Gc 7890a ms 5975

The shadow-dried powder of the two samples (120 gm of root and 150 gm of flower) was exposed to hydro-distillation for 4 h by a Clevenger device. The obtained oil was again dried with anhydrous sodium sulfate and then later kept at 4°C.
GC-MS was carried out by Agilent GC (7890A)/MS (5975) with a capillary column, He gas carrier with a flow rate of 1.5 ml/min, flame ionization detector, and a split ratio of 1:25. The temperature was set at 50 °C for the column for 1 min and then for 265 °C for the heating purpose at the rate of 2.5°C/min, then stored at 265 °C for 20min. detector temp at 300 °C, injector temp at 265 °C flow of Helium at 35 ml/min with the airflow rate of 400 ml/min. The MS set off at 70 eV ionization energy. Retention times have been recorded and calculated by utilizing the n-alkanes retention times which have been injected in the same condition after the oil (www.agilent.com). The final found chemical compounds were reported by the “Agilent’s ChemStation Integrator” algorithm (www.agilent.com).

High-pressure catalytic tests were performed in a fixed-bed plug-flow reactor consisting of a quartz tubule (Φ_inner=7 mm) inserted into a stainless steel housing. A condenser along with a gas–liquid separator was mounted at the reactor outlet. Typically, 1.3 g of oxalate was diluted with up to 2 g of SiC to achieve isothermal plug-flow conditions followed by in situ TPDec in H₂ at 0.1 MPa (30 ml min⁻¹) and 370 °C for 1 h (after oxalate decomposition, the amount of activated catalyst is ∼0.5 g). The reactor was subsequently cooled to a temperature below 100 °C in flowing hydrogen before adding CO so as to produce a syngas feed with the desired H₂/CO ratio. Metal carbonyls (mainly, Ni(CO)₄) were removed by passing the CO feed through a zeolite 4A trap at high temperature before introduction into the reactor. Typical flow rates were H₂/CO=24/16 ml min⁻¹ providing a GHSV=3,600 h⁻¹ (gas hourly space velocity). After pressurizing the system to 40 bar, the temperature was raised using low heating rates of 1 °C min⁻¹ up to 200 °C and kept overnight under these conditions. Catalytic activities and product selectivities were determined after stabilization for at least 12 h. The CO conversion and product selectivities were measured by online GC–MS (Agilent 7890A GC/5975 MS).