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Volume 42, Issue 5
Displaying 1-16 of 16 articles from this issue
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Manabu IGAWA, Shin OGAWA, Hiroshi OKOCHI1993 Volume 42 Issue 5 Pages 259-264
Published: May 05, 1993
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn the surface water analysis, the existing forms of iron and aluminium are apt to change during the preservation period and the filtration. The sample should be filtered within a day after the sampling and the sample volume should be small to avoid gel layer formation during filtration. Size distribution of metal in surface water was evaluated by filtration method. Sodium, potassium, calcium and magnesium are dissolved predominantly as free ions, whereas aluminium and iron are existing as particulate matters in surface water samplesView full abstractDownload PDF (613K) -
Yasuhisa SHIBATA, Kunio HIROTA, Hiroyuki MIYAGI, Yoshinori TAKATA1993 Volume 42 Issue 5 Pages 265-271
Published: May 05, 1993
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSInterference in the analysis of undiluted patient serum samples with dialysis by chloride ion-selective polymeric membrane electrodes (Cl-ISEs) was studied. The sensing membrane of Cl-ISE was prepared by using methyltridodecylammonium salt and 1-tetradecyl alcohol as a sensing material and a plasticizer, respectively. In the case of new Cl-ISE, fast response and good correlation to the reference method (chloride counter) were obtained. On the other hand, the used Cl-ISE showed slower response to the patient serum samples with dialysis compared to standard solutions and patient serum samples without dialysis. In many cases, the analytical values of patient serum samples with dialysis by used Cl-ISE were 10 mmol/l or more higher than that of chloride counter. It was shown that the new Cl-ISE had changed to become easily responsive to lipophilic anions and organic acid compounds after the immersion in control serum samples. The patient serum samples with dialysis were analyzed by the gel permeation chromatog-raphy(GPC) using a UV detector and many peaks which could not be observed in the measurement of patient serum samples without dialysis were detected. The used Cl-ISE was applied to the detector of GPC and the patient serum samples with dialysis were analyzed. Two peaks (retention time: 12.4 and 16.4 min) based on the compounds whose molecular weights are larger than Cl- (retention time: 18.8 min) were observed. The used Cl-ISE covered the surface of sensing membrane with dialysis membrane (fractional molecular weight: 1000) was applied to the detector of GPC and no peak was observed. Therefore, it was suggested that the molecular weights of interfering substances in patient serum samples with dialysis were over 1000.View full abstractDownload PDF (1132K) -
Hisae NAKAHARA, Shinichi KINUGASA, Shigeru HATTORI, Masaharu MUKOUYAMA ...1993 Volume 42 Issue 5 Pages 273-278
Published: May 05, 1993
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSNarrow distribution of oligo(methyl acrylate)s with a degree of polymerization (n=2 to 10) was obtained by the use of preparative gel permeation chromatography. The ratios of weight average molecular weight (Mw) to number average molecular weight (Mn) were less than 1.01 for all prepared oligo(methyl acrylate)s. Oligo(acrylic acid)s (n=26)were obtained by the hydrolysis of the oligo(methyl acrylate)s. The specific refractive in-dex increment (dn/dn) was apparently independent of the degree of polymerization of prepared oligo(methyl acrylate)s and oligo(acrylic acid)s. In the measurements of vapor pressure osmometry of the prepared oligo(methyl acrylate)s and oligo(acrylic acid)s, it was found that a calibration coefficient K increased slightly with Mn in benzene and in dioxane at 45°C.View full abstractDownload PDF (690K) -
Nobuo NAKANO, Takeo HARA, Yasumasa TAKEUCHI, Kunio NAGASHIMA1993 Volume 42 Issue 5 Pages 279-283
Published: May 05, 1993
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA galvanic sensor for monitoring nitorogen dioxide was developed using the composite of silver ion conducting solid electrolyte and polymer (copolymer of stylene and butadiene). The sensor, which is expressed as Au/Ag6I4WO4+polymer/Ag0.7V2O5 +Ag6I4WO4+polymer, is a rectangular prism 25 mm long, 25 mm wide and 0.4 mm high. The working electrode was made by sputtering of gold in argon. The Ag6I4WO4 silver-ion-conductive solid electrolyte was formed into a sheet using polymer and Ag0.7V2O5+Ag6I4WO4 electrode was laminated as the counter electrode. The used polymer was a copolymer of styrene-butadiene. The thickness of the deposited gold, electrolyte sheet and Ag0.7V2O5+Ag6I4WO4 electrode are 25 rim, 0.3 mm and 0.1 mm, respectively. The detector is able to work at room temperature. When the sample gas impinges at 300 ml min-1 on the gold cathode, the current flowing through the external circuit is linearly related to the concentration of nitrogen dioxide up to about 8 ppm and the lower detection limit is 0.3 ppm. The response time was about 3 min. The gas sen-sitivity of the sensor using this solid electrolyte sheet was stable for a long period. From the results, it is concluded that this sensor maintains stable output current for at least 200 days at room temperature.View full abstractDownload PDF (556K) -
Yuichi KOIKE, Yuzuru NAKAGUCHI, Keizo HIRAKI1993 Volume 42 Issue 5 Pages 285-291
Published: May 05, 1993
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe vertical distributions of Se(IV) and organic selenium in open sea are similar to those of nutrients. It was therefore considered that Se(IV) and organic selenium in sea water were supplied from the decomposition of marine biological material. In this study, marine planktons were used as biological material. Some pretreatment procedures were investigated for the chemical speciation of selenium in marine plankton samples. Selenium was determined by 2, 3-diaminonaphthalene (DAN) fluorometry. The interference of coexistent fluorescent materials for the fluorescence spectrum of 4, 5-piazselenol (Se-DAN complex) was effectively removed by back-extraction with concentrated nitric acid, followed by a wet-ashing method, and dilution with distilled water to 80 times the initial sample solution. The contents of selenium species in plankton body fluid changed with time. The sample pretreatment must therefore be carried out immediately after plankton thawing.View full abstractDownload PDF (1134K) -
Hiroshi NISHIDA1993 Volume 42 Issue 5 Pages 293-298
Published: May 05, 1993
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAluminium reacts with 8-quinolinol to form a light-yellow soluble complex with a maximum absorption at 380 nm in a 40% v/v aqueous pyridine solution. The color development of the complex was applied to a spectrophotometric determination of aluminium. Bcer's law holds for 1150 μg of aluminium in 25 cm3; the apparent molar absorptivity at 380 nm is 6.3 × 103 dm3 mol-1 cm -1. In the presence of interfering foreign cations (such as iron, copper and zinc) aluminium can be successfully determined by measuring the absorbance of a sample solution against water at 380 nm and by solving a given equation, 1/(b+ k) =1/(A+k-ax), for x, where A is the absorbance of the sample solution, b the sum of their absorbances for 8-quinolinol complexes of foreign cations and 8-quinolinol, a the absorbance per 1.0 μg of aluminium obtained from the calibration curve; x is the amount (μg) of aluminium, and k is any value. When a suitable value is given for k, an approximate value of x can be graphically estimated from the correlation between the x values and the 1/(b+k) values obtained by substituting some arithmetically increasing values into x for the equation. Although by using this calculation approach it is impossible accurately estimate the value of x, a reasonable good approximation can be obtained. By the proposed method, in the presence of interfering foreign cations up to seven components (such as iron, copper and zinc) 161 lug of aluminium in synthetic sample solutions can be selectively determined with recoveries of 99103% and a relative standard deviation of 0.035% without any interference from thier foreign cations. The analytical procedure of this method is both simple and fast.View full abstractDownload PDF (651K) -
Norio KANEKO, Naoyuki SHINOHARA, Hiroyuki NEZU1993 Volume 42 Issue 5 Pages 299-304
Published: May 05, 1993
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA spectrophotometric determination of dicyclohexyl-18-crown-6 (crown ether: CE) in electrodeposited tin was studied using tetrabromophenolphthalein ethyl ester (TBPE), which is an ion association reagent of organic cations. CE reacts with the potassium ion (K+) to form a CE·K+ complex cation, which can be extracted into chloroform as a 1 : 1 ion pair with TBPE at pH 8. The calibration curve was prepared as follows: 110 ml of a standard CE solution (1 × 10-5 M) was taken in 50 ml volumetric flask; 25 ml of a buffer solution (pH 8, concentration of K+: 0.8 M) and 2 ml of a TBPE solution (4 × 10-3 M) were then added. The solution was diluted to 50 ml with water and then transferred into a separatory funnel. Ten milliliters of chloroform was added; the mixture was shaken for 3 min. After phase separation, the absorbance of the organic phase was measured at 607 nm against chloroform. The molar absorptivity was 3.1 × 105l mol-1 cm-1, and the relative standard deviation was 2.4% for five determinations of 2 × 10-6 M CE. A linear relationship between the absorbance and the concentration of CE was obtained over the range of 2 × 10-7 M to 2 × 10-6 M.View full abstractDownload PDF (865K) -
Kenji YAMAZAKI, Haruo TSUJI, Kenji CHAYAMA, Yuzo TAMARI, Yuzuru KUSAKA1993 Volume 42 Issue 5 Pages 305-309
Published: May 05, 1993
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe separation and determination of trace elements in calcite by ICP-AES were examined. Trace elements (Al, Bi, Cd, Co, Cr, Cu, Fe, La, Mn, P, Sn, Sb, Ti, V, Y, Zn and Zr) in calcite were separated from calcium by the following procedure: calcite (0.3 g) was resolved by hydrofluoric, nitric and perchloric acids. The resolved solution was diluted by water (200 ml), and adjusted to pH 1. Carrier indium (30 mg) was then added to the solution. The pH of the solution was adjusted to 9 with diluted aqueous ammonia (300 ml) ; thioacetamide (0.1 g), which makes the sulfide ion, was then added to this solution. Trace elements were then coprecipitated with the indium sulfide. This precipitate was resolved by aqua regia, and the trace elements were analyzed by ICP-AES. The coprecipitation ratio of the trace elements was 89100%. The present method was efficient for the determination of elements (Cd, Co, Cu, Mn and Zn) that form complexes with ammonia. The analytical values of trace elements in calcite agreed with those determined by other methods. However, the determination of cobalt, antimony, titanium and lanthanum was interrupted by a large amount of iron in sediment samples.View full abstractDownload PDF (699K) -
Tomoko YOSHIDA, Shinichiro OKAWA1993 Volume 42 Issue 5 Pages 311-316
Published: May 05, 1993
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAn ion-chromatography method was established for the determination of cadmium us-ing postcolumn derivatization with 10-(2-pyridylazo)-9-phenanthrol (PAP) in a nonionic surfactant solution of Brij 35. The optimum conditions for determining cadmium were: An eluent containing, 0.25 mol dm-3 lactic acid (pH 3.30) with a flow rate of 1 ml/min; for the postcolumn derivatization, a 2×10-4 mol dm-3 PAP solution containing 5% (v/v) dioxane, 4% (w/v) Brij 35, 0.0198% (w/v) sodium borate and 0.0214% (w/v) sodium hy-droxide, at a flow rate of 0.3 ml/min; pH at drain, 10.3±0.1; analytical column, Shimpack IC-C1 (5.0 mm i.d. ×150 mm); oven temperature, 40°C; injection volume, 20 μl; de-tection at 545 nm. A linear relationship was observed between the peak height and the amount of cadmium within a range of 40 to 200 ppb. The relative standard deviation was 1.29% (n=6) for a cadmium concentration of 80 ppb. The detection limit of cad-mium was 14.5 ppb (S/N=3). The present method was successfully applied to the determination of cadmium in the Oyster Tissue (NIST 1556a).View full abstractDownload PDF (685K) -
Tsunetaka BANBA, Hiromichi HAGIYA, Yukito TAMURA, Chushiro YONEZAWA1993 Volume 42 Issue 5 Pages 317-323
Published: May 05, 1993
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAnalytical methods have been developed and evaluated for supporting the characteriza-tion tests of actual high-level radioactive waste glasses. The experiments were carried out by using a simulated waste glass sample and the NIST Standard Reference Materials. Sample solutions for the determination of Si and B were prepared by decomposition of a 0.1 g powdered glass sample by fusion with sodium peroxide, and then the solutions were analyzed by the inductively coupled plasma atomic emission spectroscopy (ICP-AES). Other sample solutions both for the atomic absorption spectrometry (AAS) determination of Li and Na and for the ICP-AES determination of Al, P, Ca, Fe, Zn and Zr were prepared by the decomposition of a 0.1 g powdered glass sample with hydrofluoric acid-per-chloric acid mixture. Four kinds of the NIST Standard Reference Materials were ana-lyzed to evaluate the reliability of the analytical methods. Consequently, it was evident that the repeatability of these methods were less than 6%, and that the analytical values of the NIST Standard Reference Materials were within 7% of their certified values.View full abstractDownload PDF (1013K) -
Satori UTSUMI, Shigeo MTSUNO, Akinori ISOZAKI1993 Volume 42 Issue 5 Pages 325-327
Published: May 05, 1993
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe present paper deals with a simple method for the indirect determination of chloride ion based on the measurement of silver by AAS. A sample solution (10 ml) containing less than 1×10-4 M (3.6 ppm) chloride ion is placed in a glass tube with a stopper. One milliliter of 0.1 M nitric acid and 1 ml of 1×10-3 M silver nitrate are added, and mixed. After standing for 10 min, the AgCl-precipitate is filtered with suction through a 0.45 p.m membrane filter. The absorption of silver ion in the filtrate is measured at 328.1 nm by an atomic absorption spectrometer. If some interfering ions such as iodide, thiosulfate and sulfide exist in the sample solution, the resulting AgCl-precipitate can be used for the determination of chloride. The precipitate on the filter is washed with water, dissolved completely in aqueous ammonia and the absorption of silver is measured at 328.1 nm. The relative standard deviation obtained from the filtrate method for the determination of 2.3 ppm chloride ion in an underground water sample was 1.9% (n = 10).View full abstractDownload PDF (395K) -
Etsuko FUJIMOTO1993 Volume 42 Issue 5 Pages 329-332
Published: May 05, 1993
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSPolarized attenuated total reflection FT-IR spectra of fibers (silk, nylon 6, 6, cotton and polyester) adsorbed by oily substances (oleic acid and triolein) were measured. In these spectra a new band appeared near 1700 cm-1 which is lower 57 cm-1 than the band assigned to the C=O stretching vibration mode of oily substances, for the cases of silk, nylon and cotton. This band may be due to oily substances adsorbed on fibers. As silk and nylon were adsorbed by oily substances, the relative intensity of the amide II band, which is assigned to the deformation vibration mode of NH oriented perpendicularly to the fiber axis, decreased and the line shape of this band became broad toward the high wavenumber. On the other hand, the relative intensity of the amide II band due to NH oriented at random increased and the peak of this band shifted to the lower wavenumber. These facts show that C=O of oily substances adsorbs on NH of silk and nylon. On these spectral evidences, it may be concluded that a mechanism for the adsorption of oily substances on fibers is the chemical adsorption caused by the hydrogen bonding formed between C=O of oily substances and NH or OH of fibers.View full abstractDownload PDF (479K) -
Shunichi UCHIYAMA, Tsuyoshi MIZUNUMA, Yasushi HASEBE, Shuichi SUZUKI1993 Volume 42 Issue 5 Pages 333-335
Published: May 05, 1993
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSControlled potential coulometry with carbon felt electrodes has been applied for the absolute determination of reduced nicotinamide-adenine dinucleotide (NADH) using hexacyanoferrate(III) ion and vitamin K3 mediators. The reduced forms of mediators produced by the NADH addition are completely oxidized to original oxidized forms at the working carbon felt electrode impregnated with electrolyte containing mediator. The oxidation of vitamin K3 by NADH takes place rapidly when diaphorase is contained in an electrolyte. But, the reduced form of vitamin K3 undergoes air oxidation during electrolysis and the current efficiency of NADH obtained by using vitamin K3 mediator was then below 90%, consequently, the absolute determination of NADH could not be carried out by using vitamin K3 mediator. On the other hand, an absolute coulometric determination of NADH were possible when hexacyanoferrate(III) ion mediator is used, because the oxidation rate of NADH by high concentration hexacyanoferrate(III) ion ( <0.1 M) is sufficiently high, even when diaphorase is not used. Moreover, the produced hexacyanoferrate(II) ion by the reduction of hexacyanoferrate(III) ion by NADH is stable to air oxidation and the current efficiency of NADH was found to be attained more than 99%.View full abstractDownload PDF (452K) -
Yukio TOIDA, Kazuo WATANABE1993 Volume 42 Issue 5 Pages T65-T69
Published: May 05, 1993
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA spectrophotometric method has been studied for a simple and accurate determination of trace levels of boron in high purity graphite. An appropriate weight (less than 2 g) of sample was taken in a silica dish mixed with calcium hydroxide prepared from pure calcium, and ashed in a muffle furnace. The residue was dissolved in 10% acetic acid. After the addition of glycerol, the solution was evaporated to dryness. To the residue were added curcumin-acetic acid and sulfuric-acetic acid. The mixture was diluted with ethanol, and the absorbance at 555 nm was measured. The relative standard deviation was 3% for samples with 2 μg-1 levels of boron. The results on CRMs JAERI-G5 and G6 were in good agreement with the certified values.View full abstractDownload PDF (584K) -
Miyuki TAKENAKA, Shoji KOZUKA, Yoshimi HASHIMOTO1993 Volume 42 Issue 5 Pages T71-T75
Published: May 05, 1993
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSSome analytical procedures were studied for the determination of ultratrace concentra-tions of Na, K and Fe in photoresist used ULSI by GFAAS. These procedures were as follows: 1) acid decomposition (HNO3+HClO4); 2) tetramethylammonium hydroxide (TMAH) digestion; 3) dilution by acetone; 4) extraction with HC-4-methyl-2-pentanone (MIBK) for Fe; and 5) extraction with hot water for Na and K. The results of this analysis showed the observed values by these procedures were in good agreement with each other. The detection limits were Na, K: 0.01 ppb, Fe: 0.1 ppb respectively.View full abstractDownload PDF (762K) -
Akira KOBAYASHI, Yoshiharu TAKASHIMA, Isao UMEDA1993 Volume 42 Issue 5 Pages T77-T81
Published: May 05, 1993
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA capillary GC method was developed for the determination of 21 active ingredients, including nine pyrethroidal insecticides, in the commercially available insecticide formulations (aerosol, mosquito coil and mat). These active ingredients were separated on a DB-17 fused silica capillary column (0.53 mm i.d. and 30 m in length), and determined at 100→260°C using benzyl benzoate as an internal standard. When d-tetramethrin and d-phenothrin were admixed in insecticide formulations they could not be separated from each other, but could be separated on a DB-23 fused silica capillary column (0.53 mm i.d. and 15 m in length). The results of this determination agreed with those obtained using packed columns.View full abstractDownload PDF (667K)
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