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Yasushi NAKAMURA, Yoshinori NOTO
1982 Volume 31 Issue 8 Pages
413-417
Published: August 05, 1982
Released on J-STAGE: February 16, 2010
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Trace hafnium in zirconium metal and its alloy was determined by using inductively coupled plasma emission spectrometry system which was a combination of derivative method with wavelength modulation and Echelle spectrometer. The analytical procedures established were as follows: 1.0 g of sample was decomposed with 10 ml of hydrofluoric acid (1+6) and 8 ml of hydrochloric acid, then diluted with water to 100 ml. Hafnium contents were measured by the I.C.P. system without separating zirconium. Hf II 264.141 nm was selected as an optimum analytical line and there was no spectral interference by close line; Zr II 263.909 nm owing to the high spectral resolution of this instrumental system. Coexistence with 10000 ppm of zirconium depressed intensity of hafnium by about 20 % and therefore the calibration needed the coexistence of zirconium in same concentration as sample solution. Glass nebulizer could be useful with no corrosion when the amount of hydrofluoric acid was smaller than the equivalent to zirconium. Analysis of NBS and JAERI standard samples showed good agreement with the repeated values and relative standard deviations ranged from 2.0 % to 4.6 %. Detection limit of hafnium was 10 ppm.
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Kazuo MAKINO, Nobuyuki KASHIHIRA, Kuwako KIRITA, Yoshichika WATANABE
1982 Volume 31 Issue 8 Pages
417-422
Published: August 05, 1982
Released on J-STAGE: February 16, 2010
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A rapid and sensitive method has been developed for the determination of dithiocarbamate fungicide residues in environmental samples. The method consists of the digestion of sample in 6 N hydrochloric acid in the presence of stannous chloride and the cryogenic trapping of carbon disulfide at liq. O
2 temperature, followed by gas chromatographic analysis with a flame photometric detection. Chromatographic separation is achieved with a PTFE column (FEP, 4 m × 3 mm I.D.), a half full of 5 % polyphenyl ether (PPE) on Chromosorb W(AW-DMCS) and a half full of 25 % tricyanoethoxy propane (TCEP) on Chromosorb W(AW-DMCS), isothermally at 61°C with a nitrogen carrier gas flow rate of 50 ml/min. Neither hydrocarbons nor sulfur compounds interfere. Recoveries from spiked samples are 92.0 % for diethyl dithiocarbamate in soil, 95.5 % for ziram in onion, and 94.9 % for maneb in tomato juice. Concentration of dithiocarbamates in soil, onion, and tomato juice, expressed as CS
2, are determined with the relative standard deviation of
ca. 3 % for most sample tested. The limit of determination is as low as 0.2 ppb on a 10 g sample basis.
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Naohiko SAWATARI, Yoshikazu HIROSE, Hideyuki TANABE, Sueshige ISHIDA
1982 Volume 31 Issue 8 Pages
422-427
Published: August 05, 1982
Released on J-STAGE: February 16, 2010
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Total nitrogens in high carbon containing environmental samples, such as sludge and night soil wastewater, were determined by coulometric titration method after converting the nitrogen to ammonia. The sample was thermally cracted and reduced with hydrogen over a newly developed, highly active Ni-Al
2O
3 catalyst. The catalyst was not deactivated by cracking products, and was usable more than several hundred times without regeneration. In the case of samples containing NO
2- or NO
3-, a good recovery of nitrogen was obtained by carring out the thermal cracking after adding acid (sulfuric acid, phosphoric acid) into the samples. The coefficient of variation was less than 3 % for solid samples having 2.46 % nitrogen contents. The coefficient of variation was less than 2 % for liquid samples having 100 ppm nitrogen contents. Every determination was made within 5 min.
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Iwao ABE, Keiji IZUMI, Shigefumi KURAMOTO, Soichiro MUSHA
1982 Volume 31 Issue 8 Pages
427-431
Published: August 05, 1982
Released on J-STAGE: June 30, 2009
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The rings of Yakusugi (
Cryptomeria japonica, about 1800 years old) on eight points yielding from 1084 to 1474 years which were determined their dates by counting one by one from the cortex into the heart were treated chemically to take out amino acids by washing, hydrolysis, ion-exchange clean-up, derivatization and analyzed enantiomeric mixtures by gas chromatography using Chirasil-Val glass capillary column. Then, ring ages were determined from the D/L ratio of aspartic acid (Asp) by two different methods making two corresponding calibration curves. Racemization was observed in alanine (Ala), valine (Val), Asp, and phenylalanine (Phe). As it was proceeded only a little in Val, irregular with ages in Ala and Phe, availability was found in Asp in a reasonable agreement with ages what we derived from. Ring age was calculated from the D/L ratio of Asp by next two methods and compared with the corresponding ring dated.
(I) Calibration curve from one ring dated and racemization through analytical step.
(II) Calibration curve from two rings dated 1084 and 1474 years.
The dated ages of the rings by these two methods were closely related to the ring ages and, especially, relative error % was much more sufficient in the case of (II). The standard error estimated on (I) and (II) are 39.8 years and 29.6 years, respectively. It is suitable method that Asp racemization reaction could be determined of dating tree rings.
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Yasuyuki MIURA, Hiroshi ISHIYAMA, Tomozo KOH
1982 Volume 31 Issue 8 Pages
432-437
Published: August 05, 1982
Released on J-STAGE: February 16, 2010
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A method has been developed for the determination of silver(I), copper(II), and mercury(II) in their mixtures. It is based on the consumption of thiocyanate by silver(I), copper(I), and mercury(II) which form insoluble precipitates of silver(I) thiocyanate and copper(I) thiocyanate, and non-dissociative species of mercury(II) thiocyanate, respectively; the excess of thiocyanate is determined spectrophotometrically with iron (III). The method consists of three procedures. In procedure I, the consumed thiocyanate corresponds to the amount of silver(I) because mercury(II) is allowed to be masked by cyclohexane-1, 2-diamine-
N, N, N', N'-tetraacetic acid. In procedure II, where the masking agent for mercury(II) is not added, the consumed thiocyanate corresponds to a sum of silver(I) and twice as much as mercury(II). In procedure III, the consumed thiocyanate corresponds to the amount of copper(II) because copper(II) is reduced to copper(I), and silver(I) and mercury(II) are reduced to their metallic states by L-ascorbic acid simultaneously. The three metals in mixtures give the following equivalents in each of the three procedures:
Procedure I _??_Ag (I)
Procedure II _??_ Ag (I) +2 Hg (II)
Procedure III _??_ Cu (II)
The method could be successfully applied to the determination of silver(I), copper(II), and mercury(II) in dental amalgam and silver solder.
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Indirect determination of fluoride ion
Akira KITO, Koji KOMATSU
1982 Volume 31 Issue 8 Pages
438-443
Published: August 05, 1982
Released on J-STAGE: February 16, 2010
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A method of gas-liquid chromatographic analysis of metal chelates has been applied to the determination of fluoride ion. A specified excess of beryllium (II) and 3-methyl-2, 4-pentanedione {(3MeAA)H} are added to a sample solution containing fluoride ion. The fluoride ion is converted to BeF
42- and the remaining beryllium(II) to bis(3-methyl-2, 4-pentanedionato)beryllium(II) {Be (3MeAA)
2}. The gas-liquid chromatographic analysis of the Be(3MeAA)
2 can lead to the indirect determination of the fluoride ion. The recommended procedure is as follows. One ml of a sample solution containing (0.20.5) mg/ml {(200500) ppm} of fluoride ion is taken into an about 15ml vial (73.5 mm × 20.5 mm o.d.). To the solution are added 1.00 ml of aqueous beryllium(II) chloride {0.25 mg/ml as Be(II)}, 3.00 ml of a buffer solution of 1 M acetic acid-1 M sodium acetate (pH 5.0), and 1.00 ml of a benzene solution containing 37.9 mg of (3MeAA)H and 1.5 mg of tetradecane as an internal standard. The whole solution is shaken for an hour and allowed to stand for five min. The liberated Be(3MeAA)
2 in the upper benzene extract is analyzed under the following gas-liquid chromatographic conditions. For determining small amount of fluoride ion,
i.
e., (0.010.25) mg/ml {(10250) ppm}, a benzene solution containing 2.0 mg of tetradecane is used. The coefficients of variation less than 5 % are obtained in the case of 0.1 to 0.3 mg/ml of fluoride ion. Phosphate and aluminum(III) interfere with the determination, but the other ions commonly encountered do not interfere significantly. Gas-liquid chromatographic conditions are as follows-column: 75 cm × 3 mm i.d., stainless steel tube, packed with 0.5 % Micro wax on silanized glass microbeads (60/80 mesh); column temperature: programmed from 95 to 195 °C at 6 °C/min; helium flow rate: 30 ml/min; detector: flame ionization detector; injection volume; 6μl; sensitivity: 1/10; attenuator: 1/64.
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Shogo SUZUKI, Shoji HIRAI
1982 Volume 31 Issue 8 Pages
443-449
Published: August 05, 1982
Released on J-STAGE: February 16, 2010
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Concentration of 49 elements in NBS coal standard reference materials (SRM 1632 a and SRM 1635) and coal fly ash standard reference material (SRM 1633 a) were determined by instrumental neutron activation analysis (INAA). Each sample {
ca. (25150) mg} was irradiated for short time (2 min) at thermal neutron flux 1.5 × 10
12 n cm
-2 s
-1 and for long time (5 h) at thermal neutron flux 3.2 × 10
12 n cm
-2 s
-1 in Musashi Institute of Technology Research Reactor (MITRR). Gamma-ray spectra from short time irradiation samples were taken for 4 min after (215) min after irradiation and for 15 min after (870) min after irradiation using a Ge(Li) detector coupled to an 8192 multi-channel analyzer and a mini-computer (GAMA system). Gamma-ray spectra from long time irradiation samples were taken for about 2 h after (312) d after irradiation and for about 10 h after (1560) d after irradiation. The analyzed values were in good agreement with NBS certified values except for a few elements. In order to improved the sensitivity of detection of some elements, long time irradiation samples were also counted by means of an anticoincidence counting method or a coincidence counting method with a Ge(Li) detector and a well-type NaI(Tl) detector. Concentrations of 12 elements (Pr, Nd, Rb, Th, Cr, Ce, Fe, Hg, Zr, Sr, Ni, Zn) were determind by the anticoincidence counting method and concentrations of 3 elements (Ba, Hf, Se) were determined by the coincidence counting method.
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Makiko SUEHIRO, Masahiro IIO, Junji MORIKAWA
1982 Volume 31 Issue 8 Pages
450-453
Published: August 05, 1982
Released on J-STAGE: June 30, 2009
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Sensitivity and precision in breath
13CO
2 analysis were compared among three mass spectrometric methods. The methods were: (a)
13CO
2+ and
12CO
2+ were analyzed by scanning the magnetic field, and detected by an electron multiplier. (b)
13CO
2+ and
12CO
2+ were analyzed in a fixed magnetic field with a single electron multiplier by alternating accelerating voltages.
13CO
2 abundances in the breath samples were determined by comparing with a reference CO
2, with known.
13CO
2 abundance.(c)
13CO
2+ and
12CO
2+ were separated in a fixed magnetic field and detected simultaneously by a Faraday Cup. Reference CO
2, was used for comparison as in the method (b). The pressure of the sample CO
2, was adjusted so that
13CO
2 intensities in reference and sample CO
2 were equivalent. Detection limits of these methods in terms of
13CO
2 increase from basal abundance, Δ
13C, were, (a) 5.88 ‰, (b) 0.909 ‰, (c) 0.201 ‰, when NBS No. 20 Solenhofen Limestone was used as the reference. The precision was linearly dependent on Δ
13C and the method (c) achieved the best one which was 30 times and 5 times better than (a) and (b), respectively.
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Kuniaki KAWATA, Tatsuo UEMURA, Ikuei KIFUNE, Yasuko TOMINAGA, Kikuo OI ...
1982 Volume 31 Issue 8 Pages
453-457
Published: August 05, 1982
Released on J-STAGE: June 30, 2009
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Breakthrough volumes of 90 organic vapors on Tenax GC adsorbent at 20 °C with a flow rate of 200 ml min
-1 were measured to evaluate the capacity of Tenax GC adsorbent for the collection of trace organic compounds in ambient air at the ordinary temperature. The collection tube was a 5.5 mm i.d. × 21 cm long glass tube packed with 0.5 g of Tenax GC (60/80 mesh) supported by small plugs of quartz wool. The apparatus consisted of a Tedlar bag filled with a dilute vapor sample of the organic compound, the collection tube, a diaphram pump, a gas meter, and a flow meter. Breakthrough curve was obtained with gas chromatographic analysis using the periodic sample collected by a gastight syringe from the effluent cf the collection tube. Breakthrough volume is defined as the volume which the concentration of organic vapor in the effluent equals 10 % of the initial concentration. Test compounds were halogenated hydrocarbons, aliphatic amines, sulfur compounds, oxygen compounds, and hydrocarbons having from one to ten carbon atoms. The number of compounds that breakthrough volumes were more than 1 l, 10 l, and 100 l were 71, 47, and 4, respectively. These compounds were classified into eleven groups according to their structures, and in many groups, the logarithm of breakthrough volume showed good linear correlations with the boiling point, the reciprocal of the boiling point, the molecular weight, and the carbon number. These relations may be useful for estimating breakthrough volumes of another compounds having the similar structure.
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Kyoji TÔEI, Yoshie ONO, Toshiaki WAKIMOTO, Haruo MIYATA
1982 Volume 31 Issue 8 Pages
458-461
Published: August 05, 1982
Released on J-STAGE: June 30, 2009
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City water always contains 1 ppm or less chlorine for sterilization. The residual chlorine was determined by Michler's thioketone (4, 4'-bis-dimethylamino-thiobenzophenone) spectrophotometrically. City water (10 ml) was mixed with 1 ml of 0.2 M acetate buffer solution (pH 4) and 5 ml of Michler's thioketone solution which was prepared of 0.5 ml of concentrated hydrochloric acid, 4 mg of the ketone and 100 ml of 1-propanol in a 25 ml test tube with a ground stopper with shaking. After 10 min the absorbacne at 650 am was measured in a 10 mm glass cell. The calibration graph showed a straight line which passed through the origin and the molar absorption coefficient was 7.65 × 10
4, dm
3 mol
-1 cm
-1. Coexisting cations and anions in city water in this district did not disturb the determination. The method was applied to flow injection analysis. The reaction solution contained 40 mg of the reagent and 0.5 ml of concentrated hydrochloric acid in 1l of ethanol, and the carrier solution was made of 950 ml of 0.1 M formate buffer solution (pH 3.5), 50 ml of 0.01 M EDTA and 2 ml of 1/500 % (w/v) Triton X-405. Each flow rate was 1.7 and 1.3 ml/min, respectively. The peak height was proportional to the concentration of chlorine over the range of 01.5 ppm.
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Hiroaki KUBO, Yoshie KOBAYASHI, Toshio KINOSHITA
1982 Volume 31 Issue 8 Pages
462-466
Published: August 05, 1982
Released on J-STAGE: February 16, 2010
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A simple, rapid and reproducible method for determination of indomethacin in serum by high-performance liquid chromatography (HPLC) was developed. In preparation of sample for HPLC was used Sep-Pak C
18 cartridge and an internal standard was synthesized by mixed anhydride method from indomethacin and dimethylamine. The cartridge was washed by passing 50 ml of methanol by pressurizing through a glass syringe followed by 10 ml of ethyl ether and 50 ml of distilled water. Serum (200 μl) was deproteinized with 300μl of acetonitrile containing the internal standard, the mixture was centrifuged and the supernatant was mixed with 5 ml of acetate buffer (pH 4.0) and the mixture was passed through the cartridge. And the cartridge was washed by passing 4 ml of acetate buffer (pH 3.0) and 2 ml of distilled water. Ten milliliters of ethyl ether were passed through the cartridge and the eluate was collected and evaporated to dryness. The residue was dissolved in 100 μl of the mobile phase and a 80μl of portion of the solution was analyzed by HPLC on a Radial Pak C
18 column (10μm, 8 mm×10 cm) with 48% acetonitrile containing 0.01 M sodium acetate (pH 4.0) as mobile phase (2 ml/min) and detection at 254 nm (0.01 AUFS). The retention times for indomethacin and internal standard were 13 min and 18 min, respectively. The amount of indomethacin was determined by measuring peak height ratio. The detection limit of indomethacin was 10 ng/ml. The proposed method is reproducible for the assay of indomethacin in serum and its applicable to pharmacokinetic studies of the drug.
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Ryusuke KOBAYASHI, Mitsuya IMAI, Yoshikazu HASHIMOTO
1982 Volume 31 Issue 8 Pages
467-469
Published: August 05, 1982
Released on J-STAGE: June 30, 2009
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Some fundamental conditions of atomic absorption spectrometry combined with a technique of hydrogen telluride generation followed by its collection in a trap of liquid nitrogen have been investigated. Twenty ml of 5 N HC1 solution containing (1200) ng of tellurium(IV) is placed in the reaction vessel. Four ml of 5 % NaBH
4 solution was added to the reaction vessel over a period of 15 s. The generated hydrogen telluride is isolated by the gas trap immersed in liquid nitrogen and released by warming it up to room temperature. Then hydrogen telluride is transferred into an electrically heated quartz cell atomizer and the absorbance is recorded. Under the optimum conditions, the detection limit (S/N=2) was 1 ng and the coefficients of variation were 8.7 % in ten determinations of 100 ng of tellurium. Of the elements investigated, copper, mercury, arsenic etc. interfered much with the determination of tellurium.
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Tatsuji KIKUCHI, Shintaro FURUSAKI
1982 Volume 31 Issue 8 Pages
469-470
Published: August 05, 1982
Released on J-STAGE: June 30, 2009
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A simple method to determine concentration of CO
2 in water is studied. The CO
2-dissolved aqueous sample is introduced into a vessel to contact with air free from CO
2. Thus the gas phase is made in equilibrium with the liquid phase. The concentration in the gas phase is determined by gas chromatography. The concentration in the original sample is then calculated by the use of Henry's constant. The detailed procedures are described in the text. To investigate the accuracy of the present method, Henry's constants of CO
2 for several temperatures are determined by using a gas sample whose CO
2 concentration is known. The constants agree with the values in literatures. The present method is simpler both in operation and in apparatus than the conventional methods which use gas chromatography. Concentrations of other waterdissolved gases can also be determined by this method if Henry's constant of the system is known.
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Hiroto WATANABE, Kohei TACHIKAWA, Hideki OHMORI
1982 Volume 31 Issue 8 Pages
471-473
Published: August 05, 1982
Released on J-STAGE: February 16, 2010
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A cationic copper(II) complex ofα, β, γ, δ-tetrakis(1-methylpyridinium-4-yl)porphin was extracted with dodecylbenzene sulfonate. Polyoxyethylene nonyl phenyl ether with average 7.5 ethylene oxide units (POE-7.5) was used as an extractant, based on the fact that a dilute micellar solution of POE-7.5 separates into two phases above 0°C (the cloud point). The complex was extractable into a lower phase (about 0.6 ml) rich in POE-7.5 from 60 g of the micellar solution, and the recovery yield of the complex was 60 %. 4-Methylpyridine (4-Py) was effective in increasing the recovery yield, which rose to 95 % by adding a 1000-fold excess of 4-Py in relation to the copper(II) concentration. This is probably due to adduct formation of the complex with 4-Py. This technique, in combination with a dual-wavelength spectrophotometric method, was applied to the determination of copper(II) in water at several ppb level.
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Shigehiko HAYASHI, Kinuyo AOYAMA, Ryoko YAMADA, Keiya KOTSUJI
1982 Volume 31 Issue 8 Pages
473-475
Published: August 05, 1982
Released on J-STAGE: June 30, 2009
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A new chelating ion exchanger named “hydrox-amized Sephadex” (H-Sephadex) was prepared and its properties were investigated. H-Sephadex was prepared by the reaction of hydroxylamine with carboxy methyl-Sephadex (4.27 mmol COOH/g-gel, Pharmacia). The content of the introduced hydroxamic acid residue was 0.87 mmol/g-gel. Lead(II), copper(II), mercury(II), cadmium(II), zinc(II), and manganese(II) were collected completely from 50 ml of 1 × 10
-5 M solution of each metal salt over the pH range of 3.25.4, 4.09.6, 4.28.4, 4.79.8, 4.89.6, and 5.19.6, respectively, by stirring with 0.1 g of H-Sephadex for 30 min at room temperature. Copper was collected completely from the solutions containing 1 M sodium nitrate or calcium nitrate at pH 7.68.7, but the collection of cadmium and mercury was incomplete under similar conditions. When the collection of copper was carried out from 1 M sodium chloride, the optimum pH range was shifted to 9.6. The collection of copper, cadmium, and mercury was complete from 10
-4 M sodium citrate but incomplete from 10
-6 M EDTA at pH 5.06.9. With 0.1 g of H-Sephadex, copper, cadmium, and mercury were completely collected from (101000) ml solutions containing 5×10
-4 mmol of the metal salt at pH 5.26.9 by stirring for (3060) min at room temperature.
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Itsuo MORI, Yoshikazu FUJITA, Kimiko SAKAGUCHI, Shoko KITANO
1982 Volume 31 Issue 8 Pages
475-478
Published: August 05, 1982
Released on J-STAGE: February 16, 2010
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A simple and rapid spectrophotometric method for the determination of quinine ethylcarbonate (QNEC) with ο-hydroxyhydroquinonephthalein (Qn.Ph.) and uranium(VI) {U(VI)} has been established. This method based on the formation of association complex of Qn.Ph.-U(VI)-QNEC can be applied in the concentration range of 0120μg/10 ml of QNEC. The Sandell sensitivity is estimated to be 0.0098μg/cm
2 for QNEC at an absorbance of 0.001 at 555 nm against Qn.Ph.-U(VI) solution, and the apparent molar absorptivity is 4.1×10
4. The recommended analytical procedure is as follows : QNEC less than 120μg was placed in a 10-ml measuring flask, and 2.0 ml of 0.5 % MC solution, 0.75 ml of 1.0×10
-3 M U(VI) solution, 2.0 ml of a Walpole buffer (sodium acetateacetic acid, pH 5.3) solution and 1.5 ml of 1.0×10
-3 M Qn.Ph. solution were added. Then the mixture was diluted to 10.0 ml with water, and was kept at (2025)°C for 20 min. The difference of absorbance between the Qn.Ph.-U(VI)-QNEC solution and Qn.Ph.-U(VI) solution was measured at 555 nm against water. The mole ratio of U(VI), Qn.Ph. and QNEC in the association complex was estimated to be 1 : 2 : 2 by the molar ratio method. The proposedmethod was applied to the determination of QNEC in pharmaceutical preparations.
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Tamotsu WASA, Hiroshi YAMAMOTO
1982 Volume 31 Issue 8 Pages
T55-T60
Published: August 05, 1982
Released on J-STAGE: June 30, 2009
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A microcomputer-controlled polarograph by using two microcomputers (MEK D II, Motorola and H68/TR, Hitachi) and its data-processing system by using inexpensive electronic devices have been constructed, and programs for the system control and data processing have been developed. The selection of analytical modes (Tast, Normal pulse, Differential pulse polarography, Stripping voltammetry, etc.) and measurements were carried out by using the program control of MEK D II and the electrochemical data (
i and
E) were accumulated on the memory of the computer. A microcomputer, H68/TR connected to MEK D II was used for the data processing by BASIC language. After digital filtering of the data transferred from MEK D II, polarographic waves were detected. by comparing the slopes of the
i-
E curve. The approximate values of
id, and
E1/2 were estimated by using the linear least-squares fitting with the same manner to manual treatment. These values were then utilized for the rigorous calculation of
id,
E1/2, and
S (slope of the log plot) by means of least-squares fitting with Heyrovský-Ilkovic equation. The relative error of this data processing for artificial polarograms generated by the theoretical equation was less than ±0.1 %. The results of the computer treatment for Tast and Normal pulse polarography were in good agreement with values obtained by manual treatment. The overall precision of the system for the determination of metal ions (Pb
2+, Cd
2+, Zn
2+, etc.) was within ±2 % for
id and
E1/2, and ±5 % for
S. The execution time was about 3 min for the processing of three-step polarogram.
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Kikuo OIKAWA, Hiroko SAITO, Shigeaki SAKAZUME, Masami FUJII
1982 Volume 31 Issue 8 Pages
E251-E255
Published: August 05, 1982
Released on J-STAGE: June 30, 2009
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For the analysis of residual bromate ion, the ultrasonic extraction method was useful for taking sample solutions from bread. The large interference of chloride ion with the ion chromatographic analysis was eliminated easily by silver coated resin. The residual bromate ion was determined by the ion chromatography easily and rapidly without any complicated pretreatments.
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Masatada SATAKE, Lih-Fen CHANG, Ju Chieng YUH, B.K. PURI
1982 Volume 31 Issue 8 Pages
E257-E262
Published: August 05, 1982
Released on J-STAGE: June 30, 2009
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A new spectrophotometric method for the determination of iron(III) after adsorption of its complex on microcrystalline naphthalene has been investigated. Iron(III) forms a water-insoluble complex with 5, 7-dichlorooxine in pH range 1.5-10.0. The complex is easily adsorbed on microcrystalline naphthalene from its acetone solution. The naphthalene mixture is separated, dried and dissolved in dimethylformamide. The absorbance of the solution is measured at 476 nm. The method has been applied to the determination of iron(III) in metallic alloys and aqueous environmental samples and the results were compared with the standard 1, 10-phenanthroline colorimetric method.
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Hiroaki KUBO, Yoshie KOBAYASHI, Toshio KINOSHITA, Takashi NISHIKAWA
1982 Volume 31 Issue 8 Pages
E263-E268
Published: August 05, 1982
Released on J-STAGE: June 30, 2009
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A rapid, simple, and accurate method for the determination of tobramycin in serum by high-performance liquid chromatography (HPLC) has been developed. The method is sensitive to 0.2 μg/ml using only 20 μl of serum. The serum proteins are precipitated with methanol. To the supernatant, a counter-ion reagent is added, then an aliquot of the solution is injected into the chromatograph. The determination of tobramycin is performed by a combination of reverse-phase, ion-pair chromatography, post-column derivatization with o-phthalaldehyde, and fluorescence detection. Comparisons with a microbiological assay and with a homogeneous enzyme immunoassay gave a correlation coefficient of 0.941 and that of 0.978, respectively.
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Masataka HIRAIDE, Jun MIZUTANI, Atsushi MIZUIKE
1982 Volume 31 Issue 8 Pages
E269-E272
Published: August 05, 1982
Released on J-STAGE: June 30, 2009
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Suspended solids at the mg/l levels in fresh and waste waters are coagulated by stirring with cetyldimethylbenzylammonium chloride and sodium chloride, and quantitatively floated to the solution surface within 30 s with numerous tiny bubbles. This technique is more rapid than filtration with 0.45-μm membrane filters.
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Hitoshi WATANABE, Etsuro YOSHIMURA, Tetsuji TAIRA, Sunao YAMAZAKI, Mas ...
1982 Volume 31 Issue 8 Pages
E273-E276
Published: August 05, 1982
Released on J-STAGE: June 30, 2009
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Hydride generation mass spectrometry(HG/MS) has been developed and mass spectra of arsine and stibine were measured at various electron impact voltages. The relative intensities of their molecular and fragment peaks have been found constant at higher electron impact voltages(>70 V for arsine and >30 V for stibine) with the order of the intensities: (M-2)
+>M
+>(M-3)
+>(M-1)
+. Hypothetical intensities of fragment ions of stibine were formulated using the measured ion intensities and the isotopic ratios.
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