Two fractions of both fulvic acids (FA) and humic acid (HA) were prepared by fractionation method of Pierce and Felbeck5 involving acid hydrolysis of soil rests. This step increases recovery of both FA and HA considerably what suggest us need for slight modification of IHSS method in some cases. The weight loss, change in organic carbon content and visible spectra are figures of merit discussed. After detailed characterization these humic substances (HS) will serve as the working standards for study of interactions between organomercurials and organic part of soil.
Authors:M. Hutta, S. Rippa, J. Kandráč, and M. Chalanyová
Post-column derivatization detection system based on dithizone solubilized in cetyltrimethyl-ammonium hydrogenesulfate micellar media at pH 2.0 was devised and evaluated for selective detection of mercury(II), methylmercury and phenylmercury in reversed-phase HPLC system with photometric detection at 500 nm. This reagent solution is fully compatible with acidic organo-aqueous mobile phases generally used in RPHPLC. With the aid of the detection systematic study of the retention behaviour of three mercury species on octadecylsilica sorbent was carried out. Influence of pH, acetonitrile volume fraction, complex forming additives was investigated in detail. In mobile phase consisting of 5–30% of acetonitrile in water at pH 2.0 and 2·10–4 mol·I–1 DCTA linear calibration curves were measured in range 20–1000 ppb with correlation coefficient better than 0.99. Detection limits were 1–5 ng for this three mercury species. Interferences of copper(II) and silver(I) are negligible.
Authors:T. Prochácková, R. Góra, J. Kandráč, and M. Hutta
Sequential multistep procedure, usually used for the fractionation and characterization of soil organic matter was tested
for Hg content in the individual steps and fractions. Under general laboratory conditions serious problems have arosen during
the attempt in the Hg mass balance calculation. Several sources of Hg contamination were recognized. The most serious was
the background concentration of Hg even in research grade chemicals (what is in general not declared) and laboratory air.
The work on operational Hg speciation as non-humic bound, humic acid, fulvic acid bound proceeds from the established status-quo
on distribution of mercury of soil organic matter.
Authors:A. Paulenová, P. Rajec, J. Kandráč, G. Sasköiová, E. Tóthová, P. Bartoš, V. Švec, and R. Góra
Complexation equilibrium of metals by three humic acids of different origin with ultrafiltration method was investigated at pH 4 a 5 and ionic strength I = 0.1M NaClO4. Commercial (Aldrich) and two original humic acids (peat and soil, obtained by six step isolation process from the material from Trnava county, close to the NPP Jaslovské Bohunice) were used in this study. For the evaluation of the results, the model of metal ion charge neutralization upon humic acid functional group proposed by the Kim and Czerwinski was used. Complexation constants were calculated using the terms of this model (operational concentration, loading capacity). The values of log = 5.39±0.16 for yttrium, 6.15±0.16 for americium and 5.20±0.08 for lead were found. Correlation of free metal concentration and ratio of molar fraction of complexing functional groups confirms the validity of charge neutralisation model for metal and polyelectrolyte complexation study.