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Volume 25, Issue 11
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Organometallic compoinds. XKeiichi TANIKAWA1976 Volume 25 Issue 11 Pages 721-725
Published: November 10, 1976
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA difference in detection sensitivity of β-diketone-metal chelates by gas chromatography is produced by the difference in the metal present, irrespective of the difference in ligands or of detectors and the reason for it was examined by gas chromatography-mass spectrometry (GC-MS). When the chelates of copper (II) and iron (III), which show poor sensitivity in gas chromatography, were introduced directly into the ion source of a mass spectrometer, their ionic intensity was large but the ratio of molecular ion to total ion was smaller than that of the chelates of rhodium (III) and chromium (III), which show good detection sensitivity. When the sample was heated for gasification and collected in a gas reservior for mass spectrometry, chelates of copper (II) and iron (III) showed great disintegration of the molecular ion and a large number of fragment ion species was produced. Ratio of molecular ions to total ions was greater in rhodium (III) and chromium (III) chelates, with smaller number of fragment ions. Thus the difference in detection sensitivity according to the kind of a metal present was related to the ratio of molecular ions present to total ions of the metal chelates, and the difference in the detection sensitivity of β-diketone-metal chelates in gas chromatography is affected largely by thermal stability of the chelates rather than by ionization efficiency of FID and ECD detectors or to the stability of these chelates to ionization.View full abstractDownload PDF (861K) -
Wataru YOSHIMURA1976 Volume 25 Issue 11 Pages 726-730
Published: November 10, 1976
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA square wave polarograph of Shimadzu type PR-50 was used and the mercury pool at the electrolytic cell was used as an anode. To a solution (25 ml500 ml) containing 0.60 μg3.15μg of antimony is added 32mg of zirconium oxychloride and pH of the solution is adjusted to 9.7 with ammonia water. The precipitate is separated by filtration and then dissolved in 25 ml of 4N hydrochloric acid. The solution is diluted to 50 ml with distilled water. A portion of this solution is subjected to the polarographic determination. The results are as follows, a liner relationship exists between the antimony concentration and the wave height over the range of 0.60 μg3.15μg of antimony, zirconium hydroxide is the most effective in collecting antimony when pH is adjusted to 9.7 with ammonia water, effect of various kinds of foreign ions was examined. Bismuth, copper, and iron ions interfere remarkably, the coefficient of variation of this method is 0.79%, the temperature coefficient in this method is negative value of -0.77%/degree, it takes about 3 hours in the analysis by the present method and 0.005 ppm of antimony in a sample solution can be determined.View full abstractDownload PDF (770K) -
Mamoru TOMINAGA, Yoshimi UMEZAKI1976 Volume 25 Issue 11 Pages 731-736
Published: November 10, 1976
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA trace amount of vanadium was determined by using a heated graphite atomizer (HGA-2100). The optimum conditions were; drying at about 120°C for 60 s, charring at about 1300°C for 30 s, atomizing at about 2500°C for 20 s, and Ar flow rate of 80 ml/min. The calibration curve was linear in the range of (0.055.0)mg/l. The sensitivity (1% absorption) was 9×10-10g For the determination of vanadium (1mg/l), interferences of salts of metals, in the presence of 1000-fold amount as metal, were not serious except for cupric chloride, ferric chloride, ferric nitrate, potassium nitrate, sodium chromate, and ammonium molybdate. It is supposed that the interferences with these salts are owing to the formation of nonvolatile vanadium compounds. The addition of aluminum chloride was effective for the suppression of interferences with iron, copper, and chromate, presumably because of the increased population of vanadium atom by the formation of stable aluminum oxide. Interferences with molybdenum and potassium could not be suppressed by aluminum salts. For the determination of vanadium in water, the following method is recommended. After successive injections of 20μl of sample and 20μl of 5% aluminum chloride solutions into the graphite tube, vanadium was determined directly under the conditions mentioned above. This method gave a fairly good agreement with the standard addition method.View full abstractDownload PDF (979K) -
Yukio ONO, Yoshiko HAYAMA, Shigeyuki TANAKA1976 Volume 25 Issue 11 Pages 736-742
Published: November 10, 1976
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSMass spectrometric identification of pyrolyzates from quaternary ammonium salts was investigated with a Hitachi RMU-6E spectrometer coupled with a K-53 gas chromatograph {5% OV-101, 2m × 3 mm i. d., (100 250)°C, 4°C/min}. Gas chromatography was carried out on a Shimadzu GC5A PF equipped with an FID {5% OV-101, 2m × 3 mm i. d., (100280)°C, 4°C/min}. Aqueous solutions of alkyl- and benzyl-trimethylammonium salts, benzylethyl- and benzylphenyl-dimethylammonium salts, benzalkonium salts and alkylpyridinium salts were applied to a gas chromatograph with the temperature range of (250300)°C at the injection port. Gas chromatographic and GC-MS methods gave identical chromatograms. Long chain quaternary ammonium compounds such as alkyltrimethylammonium salts and alkylpyridinium salts gave alkyldimethylamines and alkyl halides by pyrolysis. Quaternary ammonium compounds with ethyl, phenyl or benzyl groups attached to the nitrogen atom yielded different decomposition products. The carbon-nitrogen bond cleavage occurs preferentially in the following decreasing order; benzyl>methyl>ethyl: Pyrolysis of benzalkonium chlorides at 300°C yields methyl chloride, benzyl chloride, a series of alkyldimethylamines and alkylbenzylmethylamines. The mechanisms of pyrolysis for these salts were discussed from the above results.View full abstractDownload PDF (1212K) -
Yoshikazu HASHIMOTO, Katsuyuki UENO1976 Volume 25 Issue 11 Pages 742-747
Published: November 10, 1976
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple method was developed for preparation of standard hydrogen cyanide gas of very low concentration. This method is based on generation of hydrogen cyanide from the potassium cyanide aqueous solution which was prepared with potassium cyanide and appropriate buffer agents. The gas generation bottle consists of a Greenburg-Smith impinger whose impaction nozzle is cut to be shortened so as to keep a definite distance from the surface of the solution. The bottle is connected to a preheating bottle and both two bottles are placed in a water bath with a temperature controller. The generated gas was diluted in the air stream of constant flow. The rate of gas generation depends on pH, concentration, and temperature of the potassium cyanide solution. The temperature dependence of this method is much less than that of permeation tube method. A linear relationship was seen between concentrations of the solution and those of generated gas in the air stream, in logarithmic scale. The concentration of the standard gas reached to a constant level within about 30 min after starting air flow. For example, the coefficient of variation of the concentration of generated gas is 3% at 1.24 ppm.View full abstractDownload PDF (1028K) -
Hiroshi OGINO, Shigetaka SUZUKI, Shun ARAKI1976 Volume 25 Issue 11 Pages 747-752
Published: November 10, 1976
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe following chemiluminescent reaction of nitrogen monoxide with atomic hydrogen generated by microwave discharge (2450 MHz) was applied to the determination of nitrogen oxides, NOx (NO+NO2).
H+NO+M→HNO(1A")+M
HNO (1A")→HNO (1A')+hυ
where M is a third-body molecule. The emission intensity is proportional to atomic hydrogen and nitrogen monoxide concentrations;
I=I0[H] [NO]
If [H] is made large compared with [NO], the emission intensity (I) is proportional to the concentration of nitrogen monoxide, because [H] can be assumed to be constant.
Nitrogen dioxide is rapidly reduced to nitrogen monoxide with an excess of atomic hydrogen, and nitrogen monoxide produced react with atomic hydrogen. The emission intensity is proportional to the sum of concentrations of nitrogen monoxide and nitrogen dioxide because both oxides in eqimolar yield the same response.
The apparatus consists of a microwave generator, a reaction cell, a photomultiplier (Hamamatsu TV, R-712) and an optical filter (Toshiba, VR-69). Operating conditions are as follows: Cell temperature; 35°C, Cell pressure; 5.5 torr, Microwave generator power; 50 W, Hydrogen gas flow rate; 30 ml/min, Sample gas flow rate; 70 ml/min.
The working curve is linear to the concentration of nitrogen oxides NOx up to 2500 ppm and the detection limit is about 0.1 ppm under present operating conditions.
Carbon monoxide, carbon dioxide, methane, sulfur dioxide, and nitrous oxide have little or no interference with the determination.View full abstractDownload PDF (879K) -
Hiroshi UCHIDA, Kiyoshi IWASAKI1976 Volume 25 Issue 11 Pages 752-756
Published: November 10, 1976
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA laser microprobe technique has been developed for analysis of metals below microgram amounts. Metal diethyldithiocarbamate (DDTC) was extracted into chloroform cantaining trace dithizone as coloring material, and wholly dropped on a filter paper with continuous blow of warm air. The dispersed chelate was concentrated into a center by permeation with chloroform from hem of the paper. Metals on five suitable points for analysis, selected on the colored spot, were evaporated by a laser beam, and excited by a high voltage spark discharge. Qualitative analysis could be done on the photographic plate, summing up intensities obtained on the five points. The detectable amounts were 10 ng for Pd, Ag, and Co, 100 ng for Cr, Ni, Pb, and Bi, and 1 g for Mn, Fe, Cu, Zn, Cd, In, and Tl. Quantitative analysis was examined for Ag and Pd under the suitable conditions investigated (amounts of dithizone added in chloroform and spark discharge). Calibration curves were obtained between the log amounts, from 1 ng (Pd) or 3 ng (Ag) to 300 ng, initially added into aqueous phase, and log intensity with the variation coefficient of 19.3 and 24.0% on 30 ng, respectively. Utility of internal standard method and effects of coexisting element were also discussed.View full abstractDownload PDF (936K) -
Hisashi OKA, Tsugio KOJIMA1976 Volume 25 Issue 11 Pages 757-760
Published: November 10, 1976
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSTwo procedures have been presented for the analysis of fatty acid alkanolamides by a programmed temperature gas-liquid chromatography. In the direct method, the samples were converted directly to trimethylsilyl derivatives with N, O-bis(trimethylsilyl)acetamide(BSA) and the products were analysed on a column (1m×3mm) packed with 2% of OV-1 on Chromosorb W DMCS {(80100) mesh} and operated with temperature programming from 80°C to 250°C at 8°C/min. Using the peaks of fatty acid alkanolamides, the distribution of long alkyl groups can be determined. In the hydrolysis method, the samples were hydrolysed with 6N hydrochloric acid. The resulting amine and fatty acids were converted simultaneously to trimethylsilyl derivatives with BSA and chromatographed in the same manner as the direct method. Using the peaks of fatty acids, the distribution of long alkyl groups in the original amide sample can be easily determined. These procedures have been applied successfully for determining the type of hydrophilic groups and the composition of hydrophobic groups of fatty acid alkanolamide type non-ionic surfactants.View full abstractDownload PDF (647K) -
Shizuko HIRATA, Osamu TAKIMURA1976 Volume 25 Issue 11 Pages 760-763
Published: November 10, 1976
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSea water {(45)1} was filtered with a 0.45 μm milipore filter and cadmium contained in suspended substances gathered on the filter was dissolved by conc. nitric acid. A sample solution (20 μl) was atomized by passing high electric current through the atomizer. The concentration of cadmium was determined by using of the calibration curves which were made by measuring the absorption peak heights of cadmium at 2288Å. Alkali metals which show strong background absorptions near the analytical line of cadmium did not interfere with the determination of cadmium, even in the presence of 100000-fold. This may be due to the difference of volatilities. Background absorptions by substances contained in the milipore filter and by suspended substances were corrected by using of the deuterium lamp. The sensitivity for 1% absorption was 0.2 ppb of cadmium. The coefficient of variations for the repeated analysis of 5 times was found to be within about 6%.View full abstractDownload PDF (560K) -
Masaru SATOUCHI, Tsugio KOJIMA1976 Volume 25 Issue 11 Pages 764-769
Published: November 10, 1976
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSElectron capture coefficients (K) for halobenzenes were calculated at various temperatures from data obtained by using electron capture techniques. The electron affinity(EA) of halobenzenes through a non-dissociative process and the activation energy(E) for a dissociative process were calculated from a plot of K vs. 1/T. The dissociative electron capture reaction for halobenzenes probably proceeds through anion radical intermidiates and the reaction mechanism is similar to the SN 2 displacement for aromatic compounds. In the cases of chlorinated benzonitriles and acetophenones, the electron affinity increases. The increase is probably due to the stabilization of the anion radical by the inductive effect of chlorine atom. The values of E for halobenzenes substituted with electron-accepting groups(cyano-, acetyl- and nitro-) were lower than for the non-substituted analogues. These groups appear to contribute to the resonance stabilization of the anion radical. An increase in the value of E for the methyl halobenzenes and a decrease in E for the chlorinated halobenzenes were observed.View full abstractDownload PDF (850K) -
Yuroku YAMAMOTO, Takahiro KUMAMARU, Tetsuo EDO, Junji TAKEMOTO1976 Volume 25 Issue 11 Pages 770-775
Published: November 10, 1976
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe sodium borohydride tablets were prepared by molding the mixture of sodium borohydride, kaolin and dilute ammonia water. A possible loss of arsine at the initial stage of the reduction could be avoided by wrapping the tablet with a wafer sheet. The tablets were stable at least for three weeks by storage in a desiccator. Potassium iodide was found to eliminate interferences by diverse metal ions without lowering the sensitivity and the rate of reaction. The nitrogen-hydrogen flame was useful instead of an argon-hydrogen one. The linearity of the absorbance (193.7 nm arsenic line) vs. concentration was good up to 0.05 μg/ml. The sensitivity for 1% absorption was estimated to be 0.51 μg/l and precision to be 2.5% from ten determinations of 50 ppb of arsenic. This method was applied to the analysis of water samples. Results were satisfactory when compared with those given by several known methods.View full abstractDownload PDF (1115K) -
Studies on fluorometric analysis of phenol derivatives. VIITsunetoshi KAITO, Kazuhiko SAGARA, Yuji ITO1976 Volume 25 Issue 11 Pages 776-781
Published: November 10, 1976
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSButylhydroxyanisole(BHA) reacted with 1-nitroso-2-naphthol in the presence of nitric acid and traces of sodium nitrite, to form a fluorescent product which has the maxima of the excitation and emission spectra at 467 and 552 nm in chloroform solution, respectively. Acetaminophen(AAP) also showed a similar fluorescence to BHA. Based on these results, fluorometric determination of BHA and AAP were established. A linear relationship was observed between the amount of BHA or AAP in the test solution and the intensity of fluorescence up to 20 μg. The fluorescence characteristics of similar compounds were investigated. On the deter mination of BHA, the fluorescence intensity of 2-tert-butyl-4-hydroxyanisole was equal sensitivity with that of BHA. Other antioxidants and preservatives did not interfered with the test. On the determination of AAP in pharmaceutical preparations, coexistent components such as salicylic acid derivatives, aminopyrine, sulpyrin and riboflavine did not interfered. The fluorescent products were assigned to be 8-tert-butyl-10-methoxy-5H-benzo[a]phenoxazine-5-one and 10-acetamido-5H-benzo[a]phenoxazine-5-one from their analytical data.View full abstractDownload PDF (960K) -
Jun-ichi ITOH, Makoto YAMAHIRA, Takao YOTSUYANAGI, Kazuo AOMURA1976 Volume 25 Issue 11 Pages 781-784
Published: November 10, 1976
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA new highly sensitive method for spectrophotometric determination of small amounts of lead(II) has been developed. Water-soluble porphyrin, tetraphenylporphine trisulfonic acid(TPPS), formed a complex with lead(II) ion in alkaline solution. The complex had the Soret band (ε=2.75×105) at wavelength of 464 nm, which was well separated from that of free TPPS (413 nm). The highest and constant absorbances were obtained in the range of pH 9.810.5. In the presence of 10-folds excess of TPPS, lead(II) ion formed the complex quantitatively within 1 minute at 70°C. In alkaline solutions, metal ions of Cu(II), Cd(II), Fe(II), Mn(II), Hg(II) and In(III), also formed the complexes with TPPS, and interfered with the determination. However, these metal ions, except In(III) and Mn(II), were successfully masked by cyanide ion. The recommended procedure was as follows.
Take 20 ml of sample solution containing (110) μg of lead(II) into a 50 ml beaker and add 0.5 ml of 20% potassium cyanide solution and 1 ml of borate buffer solution (pH 10.2). Heat the solution up to 70°C and add 2.5 ml of 1×10-4 M TPPS solution and allow to stand for 5 min at 70°C. After cooling to room temperature, dilute the solution to 25 ml. Measure the absorbance at 464 nm against water.
Beer's law confirmed over a range of (0.050.5) μg Pb2+ ml-1 and sensitivity (Sandell index) was 0.000947 μgPb2+ cm-2, which is more sensitive than the dithizone method (0.003 μgPb2+ cm-2). The relative standard deviation for 0.414 μgPb2+ ml-1 was 1.1%.View full abstractDownload PDF (674K) -
Hiroshi OGURO1976 Volume 25 Issue 11 Pages 785-789
Published: November 10, 1976
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn the atomic absorption spectrophotometry of chromium by using air-acetylene flame, the absorption of chromium was increased in the presence of various perchlorates, especially ammonium perchlorate, and it was increased by twice for 1.0 M ammonium perchlorate. The enhancing effect was applied to the elimination of the interferences of iron, various coexisting cations and some acids on the determination of chromium in standard steels. The absorption of chromium was increased by 11% on the presence of (50200) ppm iron but in the presence of iron above 200 ppm, that was gradually decreased with increasing the concentration of iron and that was decreased by 75% on 10000 ppm iron. Nickel, lead and molybdenum ions (100 ppm) decreased the absorption of chromium, but other common cations (100 ppm) increased it. The interferences of coexisting cations and the enhancing effects of 0.1 M hydrochloric, hydrobromic, hydroiodic, nitric and perchloric acid were eliminated by the addition of 1.0 M ammonium perchlorate, but the depressing effects of 0.1 M sulfuric and phosphoric acid were not. The calibration curve for chromium in the presence of 1.0 M ammonium perchlorate was linear in (010) ppm range with the twice sensitivity of that for chromium alone. The atomic absorption spectrophotometry of chromium in the standard steels were made by using air-acetylene flame, provided that the ammonium perchlorate was added to the sample and standard solutions in the same concentration. The analytical values in the standard steels were in fair agreement with the certificate values. The coefficient of variation by proposed method for a sample containing 1.0% chromium was 0.78%.View full abstractDownload PDF (828K) -
Masakuni ZORAKU, Yosaburo OKURA1976 Volume 25 Issue 11 Pages 790-794
Published: November 10, 1976
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSOf organophosphorus insecticides, parathion, methyl parathion, EPN and methyl demeton are legal items to be determined in industrial wastes. The former three were possible to be determined simultaneously by gas chromatography or colorimetry after extracted. into n-hexane. but methyl demeton had to be determined with another colorimetric method after extracted into chloroform. The authors have developed a method for simultaneous determination of the four insecticides as follows. The four insecticides in a 200 ml of sample solution, which was previously adjusted to pH lower than 4 with hydrochloric acid, were extracted into n-hexane containing 10% chloroform. The organic phase, after dried with dehydrated sodium sulfate, was concentrated to 5 ml with a Kuderna-Dannish distillator. To remove contaminants, such as oil, dyestuff, etc., the concentrate was applied on a column of florisil activated at 130°C for 12 hours. Elution was carried out with n-hexane containing 2% acetone for the former three, and then with a mixture of one part of acetone and two parts of n-hexane for methyl demeton. Both effluents were combined and concentrated. An aliquot was injected into a gas chromatograph equipped with a flame photometric detector. The lower limit of determination was 0.001 ppm, and the recoveries, after column chromatography with a sample size of 200 ml of water or 10 to 20 g of solid, were 85 to 95% for the former three and 55 to 60% for methyl demeton.View full abstractDownload PDF (820K) -
Taitiro FUJINAGA, Tohru TAKENAKA, Teruko MUROGA1976 Volume 25 Issue 11 Pages 795-799
Published: November 10, 1976
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe aim of the present work was to investigate the course of cultural exchange from the interpretation of the results obtained by physical and chemical analyses of archaeological amber products excavated in Japan; elemental analyses and infrared spectroscopy were carried out and the results were discussed in the present paper. Geological specimens, the origins of which are well known, were collected from Kuji, Ashikajima, Choshi, Hatoyama, Nagasaki, Inubosaki, Toriakeura, Gifu, Fushun, Palmnicken, Dominica and Dalmatia. Archaeological amber samples of unknown origin were excavated from Tomio-maru-yama old tomb, Ueno old tomb and Jionji-wakimoto old tombs in Nara and Awashimadai remains in Chiba. The composition of geological samples were found to be C:H:O=43208:70350:4, and archaeological samples to be 1956:2991:4 from the results of elementary analyses. The infrared spectrum of individual amber showed a characteristic pattern depending upon its provenance as was reported in the previous report. The archeological amber samples from Tomio-maru-yama old tomb (bead), Ueno old tomb (bead) and Jionji-wakimoto old tombs (bead) T0079, T0216 were found to have the provenance of Kuji in Iwate. And the amber artifacts excavated from Awashimadai remains No. 3-1 and ST5511 were identified as Choshi origin.
From these results, it was concluded that the amber produced from Kuji were widely distributed in the Kinki-district at the Tumlus period.View full abstractDownload PDF (840K) -
Yoshinori KIDANI, Shinobu NAGA, Hisashi KOIKE1976 Volume 25 Issue 11 Pages 800-802
Published: November 10, 1976
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn order to examine the effect of the substituting groups in the mass spectrometry of divalent metal oxinates, nickel (II) chelates of 5-chloro-7-halogenooxine (halogens : chlorine, bromine and iodine) were studied.
Measurements were made with a Hitachi double focus mass spectrometer RMU-7, by means of the direct inlet system. The conditions are: ionization voltage 70 eV, ion accelerating voltage 1800 V, total emission current 80 μA and ion source temperature 250 °C.
The ligands, 5-chloro-7-halogenooxine, show two fragmentation processes: (1) removal of CO from the molecular ion, followed by the loss of the halogen radical at 7-position, and (2) removal of the halogen radical at 7-position, followed by the loss of CO and the halogen radical at 5-position. Every nickel chelate loses one ligand radical from a 2:1 molecular ion to give 1:1 fragment ion. However, nickel chelates of 5-chloro-7-bromo- and 5-chloro-7-iodooxine were observed to lose bromine or iodine radical, while this phenomenon was not observed with 5, 7-dichlorooxine nickel chelate. The fragment ion derived from the 1:1 fragment ion by the loss of CO released the chlorine radical firstly to give 5-chlorooxine. However, 7-iodooxine lost the iodine radical firstly and then nickel was removed. In bromooxine, both fragmentation processes were observed simultaneously.View full abstractDownload PDF (383K) -
Kunishige HIGASHI, Kazuyoshi HAGIHARA1976 Volume 25 Issue 11 Pages 803-805
Published: November 10, 1976
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSTo keep marine environment clean, it is important to clarify the source of oil pollution.
For this purpose, discrimination of oils was studied by gel permeation chromatography. Molecular weight distribution of oil samples diluted with tetrahydrofuran was measured by high speed liquid chromatography. A column (50 cm in length and 7.9 mm in internal diameter) packed with HSG-15 was used. And chromatograms were recorded by measuring the absorbance of the eluates at 254 nm. The eluates were obtained under 50 kgs/cm2 pressure of tetrahydrofuran as an eluent. Chromatograms of eight kinds of crude oils were recorded. It was found that the discrimination of each oil of Iranian light, Minas, Marhan and Khafiji from other crude oils was possible. The profiles of the chromatograms of Iranian heavy, Kuwait, Futo and Oman were similar to each other. To study the effect of weathering on the properties of the spilled oil, crude oils were stored on the synthetic sea water for three years. The chromatograms of the weathered crude oils were similar to their unweathered oils. The proposed method could be applied to the identification of spilled oil samples with good results. Sensitivity and reproducibility of this method were satisfactory.View full abstractDownload PDF (476K) -
Fumiaki GOSHIMA, Sumiko MIO1976 Volume 25 Issue 11 Pages 805-807
Published: November 10, 1976
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA sensitive spot test of proline on a sheet of thin layer of Japanese acid clay was investigated. The procedure is as follows: A sample solution (5 μl) of amino acids was placed on a sheet of thin layer of thin layer of, Japanese acid clay.
After drying, a ninhydrin reagent (0.5% ninhydrin in 95% ethanol) was sprayed on that plate, which then was heated at ( 100110) °C for 5 minutes. A yellow spot of proline appeared. After cooling, the plate was sprayed with 2% Na2SO3 and then reheated at the same temperature for 10 minutes. The yellow spot turned reddish purple similar to that produced by hydroxyproline. This method was more sensitive than an ordinary method and the limit of detection of the colored spot is 0.05 μg of proline. Then the colored spot were treated with a drop of 1 N NaOH. A reddish purple spot of proline remained, while the colored spot of other amino acids disappeared. However, this specific colored spot of proline also faded gradually.
A purple spot remained on the plate faintly when more than 10 μg of hydroxyproline was present in the sample solution. In this way, 2.5 μg of proline in 5 μl of a mixture could be detected by the reddish purple color in the presence of 4 times amounts of hydroxyproline. Therefore, this reaction provided a method of a sensitive spot test of micro amounts of proline in amino acids mixture.View full abstractDownload PDF (391K) -
Jun'ichiro MIURA, Hideki ISHII, Hiroto WATANABE1976 Volume 25 Issue 11 Pages 808-809
Published: November 10, 1976
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSNickel was extracted with 1-(2-thiazolylazo)-2-naphthol (TAN) into the surfactant phase separated from the micellar solution of Triton X-100 at the temperature above 70°C, the cloud point of the micellar solution. An aliquot of a nickel solution (<6 μg of nickel) was placed in a test tube which has previously been weighed. Two mililiters of phosphate buffer solution (pH 7.0) and 2 ml of TAN solution (TAN, 0.02 g: Triton X-100, 20 g: water, 80 g) were added to the solution in the test tube, then the mixture was made up to 25 ml with water. This solution was kept at 95°C for 30 min in a hot-water bath. The nickel-TAN chelate extarcted in the surfactant phase (0.5 ml) precipitated at the bottom of the test tube. At 95°C the standing time required to reach a constant absorbance was 20 min. At room temperature the total quantity in the test tube was adjusted to 5.00 g by removing a supernatant solution, then the surfactant phase was redissolved in the supernatant solution remained in the test tube. The absorbance was determined at 595 nm (a maximum wavelength of nickel-TAN chelate) in a 1-cm cell. The initial volume of an aqueous solution could vary from 20 to 40 ml without affecting the absorbance.View full abstractDownload PDF (321K)
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