Chemical distillation system with in situ analytics
An automated distillation system includes a distillation process under vacuum, a sampling device for extracting a vapor sample of distillate, a gas analyzer for measuring a property of the vapor sample, and a controller for analyzing the property and appropriately adjusting one or more parameters of the system, such as a level of vacuum, in response to the analysis.
1 . A distillation system comprising:
a feedstock supply comprising a feedstock liquid including a volatile compound;
an evaporator in fluid communication with the feedstock supply, the evaporator comprising a sample port and configured to vaporize the volatile compound;
a condenser in fluid communication with the evaporator, the condenser configured to condense the vaporized volatile compound into a distillate;
a vacuum pump configured to reduce a pressure within the evaporator to less than 750 torr;
a sampling device in fluid communication with the sample port of the evaporator and configured to withdraw a sample of the vaporized volatile compound, the sampling device comprising a gas analyzer configured to measure a property of the sample; and
a controller in communication with the gas analyzer and configured to analyze the property of the sample and adjust a parameter of the system in response to the analysis of the property:
wherein the sampling device further comprises:
a sample loop comprising an outlet in fluid communication with the gas analyzer and an inlet in fluid communication with the sample port of the evaporator;
a second vacuum pump in fluid communication with the sample loop via a vacuum valve and configured to produce a pressure within the sample loop that is equal to or less than the pressure within the evaporator;
a carrier gas port configured to introduce a carrier gas into the sample loop;
an internal standard port configured to introduce an internal standard gas into the sample loop; and
a plurality of valves; and
wherein the sampling device is configured to operate in a collection mode wherein, via the plurality of the valves, the second vacuum pump, the inlet of the sample loop, and the internal standard port are isolated from the outlet and the carrier gas port is not isolated from the outlet.
2 . The system of claim 1 , wherein the gas analyzer is a gas chromatograph.
3 . The system of claim 1 , wherein the volatile compound comprises cannabinoids.
4 . The system of claim 1 , wherein the parameter is a pressure within the evaporator and the controller is configured to modulate operation of the vacuum pump.
5 . The system of claim 4 , wherein the controller is further configured to independently adjust a second parameter of the system in response to the analysis of the property.
6 . The system of claim 5 , wherein the second parameter is a temperature of the feedstock supply, a supply rate of the volatile compound from the feedstock supply, a temperature of the evaporator, or a temperature of the condenser.
7 . The system of claim 1 , wherein the evaporator is a wiped film evaporator.
8 . The system of claim 7 , wherein the parameter is a wiper rotational speed of the wiped film evaporator.
9 . The system of claim 1 , wherein the parameter is a temperature, pressure, or flow rate within the sampling device.
10 . The system of claim 1 , wherein the sampling device further comprises a heater configured to prevent condensation of the vaporized volatile compound.
11 . The system of claim 10 , wherein the parameter is a temperature within the sampling device and the controller is configured to modulate operation of the heater.
12 . The system of claim 1 , wherein the parameter is a pressure within the sampling device and the controller is configured to modulate operation of the second vacuum pump.
13 . The system of claim 1 , wherein the plurality of valves comprises:
an inlet valve at the inlet of the sample loop;
a vacuum valve between the second vacuum pump and the sample loop; and
a first internal valve, a second internal valve, a third internal valve, and a fourth internal valve each positioned within the sample loop;
wherein, in the collection mode
the inlet valve and the vacuum valve are in an open position and the first internal valve and the second internal valve are in a closed position to draw the sample into a portion of the sample loop that is isolated from the internal standard port, the carrier gas port, and the outlet;
the third internal valve is in a closed position to isolate the internal standard port from the carrier gas port and the outlet; and
the fourth internal valve is in an open position between the carrier gas port and the outlet; and
wherein the sampling device is further configured to operate in an analysis mode wherein
the inlet valve, the vacuum valve, and the fourth internal valve are in an closed position; and
the first internal valve, the second internal valve, and the third internal valve are in an open position to allow the carrier gas and the internal standard gas to mix with the sample and flow to the outlet.