First, the rotary evaporimeter temperature control setting basis
Rotary evaporator is a commonly used laboratory equipment, mainly used for heat-sensitive substances evaporation, concentration, separation and other operations. In the use of rotary evaporimeter, temperature control is very critical. Generally speaking, the temperature setting of rotary evaporator should be considered according to the following aspects:
1. operation requirements: different experimental operations have different temperature requirements, such as liquid chromatography needs to be heated to a certain temperature for analysis.
2. sample characteristics: different samples of boiling point and evaporation temperature is different, need to set the temperature according to the actual situation.
3. equipment performance: rotary evaporator heater performance is different, some may not be able to reach high temperature, need to be measured in specific experiments.
4. safety considerations: rotary evaporator temperature is too high may be dangerous, need to set safety measures.
Second, the common rotary evaporimeter temperature control method
1. manual adjustment method: manual control of the temperature of the heater, need to regularly check whether the temperature is stable, the number of adjustments is also relatively large, not suitable for precise control.
2. PID control method: the use of PID controller to control the temperature, can be adjusted according to the real-time feedback information on the size of the heater's power, so that the temperature is more accurate.
3. program control method: by writing program, preset temperature curve, using automatic control to maintain temperature stability.
Third, rotary evaporator temperature control precautions
1, for volatile, flammable, explosive and other samples need to take special temperature control, and in the operation process to strengthen the monitoring, to ensure the safety of operation. 2, when the temperature control is high, the temperature control of the rotary evaporator should be more accurate.
2. When the temperature control is high, attention should be paid to the impact of air on the heater, ventilation conditions should be enhanced accordingly to prevent damage to the heater. 3.
3. as far as possible to use stainless steel material heater, avoid the use of easy to rust materials, to avoid the later use of the process of material contamination.
In summary, when using rotary evaporator, the correct temperature control is very important. By choosing the correct setting basis, using the appropriate temperature control method, as well as paying attention to operational safety and material selection and other issues, can ensure the experimental effect and operational safety of rotary evaporimeter.
Accurately controlling the temperature of the rotary evaporator during experimental operations is critical to ensuring the success of the experiment and obtaining high quality fractions. Here are some methods and steps to control the temperature of the rotary evaporator:
Select a suitable heating source:
Choose a suitable water or oil bath according to the boiling point of the solvent and the desired temperature.
A water bath is suitable for lower temperature heating while an oil bath is suitable for higher temperature heating.
Calibrate the temperature control system:
Ensure that the temperature control system (e.g., thermometer or thermocouple) of the rotary evaporator has been calibrated and is giving accurate readings.
Check and calibrate the temperature control system periodically to ensure its accuracy.
Use a temperature controller:
Use a temperature controller to regulate the power of the heating source to maintain a constant temperature.
The temperature controller sets the target temperature and maintains a stable temperature by automatically adjusting the power to the heating source.
Preheating:
Preheat the evaporator bottle and condenser before adding samples to minimize temperature fluctuations.
Gradual temperature increase:
Start with the temperature set slightly below the boiling point of the solvent and gradually ramp up to the desired temperature.
Rapid warming may cause the solution to boil violently, resulting in spillage or loss of fractions.
Monitor and adjust:
Continuously monitor temperature readings during distillation and adjust the temperature of the heating source as needed.
If the temperature exceeds the set point, reduce the temperature of the heating source; if the temperature is too low, increase the temperature as appropriate.
Use temperature gradients:
For heat-sensitive substances, distillation can be performed using a temperature gradient, i.e., using different temperatures at different stages.
Maintain a constant vacuum:
Ensure that the vacuum level is stable during decompression distillation, as changes in the vacuum level can also affect the boiling point of the solvent.
Avoid vigorous stirring:
Excessive stirring may result in uneven solution temperatures and affect the accuracy of temperature control.
Use thermal insulation:
Use heat-insulating materials (e.g., insulation cotton) to wrap the evaporation flask and condenser to reduce heat loss and improve the stability of temperature control.
Through the above measures, the temperature of the rotary evaporator can be effectively controlled, thus improving the accuracy of the experimental operation and the quality of the fractions.
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