injection port and detector, 200 °C; carrier gas, nitrogen, 1.25 kg/cm2; split ratio, 1/4.5; makeup gas, 50 ml/min. Detection limits of TBTC and DBTC were 0.77 ng/g and 1.15 ng/g, respectively. The relative standard deviations of TBTC (3.0 ng) and DBTC (3.0 ng) were 3.8% (n=10) and 4.1% (n=10), respectively. The maximum concentration of TBTC and DBTC in yellow tail, sea bream, salmon, and sea tangle were 1.61 ppm and 13.60 ppm, respectively. This result suggests that organotin contamination of the sea is spreading to a vast extent.View full abstractDownload PDF (743K) -
Tsuneko OGINO, Hideki OGIUCHI, Toshiyuki HOBO, Hiroshi OGINO1988 Volume 37 Issue 9 Pages 476-480
Published: September 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe racemization method using amino acid in teeth is utilized for the estimation of age of unknown corpses in forensic medicine. A series of experiments were carried out to evaluate analytical errors depending on hydrolysis conditions of coronal dentin from the third molars of human teeth. The results of these experiments revealed that aspartic acid was racemized with the acid concentration expressed by the following equation: D/L =0.0168 +0.00103× [HCI]. In addition, it was shown that the racemization rate of aspartic acid during the hydrolysis (at 100 °C, in 6 M HCI) was 0.00085 h-1. If the hydrolysis is conducted under the proposed conditions, the variations will have a negligible effect on the estimation of age.View full abstractDownload PDF (710K) -
Tetsuo AMEMIYA, Takuya HAYASHI, Yoshimasa NIHEI1988 Volume 37 Issue 9 Pages 481-484
Published: September 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple and rapid method of liquid phase chemical modification has been developed for the XPS determination of-C=C-on polybutadiene surface by addition of Br. Polybutadiene was immersed into 7.6% (v/v) Br2/CCl4 for 10 min and washed with CCl4 for 1 min, and then dried for about 12 h. As a result, -C=C-on polybutadiene surface reacted rapidly with Br. The Br labeled polybutadiene was measured by XPS. The optimum and sensitive XPS spectra were obtained in the working pressure at 10-6 Pa by operating a Mg anode at 60 W and completing measurements within 9 min to minimize the surface degradation. It was found that the addition of Br to-C=C-reached nearly to theoretical equivalence point.View full abstractDownload PDF (631K) -
Application to aluminium metalMasakazu DEGUCHI, Yoshiki KURIOKA, Kiyotoshi MORISHIGE1988 Volume 37 Issue 9 Pages 485-488
Published: September 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA fluorometric method for the determination of trace amounts of Ga with 2-hydroxy-1-naphthaldehyde-semicarbazone (2-HNS) was applied to the analysis of aluminium metal and its alloy. To a sample solution containing less than 5.0 μg of gallium, were added 0.1% sodium fluoride solution (Ga 05.0 μg : 50 μl, Ga 01.0μg: 20 μl. Ga 00.2μg: 5 μg μl), 2 ml of 2-HNS solution in DMF (Ga 05.0 μg : 0.05%, Ga 01.0 μg : 0.025%, Ga 00.2μg: 0.01%) and 1 ml of 2 w/v% ammonium acetate solution. The pH of the solution was adjusted to 3.0+0.1 with hydrochloric acid or ammonia water, and the solution was diluted to 25 ml with water. The fluorescence intensity was measured at 450 nm (λex: 395 nm) against the standard quinine sulfate solution (10, 2 or 0.5 μg/ml). Gallium was separated from interfering elements by extracting with isopropylether, and the method was then found to be applicable to the determination of gallium above 0.1 ppm in practical samples.View full abstractDownload PDF (713K) -
Tadao SAKAI, Noriko OHNO, Toshiaki MORI, Hideto SASAKI1988 Volume 37 Issue 9 Pages 488-491
Published: September 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA sensitive spectrophotometric method for the determination of Pd(II) in dental alloys is proposed. It is based on the reaction of 3-(2-pyridyl)-5, 6-diphenyl-1, 2, 4-triazine (PDT) and Pd(II) and on the formation of a 1:1 ion associate with tetrabromophenolphthalein ethylester (TBPE) which is extractable into 1, 2-dichloroethane at pH 56. A required amount of the dental alloy sample (0.10.5 g) was dissolved in 5 ml of concentrated nitric acid by heating and the resulting solution was evaporated to dryness. The residue was dissolved again in 5 ml of 1 M hydrochloric acid by heating. The solution was filtered, and the filtrate was diluted to 100 ml with 1 M hydrochloric acid. A sample solution containing up to 10 μg of Pd was transferred into a 50 ml-volumetric flask. To it, 1 ml of 5 × 10-3 M PDT solution, 2 ml of 3 × 10-3 M TBPE solution and 15 ml of buffer solution (pH 5.5) were added and the mixture was diluted to 50 ml with distilled water. After standing for 10 min, the solution was transferred into separatory funnel. It was shaken with 10 ml of 1, 2-dichloroethane for 10 min. After the organic phase was centrifuged to remove droplets of water, absorbance of the organic phase was measured at 610 nm against the reagent blank. The calibration curve was linear over the range 20200 ppb of Pd(II) and the apparent molar absorptivity was 10.8 × 104 1 mol-1 cm-1; Sandell sensitivity, 0.00098 μg cm-2; and the standard deviation, 1.5%. Although Co(II), Fe(II), Cu(II), Rh(III) and Ru(II) interfered with the determination of Pd(II) in the general procedure, these interferences could be reduced by adding appropriate masking agents.View full abstractDownload PDF (563K) -
Jyoji KUNIYA1988 Volume 37 Issue 9 Pages T87-T91
Published: September 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe thin layer chromatographic behevior of various additives for lubricating oil was studied. Zincdialkyldithiophosphates (ZnDTP) were successfully separated on a RP-8 plate based on the affinity of the alkyl groups of ZnDTPs. Development was carried out with water-acetone mixtures as a mobile phase. 2, 6-Dichloroquinonechlorimide was used as the coloringreagent. Polymer additives were separated on a RP-8 plate with dichloromethane-methanol mixtures as the solvent. Among polymer additives, polyalkylmethacrylates could be detected with spraying sulfonic acid followed by heating at 150 °C. To be removed metallic ions, an aliquot of hydrochloric acid was added to metallic detergents in benzene-methanol solution, then separation was carried out on a Silicagel-60 plate with benzene-methanol mixtures. Sulfonic acid and Pinacryptol Yellow were used for detection. Succinic acid derivertives, organic dispersants, were separated on a Silicagel-60 plate with ethylether-benzene-acetic acid mixtures. Detection was achieved by spraying ninhydrine, and heated at 120 °C in a oven. These procedures described above has been applied to the analysis of commercial lubricating oils which indicates that the TLC are useful for the separation of additives in lubricating oils.View full abstractDownload PDF (908K) -
Masakuni TAKEUCHI, Minoru HOSOYA1988 Volume 37 Issue 9 Pages T92-T95
Published: September 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe time required for the analytical procedure was shortened by simultaneous distillation with methyl borate and drying of the absorbent (1 % NaOH solution) using a home-made rapid distillation apparatus. After the dried salt had been dissolved with a mixture of hydrochloric acid-acetic acid, color was developed by the addition of Curcumin-acetic acid solution and sulfuric acid-acetic acid mixture. After stading for 20 min, the solution was diluted to 100 ml with 75 ml of methanol and 15 ml of distilled water, and the absorbance was measured at 548 nm after 10 min. The blank of absorbance could be reduced from 0.094 to 0.048 and the detection limit was reduced from 0.04 ng/g to 0.02 ng/g of boron. Concentration below 5μg/100 ml of boron obeyed the Beer's law and molar absorptivity is 1.62 × 105 1 mol-1 cm-1. Relative standard deviations for the determinations(n=6) of boron in high purity iron ( JSS 002-1, B 0.00007%) and steel ( JSS 361-3, B 0.0028%) were 8.0% and 1.8%, respectively.View full abstractDownload PDF (548K)
- |<
- <
- 1
- >
- >|