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Volume 34, Issue 2
Displaying 1-14 of 14 articles from this issue
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Hitoshi KOIZUMI, Hiroki KOSHIYAMA, Yoshihito SUZUKI1985 Volume 34 Issue 2 Pages 63-67
Published: February 05, 1985
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSA high performance liquid chromatography (HPLC)with a Raman spectrometric detector is described. In order to obtain high sensitivity, utilization of the resonance Raman effect was attempted. Seven 4-dimethylaminoazobenzene-4'-sulfone amides were derivatized from the reactions of 4-dimethylaminoazobenzene-4'-sulfonyl chloride with primary and secondary amines. These derivatives were separated successfully with a Zorbax ODS column (4.6φ×250mm). A mixed solvent of 70% (v/v) acetonitrile/water was used as a mobile phase. Chromatogram was obtained by measuring the intensity of resonance Raman scattering at 1136cm-1 with 488.0nm line of Ar+laser at 300mW output. A flow cell (0.9mm i.d.) was employed and its effective cell volume was 3.7nl. A detection limit for the methylamine derivative was 53.8ng. As the flow cell has a micro volume, this method will be applicable to HPLC of micro or semi-micro scale.View full abstractDownload PDF (646K) -
Fumio HIROSE, Takeshi KOBAYASHI, Shinichi HASEGAWA, Haruno OKOCHI1985 Volume 34 Issue 2 Pages 67-72
Published: February 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSHydride-generation atomic absorption spectrometry for the determination of trace amounts of arsenic and bismuth in nickel-base and cobalt-base heat-resisting alloys was studied. 0.5g of the sample was dissolved with a mixture of 5ml nitric acid-5ml hydrochloric acid-1ml hydrofluoric acid. Hydrofluoric acid up to 1.5ml did not interfere with the measurement. The sample solution was diluted to 50ml with water. One thousand μl of the solution was injected to the generator cell using a micro-pipette. Seven ml of 0.2M EDTA solution was added to remove the interference from the elements in samples and then 10ml of 0.8M hydrochloric acid were added. After the generator cell was set to the hydride-generation system and the system was purged with argon, 4ml of 3% sodium borohydride solution were added. Generating hydride was introduced to a quartz tube cell atomizer and atomized at 900°C by using an air-acetylene flame, and then arsenic and bismuth were determined. This method could be applied to many kinds of heat-resisting alloys. The limit of detection was 0.5ppm for arsenic and 0.2ppm for bismuth.View full abstractDownload PDF (922K) -
Determination of medazepam and sulfisomidineToshiyuki MITSUI, Toshiyasu MATSUOKA, Yoshikazu FUJIMURA1985 Volume 34 Issue 2 Pages 72-76
Published: February 05, 1985
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSErio Green B forms an ion association complex with medazepam at pH 4.10 which can be extracted into chloroform. Sulfisomidine reacts with α-chloro-p-xylene to form p-methyl benzyl derivative, which is extracted into dichloromethane at pH 2.56 in the presence of Tropaeoline OO forming an ion association complex. The procedures for the determination are as follows. Medazepam: In a 15-ml test tube, place 5ml of chloroform solution of a sample containing less than 17.5μg/ml of medazepam, 0.5ml of Erio Green B solution (8.77mg/ml), and 2ml of buffer solution (pH 4.10). Shake the solution for 3min mechanically and centrifuge for 3min. Take the chloroform phase, and measure the absorbance at 637 nm with 1-cm glass cells. Sulfisomidine: Place 15ml of acetone solution of a sample containing less than 564μg of sulfisomidine, 2ml of 1.39 × 10-1M α-chloro-p-xylene acetone solution, 3ml of 3% sodium carbonate solution, and 59ml of acetone in a 30-ml Erlenmeyer flask. Warm it on a water bath for 15min, making up for the evaporated acetone, and warm at 80±3 °C for 15min without adding acetone. After cooling, add 10ml of dichloromethane. Shake it for 30 s and centrifuge for 2 min at 3000rpm. In a 15-ml test tube, place 5ml of the dichloromethane phase, 2ml of a saturated Tropaeoline OO solution, and 2ml of buffer solution (pH 2.56). Shake the solution for 3min mechanically, and centrifuge for 2min at 3000rpm. Take 2ml of the dichloromethane, and 0.5ml of methanol solution of 10% hydrochloric acid and measure the absorbance at 543nm with 1-cm glass cells. Other compounds, such as nitrazepam, oxazepam, diazepam, Ca (II), Mg (II), Fe (III), Ni(II), Al(III), glucose, lactose, urea, L-leucine, and L-phenylalanine have not interfered with the determination of medazepam. For the determination of sulfisomidine, sulfadimethoxine, sulfamethoxazole, sulfamethizole, Fe (III), Ca (II), Cu (II), Al (III), glucose, and lactose have not interfered.View full abstractDownload PDF (707K) -
Isao YOSHIDA, Keihei UENO1985 Volume 34 Issue 2 Pages 77-81
Published: February 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe reagent, abbreviated as 2-nitroso-5-(N-propyl-N-sulfopropylamino) phenol (N-PSAP) below, is a water soluble derivative of nitrosophenol. A direct photometric method is given for determination of cobalt in commercial nickel salts quickly and accurately. Take sample solution into a volumetric flask.. Add 5ml of 0.01M cetylpyridinium bromide and 5ml of 0.001M of N-PSAP. After the pH value of the solution is adjusted to 48, add 5ml of 0.2M iminodiacetic acid. After standing for a while, 5ml of 6M hydrochloric acid is added to this mixture and the solution is made up to 50ml with water. Here, the final concentration of cobalt should be 5×10-71.5×10-5M. The optical absorbance of the resulting solution is measured at 490nm against the reagent blank. The molar absorptivity of the cobalt complex is 5.3×104dm3mol-1cm-1. The relative standard deviation is 1.2%(n=8) at 5×10-6M of cobalt. Twenty fold molar amounts of coexisting Al(III), Ba(II), Ca(II), Cd(II), Cr(III), Cu(II), La(III), Mg(II), Mn(II), Pb(II), Sr(II), Zn(II), Zr(IV), As(V), B(V), C2O42-, P(V), CN-, and F-and six hundred fold molar amounts of Ni(II) do not interfere. The addition of 1ml of 2M citric acid masks the interference caused by Fe(II) of<20 fold molar amounts. Both the molar-ratio and the continuous variation methods show that the composition of the cobalt complex is Co:N-PSAP =1:3. Spectrophotometric observations give first and second acid dissociation constants of N-PSAP as follows: p Ka1=2.74 and p Ka2=8.45(I=0.1, with NaClO4, at 20°C).View full abstractDownload PDF (815K) -
Satori UTSUMI, Midori KOTAKA, Akinori ISOZAKI1985 Volume 34 Issue 2 Pages 81-86
Published: February 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSIodide ion is oxidized to iodine with hydrogen peroxide in sulfuric acid solution. Bromide and iodide ions are oxidized to bromine and iodate ion with potassium permanganate in sulfuric acid solution. Iodine or bromine in carbon tetrachloride is quantitatively converted into triiodide ions in aqueous phase by the back-extraction with an excess of potassium iodide solution. The analytical procedure for iodide ion is as follows. To 10 ml of a sample solution containing iodide ion up to 10 ppm in a separatory funnel, 1 ml of 4.5 M sulfuric acid and 1 ml of 3 % hydrogen peroxide are added. After standing for 5 min, 5 ml of carbon tetrachloride is added to the funnel and it is shaken for 30 s. The carbon tetrachloride phase is transferred to the other funnel and 5 ml of 0.05 M sulfuric acid is added. The mixture is shaken for 30 s to wash the organic phase. Then, the organic phase is transferrd again to the other funnel and 10 ml of 0.5 M potassium iodide solution is added. The mixture is shaken for 30 s. The absorbance of the aqueous phase is measured at 350 nm with a quartz cell against water. For the determination of bromide ion, 1 ml of 3 M sulfuric acid and 1 ml of 0.015 M potassium permanganate are added to 10 ml of a sample solution containing bromide ion up to 10 ppm in a separatory funnel, and allowed to stand for 5 min. The subsequent procedure is the same as that for iodide ion described above, except for the washing of organic phase with 5 ml of 0.5 M sulfuric acid. The relative standard deviation for the determination of 63.3 ppm bromide ion in sea water sample was calculated to be 1.3 % for 10 repeated measurements.View full abstractDownload PDF (1005K) -
Kitaro SHIGETA, Tadashi KIKUCHI, Keiichi FURUYA1985 Volume 34 Issue 2 Pages 87-90
Published: February 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe determination of oxygen in silicon nitride powder and aluminium nitride powder was studied by means of vacuum heating method, and the oxygen values were compared with those obtained by inert gas fusion and activation methods. Ten milligrams of sample powder enclosed in a degassed graphite capsule was heated at 1850°C in vacuum. The extracted carbon monoxide was trapped at a liquid nitrogen trap after oxidation with copper oxide to carbon dioxide. After nitrogen was pumped out, carbon dioxide was released from the trap, and its quantity was measured by means of an oil manometer. The influence of sample weight and extraction temperature on the determined oxygen values were investigated in the range of 540mg for sample weights at 15502050°C for extraction temperatures. Larger sample weight required a longer gas extraction time, but it did not cause any deviation of oxygen values. There was no influence of extraction temperature. Lower extraction temperature required a longer gas extraction time, and higher temperature suffered from a larger background value. Under best conditions, where 10mg of sample was analyzed at 1850°C in 2030min, the oxygen values in five kinds of silicon nitride by vacuum heating method were in good agreement with those values obtained by inert gas fusion or activation methods.View full abstractDownload PDF (735K) -
Kunio NAGASHIMA, Masatoshi MATSUMOTO, Shigetaka SUZUKI1985 Volume 34 Issue 2 Pages 91-94
Published: February 05, 1985
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSGas-liquid separation and a second-derivative spectrophotometer (Model UO-1; YANACO) are used for continuous determination of nitrite. The sample is pumped at the flow rate of 4 ml min-1 to the mixing coil (50 °C, volume 4 ml), where a 13 M phosphoric acid containing 0.13 M sodium iodide is mixed at the rate of 1 ml min-1 and the nitrite is reduced to nitric oxide. Then the mixture containing nitric oxide is fed through a gas-liquid separator {outer tube (glass, 4 mm i.d.), inner tube (pore size 1 μm, microporous Teflon tube, 2 mm o.d., 1 mm i.d.), length 50 cm, 90 °C}. The evolved nitric oxide is purged with nitrogen (150 ml min-1, 90 °C) into a heated optical cell (150 °C, light pass length 25 cm, cell volume 80 ml) of a second-derivative spectrophotometer where the second-derivative absorbance at 214.0 nm is continuously recorded. The response appeared within 1 min after sample was introduced and the equilibrium response was reached for 5 min. The conversion of nitrite to nitric oxide was quantitative between 5×10-71×10-3 M nitrite. The relative standard deviation (n=6) was 2.1 % for 10-5 M nitrite. The water vapor evolved from the gas-liquid separator had no influence on this method, therefore water vapor scrubber is unnecessary in this system. No gas which absorbs the light in the region of 200240 nm was evolved except of nitric oxide by this experimental condition used. The method was applied to artificial sea water.View full abstractDownload PDF (617K) -
Tomozo KOH, Yohko KASAHARA, Tsutomu OKAZAKI, Yasuyuki MIURA1985 Volume 34 Issue 2 Pages 95-99
Published: February 05, 1985
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSA spectrophotometric method was proposed for the determination of micro amounts of cyanide, which is based on the formation of thiocyanate and its extraction into 1, 2-dichloroethane as an ion pair with Methylene Blue. A recommended procedure is as follows. Pipette 2ml of a phosphate buffer (pH7.5), 2ml of 1.3×10-3 M Methylene Blue, and 10ml of 1, 2-dichloroethane solution of 0.1 M elementary sulfur into a 50-ml separatory funnel. To this mixture, add 10ml of cyanide solution up to 1×10-5 M, then shake the funnel for 4 min to extract the ion pair between Methylene Blue and thiocyanate. After standing for a given period of more than 15 min, transfer the organic phase to a 15-ml glass stoppered tube and add small amounts of sodium sulfate. Shake the mixture vigorously by hand until the phase becomes transparent, and measure the absorbance of the organic phase at 657 nm against dichloroethane. The reaction of cyanide in the aqueous phase with sulfur in the organic phase proceeds to stoichiometric completion over the pH range of 7.7 to 8.0 under the conditions as in the procedure; one mol of thiocyanate is produced from 1 mol of cyanide and the thiocyanate formed is extracted as an ion pair with Methylene Blue into the organic phase. The apparent molar absorptivity for cyanide ion at 657 nm is 8.67×10-4 cm-1 mol-1?, the Sandell sensitivity is 3.0×10-4μg CN-cm-2 (for an absorbance of 0.001), and linear calibration graphs are obtained up to 1.0×10-5 M cyanide (2.6μg CN-in 10ml). From eleven measurements for 10-ml aliquots of 6×10-6 M cyanide, the mean absorbance value was 0.517 against a reagent blank, with a standard deviation of 0.005 absorbance unit and a relative standard deviation of 1.0%.View full abstractDownload PDF (884K) -
Hidemi TODORIKI, Tokishi HAYASHI, Takashi AKAMATSU1985 Volume 34 Issue 2 Pages 100-104
Published: February 05, 1985
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSA sensitive high performance liquid chromatographic method has been developed for the determination of glyoxalic acids, one of α-keto acids. This acid was prepurified using a column of carboxyl-CPG and derivatized with ο-phenylenediamine into 2-quinoxalinol derivative, which was extracted into ethylacetate. The 2-quinoxalinol derivative and internal standard were separated by reversed-phase paired-ion chromatography using a 250×4.0 mm i. d. column packed with LiChrosorb RP-8 (5μm). This method is sensitive, selective, and reproducible.View full abstractDownload PDF (858K) -
Jia Chen Chu, Yukihiro NOJIRI, Tetsuya HASEGAWA, Hiroki HARAGUCHI1985 Volume 34 Issue 2 Pages 104-108
Published: February 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSSimultaneous multielement analysis of certified reference material "Hair", which was issued from the National Institute for Environmental Studies, has been investigated by inductively coupled plasma atomic emission spectrometry (ICP-AES). The hair sample was dried at 85°C for 4h, and cooled for 30min in a desiccator. The sample (ca. 250mg) was digested with HNO3-HF-HClO4 or ashed at 450600°C. The acid digestion was performed in a sealed Teflon vessel at 140°C for 4h. The ashed sample was treated with HCl and HF to dissolve the sample. The digested or ashed sample was finally diluted to 25ml. The spectral interference and analytical figures of merit were examined to evaluate the analytical feasibilities of ICP-AES for hair analysis. Trace metals (Al, As, Ba, Ca, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, P, Pb, Sr, Ti, and Zn) were detected in the hair sample, and the analytical results were compared with the reported values. The measured values for most elements were reasonable, although the concentrations of Ca, Al, Fe, and Ti were very high probably because of the contamination in the preparation procedure of the certified ard reference material.View full abstractDownload PDF (802K) -
Hideharu SHINTANI, Kusuo TSUJI, Takuma OBA1985 Volume 34 Issue 2 Pages 109-113
Published: February 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSIon chromatography using conductivity detection (CD) has previously been reported. We have reported the determination of serum cations and pretreatment of serum for ion chromatography using CD method. Recently, indirect photometric ion chromatography, which analyzed cations by the difference of UV absorbance between UV absorption-having mobile phase and non UV absorption-having samples, using UV detection in place of CD was reported. We studied analytical conditions by UV detection method for the determination of serum cations using pretreatment of serum described in our previous report. The CD method and UV methods were compared as well as the comparison of a determined amount of serum cations. Analytical conditions for UV method were as follows: column; strong cation exchange resin ASC4000, mobile phase; 1.28mM copper (II) sulfate pentahydrate for sodium and potassium determination and 3.2mM copper (II) sulfate pentahydrate for calcium and magnesium determination, detection; 218nm. Serum pretreatment was as follows: untreated serum or acidified serum (below pH3.5) was ultrafiltrated. The ultrafiltrate was neutralized, diluted and injected into column of high performance liquid chromatography (HPLC). The use of more than 4mM of copper (II) sulfate pentahydrate as mobile phase was not successful, because the relation between the response and concentration of cations injected could not be maintained. A significant difference in the determined concentration of serum cations between UV and CD method was not obvious. The higher sensitivity was attained when the solution of 0.5to 1.5mM copper (II) sulfate pentahydrate and 0.5to 5mM cobalt (II) sulfate heptahydrate, nickel (II) sulfate hexahydrate, zinc (II) sulfate heptahydrate or cobalt (II) diammonium sulfate hexahydrate was used as the mobile phase in UV method.View full abstractDownload PDF (732K) -
Kiwao KADOKAMI, Ryota SHINOHARA1985 Volume 34 Issue 2 Pages 114-118
Published: February 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe trace determination ofn-alkanes in seawater was developed for investigating their background level. Water sample (101) was passed through XAD-2 resin column (1.5cm i.d. × 10cm), after perdeuteratedn-alkanes (C16, C20, C24, and C32) had been added to the sample as internal standards.n-Alkanes adsorbed on the resin were extracted in a Soxhlet extractor with dichloromethane. The extract was concentrated to 1 ml with a Kuderna-Danish evaporator. The concentrate was examined by a gas chromatograph mass spectrometer with a multiple ion detector (GC/MSSID). Precision of the absolute calibration curve method was compared with that of the internal standard method in the temperature programmed chromatography. The relative standard deviation of the absolute calibration curve method and the internal standard method was 9.6% and 4.5%. For recovery test, 1μg of each n-alkane (C13to C32) was added to 5l of 3% sodium chloride solution. n-Alkanes were recovered from the solution by the XAD-2 resin extraction method. Determination was carried out by internal standard method after addition of perdeuterated n-alkanes to the concentrate. The recoveries of low molecular weight n-alkanes (C13to C20) were from 14% to 60% and the those of high molecular weight n-alkanes (C21to C32) more than 70%. One μg of cach n-alkane (C13to C32) and perdeuterated n-alkane (C16, C20, C24, and C32) were added to 5l of water sample and over-all recovery tests of n-alkanes were performed, because the accuracy and the precision of this method were determined. The average recovered amount of n-alkanes was 1.04μg and the average of standard deviations was 0.06μg. n-Alkanes in seawater sample were determined by this method, and the sum of concentrations of n-alkanes (C13to C32) was 2.78ppb.View full abstractDownload PDF (749K) -
Taizo TSUDA, Hiroshi NAKANISHI, Shigenobu KOBAYASHI, Takashi MORITA1985 Volume 34 Issue 2 Pages T13-T16
Published: February 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThree different pretreatment methods were compared with each other for gas chromatographic determination of methyl mercury in fish meat samples. The methods were as follows. (A) Organic interferences were removed from a homogenized sample by acetone wash followed by benzene wash. Protein-bound methyl mercury was released by addition of hydrochloric acid and extracted into benzene. (B) Hydrochloric acid was added to a homogenized sample. Methyl mercury was extracted into benzene and then into aqueous cysteine solution to eliminate organic interferences. The extract was acidified with hydrochloric acid to liberate methyl mercuric chloride, which was re-extracted into benzene. (C) A homogenized sample was digested with a potassium hydroxide-ethanol solution. Methyl mercury was extracted into chloroform after acidification of the digested solution, and then into aqueous cysteine solution. Methyl mercuric chloride was extracted into benzene in a same manner as the method (B). The methyl mercuric chloride was measured by using a gas chromatograph equipped with an electron capture detector. The method (C) gave good analytical results in accuracy and reproducibility. The time required to analyze was little different among three methods.View full abstractDownload PDF (592K) -
Toshio OZAWA1985 Volume 34 Issue 2 Pages T16-T19
Published: February 05, 1985
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSBy using a micro-pipette in the duplication method, the visual colorimetric determination of copper and iron has been improved. For the visual comparison of color intensity, a pair of vessels (2cm W×2cm L ×15cm H) were used: one is for sample and the other for reference. Sample solution was taken in vessel (I), mixed with suitable color-producing reagents, and then, made to 20ml with water. Into vessel (II), the same color-producing reagents was taken and made to 20ml, to which the standard solution of the analyte was added drop by drop with the micropipette, until the same color as the sample solution was duplicated in the reference. Copper in brass and aluminium alloys, was determined by using EDTA and DDTC, respectively, and by using 20mg/ml and 500μg/ml of copper standard solution for the duplication, respectively. For iron in brass and aluminium alloys sulfosalicylic acid was used as the color-producing reagent, and the duplication was made by adding 1.0mg/ml of iron (III) standard solution. Although the metal concentration in the duplications were not equal to those in the samples, the linear relation between both concentrations is valid for a calibration curve. The concentration range for calibration curves for Cu-EDTA, Cu-DDTC, and Fe-sulfosalicylic acid, should be less than 300μg/ml, 3μg/ml, and 5μg/ml, respectively. The standard addition could be applied to the present duplication method to improve accuracy in the analysis of actual samples. Precision of this method was within ±5 %.View full abstractDownload PDF (685K)
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