Sakingo Imai

Preparation of dithiocarbamatecellulose derivatives and their adsorption properties for trace elements

Tosylcellulose was treated separately with aniline, benzylamine, n-butylamine and piperazine to give four different aminocelluloses which were further treated with carbon disulfide to furnish four dithiocarbamatecelluloses (AND, BZD, BUD and PID). A comparative study was made of their performance as adsorbents for several kinds of metal ions. PID, which has the highest degree of substitution of the dithiocarbamate group of the four derivatives obtained, was investigated for its adsorption behavior towards Ag+, As5+, Cd2+, Co2+, Cr3+, Cr6+, Cu2+, Fe3+, Hg2+, Mn2+, Pb2+, Sb5+; Se4+, Te4+ and Zn2+. PID showed good adsorption characteristics with relatively large capacities for Ag+, Cr6+, Cu2+, Hg2+, Pb2+ and Se4+ ranging from 9.5 to 370 mg g-1 of resin.

Fluorimetric determination of aluminium in serum

A convenient fluorimetric method for the routine determination of aluminium in serum has been developed using lumogallion [4-chloro-3-(2,4-dihydroxyphenylazo)-2-hydroxybenzene-1-sulphonic acid]. Losses of aluminium during deproteinisation of the serum were prevented by treatment with a combination of 20 or 30% m/V trichloroacetic acid (TCA) and 5% m/VTCA. Iron(III) was removed by extraction into chloroform with capriquat (methyltrioctylammonium chloride) as an Fe3+-lumogallion-capriquat ternary complex. The interference from Cu2+ was eliminated by using thiosulphate as a masking agent. The detection limit was 3.6 ng ml-1 and the calibration graph was linear up to 1.4 micrograms ml-1 of aluminium. Using the proposed method, the average concentration of aluminium in the serum of healthy subjects was found to be 6.8 ng ml-1, in agreement with values reported in the literature.

Neutron activation analysis of biologically essential trace elements in environmental specimens using pyrrolidinedithiocarbamate extraction

A new radiochemical group separation method using APDC reagent in the extraction procedure has been developed. The method has been applied to the radiochemical separation for activated biological samples and also to the preconcentration technique for sea water samples. The transition elements are extracted into chloroform phase from the pH 3.0 aqueous phase and only manganese is subsequently extracted from the pH 7.0 aqueous phase. The validity of the method is demonstrated by analyzing the NBS standard reference materials. In the specimens preconcentrated from the sea water samples adjusted pH to 5.5, vanadium, manganese, copper and zinc can be determined.

Determination of traces of gaseous acrolein by collection on molecular sieves and fluoremetry with o-aminobiphenyl

Abstract A fluorimetric method for determining traces of atmospheric acrolein has been developed using molecular sieves 3A and 13X to collect the vapour and o-aminobiphenyl as the fluorescent reagent. Gas samples up to 60 l can be used with 2 g each of molecular sieves 3A and 13X at room temperature, and up to 0.056 μg of acrolein can be recovered, o-Aminobiphenyl shows high selectivity towards acrolein; only methyl vinyl ketone and crotonaldehyde interfere slightly. The method is simple and practical, with errors less than about 5%.

A field study of the incorporation of atmospheric ion species into raindrops

Abstract Urban atmospheric ion species are incorporated into raindrops near the ground. Rain was collected from July 1993 through June i994 at the midtown in Kobe City and at the top of Mt. Maya which is located adjacent to the town at an altitude of 700 m. The incorporated H+ was about one-half of the total deposited amount of H+ at the midtown. The ratios of the incorporated ions other than H+ to the total deposited amount of ions at the midtown ranged from 0.09 to 0.3i. Therefore, the majority of ions deposited at the midtown was supplied from clouds. Sodium ion (Na+), Ca2+ and Mg2+ in suspended particulate matter (SPM) were more abundant during the rain period than the non-rain period. When the SPM concentration was high, the pH of raindrops was lowered by acidic components such as SO2 which had increased in the atmosphere. Generation of H+ ion in raindrops near the ground could be due to the incorporation of SO2 supplied from diesel exhaust gas.

Sorption of uranium by cellulose derivatives

The sorption behaviour of uranium was investigated by batch and column methods using four cellulose derivatives, two having an amino group and two having an amino group plus a dithiocarboxylate group. All four derivatives showed maximum uranium sorption from pure water in the neutral region or from artificial sea water in the acidic region. In the batch method, quantitative removal of 100 µg of uranium from 50 ml of water at pH 5.0 was achieved by equilibration with 50 mg of any of the four sorbents. The percentage removal under these conditions decreased gradually with increasing concentration of uranium above 100 µg per 50 ml. A similar high percentage removal of uranium was achieved using artificial sea water. In the column method, quantitative removal of 5 µg of uranium from 1 l of water at pH 6.7 was achieved with 200 mg of either of the two sorbents. Similar quantitative removal of uranium was achieved from 1 l of artificial sea water at pH 5.4 with 500 mg of either of the two sorbents. Several 1-and 10-l portions of natural sea water, adjusted to pH 5.0, were passed through the column, which was packed with a mixture of 500 mg of either of the two sorbents and 1 g of cellulose powder. The results indicated that uranium was quantitatively removed from the 1-l portions, while approximately 50% was removed from the 10-l portions.

Gas-liquid chromatographic determination of polycyclic aromatic hydrocarbons in airborne particulates

This paper describes a method for the routine determination of 13 typical types of 3–5 ring polycyclic aromatic hydrocarbons (PAHs), occurring in airborne particulates, using gas-liquid chromatography (GLC) with a packed column. The PAHs were completely separated except for the overlap of benzo[k]fluoranthene and benzo[e]pyrene under the proposed GLC conditions. Cyclohexane and a cyclohexane-chloroform (8 + 2) solvent system for column chromatography (CC) were the most effective of the five solvent systems in eliminating interfering components. The average recoveries of the 13 types of PAHs by a CC procedure were in the range 81–103%. An internal standard (1,3,5-triphenylbenzene) method was used to calculate the concentrations of PAHs.

Emission spectrographic determination of trace elements in atmospheric particulate matter

Abstract Air containing particulate material was passed continuously for one month through a low-volume air sampler equipped with a cyclone to exclude particulates greater than 10 μm in diameter. The samples and filters were ashed in a low-temperature plasma and, after addition of In2O3 support, palladium internal standard and graphite buffer, the ashes were analyzed by a.c. are emission spectrometry. Standard samples were prepared from a commercial standard containing 49 elements. The procedure allows the determination of 14 trace metals (Ag, Al, Cr, Cu, Fe, Ga, Mn, Mo, Ni, Pb, Sn, Ti, V, Zn) with relative standard deviations of 1.4–15.1%. The procedure has been applied successfully to monthly determinations of the average atmospheric concentrations of these elements in Kobe City for the past three years.