The preparation of a certified reference material of polar pesticides in freeze-dried water (CRM 606)

The preparation of a certified reference material of polar pesticides in freeze-dried water is described. The pesticides selected were atrazine, simazine, carbaryl, propanil, linuron, fenamiphos and permethrin which were added to 6000 litres of tap water at 50–80 μg · L–1 (200–320 μg · L–1 for permethrin) level in presence of NaCl (2.5 g · L–1) prior lyophilization. After the freeze-drying process the residue was rehomogenized, filled into amber glass bottles and stored at –20 °C, +4 °C and +20 °C. All pesticides were determined by HPLC/diode array detector, except permethrin which was determined by GC/ECD. The results obtained for atrazine, simazine, carbaryl, propanil, linuron and fenamiphos showed no within- or between-bottle inhomogeneity, however the material was non-homogeneous for permethrin and therefore this was withdrawn from further studies. With respect to the stability for over one year, all pesticides were stable at –20 °C. At +4 °C all pesticides were stable for at least 9 months and at +20 °C the stability was demonstrated only during the first month of storage. The content (mass fractions) of atrazine, simazine, carbaryl, propanil and linuron in freeze-dried water (CRM 606) was certified by an interlaboratory testing and a certification campaign.

Preparation of manganese oxide - graphite electrodes by electrophoretic deposition

Manganese oxide is a promising active material for supercapacitors (SCs) with pseudocapacitance due to its high capacitance and its environmentally friendly character. This paper deals with the preparation of electrodes for supercapacitors consisting of manganese oxide supported onto graphite by electrophoretic deposition. Manganese oxide powders were characterized and dispersed in water by controlling the colloidal and rheological behavior in order to obtain stable suspensions. Optimized manganese oxide suspensions were deposited onto graphite electrodes by electrophoretic deposition. The deposited mass per unit area in the electrodes was optimized by controlling the applied current density and the deposition time. It has been demonstrated that the introduction of a binder helped to improve the adherence to graphite; otherwise the deposit thickness obtained by EPD is limited and no films can be obtained by simply dipping. These conditions allowed us to obtain more homogeneous deposits with higher specific energy than without binder.