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Volume 32, Issue 12
Displaying 1-21 of 21 articles from this issue
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Osamu FUJINO, Shigeru MATSUMURA, Masakazu MATSUI1983 Volume 32 Issue 12 Pages 713-717
Published: December 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe calibration curves, obtained as the absorbances of rare earth elements (REs) measured in the rangeof (0.255.5)×10-4M with atomic and ionic lines, suggest that REs are considerably ionized in a dinitrogen monoxide-acetylene flame. Therefore, the salts ofalkali metals ionized easily in the chemical flame werea dded to examine their matrix effects on the ionizationof REs. The salt concentrations studied were from 1×10-4M to 5×10-2M at (0.54)×10-4M of REs. When the concentrations of alkali metals were increased, the absorbance of the atomic line for REs increased, whereas the absorbance of the ionic line reduced to near nil. A similar tendency was found in the matrix effect between the REs and the coexisting common elements. Such matrix effects depend not only on the salt concentration but also on the ionization potential of the coexisting metal; higher salt concentration and lower ionization potential cause large rmatrixeffects. The results suggest that there exist electrolytic dissociation equilibria among the neutral atom and ion of REs and the electron in the dinitrogen monoxide-acetylene flame. The ionization fractions of REs in the dinitrogen monoxide-acetylene flame were calculated from absorbance behaviors of REs with and without alkali metal, and they were ionized around 79%, 65%, 42%, 35%, and 18% for europium, dysprosium, erbium, ytterbium, and scandium respectively, at the concentration of 1×10-4M. In the above calculation, it was assumed that the amounts of oxides of REs were large enough to discuss the equilibria between only atoms and ions.View full abstractDownload PDF (725K) -
Kunio NAGASHIMA, Masatoshi MATSUMOTO, Shigetaka SUZUKI1983 Volume 32 Issue 12 Pages 717-722
Published: December 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSHydrogen sulfide permeation-membrane and absorption solution were used in the continuous determination of hydrogen sulfide with sulfide ion-selective electrode. Fluorophore (Sumitomo Electric Ind., Tokyo; Pore size 0.22μm, diameter 7.0mm) was use das hydrogen sulfide permeation-membrane. A 0.5 N NaOH-8 wt% sodium salicylate-1.8 wt% L-ascorbic acid-2 × 10-7M sulfide ion; mixed solution was used as a absorption solution for hydrogen sulfide (This solution inhibits the air oxidation and produce a stable electrode potential). Hydrogen sulfide impinge onto the permeation-membrane, through which the hydrogen sulfide is absorbed into absorption solution. The volume of absorption solution in the absorption pass cell is about 0.15ml. The response time of this system for hydrogen sulfide was about 50 s. The absorption efficiency of hydrogen sulfide was constant, that is 88 %, at constant flow rate of both sample gas(40ml min-1) and absorption solution (7.4ml h-1) between 200 ppm and 0.1 ppm. In this range Nernst equation was valid with a coefficient of variation of less than 1 %. Lower determination limit of hydrogen sulfide was as low as 0.05 ppm. The coexistence of various gases such as carbon dioxide, sulfur dioxide, and hydrogen chloride had no influence on this method.View full abstractDownload PDF (864K) -
Tadashi TSUKIOKA, Tetsuro MURAKAMI1983 Volume 32 Issue 12 Pages 723-729
Published: December 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA method for the determination of trace amount of LAS (linear-alkylbenzenesulfonate) in environmental waters is described, in which LAS is converted to its sulfonyl-fluoride (LAS-F) and measured by gas chromatograph equipped with electron capture detector (ECD-GC). LAS was extracted into chloroform as the ion-pair with methylene blue and the extract was evaporated to dryness. One gram of phosphorus pentachloride and 2ml of hexane were added to the residue and hexane was allowed to reflux on an oil bath at (120130)°C for effecting the sulfonylchlorination. Then, sulfonyl-chloride of LAS (LAS-Cl) was extracted with hexane, and the extract was applied to a Silicagel column. After 100ml of hexane was poured to the column, LAS-Cl was eluted by 100ml of hexane: benzene (94:6) from the column, and the eluate was evaporated to dryness. To the residue were added 0.5 g of potassium fluoride and 2ml of hexane, and hexane was allowed to reflux in an oil bath at (120130)°C for effecting the fluoro-substitution. LAS-F was extracted with hexane and measured by ECD-GC using 2% OV-17 on Gas-Chrom Q as the GC column packing. The proposed method is superior to the method measuring LAS as LAS-Cl in the following point: 1) Neither thermal decomposition nor column adsorption were observed for LAS-F, 2) improved reproducibility was obtained, and 3) the former is 50 times of sensitivity of the latter. Recovery of LAS in river water was 89% of averaged recovery (coefficient of variation: 3.3%). LAS could be detected in all of 22 samples of river water. A correlation among the analytical results of these river waters by the proposed method (GC value) and methylene blue method (MB value) was showed by the equation of
GC value=0.730×MB value -0.015 (correlation coefficient 0.963).View full abstractDownload PDF (1024K) -
Yasuharu NISHIKAWA, Keizo HIRAKI, Kiyotoshi MORISHIGE, Yuji MURATA, Ts ...1983 Volume 32 Issue 12 Pages 729-735
Published: December 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSRoom temperature phosphorometry (RTP method) has been applied to the determination of trace amount of lead by measuring RTP intensity of lead-Calcein complex on filter paper. Calcein reacts with lead in acetic medium (pH 4) to form 1:2 complex, and the complex adsorbed on filter paper shows two bands of long-lived emission at room temperature, which can be atributed, respectively, to room temperature phosphorescence and to delayed fluorescence arising from triplet upper singlet thermal activation (TADF). A dominant characteristic emission is RTP {Ex: 490nm/Em: 620nm, τRTP: (4.5±0.1)ms}. The procedure for the determination of lead was established as follows: one μl of (10-710-3) mol dm -3 -lead solution was spotted on the filter paper (Toyo, No. 51) with a microliter syringe. Then, 1μl, 1 of 2×10-4 mol dm-3-Calcein dissolved in 0.1mol dm-3 -CH3COONH4 and CH3COOH buffer solution (pH 4) was spotted on the spot. Care was taken to maintain the spot size (5mm diameter) as constant as possible. The filter paper was dried at 50°C for 20min with an air dryer. The sample was then directly mounted on a sample holder, and the holder was fitted into the phosphoroscope accessory instead of the normal cap and cylinder used for the dewar flask assembly. The RTP intensity of the spot was measured at constant temperature{(1020)°C}, Ex: 490nm, Em: 620nm. There relationship between the intensity of RTP and concentration of lead was linear over a wide range from (0.120)ng (spot size: 5mmφ). The coefficient of variation of the measurement for sample containing 2 ng lead per spot was less than 3% (5 determinations). Iron (III), cobalt (II), and copper (II) interfered with the RTP measurement of lead, but it was found that lead could be selectively collected on zinc sulfide paper, therefor, this RTP method was applicable to the quantitative analysis of lead in natural water without any interference of cation. In practice, natural water sample adjusted at pH 4 was filtered through the zinc sulfide paper, then lead concentrated on the paper was dissolved in 10 cm3, of 4 mol dm-3 nitric acid by heating at 80°C_for_5min. Afterfiltration of the solution with No. 5C filter paper, lead in the solution was determined by the RTP method. Trace amount of lead in Pepperbush and water samples was determined by this method with satisfactory results.View full abstractDownload PDF (1031K) -
Shigeru TANAKA, Takayuki YOSHIMORI, Yoshikazu HASHIMOTO1983 Volume 32 Issue 12 Pages 735-739
Published: December 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe method of solvent separation and determination for sulfate aerosol {H2SO4, NH4HSO4, and (NH4) 2SO4}was investigated. The sulfate aerosol collected on a Teflon filter is extracted by two kinds of solvents (benzaldehyde and 2-propanol). Benzaldehyde is used for the separation of H2SO4 from NH4HSO4 and (NH4)2SO4, and 2-propanol is used for the separation of NH4HSO4 from (NH4)2SO4. The extraction efficiencies of H2SO4, NH4HSO4, and (NH4)2SO4 by benzaldehyde were 96%, 3.2%, and 1.7%, and by 2-propanol were 92%, 50%, and 4.8%, respectively. These results indicated that benzaldehyde could separate H2SO4 from NH4HSO4 and (NH4)2SO4. However, the separation of NH4HSO4 from (NH4)2SO4 by 2-propanol were not sufficient. After extraction by solvents, a sample solutions in benzaldehyde and 2-propanol were reextracted or diluted with distilled water for ion chromatographic analysis. In order to prevent the effect of solvents in sample solutions for ion chromatographic analysis, a pre-column that trapped only sulfate ion and removed solvents was installed in the sample injector. The analytical precision of this method for sulfate was within 2.5%. The detection limits of atmospheric sulfate by this method was 0.005μg/m3at 40 m3 air sample volume. Atmospheric sulfate were measured by using this method in Yokohama in September, October, and December, 1982. The concentrations of H2SO4 and total sulfate in the air were (0.030.1)μg/m3 and (0.63.2)μg/m3, respectively. The percentage of H2SO4 in total sulfate was (1.36.2)%. Therefore, it is considered that most of sulfate aerosol is in neutralized chemical form such as NH4HSO4 and (NH4)2SO4.View full abstractDownload PDF (755K) -
Hideki TANAKA, Takahiko NAKANO, Yoshiaki KANAZAWA1983 Volume 32 Issue 12 Pages 740-745
Published: December 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSOn the measurement of trace amounts of chromium existed in polluted natural waters, the conditions ofcomplex formation regarding trifluoroacetylacetone (HTFA) and chromium and the gas chromatographic determination using an electron capture detector were studied. Chromium (III) was reacted with 0.17mol HTFA in benzene (20ml) for 90min with occasional shaking at room temperature. The percentage of extraction for the complex was in the range of 97% to 100%. For the conditions of gas chromatography depend on the separation of the complex, 0.32% OV-11 (60/80 mesh) column (1.6m×3mmφ) was used and the column temperature and the rate of N2 flow were setted up at 160°C and 70ml/min, respectively. The present method was well suited for the routine analysis of a natural water sample because the procedure was simple and the detection limit for total chromium was about 0.03μg/l. The coefficient of variation for chromium of 0.25μg/l was in the range of 12% to 13%. Any interference for the determination of chromium was not recognized at ordinary level of the concentration of various metal ions, salts, and dissolved organic matters existed in natural waters. On the samples highly polluted, the remarkable differences in the analytical values of chromium were observed by the using filter papers.View full abstractDownload PDF (900K) -
Akira MIYAZAKI, Akira KIMURA, Hiroaki TAO, Kenji BANSHO, Yoshimi UMEZA ...1983 Volume 32 Issue 12 Pages 746-751
Published: December 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSDemands for introduction of organic solvents into inductively coupled plasma (ICP) are increasing, because solvent extraction has been introduced for use in the pretreatment for ICP atomic emission spectrometry. Organic solvents were introduced into a low power (<1.6kw) ICP by an ultrasonic nebulizer without aerosol desolvation, and the effects on the measurements of Hg, Cd, P, Pb, Zn, Mn, Cu, Fe, V, and Mo were studied. By replacing the Teflon sample tube of the ultrasonic nebulizer (Plasma Therm, Model USN-1) with a platinum (or stainless steel)tube, the relative standard deviation of the signal intensity for organic solvents was improved to (0.51.0)%. Evaluation for more than fifty organic solvents confirmed that vapor pressure was useful to predict the ease of introduction of organic solvents into ICP. Signal enhancement (net intensity for organic solvents/net intensity for aqueous solution) for an ultrasonic nebulizer was smaller than that for a pneumaticnebulizer. This behavior might be attributed to the larger temperature lowering of the plasma by ultrasonic nebulization, since it enables more aerosol to enter the plasma than pneumatic nebulization. However, signal intensity itself for organic solvents by ultrasonic nebulization was (25) times that of pneumatic nebulization. Hence, the modified ultrasonic nebulizer without a desolvation system provided maximum 10 times improvement in detection limits as compared to those obtained by a pneumatic nebulizer. Among the organic solvents tested, amyl acetate and DIBK were recommended for ultrasonic nebulization due to the low detection limits.View full abstractDownload PDF (902K) -
Kunio SUGINO1983 Volume 32 Issue 12 Pages 752-756
Published: December 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSSulfide (H2S, HS- and S2-) in water has usually been determined by iodometric titration. But the direct iodometric titration is often interfered by coexisting substances such as sulfite, thiosulfate, nitrite ions and so on. The present paper describes the method of determination of sulfide based on the vaporization of sulfide. This method is less affected by the coexisting substances. A sample solution (50cm3) is placed in the closed vessel, which consists of an inner tube and an outer flask. Hydrogen sulfide, which is released from the sample on addition of acid, diffuses to the inner tube containing zinc acetate and zinc sulfide precipitates in this tube. And then, zinc sulfide is determined by the iodometric titration.In this method, the coefficient of variation and the mean recoveries (n=8) were 0.99%, 0.59%, 0.34%, and 0.55%, and 100.8%, 98.6%, 98.7%, and 98.6% for sulfide of 3.6mg/dm3, 8.1mg/dm3, 15.7mg/dm3, and 36.8mg/dm3 in deionized water, respectively. The interference caused by sulfite ion could be eliminated by the addition of formalin as a masking agent. The interference of thiosulfate and nitrite ions was proved to be negligible.View full abstractDownload PDF (638K) -
Toshio SUZUKI, Masato SUWABE, Kiyoshi SAWADA, Fumio SHIRAI1983 Volume 32 Issue 12 Pages 757-760
Published: December 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSIn the study of thallotoxicosis, it had become necessary to determine accurately a low thallium contentin the tissue samples. Then, a method was studied for the determination of thallium in the human internal organs. The determination method of thallium is as follows. After digestion of the sample with nitric and sulfuric acids and hydrogen peroxide, the solution was evaporated to dryness. The residue was dissolved in dilute hydrochloric acid and saturated bromine water was added to oxidize thallium to the trivalent state. Acidity was adjusted to about 0.5N hydrochloric acid solution and thallium was extracted with 5ml of 1w/v% trioctylmethylammonium chloride (Capriquat) solution in xylene. Extracted thallium in the organic phase was directly determined by graphite furnace atomic absorption spectrometry. This method wasapplied to the determination of thallium in the toxichuman internal organs. Good results were obtained by the proposed method. The chemical species for the extraction of thallium was studied. The species extracted could be formulated as follows: (R3CH3N)-TlCl4 (R=octyl radical).View full abstractDownload PDF (566K) -
Shigeki DAISHIMA, Yoshio IIDA, Akihiro SHIBATA, Keiichi FURUYA1983 Volume 32 Issue 12 Pages 761-765
Published: December 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA rapid method for the determination of benzo [a]pyrene (B [a] P) in engine exhaust and airborne particulates has been developed by gas chromatography mass spectrometry (GC/MS) using negative ion chemical ionization(NCI). Particulate on a glass or quartz fiber filter is extracted with ethanol/benzene with the aid of an ultrasonic generator. To the neutral fraction of the extracts hexabromobenzene is added as an internal standard, and the solution is concentrated to 0.5ml. Oneμl of this solution is introduced through a splitless injector into a GC/MS equipped with a 5m SE-54 fused silica capillary column. Methane is used as a reagent gas. The ionization chamber pressure and ion source temperature are 0.2 Torr and 250°C. The mass fragmentograms are recorded atm/z 252 and 79 corresponding to M- of B [a] P and Br- of hexabromobenzene, respectively. Amount of B [a] P is calculated from the ratio of the peak area of B [a] P to that of an internal standard. Since M- of B [a] P was formed about 60times more than that of benzo [e] pyrene(B [e] P) in NCI mode, B [a] P could be measured selectively without complete separation from B [e] P. Results obtained by the proposed method were in fair agreement with those by HPLC-fluorescence detection method. It was found that the determination limit of this method was about 50pg with relative standard deviation of (16)% and the time required for a GC/MS measurement was within 10min.View full abstractDownload PDF (791K) -
Makoto KURIHARA1983 Volume 32 Issue 12 Pages 766-768
Published: December 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe 4-aminoantipyrine method is adopted in Japan Industrial Standard (JIS K 0102) as a method for the determination of phenols in industrial waste water because of its high sensitivity and good reproducibility. However, a troublesome problem arised in the laboratory waste water treatment. Namely, hexacyanoferrate (III) ion which was used as an oxidizing agent in the reaction of phenols with 4-aminoantipyrine could not be decomposed under the common alkaline chlorination process for the waste water containing cyanide. The 4-aminoantipyrine method with iodine instead of potassium hexacyanoferrate (III) was reformed. To 100 ml of sample solution containing not more than 0.05 mg of phenol taken in a 300ml separating funnel, 3ml of ammonium buffer solution (pH 10), 2.0ml of 4-aminoantipyrine solution and 7 ml of 0.05M iodine solution were added. The mixture was allowed to stand for 3 min and then shaken for 2 min with 10.0ml of chloroform. The absorbance of chloroform phase was measured at 460 nm. The analytical curve for phenol was linear in the concentration range of 1μg to 50μg. The precisions (C. V.) were 6.1%, 0.9%, and 0.7% for phenol of 2μg, 20μg, and 50μg, respectively.View full abstractDownload PDF (381K) -
Effects of relative humidity on the weight of samples and how to take the countermeasureMasataka NISHIKAWA, Keiko MIYASAKA, Tsuguo MIZOGUCHI1983 Volume 32 Issue 12 Pages 768-770
Published: December 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSAfter airborne particulates are collected with a high volume sampler or a low volume sampler, it is prescribed that those samples are weighed in the atmosphere at 20°C and 50% relative humidity. Therefore, an experimental apparatus for the easy control of humidity was developed. From of the results of weighing of blank filters under the various values of humidity, it was proved that filters of cellulose ester had the properties of larger moisture-adsorption than those of glass fiber. The weighing of airborne particulates collected on filters is difficult because of moisture-adsorption of those. But the samples were able to be easily and accurately weighed by being tightly covered with aluminum leaves in the box for conditioning of the samples before weighing of those. The results of weighing with this method were independent of various values of humidity in the room where those samples were weighed.View full abstractDownload PDF (441K) -
Takashi TANAKA, Kazuo HIIRO, Akinori KAWAHARA, Shinichi WAKIDA1983 Volume 32 Issue 12 Pages 771-773
Published: December 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSHypophosphite, phosphite, and phosphate ions were determined by ion chromatograph equiped conductivity detector. Well separated chromatograms of the each anions were obtained by using a mixture of 0.003M sodium bicarbonate-0.0024M sodium carbonate solution (pH 10.3) as eluent. When the detector sensitivity was set at 1μS/cm and 100μl sample was injected into the system, (0.050.5) mgP/1 of hypophosphite, (0.11.5)mgP/1 of phosphite, and (0.23)mgP/1 of phosphate were determined. The coefficients of variation of peak hights of hypophosphite, phosphite, and phosphate as 0.5 mgP/1 of each ten samples were 1.5%, 1.4%, and 4.1%, respectively. The method was applied to determination of hypophosphite and phosphite in plating solutions.View full abstractDownload PDF (422K) -
Masaru NIITSU, Katsuya TAKAI, Nobuhiko IRITANI1983 Volume 32 Issue 12 Pages 773-775
Published: December 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSEffects of various anions on the solvent extraction of chromium (III) with 1-(2-pyridylazo) -2-naphthol(PAN) were studied and remarkable effects on the extraction were found in the presence of perchlorate ion. The procedures were carried out as follows: the mixture of aqueous solution containing chromium (III) and acetate buffer (pH 3.1) and 1cm3 PAN-methanol solution (0.2%) was heated at 363 K for 120min.After cooling to room temperature, 10cm3 of chloroform was added to extract the chromium (III)-PAN complex. The concentration of extracted complex depended on the acetate buffer concentration in the aqueous phase. Similarly the effects of the various anions on the extraction were studied. It was found that the spectra of the complex changed greatly in the presence of perchlorate ion and the intensity of absorption increased considerably. Furthermore, the extraction achieved quantitatively above 1mol dm-3 of the anion.View full abstractDownload PDF (488K) -
Masahiro TACHIBANA, Toshiaki IMAMURA, Mikihiko SAITO, Kenyu KINA1983 Volume 32 Issue 12 Pages 776-778
Published: December 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSTAMSMB {2-(2-thiazolylazo) -4-methyl-5-sulfo-methyl-aminobenzoic acid} was used in a spectrophotometric flow injection system for the determination of copper in serum (0.7ppm to 1.5ppm). For the determination of copper in serum, a 20μl of deproteinized sample is injected into a carrier stream of acetate buffer solution (pH5) containing 0.1% Brij-35. The carrier stream meets a reagent stream of TAMSMB (10-5M) solution at confluence point.After mixing coil (0.5mm i. d.×200cm), the absorbance at 585 nm of the effluent was continuously measured by a spectrophotometer with a 8μl flow-through cell. Sampling rate was 70 samples per hour. Calcium (II), Magnesium (II), and iron (III) did not react with under the proposed condition. The method was satisfactorily applied to the variety of serum samples.View full abstractDownload PDF (353K) -
Tohru WAINAI, Hiroshi KANEMOTO, Kiyoshi MASHIMO1983 Volume 32 Issue 12 Pages T123-T128
Published: December 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSAn anionic linear alkylbenzenesulfonates (LAS) surfactant is a mixture of n-alkyl chains with sulfonated phenyl group attached at various positions on normal chain length range of 10 to 14 carbons, and the distribution has a considerable influence on the abilities of a synthetic detergent. The isomeric sodium dodecylbenzenesulfonates (2φ6φDBS) which are principal constituents in LAS and sodium 2-alkylbenzenesulfonates with phenyl group attached at 2-position on C10 to C14, n-alkyl chains were synthesized. The chemical shifts in the 13C-NMR spectrum for each LAS were assigned. On the basis of the above chemical shifts, the analysis of a commercial LAS was investigated from the quantitative 13C-NMR spectrum, which was measured by the gated decoupling technique with a relaxation reagent, H2[Gd (DTPA)], added for the suppression of long spin-lattice relaxation time and nuclear Overhauser effects. The analytical result of the LAS by the 13C-NMR method agreed fairly well with that of the original linear alkylbenzenes obtained by GC method. In particular, 5φ and 6φLAS that were difficult to separate by the GC method could be determined by this method.View full abstractDownload PDF (867K) -
Junichi SHIDA, Noriyoshi IWABUCHI, Akira SUGIMOTO, Tsutomu MATSUO1983 Volume 32 Issue 12 Pages T129-T132
Published: December 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe ion-associate of 12molybdophosphate with basic dye is precipitated in a nitric-acid medium. The precipitate is floated with a mixture of organic solvents at the phase boundary, and separated from the excess of reagent (flotation). The adaptability of four basic dyes (Rhodamine B, Safranin O, Neutral Red, and Malachite Green) to the flotation-spectrophotometric determination of phosphate ion has been studied. The standard procedure is as follows: to a 20-cm3 portion of the sample solution (previously neutralized) containing less than 3μg P in a 100-cm3 separatory funnel, 10 cm3 of 4mol dm-3 nitric acid solution, 10 cm3 of 0.1mol dm-3 ammonium molybdate solution, 5cm3 of 1mol dm-3 potassium nitrate solution, and 1cm3 of 2×10-3mol dm-3 basic dye solution are added, and the solution is diluted to 50cm3 with water. Add about 10cm3 of a mixture of methyl isobutyl ketone and cyclohexane. Shake for 10min, allow the phases to separate, and discard the aqueous phase carefully. Then, back-extract the excess of reagent with water. Repeat the washing with water until the washings are colorless. Add Zephiramine solution (5 cm3 of 5.0×10 -3mol dm-3 Zephiramine and 5cm3 of 0.5mol dm-3 nitric acid) or polar solvent (ethanol or N, N-dimethylformamide) to dissolve the precipitate, and transfer the solution into a 25-cm3 volumetric flask. Dilute to the mark with water and measure the absorbance against a reagent blank. Rhodamine B has the most excellent sensitivity (molar absorptivity is 3.2×105mol-1cm-1dm3 at 558nm), and Neutral Red is superior to the other dyes in precision. The molar ratio of basic dye to 12molybdophosphate in each ion-associate is found to be 3:1. Arsenic(V), germanium(IV), and silicon (IV), which form heteropolyacids like phosphorus (V), interfere in the determination of phosphate ion.View full abstractDownload PDF (586K) -
APPLICATION OF XANTHENE DERIVATIVES FOR ANALYTICAL CHEMISTRY. Part XXXIVYoshikazu FUJITA, Itsuo MORI, Shoko KITANO1983 Volume 32 Issue 12 Pages E379-E386
Published: December 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA color reaction between pyrogallol red(PR) -molybdenum(VI) complex and protein was investigated. A spectrophotometric method using the PR-molybdenum(VI) complex could be used in the concentration range of 0 - 400 μg/10 ml of albumin, where the Sandell sensitivity was calculated to be 0.0048 μg/cm2 for albumin at 600 nm. A detection test of protein on a spot plate was also studied. The proposed method was applied to the determination of urinary protein; analytical results were satisfactory.View full abstractDownload PDF (693K) -
A. ALONSO, M. GALLEGO, M. VALCARCEL1983 Volume 32 Issue 12 Pages E387-E394
Published: December 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe analytical applications of salicyloylhydrazones of di-2-pyridyl ketone (SHDPK) and 2-benzoylpyridine (SHBP) are described. A rapid, sensitive atomic absorption spectrophotometric method for the determination of trace amounts of Pb(II) is presented. Both reagents form stable cationic complexes with lead. These complexes are quantitatively extracted into isobutyl methyl ketone (IBMK) in the presence of perchlorate as ion-pair. The lead-SHDPK complex formed in an acid medium (pH=4.5) has been used for the determination of lead in water samples.View full abstractDownload PDF (622K) -
SENSITIVE DETERMINATION METHOD OF CREATINE PHOSPHOKINASE ISOENZYMES BY BIOLUMINESCENT LIGHT EMISSIONKayoko ODA, Shigeru YOSHIDA, Shingo HIROSE, Tatsumori TAKEDA1983 Volume 32 Issue 12 Pages E395-E401
Published: December 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSIsoenzymes of creatine phosphokinase (CPK-MM, -MB and -BB) were separated by anion-exchange chromatography, with use of stepwise gradient. The separated isoenzymes were subsequently mixed with the reagents necessary for producing nicotinamide adenine dinucleotide, reduced form (NADH). The produced NADH was measured by flow injection analysis for bioluminescent assay. The lower limit of the detection of NADH was at femtomole level. As the results, the determination of CPK-MB and -BB of low activity without the effects of serum background was possible. The reproducibility was good with the coefficient of variations in the range 2.5 - 3.0 % for CPK-MM, 4.0 - 5.2 % for -MB and 7.0 - 8.1 % for -BB.View full abstractDownload PDF (569K) -
Makoto NOSHIRO, Tomio YARITA, Shigeaki YONEMORI1983 Volume 32 Issue 12 Pages E403-E406
Published: December 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSFor the determination of trace fluorine in organic compounds such as fabrics finished with water and oil repellants, a rapid and highly sensitive method is established. Organic fluorine was decomposed by sodium biphenyl reagent and the fluoride was determined by trimethylsilyl fluoride-gas chromatographic method. Analytical results of the present method show good agreement with those of conventional methods.View full abstractDownload PDF (322K)
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