All issues
Volume 36, Issue 2
Displaying 1-18 of 18 articles from this issue
- |<
- <
- 1
- >
- >|
-
Akifumi YAMADA, Kazunori HODOUCHI, Koichi KATOH, Yoshikiyo KATOH1987 Volume 36 Issue 2 Pages 67-72
Published: February 05, 1987
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSVoltammetric sensor with a small silver electrode (0.3 mm in diameter and 99.99% in purity) has been applied to the analysis of chloride in sea sand and cement pastes. The voltammetric sensor consisted of a silver electrode (working electrode), a lead/lead(II) sulfate electrode (reference electrode) and a stainless-steel electrode (counter electrode). The sensor was connected to the voltammetric analyzer. Alumina of various particle size (0.05, 1 and 8μm) was used to polish an electrode surface; well-reproduced currents were obtained at the polished electrode with 8 μm alumina in a concentration range of 0.051.0% of chloride. Pretreatment of the electrode for the electrochemical activation was also examined; good results were obtained in 2% NaCl solution. For the determination of chloride in sea sand, a 30 g of sea sand was added in 50 ml of water, and the mixture was agitated for 10 min in order to extract chloride. An aliquot was then added into 0.1 mol dm-3 NaNO3 solution and the current due to chloride was measured. Chloride content was also determined by Mohr method; a correlation between the results of voltammetric and Mohr methods was found to be excellent with a correlation factor of 0.994. As for the analysis of chloride in cement paste, cement paste was filtered by aspirator, and a portion of the filtrate was added into 0.1 mol dm-3 phosphate buffer (pH 7.0) or acetate buffer (pH 4.6) solutions. Tast polarogram of the combined solution was measured; concentration of chloride was determined from the electric current due to the oxidation of chloride. Chloride in cement paste was also determined by the Mohr method; the results were in excellent agreement with those obtained by the voltammetric method and a correlation factor was 0.994. Effect of a water-cement ratio on the determination of chloride content was examined; the variation of the current was ±2.3%, while the water-cement ratio varied from 0.56 to 1.67.View full abstractDownload PDF (903K) -
Teruhiko HAGIWARA, Kazuyuki AKIYAMA1987 Volume 36 Issue 2 Pages 73-76
Published: February 05, 1987
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSA method for HPLC determination of digoxigenin (DO), digoxigenin monodigitoxoside(D1) and digoxigenin bisditoxoside (D2) in digoxin tablet was developed and applied to the determination of these digoxin hydrolyzed products in the chloroform extract of dissolution test solution of the tablet. Digoxin hydrolyzed products were separated at 40 °C on an Inertsil ODS column by using mixed solution of acetonitrile-methanol-water (11 : 7 : 35) as mobile phase, and were detected at 225 nm. Ethyl benzoate was used as an internal standard. In six brand of tablets, D0, D1 and D2 were found to be 0.131.84, 0.160.29 and 1.604.19 μg/tab., respectively. The chloroform extract of dissolution test solution was found to contain 42.546.4% D0, 17% D1, 20% D2 and 15.720.2% digoxin.View full abstractDownload PDF (595K) -
Shoji MOTOMIZU, Ikuo SAWATANI, Takashi HIRONAKA, Mitsuko OSHINIA, Kyoj ...1987 Volume 36 Issue 2 Pages 77-81
Published: February 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSRapid and sensitive determination of chloride, sulfate and nitrate ions in river water was achieved by ion chromatography with UV photometric detector. Comparison of elution ability of eluent ions was made by using phthalate, hemimellitate, trimellitate, trimesate and pyromellitate ions at pH 7.5. Trimellitate solution (1, 2, 4-benzenetricarboxylate, 4×10-4 M) is superior to other eluent ions because of its strong light-absorption at longer wavelength beyond 250 nm, suitable ability of elution for chloride, sulfate and nitrate ions, low price, high purity and easy availability. An anion exchange column (TSK gel IC-Anion-PW, 4.6 mm i.d.×50 mm) was used. Twenty microliters of sample solution was injected and decrease in absorbance of the trimellitate eluent at 250300 nm was detected. The calibration curves were linear in the range of (0.810)×10-4 M for chloride, (0.44)×10-4 M for sulfate and (0.120)×10-4 M for nitrate. By the proposed method, chloride, sulfate and nitrate in river water were determined within four min. The relative standard deviations of ten measurements of tap water were 0.35% for chloride, 0.56% for sulfate and 1.3% for nitrate, respectively.View full abstractDownload PDF (698K) -
Kazuhiro TANABE, Takao KAWASAKI, Masako MAEDA, Akio TSUJI, Masahiko YA ...1987 Volume 36 Issue 2 Pages 82-87
Published: February 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA highly sensitive chemiluminescence assay for NAD(P)H have been developed. The principle of present method is as follows; NAD(P)H reduced molecular oxygen to O2- and hydrogen peroxide (H2O2) in the presence of 1-methoxy-5-methylphenazinium methylsulfate (1-MPMS) as electron mediator. The produced O2- and H2O2 could be assayed by chemiluminescence reaction using isoluminol (IL)-microperoxidase (m-POD). A linear relationship between chemiluminescence intensity and NAD(P)H (log/log) was obtained ranged from 10-9 M to 10-5 M, and the detection limit was about 100 fmol/assay. The relative standard deviation of NADH and NADPH were 1.15.8 and 1.47.6%, respectively. This chemiluminescence reaction has been applied to the determination of total bile acids in serum, enzyme activity of glucose-6-phosphate dehydrogenase and glucose in blood. Plasma samples were assayed for total bile acids and glucose by both conventional and present method. The results showed good agreement by the correlation coefficient {r=0.96 for total bile acids (n=83) and r=0.99 (n=100) for glucose}.View full abstractDownload PDF (1052K) -
Kazuhisa YAMAYA, Nagisa OOSAKO, Hiroshi SHIOTA, Shoji KONDO, Minoru YO ...1987 Volume 36 Issue 2 Pages 88-92
Published: February 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSFluoride ion in aqueous matrix is determined at the parts per billion level by a combination of trimethyl-fluorosilane (TMFS) generation, concentration in cryogenic column and gas chromatographic determination with flame ionization detector. A 50 cm3-aliquot of a sample solution is transferred into a reaction vessel. To it are added 22 cm3 of hydrochloric acid and 3 cm3 of hydrochloric acid saturated with trimethylchlorosilane (TMCS). The produced TMFS is stripped from solution by passing nitrogen through a sintered glass filter ball(flow rate : 50 cm3 min-1). Then, it is collected for 14 min in a concentrating column cooled in a acetone-dry ice bath. The TMFS thus collected is injected all at once into the CC column (packing: 2% OV-3 on Uniport HP) and the fluoride is determined from the calibration curve for computing peak area. The proposed method is applied to determine 0.3 to 10 ppb of fluoride in aqueous solution. The average value obtained by measuring of the 10.0 ppb standard solution with the 95% confidence limit is 10.0±0.18 ppb. Most ions encountered in natural samples do not interfere.View full abstractDownload PDF (890K) -
Toshiaki NOMURA1987 Volume 36 Issue 2 Pages 93-97
Published: February 05, 1987
Released on J-STAGE: November 18, 2010
JOURNAL FREE ACCESSThe frequency of a piezoelectric quartz crystal varies in proportion to the mass change of the crystal electrodes. Barium sulfate produced by the reaction of sulfate with barium adsorbs on the electrodes of the crystal and decreases the frequency of the crystal with increasing mass of the electrodes. Thus the sulfate in water of the range 5100 μM (0.541 ppm) could be determined by using the calibration graph prepared with the satndard solution with a good reproducibility. Barium sulfate adhered could be removed with EDTA solution and only phosphate interfered.View full abstractDownload PDF (862K) -
Takeo IWAMOTO, Masahiko YOSHIURA, Keiji IRIYAMA1987 Volume 36 Issue 2 Pages 98-102
Published: February 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSMethionine (Met) in blood serum was determined by HPLC with the electrochemical detector in which an anodically treated glassy carbon (GC) electorde was used. The result were compared with those obtained with an untreated GC electrode. The oxidation current of Met appeared at the potentials more positive than +1.2 V using an untreated GC electrode, but the peak height was very small and nonreproducible. The response of the electrode was improved by preanodizing for 2 min at +1.9 V in 0.2 M phosphate solution (pH 6.5). The peak current showed linearity from 1 ng to 500 ng at the potential of +1.7 V with 0.02 M phosphate buffer (pH 3.0) used as a mobile phase. Reproducibility of relative standard deviation was as small as 1.31% (n=20) in the continuous injection of 100 ng samples. The detection limit of Met with the treated electrode was 360 times lower than with the untreated electrode. The treated electrode could be used without any deterioration for one week, 8 h per day.View full abstractDownload PDF (838K) -
Takayuki KANEDA, Satoshi TAKANO1987 Volume 36 Issue 2 Pages 103-108
Published: February 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSSimple and rapid methods have been developed for the determination of water hardness by colorimetry using ο-cresolphthalein complexone as a color development agent. In the determination of calcium hardness, 8-hydroxyquinoline-5-sulfonic acid was used as a masking agent for magnesium, whereas sodium citrate was used for the determination of total hardness in order to equalize the molar absorptivities of calcium and magnesium. To a transparent cylindric measurement vessel with 25 ml volume, a 20 ml of water sample and a reagent for the determination of calcium or total hardness were added, and the vessel was vigorously shaken for a miunte. The determination of calcium hardness (25150 ppm as CaCO3) and total hardness (25200 ppm as CaCO3) were easily carried out by comparing the color of sample solution to a standard color scale. In the presence of a yellow dye, color of the sample solution turns from yellow to red with an increase of water hardness. The results of the determination of calcium and total hardness in water by the proposed method agreed well with those by AAS.View full abstractDownload PDF (926K) -
Takayuki KANEDA, Satoshi TAKANO1987 Volume 36 Issue 2 Pages 109-113
Published: February 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA simple and rapid method has been developed for the determination of iron in water by colorimetry using disodium bathophenanthroline disulfonate as a color development agent. It was found that suspended iron in water such as ferric hydroxide and ferric oxide could be dissolved and ionized with oxalic acid rapidly. To a transparent cylindric measurement vessel with 25 ml volume, a 20 ml of water sample and 20 mg of oxalic acid were added, and the vessel was vigorously shaken for a minute. Then, a mixture of L-ascorbic acid, disodium bathophenanthroline disulfonate and a blue dye were added and the vessel was shaken for 2 min. The determination of iron of 0.050.5 ppm was easily carried out by comparing the color of sample solution to a standard color scale. In the presence of the blue dye, color of the sample solution turns from blue to purple with an increase of iron. The determination of iron was interfered with Cu(II) and a large amount of Ca(II), however the addition of EDTA after color development could eliminate these interferences. The results of the determination of iron in water by the proposed method agreed well with those by AAS.View full abstractDownload PDF (826K) -
Shigeru TANAKA, Masaru NAKAMURA, Yoshikazu HASHIMOTO1987 Volume 36 Issue 2 Pages 114-117
Published: February 05, 1987
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSThe method described has the advantages of easy preparation and rapid measurement of samples as compared with the other method, and enables the simultaneous determination of arsenic and antimony. One milliliter of zirconium oxychloride solution (10 mg Zr/ml), a coprecipitant, was added to 100 ml sample solution, then pH of the solution was adjusted to 9 with ammonia water. After collected on a Toyo No. 5C filter paper, the precipitate was dried in a desiccator for XRF analysis. Precipitation recoveries of arsenic(III) and antimony(III) in spring water with zirconium hydroxide were sufficient, while those of arsenic(V) and antimony (V) were not due to the interference of foregin ions. Therefore, arsenic(V) and antimony(V) were reduced to arsenic(III) and antimony(III) by adding 1 g potassium bromide and 1 ml hydrochloric acid to the sample and boiling it at 80 °C for 1 h, so that the sufficient recoveries were obtained. The linear range of calibration curves for arsenic and antimony by this method was within 200 μg. The limits of detection were 0.3 μg for arsenic and 6.1 μg for antimony in case of 100 ml sample volume. The analytical results of arsenic and antimony in spring waters at several sites in Japan by this method were in good agreement with those obtained by the hydride generation AAS.View full abstractDownload PDF (809K) -
Takashi IMAGAWA, Akira MIYAZAKI1987 Volume 36 Issue 2 Pages 118-120
Published: February 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSAs chlorinated hydrocarbons are said to be converted to more stable compounds by combustion, chloroform was injected into a gas chromatograph equipped with a flame ionization detector (FID) to examine the products. The exaust gas from the FID was sampled by a florisil column and the acetone eluate was analyzed by GC with an electron capture detector or a mass spectrometer when factors such as sample size, flow rate of air and hydrogen supplied to the detector were varied. Injection of 2 microliters of chloroform into a FID through a packed column resulted in formation of hexachlorobenzene together with hexachloroethane, hexachlorobutadiene, pentachlorobenzene and octachloronaphthalene. Formation of hexachlorobenzene was suppressed by making the sample size smaller, in creasing the flow rate of hydrogen or decreasing the flow rate of air in the detector.View full abstractDownload PDF (578K) -
Eiko NAKAMURA, Hiroshi NAMIKI1987 Volume 36 Issue 2 Pages 120-122
Published: February 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSNanogram per liter levels of mercury in water was determined by flameless AAS after preconcentration from a large sample volume, on KMnO4-coated glass beads as previously reported. Take 5 l of the sample in a glass bottle and add 15 ml of H2SO4 and 10 ml of H2SO4 (1M)-SnCl2(5%) solution. Pass mercury-free air into the sample at a flow rate 5 l/min for 20 min. Collect the generated mercury on the KMnO4-coated glass beads packed in a glass tube. Determine mercury as in the previous report. As these glass beads could collect mercury completely at high flow rates, complete generation and collection of mercury from a large sample volume could be done in a short time. Mercury in potable and deionized water determined by this method gave results of 23 ng/l.View full abstractDownload PDF (558K) -
Kazuaki ITO, Hiroshi SUNAHARA1987 Volume 36 Issue 2 Pages 123-125
Published: February 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDetermination of ammonium and nitrate ions in activated sludge process waters was examined by using plastic-membrane ammonium- and nitrate-selective electrodes. Magnesium sulfate solution was added to the samples for adjustment of ionic strength. Consequently the sample solutions contained 2.5×10-2 M MgSO4. Results obtained for ammonium ion (NH4+-N, 125 mg/l) were a little higher than those by ion chromatography and coulometric titration method. Results for nitrate ion (NO3--N, 136mg/l) were slightly higher than those by ion chromatography. These results could be attributed to interference by potassium and chloride ions (determined by ion chro-matography) for ammonium- and nitrate-selective electrodes, respectively. Thus, the present method is useful for routine analysis and successfully gives quick results on the effectiveness of nitrofication-denitrofication process.View full abstractDownload PDF (489K) -
Toshiaki HATTORI, Sigeru KUSUMI, Masaaki SUZUKI, Mitsuhiko TAGA, Hitos ...1987 Volume 36 Issue 2 Pages 125-128
Published: February 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe reactions of copper(II), nickel(II), lead(II), cadmium(II), zinc(II), silver(I) and thallium(I) ions with sodium diethyldithiocarbamate (DDTC) were examined by thermometric titration for the determination of these metal ions. The divalent metal ions reacted with DDTC in a molar ratio of 1 : 2 and monovalent thallium ion reacted in that of 1 : 1. But the titration of silver(I) ion exhibited a nonstoichiometric end point before the equivalence point. The divalent metal ions in the range of 40120 μmol can be determined within 1% error in acetate buffer solution at pH 5.0. The heats of precipitation of Cu(II)-, Ni(II)-, Pb(II)-, Cd(II)- and Zn(II)-DDTC were measured.View full abstractDownload PDF (628K) -
Sadayuki MATUDA1987 Volume 36 Issue 2 Pages 129-130
Published: February 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe apparent binding constant (Kapp) of calcium (II) with 2, 7-bis(4'-chloro-2'-phosphonophenylazo)-1, 8-dihydroxynapthalene-3, 6-disulfonic acid (chlorophos-phonazo III) was determined in the pH range of 6.08.0 by spectrophotometry at 20°C. In the presence of 0.1 M KCl, Kapp increased by a factor of 50 between pH 6.0 and 8.0. However, the pH dependency of Kapp above pH 7 was slightly smaller than that of Kapp below pH 7. At pH 6.8 Kapp was 1×106 M-1. The present data may be available to measure free calcium (II) concentration in biochemical experiment.View full abstractDownload PDF (328K) -
Eiko NAKAMURA, Hiroshi NAMIKI1987 Volume 36 Issue 2 Pages T5-T8
Published: February 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThough the copperized cadmium column(Cu-Cd column) method in JIS K 0102 is excellent in precision in the determination of the total nitrogen in water, some difficulty occures by the blocking of the column in the process of the Cu-Cd column reduction of the digested sample. In this paper, the phenomenon of the blocking was discussed. When the sample in a glass bottle was digested with peroxodisulfate in high alkaline medium at 120°C, 250350 mg/l of ionic silica (after diluted to 100 ml) dissolved out from the glass wall. When the solution pH was adjusted to 8.5 prior to the reduction process, the silica up to about 200 mg/l remained stable in ionic form. And the excess was changed to colloidal form by polymerization during the standing time, and resulted in the blocking of the column.View full abstractDownload PDF (651K) -
Haruo HONMA, Keiko SUZUKI, Mutsuko YOSHIDA, Hisako YANASHIMA1987 Volume 36 Issue 2 Pages T9-T14
Published: February 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSIn order to determine fluorine, chlorine and bromine in organic compounds precisely (within ± 0.3% of the theoretical values), several analytical conditions were discussed. Blank values were measured from the combustion system with or without a purification tube. In a combination of the eluent and diluting solution which were made of different lots of the same manufacturer, chloride ion blank value was 6133μVs. When the manufactures were different, the blank value was 5827μVs. Moreover, in the reagents of the same manufacturer and the same lot, but prepare at different times the value was 3404μVs. These values corresponded to 0.71.34% of the total peak areas. Thus the eluent and the diluting solution should be prepared simultaneously from the same lot of reagents Because the pH of the sample solution affected the sensitivity of detection, the combustion, absorption, and dilution of standard samples and unknown samples were performed under the same condition. The pH of eluent influenced the precision of detection. In the range of pH 10.269.87, the precision decreased with the decrease in pH. The most satisfactory precisions for the three ions were obtained at pH 10.72, but the resolution of bromide and phosphate ions tended to decrease at this pH. In this method, 4 mM Na2CO3-4 mM NaHCO3 solution(pH 10.26) was used as an eluent. Calculation was based on the sensitivity factor method. The sensitivity factors obtained by standard samples were in satisfactory precision. The relative standarddeviations of fluorine, chlorine and bromine determinations were 0.0183, 0.0070 and 0.0050, respectively.View full abstractDownload PDF (1010K) -
Studies on analytical methods by amperometric titration using a rotating platinum electrode. LIIHiromu SATAKE, Sanae IKEDA1987 Volume 36 Issue 2 Pages T15-T19
Published: February 05, 1987
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA precise method for the microdetermination of methionine in the presence of methionine sulfoxide was developed by amperometric titration using a rotating (2000 rpm) platinum electrode at the potential of +0.6 V vs. SCE. Methionine could be titrated at ca. 45 °C by potassium iodate standard solution with 0.05 ml portion at intervals of 260 s in the base solution of 0.5 M sulfuric acid-0.4 M potassium bromide. Relative errors and relative standard deviation of less than 0.3% were obtained in the sampling range of 0.0630 mg for methionine. Methionine in fifty-times amounts of methionine sulfoxide could be determined within a relative error of 3.1 %. Effects of amino acids were also investigated. The analytical procedure was as follows. Mix 5 ml of 5 M sulfuric acid, 5 ml of 4 M potassium bromide and 30 ml of distilled water into the titration cell (100 ml), and heat it to ca. 45 °C. Add exactly 10 ml of an aqueous solution of methionine (2×10-52×10-2 M). Titrate immediately the resultant solution with potassium iodate(10-410-1 M) standard solution by amperometry.View full abstractDownload PDF (778K)
- |<
- <
- 1
- >
- >|