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Volume 37, Issue 4
Displaying 1-12 of 12 articles from this issue
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Application to nickel-germanium alloysYûetsu DANZAKI1988 Volume 37 Issue 4 Pages 153-158
Published: April 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIt was proposed that Ge could be determined by phenylfluorone spectrophotometry in the presence of the above cited acids. The method was applied to Ni-Ge alloys (Ge>0.02%). When color development, nickel up to 50 mg did not interfer with germanium determination. Procedure: A sample below 600 mg was digested with 10 ml of sulfuric acid (1+1), 10 ml of nitric acid (1+1) and 2 ml of hydrofluoric acid in a platinum dish. A 20 ml saturated boric acid solution was added. The solution was diluted to 100 ml (solution A). A 10 ml aliquot of solution A was diluted to 100 ml (solution B). Furthermore, a 10 ml aliquot of solution B was diluted to 100 ml (solution C). When the Ge content in the sample taken was below 1.05 mg, a 10 ml aliquot of solution A was mixed with 4.1 ml of a hydrofluoric acid-saturated boric acid solution (1 : 40), 10 ml of 20 w/v% urea solution, 10 ml of hydrochloric acid, 10 ml of 0.25% polyvinylalcohol solution, and 15 ml of 0.04% phenylfluorone solution.The mixture was diluted to 100 ml with water. The absorbance was measured at 505 nm after standing for 30 min. When the Ge content in the sample taken was 1.0510.5 mg, a 10 ml aliquot of solution B and 5 ml of a hydrofluoric acid-saturated boric acid solution (1 : 46) were used for the germanium determination. When the Ge content in the sample taken was 10.5105 mg, a 10 ml aliquot of solution C and 5 ml of a hydrofluoric acid-saturated boric acid solution (1 : 40) were used.View full abstractDownload PDF (829K) -
Masaji KUBO1988 Volume 37 Issue 4 Pages 159-163
Published: April 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSStoichiometric indirect AAS was developed to determine Ni in stainless steel. Stainless steel sample (0.3 g) was dissolved in 15 ml of aqua regia. The solution was evaporated to about 6 ml, and diluted to about 70 ml with water. After adding 30 ml of 45.7 w/v% citric acid solution for masking iron, pH of the solution was adjusted to 7.37.5 with 15 M ammonium hydroxide. To the solution a certain amount of dimethylglyoxime standard solution (10 mg/ml) was added which was expected to precipitate about 90% of Ni in the sample. Then, 2 ml of 15 M ammonium hydroxide was added. The content was made up to 250 ml with water, and left standing overnight. Nickel content in the filtrate was determined by flame AAS using Ni analytical line of 341.5 nm, using standard addition method for calibration. On the other hand, Ni content in the precipitate could be calculated from the amount of dimethylglyoxime added, because they react with each other stoichiometrically. Thus, Ni content in the original stainless steel sample was obtained by summing the Ni contents in those two phases. The analytical precision of this method in terms of standard deviation on the duplicated analyses of various stainless steel standard samples was about 0.037%, which was comparable with that of gravimetry based on JIS G 1216.View full abstractDownload PDF (566K) -
Removal of interference from chlorideMitsuhiko TAGA, Osamu SAKURADA, Hideaki TAKAHASHI1988 Volume 37 Issue 4 Pages 164-168
Published: April 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSChloride interference on the tin signal in graphite furnace AAS have been investigated with various chloride salts at different concentrations in sample matrix, and X-ray photoelectron spectroscopy (XPS) was applied to determine the mechanism of the chloride interference. In XPS measurements, graphite specimens immersed in the sample matrix were heated to 600 °C to estimate the amount of chloride remaining on the graphite surface. It was found that negative interference on Sn signal occurred in the presence of metal chlorides and that this interference was removed by the addition of ammonium salts. Ammonium nitrate and ammonium oxalate were the most suitable matrix modifier for determination of tin by graphite furnace AAS. The XPS measurements showed that chloride remained on the graphite surface at 600 °C in the presence of metal chloride in the sample matrix, but with the addition of ammonium nitrate to sample matrix, chloride disappeared at 200 °C. The interference from chloride could be caused by the formation of tin chloride before atomization. The addition of an ammonium salt possibly causes chloride vaporization as ammonium chloride, and prevents the formation of tin chloride.View full abstractDownload PDF (628K) -
Chozo YOSHIMURA, Takayosi HUZINO, Tadashi OHNISHI1988 Volume 37 Issue 4 Pages 169-173
Published: April 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA liquid substitution reaction between EDTA and metal chelates in nonaqueous solvents and analytical application were investigated. N, N-Dimethylformamide (DMF) was used as a solvent because of high solubility of the following metal chelates(metal/8-mercapto-quinoline chelate, metal/5, 7-dibromo-8-hydroxyquinoline chelate, metal/8-aminoquinoline chelate, metal/ diethyldithiocarbamate chelate, metal/pyrrolidine-N-dithiocarbamic acid chelate). Suitable titration rate was 0.51.0 cm3 min-1. Titration was carried out at room temperature except the diethyldithiocarbamate chelate which was titrated at 50 °C, due to the slow reaction rate between EDTA and the chelate in DMF. The molar ratio between the metal chelates and EDTA was obtained either at 2 : 1 or 1 : 1(metal/5, 7-dibromo-8-hydroxyquinoline chelate, metal/diethyldithiocarbamate chelate, metal/pyrrolidine-N-dithiocarbamic acid chelate). The reaction was considered to be substituted reaction between EDTA and ligand for metal ion in DMF. The reactivity of the ligand substitution reaction was dependent on the kind of the metal chelates. Less than 2% of water, inorganic acids or organic solvent(chloroform) gave no influence on the inflection point of the conductometric titration curves. The determination limit was 2×10-3 mol dm-3. This method was easy for the preparation of sample solution and was able to determine metal chelates.View full abstractDownload PDF (754K) -
Tadao SAKAI, Yoshitaka OHSUGI, Takeshi KAMOTO, Noriko OHNO, Hideto SAS ...1988 Volume 37 Issue 4 Pages 174-179
Published: April 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAlthough cetylpyridinium cation does not form an ion associate with divalent Bromocresol Green (BCG2-) at ca. pH 7, the extractability of cetylpyridinium is enhanced only in the presence of quinidine. The proposed extraction system is based on the reaction of monovalent quinidine cation (HQuinidine+), BCG2- and cetylpyridinium cation to form a 1:1:1 ternary ion associate (HQuinidine+-BCG2--cetylpyridinium+) extractable into 1, 2-dichloroethane, moderate polar solvent. Maximum absorption wavelength of quinidine-BCG associate was at 550 nm, but the wavelength of ternary ion associate shifted to 633 nm and bathochromic effect was also observed. The linearlity of the calibration curve was improved and the molar absorptivity increased compared with cetylpyridinium-BCG extraction system. Moreover, as the optimum pH was at 8.99.6, amines such as chlorpheniramine, dibucaine and diphenhydramine did not interfere with the absorption measurement. Molar absorptivity was 35800 mo1-1 cm-1 1 for quinidine-BCG-cetylpyridinium associate at 633 nm and relative standard deviation, 1.8%. The proposed method could be applied to the spectrophotometric determination of cetylpyridinium chloride in multi-component drugs.View full abstractDownload PDF (843K) -
Hideo WATANABE, Masato AIHARA, Mitsuo KIBOKU1988 Volume 37 Issue 4 Pages 180-184
Published: April 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSMolybdenum(VI) reacts with potassium xanthate {KRX : R=alkyl groups, viz., ethyl(Et), propyl(Pt), butyl(Bu) and pentyl(Pe)} to form complexes extractable into organic solvents. The application of their extraction method with xylene in ICP-AES determination of Mo was investigated. The optimum conditions of ICP-AES were as follows : incident power, observation height of measurement, coolant gas flow rate, plasma gas flow rate, carrier gas flow rate and wavelength were 1.0 kW, 13 mm above the coil, 16.0 l/min, 1.6 l/min, 0.6 l/min and 202.03 nm, respectively. For quantitative extraction of Mo-RX complex into xylene, among the KRK examined, butyl derivative (KBuX) was found to be the most suitable complexing agent. The optimum activity is 0.1 N to 7.0 N and the minimum concentration of KBuX is 0.01 mol dm-3 in aqueous phase. Five hundred-fold amount of Fe(III) interfered negatively with the determination of Mo, whereas 50-fold amount of Li(I), Rb(I), Sr(II), Ba(II), Mn(II), Cu(II), Ni(II), Zn(II), Zr(IV), V(V) and Cr(VI) or 5000-fold amount of Na(I), K(I), Mg(II), Ca(II) and Al(III) were tolerable. The relative standard deviation for 10 measurements in the mathod ranges from 1.2 to 1.9% in the determination of 2.5, 5.0 and 10.0 μg of Mo. With this method, the detection limit (3σ) was 1.8 ng cm-3 and the results of Mo determination in the standard silicate rocks were in excellent agreement with the certified values.View full abstractDownload PDF (669K) -
Yukio SUDO, Harumi ISHIZAWA, Masako MAEDA, Akio TSUJI1988 Volume 37 Issue 4 Pages 185-189
Published: April 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDihydronicotinamide adeninedinucleotide (NADH) reduces molecular oxygen to O2- and H2O2 in the presence of electron mediator. The produced O2-and H2O2 could be measured by chemiluminescence reaction using isoluminol and microperoxidase. We have developed a chemiluminescence assay of NADH using 1-methoxyphenazinemethosulfate (1-MPMS) as electron mediator. This chemiluminescence reaction has been coupled to the assay of enzyme activities which produced NADH. A highly sensitive chemiluminescent enzyme immunoassay of 17α-hydroxyprogesterone(17-OHP) using this NADH chemiluminescence assay have been develpoed. Glucose-6-phosphate dehydrogenase (G6PDH) and glucose dehydrogenase(GDH) were used as label enzyme. G6PDH gave good results than GDH because of its high enzyme activity. The second antibody-coated-bead was used to separate the bound and free fractions. The enzyme activity of bound fraction was measured by above NADH chemiluminescence reaction. Good standard curve was obtained in the range from 40 fg to 250 pg/assay. The 17-OHP values of dried blood spot samples (3 mm i.d.) were assayed by both ELISA and the present method. The results showed good correlation {y (proposed chemiluminescent enzyme immunoassay) =0.98x(ELISA)+1.25, r=0.973, n=29}. The present method may be usefully applicable for the neonatal congenital adrenal hyperplasia.View full abstractDownload PDF (770K) -
Hitoshi KOIZUMI, Yoshihito SUZUKI1988 Volume 37 Issue 4 Pages 190-194
Published: April 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA semi-micro HPLC coupled with a resonance Raman detection was described. For sensitive Raman detection, aliphatic amines and substituted phenols were derivatized with dabsyl chloride (4-dimethylaminoazobezene-4'-sulfonyl chloride). Also aliphatic aldehydes were derivatived with dabsyl hydrazine. These derivatives were separated on semi-micro column (μS-Finepak C18, 1.5 mm i.d.×250mm). Derivatives eluted from the column were monitored continuously by measuring the intensity of resonance Raman scattering at 1136 cm-1 with the 488.0 nm line of Ar ion laser. Peak height and/or peak shape of chromatograms would be influenced by various factors such as power of laser output, photon integration time, slit width of monochromator, smoothing point number and so on. Effect of above factors on Raman detection was investigated. Under optimum conditions for Raman detection, the lower detection limit of 2 ng with n-propylamine-dabsyl amide was obtained. The lower detection limit of this method was 20-fold better than that of the conventional column used in comparison with injected amounts.View full abstractDownload PDF (648K) -
Katsushige TAKAMI, Tameo OKUMURA, Hiroyasu YAMASAKI, Masao NAKAMOTO1988 Volume 37 Issue 4 Pages 195-201
Published: April 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSLiquid solid extraction of ultra trace levels of organic compounds in water samples were studied by using cartridges packed with styrene-divinylbenzene copolymers (SDBC). Adsorbability of 5 porous adsorbents for organic compounds were evaluated by the use of collection efficiency of total organic carbon (TOC) from water samples. Adsorbents, washed with ethanol, were packed into a heat shrinkable PTFE tubing (1.6 cm i.d.) and each end of the tubing were fixed with glass-sintered filters. The Cartridges (1.6 cm×12 cm) prepared were washed with diethylether by using a Soxhlet extraction apparatus prior to use. A 20 l of tap water, treated with sodium sulfite, was passed through the cartridge at less than 5 l/h of flow rate. The tap water before and after passing through the cartridge were decarbonated by bubbling pure air and analyzed by a TOC analyzer, and collection efficiencies for TOC were calculated. Recovery test of fifty organic compounds (pesticides, alkyl alcohols, etc.) were examined by using a cartridge packed with a SDBC (SP-800) of high surface area. One to ten μg of the compounds were injected into the top of the cartridge and 20 l tap water was passed through the cartridge. The compounds retained in the cartridge were eluted with methanol and diethylether. The organic compounds in the combined eluates were extracted with hexane/ethylether (1 : 1, v/v), dehydrated, condensed and then analyzed by GC or GC/MS. High collection efficiencies were obtained for SP-800 and SP-207 adsorbents with 800 m2/g and 400 m2/g surface area, respectively. Recovery for organic compounds were 63.5129% with 2.122.6% of relative standard deviation.View full abstractDownload PDF (1097K) -
Hiroshi MATSUMOTO, Mitsunojou ICHISE, Tsugio KOJIMA1988 Volume 37 Issue 4 Pages 202-206
Published: April 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSFourier transform spectrometer was applied to a spatially incoherent extended and pulsed source. The triangle common path interferometer having two sides of about 70 mm long was coupled with a image intensifier (I.I.) interfaced to a 16 bit microcomputer by the 512 channel Reticon linear array. The tube type I.I. having very high optical gain showed image distortion, though the proximity focus I.I. did not show this at all. Inequities of sampling intervals of the interferogram in the former I.I. caused the distorsion of calculated spectra. Fourier transformation was modified by using measured friges of equal thickness of a He-Ne laser. Despite of widening the aperture for the source, the resolving power was kept constant and the spectral peak height increased almost proportionally. Single pulse (a frequency doubled ruby laser; 347 nm, 20 mJ, 10 ns)-excited Ramman spectra of acetonitrile and methanol were obtained with a moderate intensifier gain. The methods of improving the resolving power (about 100 cm-1) were discussed. A new possibility for rejecting fluorescence and Rayleigh scattering was mentioned.View full abstractDownload PDF (675K) -
Kunio NAGASHIMA, Takashi ISHIMATSU, Shigetaka SUZUKI, Toshiyuki HOBO1988 Volume 37 Issue 4 Pages 207-209
Published: April 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe sample solution containing ammonium ion and diethyl amine is pumped at the flow rate of 8 ml min-1 to the mixing joint, where a reaction solution (1% sodium hydroxide solution) is mixed at the rate of 4 ml min-1. Then the mixture containing ammonia and amine is fed into a gas-liquid separator. The ammonia and amine permeate through three Teflon membranes (0.80 μm pore size, 0.1 mm thick, 82% porosity) into an absorption solution (10-2 M ammonium chloride solution) flowing at 2 ml min-1. Since the porous wall of inner Teflon membrane is coated with an Armeen SD, aliphatic primary amine (C15), when ammonia and amine pass through the pore, the difference in the passing time between ammonia and amine can be observed. The response time of ammonia and diethyl amine were about 3.5 min and 4.8 min, respectively. Therefore, the ammonium ion could be determined separately from diethyl amine. The pH of absorption solution is measured with a glass electrode. The Nernstian response of electrode potential is valid with a relative standard deviation of less than 5% in the range between 1×10-1 and 1×10-4 M.View full abstractDownload PDF (470K) -
Haruo HONMA, Keiko SUZUKI, Mutsuko YOSHIDA, Hisako YANASHIMA1988 Volume 37 Issue 4 Pages T55-T60
Published: April 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method for the determination of free anions in coal was developed. The qualitative analysis was performed by ion chromatography for the water extracts from two kinds of coal which were commercially available as standard samples for elemental analysis. Chloride, nitrite, nitrate and sulfate ions could be detected as main anions. To extract these anions completely, 100200 mg of each kind of coal was weighed in a quartz flask, 20 ml of deionized water was added and this mixture was refluxed with a quartz condenser for 60 min. After the coal was separated by filtration, the extract was diluted with 8 mM Na2CO3-NaHCO3 solution to 50.000 g and injected into the ion chromatograph. The precision of the results was good for chloride and sulfate ions, but not satisfactory for nitrite and nitrate ions. To determine the total amount of anions, the coals combusted gaseous products were absorbed in deionized water, the residue was stirred with deionized water and heated on a water bath. Each solution was injected into the ion chromatograph and the total amount of anions was obtained by adding both results. It was found that the amounts of free anions were 010% of those of the total anions. These values were useful as an indicator of the quality of coal.View full abstractDownload PDF (789K)
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