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General Short Path Distillation Guide

This guide provides general operational guidance for setting up, leak-testing, and running a short path distillation system. It includes recommended temperature ranges, fraction collection points, vacuum expectations, decarb notes, and vacuum pump maintenance instructions.

Link to General Short Path Distillation Guide and Info

Quick Facts

  • Process Type: General short path guidance (not a formal SOP)
  • Acceptable Vacuum for Leak Test: Below 250 microns
  • Initial Vacuum During Production Run: 500–1200 microns
  • Boiling Flask Fill Limit: 60%
  • Key Temperature Ranges:
    • DFY heater/chiller: 30–40°C
    • Mantle start: 60–70°C
    • Decarb: ~120°C
    • Body fraction: 170–200°C
  • Stirring Range: 100–500 RPM

Safety Disclaimer

  • This guide is not a standard operating procedure. Care and common sense should be used in the operating of any laboratory equipment. USA Lab is not responsible for any damages, injury or loss.

Setup Instructions

  1. Unpack all parts and inspect glass; cross-check with packing list.
  2. If any glass is broken, cracked, or missing, contact USA Lab.
  3. Clean all glass before installation and use.
  4. Lightly grease all ground glass joints with vacuum grease—excess grease can contaminate product.
  5. Vacuum leak test the system before adding product.
    1. Below 250 microns = pass.
  6. To locate leaks:
    1. Use spray bottle with ethanol.
    2. Spray each potential leak point individually.
    3. If gauge remains stable → no leak.
    4. If reading rapidly increases then decreases → leak found.
  7. Inspect leak: cracked glass, bad gaskets, loose connections, missing hose clamps.
  8. Spray again to verify fix.
  9. Once system holds vacuum below 250 microns, perform a test run with ethanol or water to ensure heating and stirring work correctly.

Production Run Instructions

Before You Begin
  • Material must be winterized; all lipids removed.
  • Fill cold trap with dry ice and alcohol.
  • Fill boiling flask no more than 60%.
Start-Up
  1. Turn on vacuum pump.
  2. Verify no leaks.
    1. 500–1200 microns is acceptable at this stage.
  3. DFY heater/chiller: 30–40°C.
  4. Heating mantle: 60–70°C.
  5. Stirring: 100–500 RPM.

Decarboxylation Notes (During Short Path)

  • Short path can be used to decarboxylate near 120°C.
  • Decarb can cause bumping; perform slowly and carefully.
  • No solvent should be present above 100°C.

Distillation Temperatures & Fractions

  • Increase mantle temperature in increments:
    • 5°C increments below 170°C
    • 2°C increments above 170°C
  • Head fraction: 120–150°C
  • Body: 170–200°C
  • Tail: 200–220°C
  • Head probe should read ~10°C cooler than mantle setting.
  • Rotate the cow (three-ball glass section) for each fraction.
Condenser Adjustment
  • Some operators increase DFY heater/chiller temperature to 70–90°C once fractions begin.
Stirring Adjustment
  • May need to increase stirring speed as solution volume decreases.

Shutdown Procedure

  1. Set mantle to 100°C when finished.
  2. Allow mantle to cool with stirrer on.
  3. Open gas ballast to I or II until mantle temp drops below 170°C.
  4. Once below 170°C:
    1. Shut off vacuum
    2. Close gas ballast

Vacuum Maintenance Instructions

Vacuum oil must be emptied, flushed, and replaced after every run.

Oil Change Procedure
  1. Drain pump.
  2. Close drain.
  3. Run pump without oil for 5–10 seconds.
  4. Drain pump again.
  5. Close drain.
  6. Add flushing fluid (FF-10).
  7. Run pump 30 minutes with KF-25 adapter on Bullseye vacuum gauge.
  8. Record vacuum level achieved.
  9. Repeat from step 1 until pump reaches similar pressure to a new factory unit.
  10. Repeat steps 1–5 but fill with Inland 19 instead of FF-10.
  11. Check ultimate pressure again before the pump is ready for use.

ZNCL Mantle Optimized Settings (Simplified Format)

To enter the settings menu:

  • Hold Heat + for 5 seconds to enter LC (menu selection).
  • Press Heat to move to the next parameter.
  • Hold Heat for 5 seconds to save changes.
  • Note: The display symbol for “T” looks like a lowercase r on the screen.

Menu 1 — LC: 3
  • T: 3
  • P: 5.0
  • I: 5
  • D: 3

Menu 2 — LC: 9
  • doT: 1
  • nP: 60

Menu 3 — LC: 103
  • Pd: 30
  • InT: 20
  • SdL: 60
  • db: 40

Contact & Support

For help with short path systems, mantles, or vacuum pumps:

📞 734-855-4890
📧 support@usalabequipment.com