Electroanalytical and chromatographic determination of pentachlorophenol and related molecules in a contaminated soil: a real case example

Electroanalytical and chromatographic methodologies have been applied for the determination of pentachlorophenol (PCP) and some of its derivatives in real soil samples contaminated by industrial discharge. The analytes were extracted with hexane from soil samples collected at different points of the site and mixed to produce a representative sample. Square wave voltammetry (SWV) experiments were carried out on either a boron-doped diamond (BDD) electrode or a gold ultramicroelectrode (Au-UME) in an analyte composed by the Britton-Robinson (B-R) buffer at pH 5.5 with the direct addition of proper amounts of the extract. The voltammetric responses revealed an irreversible anodic peak at approximately 0.80 V vs. Ag/AgCl with a peak current showing a linear dependence on PCP concentration. This linear relationship yielded a detection limit (DL) of 2×10⁻⁸ mol l⁻¹ (or 5.5 μg l⁻¹) for the BDD electrode and 6.9×10⁻⁸ mol l⁻¹ (18.4 μg l⁻¹) for the Au-UME, while the independently measured HPLC detection limit was 1.1×10⁻⁸ mol l⁻¹ (3.0 μg l⁻¹). The application of electroanalytical and chromatographic methodologies in the analysis of soil extracts revealed, besides the PCP responses, signals for some related molecules such as o-tetrachlorobenzoquinone (o-chloranil), hexachlorobenzene and tetrachlorophenol. Recovering experiments for PCP showed a concentration of 27.5 mg kg⁻¹ for the electroanalytical determinations and 26.8 mg kg⁻¹ for the HPLC analysis, values exceedingly high if considering that the maximum residue limit established for natural waters by the Brazilian Environmental Agency is 10 μg l⁻¹.     

Superfluid3He in high magnetic fields: New results

The superfluid A₁ an A₂ transitions have been studied by means of vibrating wire viscosimeters in magnetic fields up to 9.3 T. Using the technique of quick melting of polarized solid (Castaing-Nozières effect) we have succeeded in increasing the superfluid transition temperature from 2.86 to 3.23 mK, which is the highest up to now. Using this method, with some improvements, it should be possible to test some of the present theoretical models for³He. A minimum of the viscosity in the A₁ phase has been observed for the first time. Very close to the A₂ transition an anomaly in the amplitude of the viscometers seems to indicate the presence of a new phase, or some textural change due to dipole locking.Invited talk at the International Conference on Macroscopic Quantum Phenomena, Smolenice Castle, Czechoslovakia, September 18–22, 1989.The authors wish to thank C. C. Kranenburg and C. M. C. M. van Woerkens for their various contributions to the experiments. Very helpful discussions with K. S. Bedell, B. Castaing, H. Capel, P. Nozières, D. Rainer, A. Schakel, and G. A. Vermeulen are gratefully acknowledged. This work was financially supported by the Stichting voor Fundamenteel Onderzoek der Materie F. O. M.