We ran our first short path distillation with a vacuum pump, cold trap, recirculating chiller, and heating mantle on CO2 extracted material. Chiller set to 50C and heating mantle 60C. Slowly increased temp and first saw reaction in the head around 130C, didn’t see the golden main body until 245C. When the main body started to flow Does this temperature seem too high for the main body? Open any suggestions, your procedure with temps, anything will help. Thanks!
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Definitely need deeper vacuum
It looks like you have a vacuum problem. This could be your pump or a major leak in your system. Proper distillation the main body will come over at 180-200C from my experience. The deeper the vacuum and you can get the boiling point even lower.
Can you send a picture of your set up? Do have have anything to monitor your vacuum levels? Are you using the appropriate vacuum grease on all joints? This would help troubleshoot your issues.
Could be a leak issue too. If they are not using the proper grease, the boiling flask the thermometer and distillation head joints are two easy/common sources of vacuum leak. If they are reaching 245C regular silicone vacuum grease will not hold. A higher CFM or deeper vacuum pump could help overcome the leak and appear to fix the issue but double checking the connections is where I would start.
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