1L Standard Distillation Turnkey Setup
The Standard Distillation Turnkey Setup includes all the components necessary to successfully perform distillation at an entry level price point. Crossbar pictured is not included. We recommend purchasing multiple lab stands to accommodate your specific needs.
The Standard Turnkey Setup Includes:
- 1L Distillation Kit
- 1/4" FJIC x 1/4" Barb Adapter
- Poly science 7L MX Heated Circulator
- Best Value Vacs VE280 9CFM Two Stage Vacuum Pump
Distillation Quick Start Guide
This guide gives basic quick start instructions for distillation systems. It is intended to provide a starting point for learning the process. Parameters should be adjusted to suit specific needs,
Before beginning distillation, ensure the following steps have been taken:
- Vacuum Pump is in good working order. Pump should be run against dry load to allow internals to warm up. Oil should be clear. Cloudy or dark oil should be changed.
- All glass components are in good working order and ready to be assembled
- A winterization and degassing procedure has been done to prepare oil for distillation
Once all three of these steps have been completed, you are ready to begin distilling.
- Begin by placing stir bar in boiling flask and then load your material. This should be done using a funnel. A small amount of alcohol in the oil will give it a thinner consistency making it easier to transfer.
- Assemble all glassware and ensure each joint is properly greased. Do not use too much, as the vacuum pressure might pull some grease into the system. To ensure a full seal, spread grease in a circular motion by rotating glassware
- Attach circulator to condenser and set temperature to 50C. Allow circulator to reach temperature before beginning distillation.
- Connect vacuum pump to manifold. The manifold will allow you to isolate each individual component as well as let atmosphere into and out of the system.
- Connect receiving cow to cold trap.
- Connect cold trap to manifold.
- Connect vacuum gauge to manifold.
- At this point, ensure all connections are correct. Also ensure receiving cow is positioned to collect the first fraction in the far-left receiving flask. Circulator should be at its set temperature. Turn on vacuum pump to begin process.
- Turn on heat and set to 60C. Vacuum pump will begin to pull down and temperature will begin to rise. Watch the gauge to monitor vacuum pressure and stability.
- Start stir slower and increase speed with temperature.
- Once you are close to 60C, increase the temperature 20 degrees. Continue to raise the heat incrementally in 20-degree steps, increasing the set temperature as you near your set point. Increase temperatures incrementally until you reach 220C.
- You will see your first fraction somewhere between 180C and 190C or slightly before. This is the “heads” fraction.
- You will move to your second fraction when you see an increased reaction in the head, a slight color change toward golden, as well as a thickening of distillate. When this fraction hits, allow the distillate to “self-clean” the head for a minute or two then, rotate the cow to the middle receiving flask. Collect your “main body” fraction. You will see temps between 190-220C during this fraction.
- Continue to increase stirring speed as necessary. Reaction in the head may vary but it should never stop. As fluid level in the boiling flask decreases, increase stir speed.
- The final “tails” fraction is a mixture of the first and second fractions and should be saved for re-distillation later. Ideally, you want to turn the cow to the final flask before the tails fraction hits. The “tails” fraction has an obvious color change and will be darker than the “main body” fraction. You will see temps between 200-250C during this fraction.
- As fluid level in the boiling flask decreases even more, set stirring RPM higher (1000+ RPM). You may need to compensate with a bit more heat to finish of the final fraction as well.
- Once process is complete, stop heat, stop stir, and stop vacuum. Let atmosphere into the system. Be sure to properly store your distillate as exposure to air and light can cause oxidation.
Note: All units are inspected for broken glass or parts before unit is shipped. If unit arrives damaged or glass is broken (this does not include minor imperfections or scuffs in glassware), Customer MUST contact LeDAB within 3 days of delivery to file a claim and receive a replacement part. If customer DOES NOT contact LeDAB within 3 days of delivery responsibility for replacement parts falls on the customer and they must pay for replacement pieces.
Glassware Safety Disclaimer: LeDAB is not responsible for failure of glassware which must be inspected before and after every use because it may eventually develop imperfections or damage through normal usage, mishandling, and stress caused by temperature variations. If an imperfection or damage is noted while inspecting the glassware DO NOT use the glassware because it can fail causing bodily harm or damage to the surrounding area. (30 Day Limited Warranty: after this time period, any warranty issues must be resolved with the end supplier).
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