290
rately prepared, containing 0.04 M H 3 PO 4 , CH 3 COOH,
H 3 BO 3 ) and 0.2 M NaOH.
4. Ethanol (96%) for preparation of aqueous ethanolic solutions of
less soluble drugs (40% v/v).
1. Working electrode: Glassy carbon or platinum electrode of
diameter 0.7–2 mm.
2. Ag/AgCl/1 M KCl reference electrode separated from examined solution by a salt bridge.
3. Auxiliary electrode: Pt net.
4. The electrochemical cell with an inlet and outlet for argon or
nitrogen: In case of ethanolic solutions, argon is first bubbled
through the reservoir of ethanol to prevent the evaporation of
ethanol from the examined solution.
1. The electrolytic cell with separated anodic and cathodic parts
and inlet/outlet of inert gas: In case of ethanolic solution,
argon is first bubbled through the reservoir of ethanol to prevent the evaporation of ethanol from examined solution.
2. Working electrode: Glassy carbon or platinum electrode with a
large surface.
3. Ag/AgCl/1 M KCl reference electrode separated from solution by a salt bridge.
4. Auxiliary electrode: Carbon electrode present in the cathodic
compartment of the electrolytic cell (when oxidative generation
of products is measured).
1. Optically transparent spectroelectrochemical cell (more details
available in [20]).
2. 0.5–1 mL Hamilton syringe with needle.
3. Tetrabutylammonium hexafluorophosphate in acetonitrile used
as supporting electrolyte for electrochemical cleaning of the
cell.
1. GC-MS parameters: Separation on a DB-5MS chemically
bonded fused silica capillary column with stationary phase 5%
phenyl-95% methylpolysiloxane, and of dimensions 0.25 mm
i.d., 0.1 μm film thickness, 25 m and 30 m length. Gas chromatographic conditions as follows: initial temperature 57 °C,
2 min isothermal, then ramped at 10 °C/min up to 200 °C,
3 min isothermal, then ramped at 20 °C/min up to 300 °C,
and then isothermal for 20 min. Carrier gas He (purity
99.9995%), at a constant flow rate of 1.2 mL/min. Injection
volume 2 μL, splitless mode at 280 °C. Mass spectrometric
acquisition on a single quadrupole, electronic impact ionization
2.2 Cyclic
Voltammetry
2.3 Electrolysis
2.4 UV–Vis
Spectroelectrochemistry
2.5 Gas
Chromatography
Romana Sokolová and Ilaria Degano
rately prepared, containing 0.04 M H 3 PO 4 , CH 3 COOH,
H 3 BO 3 ) and 0.2 M NaOH.
4. Ethanol (96%) for preparation of aqueous ethanolic solutions of
less soluble drugs (40% v/v).
1. Working electrode: Glassy carbon or platinum electrode of
diameter 0.7–2 mm.
2. Ag/AgCl/1 M KCl reference electrode separated from examined solution by a salt bridge.
3. Auxiliary electrode: Pt net.
4. The electrochemical cell with an inlet and outlet for argon or
nitrogen: In case of ethanolic solutions, argon is first bubbled
through the reservoir of ethanol to prevent the evaporation of
ethanol from the examined solution.
1. The electrolytic cell with separated anodic and cathodic parts
and inlet/outlet of inert gas: In case of ethanolic solution,
argon is first bubbled through the reservoir of ethanol to prevent the evaporation of ethanol from examined solution.
2. Working electrode: Glassy carbon or platinum electrode with a
large surface.
3. Ag/AgCl/1 M KCl reference electrode separated from solution by a salt bridge.
4. Auxiliary electrode: Carbon electrode present in the cathodic
compartment of the electrolytic cell (when oxidative generation
of products is measured).
1. Optically transparent spectroelectrochemical cell (more details
available in [20]).
2. 0.5–1 mL Hamilton syringe with needle.
3. Tetrabutylammonium hexafluorophosphate in acetonitrile used
as supporting electrolyte for electrochemical cleaning of the
cell.
1. GC-MS parameters: Separation on a DB-5MS chemically
bonded fused silica capillary column with stationary phase 5%
phenyl-95% methylpolysiloxane, and of dimensions 0.25 mm
i.d., 0.1 μm film thickness, 25 m and 30 m length. Gas chromatographic conditions as follows: initial temperature 57 °C,
2 min isothermal, then ramped at 10 °C/min up to 200 °C,
3 min isothermal, then ramped at 20 °C/min up to 300 °C,
and then isothermal for 20 min. Carrier gas He (purity
99.9995%), at a constant flow rate of 1.2 mL/min. Injection
volume 2 μL, splitless mode at 280 °C. Mass spectrometric
acquisition on a single quadrupole, electronic impact ionization
2.2 Cyclic
Voltammetry
2.3 Electrolysis
2.4 UV–Vis
Spectroelectrochemistry
2.5 Gas
Chromatography
Romana Sokolová and Ilaria Degano