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Volume 29, Issue 3
Displaying 1-16 of 16 articles from this issue
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Determination of calcium sulfate dihydrate in atmospheric particulate by X-ray powder diffractometryToshihiro NAKAMURA, Masatoshi TAGUCHI, Hiroo SASUGA1980 Volume 29 Issue 3 Pages 159-164
Published: March 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSCalcium sulfate dihydrate in atmospheric particulates was determined by X-ray diffractometry. Synthesized CaSO4·2H2O was employed as a standard material. To reduce errors generated from the difference in crystallinity between the standard material and samples, the synthesized CaSO4·2H2O was ground to such an extent that its half width of 141 diffraction line was equal to that of CaSO4·2H2O contained in samples. Calibrating standards were prepared by filtering suspensions through glass fiber filters. The suspensions were prepared as follows: known quantities of a mixed powder {10.0 (w/w) CaSO4·2H2O, 45.0% silica gel, and 45.0% carbon} were sonically dispersed in methanol. Absorption effects of such matrix material as silica gel, carbon, and α-ferric oxide were negligible when the respective material was in the range <2000μg cm-2. A linear calibration curve was obtained over the range (20200)μg cm-2 by measuring the intensity of 141 reflection line for CaSO4.2H2O. A low volume air sampler was used for the collection of atmospheric particulates. The determination limit was 8μg cm-2, and the coefficient of variation was 12% after ten determinations at a level of 99μg cm-2 CaSO4·2H2O.View full abstractDownload PDF (897K) -
Wataru ISHIBASH, Ryoji KIKUCHI1980 Volume 29 Issue 3 Pages 165-169
Published: March 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSEffects of various sheath gases for the measurement of aluminum, calcium and copper in flameless atomic absorption have been studied. The sheath gases used for this work were helium, nitrogen, argon and sheath gases mixed hydrogen in pure sheath gases. The atomic absorption spectrophotometer was used a Hitachi Model 308, equipped with a Perkin-Elmer HGA-2100 graphite tube furnace. The results of this experiment were suggested as follows. (1) The common logarithm of atomic absorbance can be expressed by linear function for flow rates of the sheath gases. The linear function is divied into a type helium and a type argon. The nitrogen sheath gas belongs to one of the type argon. (2) A plot of logarithm of atomic absorbance vs. argon flow rates expresses the type helium at argon gas flow rate more than a constant. (3) A difference between the type helium and the type argon is recognized by the diffusion coefficient of sheath gases. (4) In H2-Ar sheath gas, the atomic absorbance [A] of aluminum has been obtained as a function of hydrogen concentration [H]. [A] =K/[H]0.52 K……constant (5) The atomic absorbance of aluminum and calcium decreases under the nitrogen sheath gas in comparison with the argon gas, or the atomic absorbance of aluminum and copper decreases under the sheath gases of hydrogen and other gas in comparison with the argon gas.View full abstractDownload PDF (796K) -
Kazuhiro KUWATA, Yoshiaki YAMAZAKI, Michiko UEBORI1980 Volume 29 Issue 3 Pages 170-175
Published: March 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe adsorption and thermal desorption characteristics of (C1C4) aliphatic amines on alkalized porous silica beads were examined for use as an analytical sampling device. The experiment was performed by using a sampling tube (5cm×7mm i. d., glass) packed with 0.8g of Porasil A {(80100) mesh} coated with 5% of potassium hydroxide and by gas chromatography with a glass column (3m×2mm i. d.) packed with Chromosorb 102 TMCS coated with 5% of potassium hydroxide. The sampling tube had an effective capacity for the low ppm or ppb level of the (C1C4) amine vapors at less than 500ml/min of the air sampling rate, though water vapor in the sampling tended to reduce breakthrough volumes of the amines. In usual cases, 6l of air could be successfully sampled without loss of the collection efficiencies for (20500)ng of the amines. The desorption of the amines was completed by passing nitrogen gas (50ml/min) through the tube at 280°C for 4min. The recoveries for (20500)ng of the amines were (81107)% and their standard deviations were less than 5%. Effect of storage time on the recoveries was not apparently observed in 24h. This simplified technique for collection and concentration of (C1C4) amine vapors could be used in the place of the prevailing condensation methods up to date.View full abstractDownload PDF (859K) -
Takushi KOITA, Haruo MIYATA, Kyoji TOEI1980 Volume 29 Issue 3 Pages 176-179
Published: March 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSFor the determination of 10 ppm or below of sulfateion in river waters, 1-anthraquinoneazo R acid was synthesized as a new precipitating and colorimetric reagent. The mixed reagent, of its barium salt and barium sulfate powder (1+100) was used to the determination of sulfate ion. By the mixed reagent, the precipitates of barium sulfate was formed quantitatively with sulfate ion from ethanolic solution (1+1), and the absorbance of the liberated reagent in its supernatant liquid was measured at 522nm. By this method, (210)ppm of sulfate ion in river waters could be determined with a recovery of (94101)%. The ions normally present in river waters gave strong interference on this determination. Chloride ion and cations were eliminated with Ag2O and a cation exchanger resin, respectively. The analytical procedure is as follows: Filter the river water samples through a membrane filter (0.45μm), and add 20mg of Ag2O to (60100)ml of its filtrate. Shake the mixture for 2h, and centrifuge for 5 min at 3000 rpm. Pass the supernatant obtained into a column containing Amberlite IR 120 B (1.5cm2×10cm). To 3ml of its eluate (pH 34) in a 10-ml stoppered centrifuge tube, add 40mg of the mixed reagent and 3ml of ethanol. Shake for 45 min with a mechanical shaker, and centrifuge the precipitate for 15min at 3000rpm, and then, take the clean supernatant liquid into a 1cm glass cell. Measure the absorbance at 522nm.View full abstractDownload PDF (584K) -
Keiro HIGUCHI, Shigeharu MONYA, Yasuaki SHIMOISHI, Haruo MIYATA, Kyoji ...1980 Volume 29 Issue 3 Pages 180-183
Published: March 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA new cationic dye, 1-methyl-4-(4-diethylaminophenylazo)-pyridinium iodide, forms, with the anionic surfactants such as alkylbenzenesulfonate and alkylsulfate, ion-associates extractable from an aqueous layer with chloroform. The concentration of the surfactants can be determined by measuring the absorbance of the extracts at 564 nm. Calibration curve obeyed to Beer's law over the range 01.5×10-5M (in chloroform) of the surfactants. And the apparent molar absorptivity is 67000 mol-1 cm-1 1 with sodium di-(2-ethylhexyl)-sulfosuccinate (SSS, 96.3% certificated by Japan Oil Chemists' Society). The determination procedure is as follows: In a 100ml separatory funnel, place 100ml of sample solution (surfactant content <7.0×10-7M), 1ml of 5×10-4M reagent, 2ml of acetate buffer solution (pH 6), 2ml of 1.5M sodium sulfate, and 2ml of 10-2M EDTA solution. Add 5ml of chloroform, and shake the funnel for 5min mechanically and allow to stand for 15min. Measure the absorbance at 564nm with 1cm glass cells. The proposed method is very simple and rapid in comparison with the Methylene Blue method (JIS method), and is useful for the determination of trace amounts of the anionic surfactants in river waters.View full abstractDownload PDF (536K) -
Akiyoshi SUGIMAE1980 Volume 29 Issue 3 Pages 184-189
Published: March 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe sample preparation method was examined for the determination of trace elements in water-soluble component of airborne particulate matter collected on a glass fiber filter. The proposed procedure is as follows. A sample disc of 50 mm in diameter is punched out from a 8''×10'' Hi-vol filter sample and placed in a 300-ml conical beaker. Five ml of cation exchange resin {Dowex 50W-X8, (50100) mesh, H-form} are added to prevent the adsorption of water-soluble metal compounds on the fiberous filter surface during the immersion of the sample disc. Seventy ml of distilled water are added and heated at the temperature (95°C) below the boiling point on the water bath for 2h. The disc is removed from the sample solution, rinsed with distilled water and discarded. The metal-adsorbed ion-exchange resin is washed with distilled water, leached with (1+3) HCl for 30 min at room temperature and filtered off on a filter paper. The filtrate is catched in a volumetric flask and diluted to 50 ml with (1+3) HCl. The solution thus prepared is subjected to inductively coupled plasma-optical emission spectrometry for the simultaneous determination of Zn, Pb, Cd, Ni, Mn, Fe, Cr, V and Cu. The method was found to yield satisfactory results and the precision of the complete analytical procedure was consistently better than±12%.View full abstractDownload PDF (798K) -
Takeshi OMORI1980 Volume 29 Issue 3 Pages 189-193
Published: March 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method is described for the quantitative determination of 11 water-soluble acid dyes permitted in Japan as food additives, and eosin by high performance thin layer chromatography (HPTLC). The analytical conditions were as follows: HPTLC plates Si 60 were used and activity of the adsorbent was preconditioned with H2SO4-solution for relative humidity at 47%. Solvent was ethylmethylketone: methanol: 28% NH3(aq)=10:5:1.25 and solvent vapor was preloaded for 5min in saturated chamber. Dyes which are unstable in concentrated ammonia solution were separated by HPTLC plates cellulose, with solvent butanol: ethylmethylketone: 1% NH3(aq): water=4:2:1:1. Each dye, between 5ng and 20ng, was determined quantitatively by the dual wavelength densitometer (sample wavelength λs=430nm, 550nm, 630nm, reference wavelength λr=700nm). The advantages of HPTLC plates are shorter analysis time, more measurement data per plate and high resolution and more improved signal/noise ratio than those of usual TLC plates, and therefore, HPTLC plates are suitable for determining small amount of substances directly on chromatograms by using a densitometer.View full abstractDownload PDF (717K) -
Katsumi YANAGI1980 Volume 29 Issue 3 Pages 194-199
Published: March 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSFor the analysis of arsenic at ppb or less level in natural waters, a new procedure was developed. 25 ml of a water sample and 3ml of 6N hydrochloric acid are taken in a reaction vessel. By using a peristaltic pump 2% sodium borohydride solution is let to flow in the vessel at a rate 1. 2ml/min. Six min flow is enough to convert the total arsenic in the vessel into arsine to be transferred by the carrier hydrogen which is evolved at the same time, to the trap of liquid nitrogen. It is also noteworthy that the acidity of 0.6N was proved to be sufficiently strong for converting As (V) into arsine as well as As (III). Then the trapped arsine is vaporized in a water bath and transferred by the flow of nitrogen (900ml/min) into a quartz cell (10mm×265mm). The cell which has been heated by an electric furnace atomizes the arsenic for measuring its atomic absorption at 193.7 nm wavelength. Calibration curve drown from peak height values of absorption signal slightly bends but is quite reproducible. The determined values are satisfactory with a coefficient of variation, less than 2.9% at the arsenic concentrations ranging from 0.08ppb to 0.6ppb. Lower limit of determination is 0.02ppb, when a 25ml sample is used. The determination is hardly affected by other ions normally present in natural waters. The applicability of this procedure to natural water samples proved to be satisfactory, giving a good recovery of arsenic in standard addition experiments. The time required for a determination is eight to ten min.View full abstractDownload PDF (888K) -
Tsunenobu SHIGEMATSU, Masakazu MATSUI, Osamu FUJINO1980 Volume 29 Issue 3 Pages 199-203
Published: March 05, 1980
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIonization behavior of europium in a nitrous oxideacetylene flame was studied by using an atomic absorption method. Europium measured in the range of (18)×10-4M by an atom line and by an ion line gave calibration curves showing a district curvature away from and near to the concentration axis respectively. This curvature suggested that europium was considerably ionized, and there existed electrolytic dissociation equilibria among europium neutral atom, ion and electron. Therefore, the salts of alkali metals which were easily ionized in the chemical flame were selected to study their matrix effect on the absorbance of europium; the salt concentrations studied ranged from 5×10-4M to 2×10-2M with 3×10-4M of, europium. The results showed that the absorbance of the atom lines for europium increased wheras the absorbance of the ion line reduced until near nil absorbance by increasing concentrations of alkali metals. A similar tendency was found between the matrix effect of some other common elements and rare earth elements and that of alkali metals. These effects depended not only on the concentration of salts but also on their ionization potential; higher metal concentration and lower ionization potential gave higher matrix effect. We have calculated the fraction of ionization of europium in N2O-C2H2 flame using absorbance readings of europium with and without alkali metals. The results showed that europium in the range of (116.4)×10-4M was ionized from 48 to 78%.View full abstractDownload PDF (522K) -
Kunishige HIGSHI, Kazuyoshi HAGIWARA1980 Volume 29 Issue 3 Pages 204-208
Published: March 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple and rapid method was studied for the characterization of spilled oils in the environment. Seven crude oils produced in the Middle East were used as sample oils. The crude oil {(520)μl} was spotted on a thin-layer of stationary phase, and developed on standing. Chromatogram of the developed oil was obtained on dual-wavelength TLC scanner (Shimadzu CS-910). Comparison was carried out on four kinds of stationary phases such as silica gel, alumina, microcrystalline cellulose, and filter paper. Discriminative capability among the oils was highest in the case of silica gel. Peak intensity of the chromatogram increased with standing time after spotting the oil, but considerable change of the profile was not observed.Development after heating the spotted oil was also studied for the analysis of high-viscous oils. The profile of the oil depended upon the temperature of developing. The profile of the chromatogram changed considerably with both measuring and reference wavelength. The discriminative capability among the crude oils was enhanced by comparing the profiles of the oils at several wavelengths.View full abstractDownload PDF (607K) -
Uranium (VI)-trioctylphosphine oxide-dibenzoylmethanehexane systemTatsuya SEKINE, Satoshi KUSAKABE, Teruyuki TOSAKA1980 Volume 29 Issue 3 Pages 209-211
Published: March 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSEffect of coextracted acids in organic solvents on the coloration of extracted metal ions with an additional complexing agent was studied in uranium (VI)-trioctylphosphine oxide-dibenzoylmethane-hexane system when the aqueous phase contained hydrochloric, perchloric, or nitric acid. The coloration was found to be more reduced in this order of the acids as well as with higher concentration of an acid. This interfering effect of the coexisting acid could be eliminated by washing the organic phase with a borate-carbonate buffer at pH 8.6.View full abstractDownload PDF (460K) -
Eiji KOYAMA, Shigeo KATSURA, Mitsuo FUKUMURA, Kozo NAGASHIMA1980 Volume 29 Issue 3 Pages 211-213
Published: March 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSFor the inductively coupled plasma (ICP) spectroscopic determination of selenium in organic selenium compounds, several milligrams of sample is treated with concentrated nitric acid in a tightly sealed glass vessel to convert selenium into water-soluble form. Then the solution is diluted and introduced to the argon plasma, and the emission intensity is measured at the wavelength of 1960.3Å (SeI). The method allows the determination of selenium in the concentration range 1ppm to 1000ppm, most conveniently 10ppm to 100ppm. The concentration of nitric acid of both sample and standard solution should be adjusted to 0.6N to 1.2N, because large amount of nitric acid reduces the spectral intensity of selenium. The standard solution of selenium is prepared by dissolving selenium in conc. nitric acid and conc. hydrochloric acid (1:3). Selenium content of the known selenols, diselenides and selenoxides were determined to check the accuracy of the present method. The coefficient of variation for the selenium analysis of these compounds was 0.5% to 0.7%.View full abstractDownload PDF (448K) -
Shuichi ETO, Ryota SHINOHARA, Azuma KIDO, Teiji HORI1980 Volume 29 Issue 3 Pages 213-216
Published: March 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSMicrodetermination of N-cyclohexy 1-2-benzothiazole sulfenamide (CHBSA) and 2-(4-morpholinothio) benzothiazole (MTBT) were developed. One litre of a water sample was extracted with 50ml each of hexane twice. The extract was dried through an anhydrous sodium sulfate column and concentrated to 1ml with a Kuderna-Danish (KD) evaporator at reduced pressure. The concentrate was analyzed by gas chromatography with a flame photometric detector (FPDGC). In case of sediment samples, 50ml of acetonitrile was added to a sample (20g). The mixture was filtered after vigorous shaking for 10min. The sediment residued on the filter was shaked with 50ml of acetonitrile again. After filtration of the mixture, all the filtrate were combined. The filtrate was washed with 50ml of hexane 3times to remove the interferences. The acetonitrile layer was extracted with 50ml each of hexane twice after 400ml of water had been added to the acetonitrile layer. Then hexane layer was treated in the similar way as water samples. When the removal of interferences was inadequate, alumina column chromatography was required. The alumina (neutral, W 200, 1% water added) column (1cmφ×10cm) was prepared with benzene. The concentrate was placed on the top of the alumina column. CHBSA and MTBT were eluted with benzene/ethyl acetate/triethylamine (16/4/1) after the column had been washed with 20ml of benzene. The first 7ml was discarded. The next 20ml was collected and concentrated to 1ml with a KD evaporator at reduced pressure. Recoveries of CHBSA and MTBT for a water sample were 92% and 82%, and these for a sediment sample were 68% and 93%, respectively. Detection limits of CHSBA and MTBT for a water sample (11) were 0.04ppb and 0.02ppb, and these for a sediment sample (20g) were 2 ppb and 1ppb, respectively. This method was applied to some environmental samples. MTBT was detected at 8ppb in one river sediment sample, while not detected in other environmental samples. No CHBSA was detected in the all samples examined.View full abstractDownload PDF (579K) -
Shoji TAGAWA, Yoshio KOJIMA1980 Volume 29 Issue 3 Pages 216-219
Published: March 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSBehavior of arsenous, arsenic, disodium methanearsonate (DSMA) and dimethylarsinic acid (DMAA) with a strong-acid cation-exchange resin was investigated. Dowex 50W×8 {(50100) mesh, hydrogen from} was used. A mixed solution, modified to pH 2, of these arsenicals was applied to the top of a short column (1.5cm×12cm) connected to a long column (1.9cm×118cm) and then eluted at a flow rate of (911)cm3cm-2h-1. The effluent was monitored for arsenic by using atomic absorption spectrophotometer equipped with graphite furnace atomizer. Arsenic, arsenous and DSMA were separately eluted with water in this order from the long column. DMAA held strongly on the short column was eluted with aqueous ammonia after the connection of the two columns was cut. Almost 100% of these arsenicals was recovered in the effluents. From an aqueous extract from a brown seaweed, Hizikia fusiforme, 4 arsenic peaks corresponding to the reference arsenic, arsenous, DSMA and DMAA were obtained by the method. This method is effectively applicable for studying chemical forms and metabolic fate of arsenic in marine organisms.View full abstractDownload PDF (574K) -
Hiroshi ONISHI, Fumie KAWASHIMA1980 Volume 29 Issue 3 Pages 219-221
Published: March 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn the analysis of wastewater for total cyanide by JIS (Japanese Industrial Standard) method, if the distillate contains small amounts of sulfide, it is treated with potassium permanganate and redistilled. Instead of this oxidative treatment, addition of a precipitant and distillation of hydrogen cyanide without removal of the sulfide precipitate was investigated. Satisfactory results were obtained by distillation of 300ml of solution containing 0 to 30μg of CN-, 1.0mg of S2-, 20mg of Bi(III) and 6ml of 3.2M (=1+4) nitric acid. About 70ml of distillate was collected in a receiver containing 20ml of 20g/l sodium hydroxide solution. The cyanide was then determined spectrophotometrically by JIS pyridine-pyrazolone method.View full abstractDownload PDF (301K) -
Takashi KORENAGA1980 Volume 29 Issue 3 Pages 222-223
Published: March 05, 1980
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple apparatus was developed for the rapid and continuous determination of chemical oxygen demand (COD) in environmental water samples based on the principle of flow injection-spectrophotometric analysis. A solution of 2.7×10-4M potassium permanganate in 3.3% sulfuric acid was pumped with a reciprocating pump into the manifold to which 20μl of sample (i. e. sodium oxalate solution) was also introduced by manual injection. After reaction, the mixture went through a quartz flow cell (10mm light path, 18μl volume) placed in a spectrophotometer operated at a wavelength of 525nm. The manifold was made entirely of polytetrafluoroethylene tubing (0.5mm inner diameter, 10m length). The signal from the spectrophotometer was continuously recorded. When a pumping rate was chosen to be 1.9ml min-1, a residence time was 1min. A sampling rate of 120 samples per hour was achieved and the apparent COD at a concentration range of (21170) mg COD l-1 was measured reproducibly. Chloride at 10 mg l-1 level was suppressed by adding 0.1% silver nitrate in the flow injection system.View full abstractDownload PDF (246K)
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