Work technique
Work technique
Laboratories
Handling volatile or air-sensitive compounds, which are often used and synthesized in our group, requires vacuum techniques. Therefore every workplace is provided with a high-vacuum equipment.
Vacuum lines
The vacuum lines were manufactured in the glass factory. Young valves seal the system. The pressure is measured with devices with a combined Pirani and Piezo sensor. A two-stage rotary vane pump provides the required vacuum of min. 5 · 10-4 mbar. As the individual partial volumes are known, the molar amount of the desired substance can be calculated by means of the ideal gas law. This enables a stoichiometric work with highly volatile liquids and even gases.
Working with elemental fluorine
Anhydrous hydrogen fluoride and elemental fluorine are handled with a stainless steel vacuum line. HF and F2 can be used stoichiometrically, furthermore a nitrogen supply is installed.
- HF gas bottle
- fluorine-resistant manometer (monel)
- U-trap filled with soda lime
- Selfmade cooling trap from PTFE tubing (polytetrafluoroethylene)
- Fluorine gas bottle containing a fluorine/helium mixture with 5 % fluorine
- 100 % fluorine from the adjacent fume hood
- Circulation pump for gas phase reactions
- Stainless steel valve
Routine measurements
The majority of the NMR spectroscopic measurements is performed on a Bruker Avance III 300 NMR spectrometer with autosampler. Manual measurements are also possible. For IR measurements a Bruker Alpha FT-IR with an ATR unit and different gas cells, including a fluorine-resistant cell with AgCl windows, is available.
