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Volume 37, Issue 6
Displaying 1-14 of 14 articles from this issue
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Jun'ichi ITO, Masaaki IWATSUKI, Michio MAEDA, Katsunori ENDO, Tsutomu ...1988 Volume 37 Issue 6 Pages 273-278
Published: June 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA study is described on the X-ray diffractometric determination of 0.52 mg silicon carbide (SiC) in a milligram sample formed into a thin layer. The preparation of thin-layer specimens was studied using SiC powders of different particle sizes. Reproducibility of diffraction patterns was examined on the prepared specimens to estimate a critical particle size required for reliable XRD analysis. Relationships of SiC amounts vs. intensity ratios of SiC to internal standard silicon were compared among specimens with different sized SiC and among different lines of SiC and silicon. An appropriate combination of the ratios gave a calibration curve common to determination of SiC through #3000 to #400. Mixed SiC specimens with α-alumina and chromite were also examined.View full abstractDownload PDF (1098K) -
Kuniaki KAWATA, Tatsuo UEMURA, Masashi KANEKO1988 Volume 37 Issue 6 Pages 279-283
Published: June 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple head-space technique for the microde-termination of volatile chlorinated hydrocarbons (VCHs) in soil and sediment was developed. The VCHs investigated were 1, 1-dichloroethylene (1, 1-DCE), trans-1, 2-dichloroethylene (trans-DCE), cis-1, 2-dichloroethylene (cis-DCE), 1, 1-dichloroethane (1, 1-DCA), 1, 2-dichloroethane (1, 2-DCA), 1, 1, 1-trichloroethane (MCF), trichloroethylene (TCE) and tetrachloroethylene (PCE). To 10g of sample in a vial (actual capacity of 70ml) was added 45 ml of 5 M sodium chloride and 5μg of perdeuterated 1, 2-DCA (d4-1, 2-DCA) as an internal standard. The vial was sealed with a Teflon-coated rubber septum and an aluminum crimp seal, followed by ultrasonic irradiation for 20 min and kept at 40°C in a water bath for 30min. Head-space gas of 0.2 ml was measured by GC/MS equipped with a 25m×0.53 mm i.d. fused silica capillary column coated with 3.0μm thickness of methyl silicone. The m/z of the selected ions were 61 and 96 for 1, 1-DCE, trans-DCE and cis-DCE, 63 for l, l-DCA, 62 for 1, 2-DCA, 61 and 97 for MCF, 62 and 130 for TCE, 61 and 166 for PCE and 102 for d4-1, 2-DCA. The recoveries of the VCHs were from 85.9 to 99.9%. The detection limits were 0.2 ng for 1, 1-DCA to 4 ng for PCE as absolute amount in the vial. This method was applied to determine VCHs in soil and river sediment.View full abstractDownload PDF (816K) -
Yuka NISHIKAWA, Kiyotoshi MORISHIGE, Tsunenobu SHIGEMATSU, Yasuharu NI ...1988 Volume 37 Issue 6 Pages 284-291
Published: June 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe acid-base equilibria of four water soluble porphyrins {α, β, γ, δ-tetrakis(4-N-methylpyridil) porphine: TMPyP, α, β, γ, δ-tetrakis(4-N-trimethylaminophenyl) porphine : TTMAPP, α, β, γ, δ-tetraphenylporphine trisulfonic acid : TPPS3, α, β, γ, δ-tetrakis(4-sulfophenyl) porphine : TPPS4} were investigated spectroscopically. They showed remarkable variation in their Q-band spectra (500700 nm) at various pH solutions, and pK values could be determined by an acid-base titration method (Hildebrand plot) at (20±1)°C. The pK values of the methylpyridyl groups or the trimethylamino groups at α, β, γ, δ-positions on the porphyrins were as follows. (TMPyP : pK4=1.17, pK3=2.10, pK2=5.99, pK1=11.27; TTMAPP : pK4=0.97, pK3=3.00, pK2=7.64, pK1=9.45). The pK values of TPPS3 and TPPS4 which have sulfonic groups at the meso-positions are different from that of TMPyP and TTMAPP, and are shifted to the narrow acidic range by effect of the acidic-sulfonic groups. The difference in the number of sulfonic groups gave different pK values between TPPS3 and TPPS4. They were pK4(3.57), pK3(4.88), pK2(5.15) and pK1(8.31) for TPPS3, and pK4(1.16), pK1(5.20) for TPPS4. The fluorescence lifetimes (τf) of five protopic species of the water soluble porphyrins (TMPyP, TTMAPP, TPPS3, TPPS4) showed remarkable variation among them. The lifetime of the species of TMPyP were 6 ns for the di-cationic species (PH42+) and the di-anionic species(P2-). The other three species mono-catonic species (PH3+), neutral species (PH2) and mono-anionic species (PH-) have long fluorescence lifetime which are twice the former. The long fluorescence lifetime (11.113.2 ns, mean : 12 ns) suggests that protoropic resonance in the pyrrol rings was retained.View full abstractDownload PDF (1044K) -
Kazuaki ITO, Hiroshi SUNAHARA1988 Volume 37 Issue 6 Pages 292-295
Published: June 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAn ion chromatographic method for the determination of trace level iodide ion (I-) in concentrated salt solutions which contain an excess of ions such as Cl-, SO42- is described. Ion chromatographic conditions were as follows : Separation column, TSKgel IC-Anion-PW (Toyo Soda; 50 × 4.6 mm i.d.; packing material, polymethacrylate; anion-exchange capacity, 0.03 meq./ml) ; Eluent, 0.1 M NaCl+5 mM sodium phosphate buffer (pH 6.7) ; Flow rate, 1.2 ml/min; Sample volume, 100μl; Detection, amperometry using a glassy carbon electrode as a working electrode (the applied potential +1.0 V vs. Ag/AgCl). Glassy carbon electrodes were pretreated by repeating anodization at +1.6 V (vs. Ag/AgCl) for 5 min followed by cathodization at -1.0 V for 2 min in a flow system (0.5 ml/min) of 0.3 M sodium phosphate buffer (pH 6.7). The iodide peak was sufficiently separated from those of electroactive inorganic anions (S2O32-, NO2-, Br-, SCN-) and anions (Cl-, SO42- etc.) in artifitial seawater (salinity 35‰). The detection limit of I- in artifitial seawater was 5 μg/l (S/N=2). Relative standard deviation was 3.0% (n= 5, I-=0.1 mg/l). The iodide peak in artificial seawater was a little broad compared to that in deionized water but the retention time was almost equal. The concentrations of I- in two seawater samples (Seto Inland Sea) were 20 and 32μg/l.View full abstractDownload PDF (672K) -
Yasuhiro HOSOI, Shoji MOTOMIZU1988 Volume 37 Issue 6 Pages 296-300
Published: June 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSColor change of tetrabromophenolphthalein ethyl ester (TBPE·H) in several alcohols and their mixtures with chloroform was studied. TBPE·H shows maximum absorption at 430 nm in chloroform, while it shows the maximum absorption near 600 nm in mixed solvents of chloroform and alcohols. The absorption near 600 nm was considered to be due to ion-pair formation. The formation of the ion pair and its dissociation reaction are considered as follows.
TBPE·H+(m+n)SKi_??_TBPE(mS)-·H(nS)+
TBPE(mS)-·H(nS)+Kd_??_TBPE(mS)-+H(nS)+
where S is an alcohol. Ion-pair formation constants (Ki) and dissociation constsnts (Kd) were obtained using methanol, ethanol, propanol and butanol as solvation molecules by spectrophotometry and conductometry. The solvation numbers obtained were 3.3 to 4.7, and the values of log Ki were -4.6 to -2.4. The values of log.Kd obtained in pure alcohols were -7 to -6, which indicates that little dissociation occurs.View full abstractDownload PDF (649K) -
Yasuhiro HOSOI, Shoji MOTOMIZU1988 Volume 37 Issue 6 Pages 301-305
Published: June 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn a weak acidic solution an acidic triphenylmethane dye, tetrabromophenolphtalein ethyl ester, exists in the protonated form, TBPE·H, which precipitated as a yellow solid. TBPE·H, however, dissolves in an acidic solution in the presence of a non-ionic surfactant, such as Triton X-100, and the TBPE·H solution turns blue (λmax=590 nm) on adding alcohols, such as methanol, ethanol, propanol and butanol. This color change was used to determine the ethanol content in alcoholic liquors. The calibration curve was not a straight line. The determinable range was from 2 to 10%(v/v) (final concentration). Alcoholic liquors (sake, whisky, shochu) were used for the determination after pretreatment with activated, carbon. This color change reaction was applied to FIA; it made it possible to analyse 45 samples per hour without pretreatment with activated carbon.View full abstractDownload PDF (683K) -
Tsutomu ISHIBA, Yukio TAKANO, Takeshi TAJIMA, Isamu ORITA1988 Volume 37 Issue 6 Pages 306-311
Published: June 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA. new technique for precise lattice parameter measurement using two-beam double crystal method of X-ray diffraction was developed for characterization of single crystals. The accuracy of the measurement was Δd/d=1×10-7 in the case of dislocation-free Si crytals, and was 1×10-6 in the case of GaAs crystals with dislocation of (34)×104 cm-2. Precise lattice parameter was measured to characterize the undoped LEC-GaAs wafers. The lattice strain was found both intra and inter wafers with an order of 10-510-4 Å.View full abstractDownload PDF (1015K) -
Hiromiti SAWAMOTO1988 Volume 37 Issue 6 Pages 312-315
Published: June 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSNickel in river waters was determined by adsorptive stripping voltammetry employing adsorption of Ni-2, 2'-bipyridine complex on the hanging mercury drop electrode (Metrohm E410 and EA290). The sensitivity of the previous method was improved. The most suitable supporting electrolyte was 0.05 M KCl with 0.01 M KOH. The concentration of 2, 2'-bipyridine was 0.1 mM. A preconcentration potential of -0.75 V vs. SCE was applied for 5 min. In the stripping process a differential pulse polarograph (Princeton Applied Research Model 174A) was used. The calibration curve was linear up to 0.1 μM, and the detection limit was 5 nM. The ralative standard deviation was 5.5% (50 nM Ni2+). Most metal ions did not interfere with the determination of nickel. The results of the determination of nickel in river waters were 32.8 nM (Kagami River) and 79.3 nM (Obushi River).View full abstractDownload PDF (602K) -
Sadanobu INOUE, Tadashi TAKAHASHI, Suwaru HOSHI, Mutsuya MATSUBARA1988 Volume 37 Issue 6 Pages 316-321
Published: June 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSN-p-Octyloxybenzoyl-N-phenylhydroxylamine (OB-PHA) reacts with Ti (IV) in above 9 mol dm-3 hydrochloric acid and forms a complex which is completely extractable into chloroform. The chloroform extract of Ti(IV) is shaken with 0.5 mol dm-3 hydrochloric acid medium in the presence of phenylfluorone and isoamyl alcohol. The product is an intensely colored ternary complex and has an absorption maximum at 530 nm with a molar absorptivity of 2.12 × 105dm3mol-1cm-1 The system obeys Beer's law up to 1.43 μg (organic phase) of Ti(IV). Considerable amounts (10 mg) of many cations and anions can be tolerated. However, the tolerance limit for both Nb(V) and Zr (IV) is 1.4-fold excess even by reduction with L-ascorbic acid. The recommended procedure for the determination of Ti(IV) in environmental materials is as follows : treat the sample with a mixture of hydrofluoric acid and nitric acid at 150 °C and evaportate to dryness. Then digest the sample with mixture of nitric acid and perchloric acid at 200°C and evaporate to dryness.Dissolve the residue in 10 mol dm-3 hydrochloric acid and dilute with water in volumentric flask. Take an aliquot of digested solution to a separately funnel and add hydrochloric acid to give 10 mol dm-3. Then dilute to fixed volume with water. Extract Ti (IV) with 10 cm3 of 0.1% OBPHA in chloroform by shaking for 3 min. Transfer the 5 cm3 of organic phase in another separately funnel. Add 2cm3 of 0.06% phenylfluorone, which was prepared by mixing 4 cm3 of N, N-dimethylformamide, 0.4 cm3 of hydrochloric acid and 40 cm3 of isoamyl alcohol, followed by addition of 5 cm3 of 0.5 mol dm-3 hydrochloric acid, and shake for 3min. Measure the absorbance of the organic phase at 530 nm against a reagent blank.View full abstractDownload PDF (1001K) -
Yosinori UJI, Yoshi SAKAI, Masataka SHIRAKI, Akio NOMA, Masako MAEDA, ...1988 Volume 37 Issue 6 Pages 322-324
Published: June 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSWe have developed a method for chemiluminescent determination of serum non-esterified fatty acids (NEFA) using acyl-CoA synthetase, acyl-CoA oxidase, iso-luminol and micro peroxidase. Since the determination of serum NEFA by the chemiluminescence method was interfered with serum bilirubin, the bilirubin oxidase was used to eliminate the effect of endogeneous bilirubin in the proposed method. The within-run precision of the proposed method gave an excellent relative standard deviation (3.1%) in the lower medical decision level of serum NEFA. Results by the proposed method (Y) correlated well with those by the conventional high sensitive enzymatic method acyl-CoA synthetase-myokinase-pyruva te kinase-lactate dehydrogenase method (X). The linear regression curve was Y=1.11X-25.4 and the correlation coefficient (r) was 0.99.View full abstractDownload PDF (442K) -
Keiji GAMOH, Eiji OKADA1988 Volume 37 Issue 6 Pages 324-327
Published: June 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA facile and rapid method for the determination of monensin in feeds by HPLC was reported. Solid phase extraction of monensin in a feed, followed by derivatization with 9-anthryldiazomethane (ADAM) was carried out. The monensin-ADAM derivative was determined with a fluorescence detector. Monensin in a feed was extracted from a mixture of methanol and acetone (9 : 1) and then the extract was filtered under reduced pressure. After the extract was evaporated to dryness, the residue was dissolved by methanol and then the solution was centrifuged for 5 min. The resulting supernatant was applied to a ODS cartridge column (Bond Elut C18), followed by washing with 20% aqueous methanol sloution and then eluting with 90% aqueous methanol to obtain the monensin fraction. Monensin in the eluent was converted into the corresponding ADAM-monensin derivative by reaction with the ADAM reagent in the presence of crown ether for 2 h at room temperature. The reaction mixture was injected to the analytical column. The conditions of HPLC was as followed; column, Shim-pack CLC-ODS (6.0 mm i.d. × 150 mm L), mobile phase, 10 mM magnesium acetate in 95% aqueous methanol: flow rate, 1.4 ml/min: column temp., 45°C detector, RF-535 (Ex 365 nm, Em 412 nm). The calibration curve was linear from 0.1 μg/ml to 1.5 μg/ml. Recoveries of monensin added to the feed at the level of 10 μg/ml were 82.8+2.1% (n=5).View full abstractDownload PDF (759K) -
Takushi ITO, Hiroki OMURA, Tetsuo SUZUKI, Akira MURATA1988 Volume 37 Issue 6 Pages 327-330
Published: June 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe 4, 5-dihydroxycoumarin with acid dissociation constants of Ka1 =2.72 × 10-3 and Ka2=2.88 × 10-14 is able to form complexes with 22 metal ions. Among these metal ions, 12 could form fluorescent complexes.The analytical procedure for the spectrofluorometric determination of Be was as follows : To a solution containing 0.11.3 μg of Be, 2.5 ml of 2×10-4M 4, 5-dihydroxycoumarin in methanol, 10 ml of methanol, and a sufficient amount of 0.5 M ammonia solution to adjust the pH of 910 were added, and this mixture was diluted to a final volume of 25 ml with water.After standing for 1 h, the fluorescence intensity was measured at 428 nm with excitation at 334 nm. The calibration curve was linear in the range of 0.11.3μg Be, and the relative standard deviation obtained from seven measurements of 0.9μg Be was 0.73%. Cr(III), Ti(IV), Mn(II) and La(III) gave serious negative errors. The molar ratio of Be to the reagent was 1:1 at pH 6.0 and 1:2 at pH 8.511.5.View full abstractDownload PDF (525K) -
Shukuro IGARASHI, Kimiyoshi UCHIYAMA, Takao YOTSUYANAGI1988 Volume 37 Issue 6 Pages 331-332
Published: June 05, 1988
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSSilver complex of α, β, γ, δ-tetrakis(4-sulfophenyl) porphine (Ag2-TPPS) was quantitatively formed within 1 min at room temperature in the pH range of 11.0 to 12.5. The complex easily relases the porphyrin in the presence of "soft base" anions such as S2-, CN-, I-, glutathione and L-cysteine within 5 min at room temperature in the above pH range. Based on this reaction, spectrophotometric determination of 10-7 mol dm-3 levels of sulfide ion was developed. The Soret band of TPPS and the Ag2-TPPS complex at pH 12.0 and I=0.5 were located at wavelength of 414 nm (ε=41.4 × 104) and at 443 nm (ε=7.9 × 104), respectively. A recommended procedure : 1.0 cm3 of 10-4 mol dm-3 TPPS solution, 10cm3 of 2.5 mol dm-3 sodium nitrate solution, 2.0 cm3 of 10-4 mol dm-3 Ag(I) solution, and 5 cm3 of 1 mol dm-3 sodium hydroxide solution are taken into a 50 cm3 of amber-volumetric flask. After standing for 5 min, 30 cm3 of sample solution containing less than 2.0μg of sulfide is added and is diluted to 50 cm3 with water. After 10 min, the absorbance at 414 nm against water is measured. The calibration curve was found to be linear in the range of 02.0 × 10-6 mol dm-3. The relative standard deviation was 3.75% for [S2-]T= 5 × 10-7 mol dm-3 (8 determinations). The detection limits was 7 x 10-8 mol dm-3 (S/N=3). The tolerance limits of diverse ions for determination of [S2-]T = 5 × 10-7 mol dm-3 were 5 × 10-4 mol dm-3 for NO3-, CI-, SO42-, K+ and Na+, and 5 × 10-5 mol dm-3 for Ba2+, Ca2+ and Fe3+. However, 5 × 10-7 mol dm-3 of I-, CN-, Cd2+, glutathione and L-cysteine were interfered. As Ag2-TPPS complex reacts rapidly with various kinds of soft bases, it is expected as a highly sensitive and selective chromogenic reagent of postcolumn detection system in the LC for these ions.View full abstractDownload PDF (289K) -
Seiji YASUDA, Kazuyoshi KAWAZU1988 Volume 37 Issue 6 Pages T67-T71
Published: June 05, 1988
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe adsorption behaviors of Ge(IV) from water samples on a commercially available boron-specific resin with 1-deoxy-1-(methylamino)sorbitol groups, Diaion CRB02, were investigated by means of batch and column methods. Germanium(IV) was quantitatively adsorbed on the resin from the solutions of pH 612. The shaking time of about 8 h was required to achieve adsorption equilibrium at 25°C. The oxoanions of As(III), As(V), Sn(IV), Sb(V), Te(IV), Te(VI), V(V), Cr(VI), Mo(VI) and W(VI) were found to be adsorbed on the resin by chelate formation or anoin exchange reactions. The batch tests showed that these oxoanions did not interfere with the adsorption of Ge(IV). In the presence of a large amount of B(III), Ge(IV) showed a considerably low recovery by competing adsorption of both elements on the resin. The column experiments were carried out using a column (5 mmφ × 105 mmH) packed with 2 cm3 of the resin. The sample solutions at pH above 7 were passed through the column at a flow rate of 1.3 cm3 min-1. The elution of Ge(IV) adsorbed on the column was accomplished by passing 20 cm3 of 1 M hydrochloric acid at the same flow rate. This column method could be applied for the preconcentration of trace Ge(IV) from a large volume of natural water samples. A sufficient recovery of Ge(IV) was obtained from the distilled water and surface water of dam to which trace Ge(IV) was spiked.View full abstractDownload PDF (843K)
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