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Volume 32, Issue 11
Displaying 1-26 of 26 articles from this issue
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Makoto NAGASE, Hiroyuki KONDO, Akira MORI1983 Volume 32 Issue 11 Pages 633-636
Published: November 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSA new determination method of ethyleneoxide (EO) in air was studied and the following procedure was established. An air contained EO was sampled with a 1l sampling bottle vacuumized. Hydrochloric acid contained 55 μmol hydrogen chloride was injected in the sampling bottle and vaporized. After the sampling bottle was kept at room temperature for 30 min, the unreacted hydrogen chloride was neutralized with ammonia. Ethylenechlorohydrine (ECH) produced from EO was purged with nitrogen at 200 ml/min for 25 min and adsorbed on 0.5 g Tenax GC (6080) mesh in an adsorption tube, which was a 22 cm×5 mm i. d. glass tube. The adsorption tube was installed in a gas chromatograph (FID), and the temperature of adsorption tube was elevated from room temperature to 190 °C in 80 s. Desorbed ECH was transferred to the gas chromatograph and determined. In this method, the average recovery of EO was 93. 1 % and the coefficient of variation, 2.5 %, and the limit of determination was 56 ng. EO in air is determined simply and precisely by this method.View full abstractDownload PDF (712K) -
Jun SAITO, Norio TERAMAE, Shozo TODA, Shigeyuki TANAKA1983 Volume 32 Issue 11 Pages 637-643
Published: November 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSField desorption mass spectrometry (FD-MS) was applied to the analysis of thermal behavior of blocked isocyanates (BIC). The isocyanates were synthesized by the reaction between urethane prepolymer and blocking agents. One of them, BIC-1 was prepared with methanol as a blocking agent, and another, BIC-2, with ε-caprolactam as a blocking agent. The field desorption mass spectra of these compounds were measured and examined in detail. As a result, the following conclusions were obtained. (1) Dissociation of blocking agents comprised in the BIC-1 or BIC-2 proceeds with an increase in temperature, and thermal degradation of the BIC-2 occurs at a lower temperature compared with that of the BIC-1. (2) In the case of the BIC-1, the temperature range of dissociation depends on the kinds of series of molecular species. For example, comparing the series of BG (1, 3-butanediol) with those of TM (trimethylolpropane), dissociation occurs at a lower temperature in the BG than the TM. On the other hand, in the case of the BIC-2, the dissociation temperatures for both the BG and TM series do not differ significantly and are in a relatively narrow temperature range. (3) As for the dissociation of 2, 4-tolylene diisocyanates, it occurs together with the dissociation of blocking agents in the case of the BIC-1, but it occurs after the dissociation of blocking agents in the case of the BIC-2. Thus, the details of thermal degradation of blocked isocyanates can be clarified from field desorption mass spectra and mass chromatograms. The FD-MS is useful for the analysis of thermal behavior of these compounds.View full abstractDownload PDF (1165K) -
Tatsumori TAKEDA, Shigeru YOSHIDA, Kayoko ODA, Shingo HIROSE1983 Volume 32 Issue 11 Pages 643-648
Published: November 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSNitrogen laser-excited fluorescence detector (Nisshin Electric Co., Ltd.) is applied to the monitoring of flow injection analysis. The conventional laser-induced technique showed large fluorescence background even with purified water. The major contributions to the blank emission are luminescence from instrumental components, scattered light and Raman scattering from water. But these scattered light are instantaneous and present only while the excitation source irradiates the sample. The combination of pulsed nitrogen laser excitation (peak power: 10kW) and time resolution in boxcar integrator led to a instrumentation capable of effectively eliminating these contribution to the blank. In relatively pure samples, few problems with this detection system were noted, however, significant interferences were observed in human sera. Fluorescence background of serum, which was mainly caused by protein, could be decreased to 20% of total background by incorporating DEAE-Sepharose column (2 mm×10 mm) into the flow injection system and by eluting with glycine buffer (pH 9.0) contained. 30 mM sodium chloride. Furthermore (110)μl injection of sample which was diluted serum to about seventeen fold with enzymatic agents and buffer solution decreased the residual fluorescence background of serum to negligibly small. In this system, makes it possible to determine NADH which was produced with enzyme reaction in serum. Using this system, concentration of lactic acid and activity acid and activity of lactic dehydrogenase in serum were determined. The reproducibility of the assay using same serum was 13.3 mg/dl, standard deviation: 0.65 mg/ dl and coefficient of variation: 4.9 % (n=6) for lactic acid and 220 U/L, standard deviation: 12.1 U/L, and coefficient of variation: 5.5 % (n=6) for lactic dehydrogenase, respectively.View full abstractDownload PDF (1278K) -
Shoji MOTOMIZU, Shoichi HAMADA, Kyoji TÔEI1983 Volume 32 Issue 11 Pages 648-653
Published: November 05, 1983
Released on J-STAGE: January 19, 2010
JOURNAL FREE ACCESSThe ion association extraction of quaternary ammonium ions with univalent anions was carried out. The extraction constants (log Kex) for these ion-as-sociates between aqueous and chloroform phases were determined. The linear relationship was obtained between log Kex and the number of carbon atoms in quaternary ammonium ion, and the contribution of a methylene group to the extraction constant, πCH2, was on the average 0.59. The order of the extractability of inorganic anions was F-<OH-<NO2-<Cl-<NO3-<Br-<BF4-<I-<SCN-<ClO4-, and the linear relationship was seen between log Kex and the crystal ionic radius of inorganic anion. If the total carbon number is assumed to be equal, the order of the extractability of cations is R-N(CH3)3+>R'4N+>(C6H5)4P+≈(C6H5)4-As+, and the differences in log Kex between the respective cations in this order averaged 1.2 and 1.1 in turn. The π values for C6H5- and C10H7- groups were 2.90 and 4.43, respectively. By using these empirical parameters, the extraction constants for several ion associates were estimated, and the extraction constants calculated were in good agreement with those obtained experimentally in this work and those reported by other workers.View full abstractDownload PDF (1087K) -
Etsu YAMADA, Masanori SATO1983 Volume 32 Issue 11 Pages 654-658
Published: November 05, 1983
Released on J-STAGE: January 19, 2010
JOURNAL FREE ACCESSThe suitable determination procedure for the routine analysis of Mn, Fe, Ni, Cu, Zn, Pb, and Cr contained in waste water of the university campus was investigated. The essential procedure consists of the condensation of trace elements as diethyldithiocarbamate (DDTC) complexes on a Millipore filter and direct multielement determination by energy dispersive X-ray fluorescence analysis. As for the condensation procedure of the elements, the following process was recommended. For the determination of total metals, waste water samples were digested with nitric acid. Then, 10 ml of 1 % DDTC was added to the solution after neutralization by ammonia or acetic acid. After standing the solution for one hour, the precipitate of DDTC-complexes was collected on a 0.45 μm Millipore filter and dried prior to the X-ray fluorescence determination. To determine Cr, the reduction of Cr (VI) to Cr (III) by using ethanol in hydrochloric acid solution was necessary before the addition of ferric ion as a carrier. Then 1 % DDTC was added to the solution after adjustment of pH to 8.5. For the determination of soluble Fe and Mn, the filtrate of sample solution was acidified with (1+1) nitric acid. Then, nickel ion as a carrier, methanol solution of 0.1 % 1- (2-pyridylazo)-2-naphthol (PAN) and ammonia buffer (pH =10) were successively added to the solution. The formed precipitate of PAN-complexes was collected by a Millipore filter and dried prior to X-ray fluorescence determination. The detection limits for Cu, Fe, Mn, Ni, Pb, and Zn are 1 ppb, 2 ppb, 6 ppb, 4 ppb, 7 ppb, and 2 ppb, respectively. The comparison of the results by X-ray fluorescence analysis with those by atomic absorption (AA) analysis for Mn, Fe, Zn, and Cu showed that the present X-ray fluorescence analysis had the sufficient correlation coefficients and comparable detection limits with AA analysis.View full abstractDownload PDF (982K) -
Takeshi KATO, Kiyoshi KANO, Hiroaki SASAKI1983 Volume 32 Issue 11 Pages 659-664
Published: November 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSUse of 2, 2'-dipyridylketone aminoethylimine (DPAI), which is prepared by refluxing an equimolar mixture of 2, 2'-dipyridylketone and ethylenediamine, in the presense of sodium L-ascorbate is proposed for a spectrophotometric determination of iron (II). DPAI reacts with iron (II) to form a water soluble complex, which has an absorption maximum at 608 nm. The calibration curve obeys Beer's law over the concentration range from 0.1 μg/ml to 5μg/ml of iron (II) at 608 nm in a range of pH 7.010.1. The apparent molar absorption coefficient of the complex is 1.71 × 104 dm3 mol-1 cm -1. The combining ratio of iron and DPAI in the complex was confirmed to be 1:2 by both the continuous variation method and elementary analysis on the isolated DPAI-iron (II) complex. Following procedure are recommended for the determination of iron (II); To a sample solution, 1 ml of 10% sodium L-ascorbate, 2 ml of 25 % ethylenediamine, 10 ml of 10-3 M DPAI are added, and pH is adjusted to 7.010.1 with acetate or ammonia buffer solution. Being boiled gently for one minute, and them cooled down to room temperature, the solution is made up to 50 ml with water. The absorbance is measured at 608 nm against reagent blank.View full abstractDownload PDF (1016K) -
Toshihiko KADOYA, Tsuneo OKUYAMA1983 Volume 32 Issue 11 Pages 664-669
Published: November 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSFor the purification of cytoskeletal proteins such as glial fibrillary acidic protein (GFA) or neurofilament proteins (NFP), the chromatography of proteins in the presence of urea should be one of the most important step, since those proteins were extracted with 2 M urea from brain tissue. Ion exchange chromatography was performed using a 6.0 × 0.75 cm I.D. column packed with DEAE-Sephadex A-50 equilibrated in 10 mM potassium phosphate buffer (pH 7.1) with or without urea, and linear sodium chloride gradient for elution of proteins. Human IgG, bovine serum albumin (BSA), and human serum proteins were used as protein samples. In the presence of urea, interaction between ion exchange resin and BSA was reduced. One M urea was equivalent to 0.02 M sodium chloride ion strength. In the case of the presence of 6 M urea, urea had effects on elution patterns of proteins. However, 2 M urea scarcely produced an effect on ion exchange chromatography of human serum proteins. Then, bovine brain 2 M urea extract, which was rich in GEA and NFP was applied to DEAE-Sephadex A-50 column chromatography in the presence of 2 M urea. This system was very useful for the purification of these proteins.View full abstractDownload PDF (1062K) -
Tsutomu FUKASAWA, Susumu KAWAKUBO, Manabu MOCHIZUKI1983 Volume 32 Issue 11 Pages 669-673
Published: November 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSIn a 20-cm3 test tube with stopper, 2.2×10-5 mol dm-3 Malachite Green (MG) was oxidized with 4.3×10-4 mol dm-3 potassium periodate under the conditions of pH 3.8 (acetate-acetic acid buffer solution) at 31°C. The absorbance change of less than 0.2 at 615 nm was measured using a thermostatted 10-mm cell against a reference absorption plate of which the absorbance was about 1.8 against water. The manganese-catalyzed reaction showed a induction period inversely proportional to amounts of manganese (II), and was approximated by zeroth order reaction after induction period. From the induction period read off, manganese (II) of 5 ng to 200 ng can be determined. The time required for each determination was ca. 30 min. Interference of coexisting elements was less than that observed in the previous study, where the rateconstant method on the pseudo-first order reaction in a more diluted MG medium was reported. Iron (III) was allowed to coexist up to 104 times than the amount of manganese (II).View full abstractDownload PDF (841K) -
Hiroshi UCHIKAWA, Rikihisa FURUTA, Yasuo MIHARA1983 Volume 32 Issue 11 Pages 673-677
Published: November 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSBy ICP-AES, cadmium in ceramic materials and ceramic products were rapidly determined with high accuracy and high sensitivity. The instrument adopted was JY 38PII having a monochrometer whose reciprocal linear dispersion is 0.26 nm/mm. The spectral line of Cd I 228.802 nm was selected for analysis, considering optimised signal to background ratio and spectral interferences by iron. The elimination of spectral interference by fine structure of NO molecular band spectra was examined by blowing inert gases against plasma. The order of this effect was Ar>He>N2. By using Ar as a blowing gas and adjusting the vertical width of entrance slit, this kind of interference was completely eliminated. This method gave the background equivalent concentration of 0.028 μg Cd/ml with little chemical and spectral interference by coexisting elements. Detection limit (2σ) was 0.0006μg Cd/ml. Determined values of standard samples dissolved by HF-HClO4 and followed by this methods corresponded to those obtained by metal (W) furnace AAS. The contents of cadmium were (0.13 1.69) μg Cd/g. Coefficients of variation were (1.926)%.View full abstractDownload PDF (869K) -
Ferron-cationic surfactants systemKatsumi GOTO, Shigeru TAGUCHI, Kanji MIYABE, Keni-chi HARUYAMA1983 Volume 32 Issue 11 Pages 678-682
Published: November 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSIt is found that the extraction constant Kex for the ion-pair extraction systems is made up of three independent constants (individual extraction constants), Kc, Ka, and Ks in accordance with the equation:
logKex=logKc+logKa+logKs……(1)
where the subscripts c, a, and s denote cation, anion, and solvent, respectively. The anion, cations, and solvents studied were 7-iodo-8-quinolinol-5-sulfonic acid (ferron), eight cationic surfactants and 1, 2-dichloroethane, dichloromethane, and chloroform. Cationic surfactants used in this work are alkyltrimethylammonium salts with alkyl chain lengths from 10 to 18 methylene groups, and several quaternary ammonium salts. Logarithm K values for several cations, anion, and solvents were calculated from experimental values of log Kex by tentatively assigning the logK values 1.0 and 1.0 to ferron and chloroform, respectively, as reference value. It was also shown that the association constant, KA and the distribution constant, KD are made up of independent constants KA, c, KA, a, (individual association constants) and KD, c, KD, a, Ks (individual distribution constants), respectively, in accordance with the equations:
logKA=logKA, c+logKA, a……(2)
logKD=logKD, c+logKD, a+logKs……(3)
where subscript c, a, and s have the same meaning as in equation (1). Experimental data, are presented to show the validity of the above three equations.View full abstractDownload PDF (963K) -
Rumiko HAYASHI, Norihisa KAWAMURA, Kiyoko HAYAKAWA, Masao ITO1983 Volume 32 Issue 11 Pages 683-687
Published: November 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSVarious conditions in the determination of trace amount of tin by benzene extraction-anodic stripping voltammetry (ASV) were examined. 0.2 μg tin (IV) was extracted as iodide from 5.5 M sulfuric acid solution with benzene. The benzene extract was back-extracted with 1.0 ml of 0.5 % hydrochloric acid. The benzene phase was removed completely by heating at 100 °C in aluminium block bath. Into the aqueous phase, 5 drops of 10 % hydroxylamine hydrochloride were added, and tin (II) was measured by ASV. The recovery and C. V. for 0.2 μg tin by this technique were 99.4 % and 0.7% (n = 6), respectively, the detection limit for tin by ASV was 0.02 μg/ (10 ml 4 M HCl). No influence of following 19 ions on the benzene extraction as tin iodide (as 0.2 μg tin) was found--Ca (II) (2.0 mg); Na (I), Mg (II), Al (III), V (V), Cr (VI), Mn (IV), Co (II), Ni (II), Zn (II), Se (IV), Cd (II), Hg (II), and PO43-(1.0 mg); Cu (II) (750μg); Ge (IV), As (V), Sb (V), and Pb (II) (100 μg). Fe (III) tends to decrease the extraction efficiency of tin. But, the influence could by removed by the addition of 0.5 ml of 20% L-ascorbic acid solution. On the determination of tin in hair, urine, and blood samples, this technique was applied to the samples digested by nitric acid, perchloric acid, and sulfuric acid. The C. V. for tin in these biological materials by this method were (0.49.8)%, and the recoveries for added tin in them were (91.698.3)%. This method was applied to the tin content in human hairs, and the mean concentration of tin were (0.40±0.24)μg/g(male, n=15), (0.87±0.46)μg/g(female, n=14).View full abstractDownload PDF (1001K) -
Keiichi FUKUSHI, Kazuo HIIRO1983 Volume 32 Issue 11 Pages 688-692
Published: November 05, 1983
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSA graphite furnace atomic absorption spectrometric method after electrolytic preconcentration of lead on a platinum net cylindric electrode and dissolution into dilute nitric acid was proposed for the determination of trace amount of lead in sea water. Effects of electrolysis potential, electrolysis time, concentration of nitric acid, dissolution time, composition and pH of electrolyte solution on the recovery of lead were examined. The optimum conditions were established as follows; for 1.01 of sample solution, electrolysis potential was 2.0 V, electrolysis time was 2 h, concentration of nitric acid was 0.16 M, dissolution time was 5 min, pH of the sample solution was about 4. Under these conditions, linear calibration curve was obtained for artificial sea water samples containing up to 5.0 μg of lead. The proposed method was applied to the determination of trace amount of lead in the coastal sea water samples in Osaka Bay sampled in February, 1983. Good agreement was observed between the results obtained by the proposed method and the graphite furnace atomic absorption spectrometric method after extraction with DDTC into MIBK.View full abstractDownload PDF (915K) -
Tokishi HAYASHI, Ayumi ODASHIMA, Hironori TSUCHIYA, Hiroshi NARUSE1983 Volume 32 Issue 11 Pages 692-697
Published: November 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSAn automated amino acid analyzer based on reversed-phase ion pair chromatography was constructed. The separation was carried out with a stainless-steel column (250 mm×4 mm I. D.) packed with LiChrosorb RP-8 (5 μm). Sodium lauryl sulfate was used as counter ion. For the monitoring of amino acids eluted from the column, a fluorescence detection method using ο-phthalaldehyde and 2-mercaptoethanol was used in this system. This analyzer was applied to the analysis of amino acids in human plasma and dried blood on filter paper. Twenty five microliters of plasma were mixed with 500 μl of 70% ethanol containing γ-aminobutyric acid (0.25 μg) as an internal standard and centrifuged. The supernatant was evaporated to dryness. The residue was redissolved with 150 μl of mobile phase 1 (0.05 M sodium lauryl sulfate adjusted to pH 3.0 with monochloroacetic acid). The resulting solution was transferred into the sample cup for the autosampler. Fifty microliters of the solution were injected to the column. In the case of the dried blood on filterpaper, 5 disks (3 mm-diameter) of the sample were placed into a small test tube. Five hundred microliters of 70 % ethanol containing γ-aminobutyric acid (0.25 μg) were added to the tube. The tube was kept in an ultrasonic cleaner for 10 min and then kept at 4 °C overnight. The mixture was centrifuged and the supernatant was evaporated. The residue was treated in a similar manner to that in the case of a plasma sample. This amino acid analyzer showed good reproducibliities in both retention time and peak intensity. Furthermore, the investigation to shorten the separation time was also carried out and the separation in only 35 min was achieved.View full abstractDownload PDF (1193K) -
Fluorometric determination of gallium with 2, 2'-dihydroxy-4, 4'-dimethylazobenzene in mixed solventKunihiro WATANABE1983 Volume 32 Issue 11 Pages 698-701
Published: November 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSFluorometric determination of gallium with 2, 2'-dihydroxy-4, 4'-dimethylazobenzene (4, 4'-DDAB) has been investigated. Gallium reacts quantitatively with 4, 4' -DDAB in the presence of ethylenediamine (en) to form a ternary complex. The optimum pH range for the formation of the ternary complex, which has a red fluorescence with an emission maximum at 588 nm, was 10.711.8. The composition of the ternary complex was Ga: 4, 4'-DDAB: en=1: 1: 1. As dioxane content in the solvent mixture of dioxane, ethanol, and water increased, the fluorescence intensity of the complex increased remarkably. The recommended procedure is as follows: Take (19) ml of a sample solution containing less than 10μg of gallium, and add 5 ml of a buffer solution (ethanol: en: HCl= 4: 1: 0.025), 35 ml of dioxane, and 1 ml of a 0.006 04 4, 4'-DDAB solution. Dilute the mixture to 50 ml with water. Measure the relative fluorescence intensity of the mixture at 588 nm with excitation wavelength of 505 nm. Using 0.01 pg/ml or 0.1 μg/ml rhodamine B solution as a setting reagent, (0.0410)μg of gallium was determined.View full abstractDownload PDF (790K) -
Hiroshi KOBATAKE, Akira OKAHIRA, Sei-ichi NIWA1983 Volume 32 Issue 11 Pages 701-703
Published: November 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA simple and accurate method for the identification of D-mannosamine in complex polysaccharides is described. The method is based on acid hydrolysis of complex polysaccharides, methyl glycosidation of the products with a cation exchange resin as catalyst, followed by acetylation, and isothermal gas-liquid chromatographic analysis of the derivatives. As the gas-liquid chromatographic column packing material, the low polar SE-30 was adequate for fractional detection of hexosamines from other contaminated components but was not so good for separation of each glycoside. On the other hand, the high polar Tabsorb® and Silar-10C were rather good for separation of each glycoside one another. The method could be powerful means for the identification of mannosamine in complex polysaccharides, especially in trace amount of polysaccharide from microorganisms.View full abstractDownload PDF (552K) -
Shoji MOTOMIZU, Shoichi HAMADA, Kyoji TÔEI1983 Volume 32 Issue 11 Pages 703-706
Published: November 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe ion association extraction of Zephiramine ion with univalent organic anions such as benzoate and benzenesulfonate was carried out. The extraction constants (log Kex) for these ion associates between aqueous and chloroform phases were determined. The contribution values of substituents (-X) on the aromatic ring of anions to log Kex, πx, were as follows:πNO2(m, p)=1.05;πCl(m, p)=1.04;πCH3=0.58;πNH2(m)=-1.58; πNH2(p)=-1.81;πOH(m)=-1.18;πOH(p)=-0.54; πOCH3(p)=0.11; πN(CH3)2(p)=0.13. The values of log Kex for sulfonate ions were 1.30 larger than those for carboxylate ions. The values of log Kex for benzoate and benzenesulfonate ions with-NH2 and -OH groups at o-position were 1.52.2 larger than the values for those with -NH2 and -OH groups at p-position. By using these empirical parameters, the extraction constants for several ion associates were estimated.View full abstractDownload PDF (659K) -
Akira NEMORI, Hideyuki SASAKI, Takatoshi KONO1983 Volume 32 Issue 11 Pages 706-708
Published: November 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSIt is well known that thioglycolic acid is used for the determination of iron, but that is now little used. The effect of coexisting elements on color development were investigated using about 30 elements in detail. It is found that many coexisting elements do not interfere and that the maximum absorption is 530 nm, the molar absorption coefficients is 3.9 × 103 mol -1 cm -1 l, the analytical sensitivity is 0.014 μg/ml and the stability of color development is over one day at least. The method using thioglycolic acid is useful for the determination of iron in the samples containing from ca. 0.1 to 60 percent iron such as lime stone, silica stone, poltland cement, and iron ore on routin work.View full abstractDownload PDF (504K) -
Haruo HONMA, Hideko OTSUKA, Kiyoko YAMAMOTO, Teruji ISHII1983 Volume 32 Issue 11 Pages 709-711
Published: November 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSThe sweat is one of the most dilute secretion in human body but contains a great number of components. An extreme usefulness of laser desorption mass spectrometry has been found for the detection and identification of many kinds of components in sweat. This method makes it possible to measure a sample directly and to detect simultaneously inorganic and organic components as positive and negative ions whose detection limit is within the range of 0.1 ppm to 1.0 ppm. The sweat was ionized by He-Ne pulse laser irradiation and its mass spectra were measured by using a laser desorption mass spectrometer, Leybold-Heraeus GmbH LAMMA-500. The positive ions detected are as follows: Na+, Na2+, Mg+, Al+, Al3+, S+, S2+, Cl+, Cl2+, K+, K2+, Ca+, Mn+, Mn2+, Fe+, Fe2+, Ni+, Ni2+, Cu+, Zn+, As+, Cd2+, Sn+, Sn2+, Pb2+, HCN+, NO2+, NO3+, NaSCN+, KOCN+, Na2Cl+, CCl2+, NaKCl+, Na3Cl2+, C2H4+, C3H+5, CH3C0H+, C2H5OH+, HCOOH+, C3H4O3+, C4H8O2+, C3H7NO2+, C3H7NO3+, C4H7N3O+, C5H9NO2+, C5H15NO2+, C6H6N2O+, C6H5NO2+, C4H8N3O2+, C4H10N3O2+, C11H8O2+, and C6H12O6+. The negative ions detected are as follows: C-C7-, F2-, Cl-, CN-, OCN-, SO4-, C4H-, NaCN-, NaCl-, SCN-, NaOCN-, KCl-, KOCN-, NaSCN-, MgCl2-, CaCl2-, P2O5-, C2H-, C2H3-, C3H-, C2H3O2-, HC3COOH-, CH4N2O-, and C3H5O3-.View full abstractDownload PDF (402K) -
Kenjiro YANAGASE, Tetsutaro YOSHINAGA, Kentaro KAWANO1983 Volume 32 Issue 11 Pages T111-T116
Published: November 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSFor multi-purpose use of the geothermal water, removal of arsenic has been required. Two kinds of techniques were employed. The first one is made up of addition of iron (III) chloride to a arsenic containing solution followed by hydrolysis and coprecipitation, and the another, addition of iron (III) hydroxide to the solution. Fresh geothermal water collected from the Ohtake bore was used. And the geothermal water was maintained the temperature at 80 °C during the experiments. Influence of pH on the arsenic removal was examined and the optimum pH was found to be 3 in both methods. Comparison of both methods showed that direct addition method of Fe (OH)3 was less effective than the FeCl3 coprecipitation method. To attain the environmentally allowed maximum concentration (0.05 ppm), iron (III) concentrations of 25 ppm (FeCl3 coprecipitation method) and 45 ppm {Fe (OH)3 addition method} were required (under standard condition: pH 3, at 80 °C, 0.5 h stirring). Stirring time affected only for the Fe (OH)3 method. Residual arsenic concentration decreased with time and after 6 h the efficiency of arsenic removal became constant. This might be explained that before use, the Fe (OH)3 colloidal particles are in the state of secondary coagulated form, and with passage of stirring time the colloidal particles are mechanically dispersed to the primary coagulated form which is active for arsenic adsorption. Treatment temperature influenced the arsenic removal. At (8050) °C, optimum pH was around 3, and the residual arsenic concentration was (0.0140. 018) ppm, however, at 20 °C, optimum pH was shifted to 5 and the residual arsenic concentration was 0.04 ppm. Silicic acid and the salts (colloidal silica) showed a kind of buffer action on arsenic removal. That is, in the acidic solution, colloidal silica interfered the adsorption of arsenic, but in the alkaline solution, desorption (or elution) of arsenic from the iron (III) hydroxide was depressed.View full abstractDownload PDF (1093K) -
Muneyuki KOORI, Shinji ITOH, Koichi SATO, Haruno OKOCHI1983 Volume 32 Issue 11 Pages T117-T121
Published: November 05, 1983
Released on J-STAGE: January 18, 2010
JOURNAL FREE ACCESSIn the case of slag samples as refractory materials, it is important to combust perfectly keeping at high temperature. The combinations of accelerators and thier optimum amounts were examined. Combination of iron and tungsten gave satisfactory results. Residual metal was produced by the addition of iron, in the center of the crucible after combustion. Since this residual metal contained a slight amounts of sulfur, the losses of sulfur due to remaining in the residual metal are negligible. Analytical values of various slag samples (blast furnace slag, converter slag, etc.), which were analysed using 0.4 g of samples, and 1.5 g of iron and 2.0 g of tungsten as accelerator, were in good agreement with those obtained by the X-ray fluorescence analysis using α-correction method, and by the gravimetric method as barium sulfate. This method is excellent with respect to precision and rapidity. The coefficients of variation were about 2 %.View full abstractDownload PDF (816K) -
Yohei HASHIMOTO1983 Volume 32 Issue 11 Pages E343-E352
Published: November 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSClassical phytomicrochemistry founded by H. Molisch using microscopic methods has been further developed by the author using modern chromatographic techniques. These include improved spot test analyses, paper chromatography, paper electrophoresis, thin layer chromatography, gas chromatography and high performance liquid chromatography. Among the new procedures in liquid chromatography, the use of a capacitance-conductance detector for weak electrolytes, and chelate derivatization of primary and secondary amines have played important roles. Increased versatility in the use of micro techniques can be expected from the methods of histochemical and enfleurage chromatographies applied to the analysis of living cellular tissue in situ. The former method involves the direct analysis of cell contents including oily substances, solutions and other visible material removed by a newly improved micromanipulator for appropriate analysis by chromatographic methods including GC/MS. The latter method was so named by reason of its similarity to a classical method used in perfumery in which volatile substances are absorbed on fresh fat and subsequently extracted by ethanol to prepare an "absolute". In the microanalytical adaptation, the fat is extracted with acetonitrile and the extract serves as a sample which is injected directly into the chromatograph or GC/MS combination without need for the removal of the solvent.View full abstractDownload PDF (1430K) -
Yoshio SHIJO, Katsuji IDE, Kaoru SAKAI1983 Volume 32 Issue 11 Pages E353-E359
Published: November 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA rapid spectrophotometric method for the determination of molybdenum(VI) in seawater based on extraction and back extraction is described. Molybdenum(VI) is extracted as the thiocyanato complex from 400 cm3 of a seawater sample into 30 cm3 of 1 × 10-2 mol dm-3 capriquat (trioctylmethylammonium chloride) benzene solution and then back-extracted into 3 cm3 of 4 mol dm-3 nitric acid-1 mol dm-3 trichloroacetic acid solution, followed by spectrophotometric determination of molybdenum (VI) as molybdenum(V) thiocyanato complex after reduction. The concentration of dissolved molybdenum(VI) in Ibaraki coast( seashore of The Pacific Ocean) seawater was found to be 11.3 μg dm-3 with a relative standard deviation of 2.1%. Other cations in seawater were found not to cause interference.View full abstractDownload PDF (672K) -
Kousaburo OHASHI, Kazuyoshi KUROSAWA, Katsumi YAMAMOTO1983 Volume 32 Issue 11 Pages E361-E365
Published: November 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe absorption spectral changes of Cu(HDz)2, Cu(I)(HDz) and socalled secondary Cu(Dz) in various mixed organic solvents were investigated, where HDz and Dz represent monoanionic and dianionic form of 3-mercapto-1, 5-diphenyl formazane (dithizone), respectively. The addition of organic solvents such as methanol, ethanol and o-xylene to the chloroform solution of Cu(HDz)2 showed the absorption spectral change caused by the formation of sec-Cu(Dz) and caused the decrease in the absorbance due to the subsequent decomposition. Cu(HDz)2 did not show the absorption spectrum of sec-Cu(Dz) by the addition of carbon tetrachloride, nitrobenzene or toluene to chloroform solution of Cu(HDz)2, but decomposed simply. The addition of other organic solvents except for chloroform and benzene to sec-Cu(Dz) showed the simple change in the absorption spectrum due to the decomposition. Cu(I)(HDz) in mixed organic solvents showed the absorption spectrum of sec-Cu(Dz) and subsequently decomposed.View full abstractDownload PDF (665K) -
Masaru NIITSU, Yoshio MUKAI1983 Volume 32 Issue 11 Pages E367-E370
Published: November 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSThe solvent extraction of alkali metal(I) and cobalt(II) from 1 mol dm-3 solutions of five alkali metal thiocyanates into 1, 2-dichloroethane with Triton X-100 was examined. The extractability of cobalt (II) was closely dependent on that of the alkali metal thiocyanate. The reason for this was considered.View full abstractDownload PDF (438K) -
Akira SANO, Yoshihiro ASABE, Shoji TAKITANI1983 Volume 32 Issue 11 Pages E371-E374
Published: November 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSAs supplemental studies on fluorophore in the reaction of epoxides with nicotinamide and acetophenone, 1, 6- and 2, 7-naphthyridine derivatives were prepared, and their fluorescence properties were compared. The result confirmed that the fluorophore has a 2, 7-naphthyridine structure, but no 1, 6-isomer.View full abstractDownload PDF (469K) -
APPICATION OF XANTHENE DERIVATIVES FOR ANALYTICAL CHEMISTRY. Part XXXVYoshikazu FUJITA, Itsuo MORI, Shoko KITANO, Yoshiyuki KAMADA1983 Volume 32 Issue 11 Pages E375-E378
Published: November 05, 1983
Released on J-STAGE: June 19, 2009
JOURNAL FREE ACCESSA simple and rapid spectrophotometric method for the determination of tubocurarine chloride(TBC) using the color reaction with ο-hydroxyhydroquinonephthalein, zirconium(IV) and fluoride ions in the presence of sodium dodecyl sulfate was established. This method without extraction could be used in the concentration range of 0 150 μg/10 ml of TBC at 515 nm; it was applied to the determination of TBC in commercial injections.View full abstractDownload PDF (532K)
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