Distillation

(short description of the project + goals)

  • Lab stand cart for distillation setup

    I want to build some sort of cart, or something with wheels to put all my distillation things on so I can easily roll it out of the way. It should permanently hold my big lab stand to hold the biomass vial, and under that I would like it to house a 10L jerrycan and a smaller lab stand to hold the heated mantle and boiling flask. Also, somewhere to put the controller/power for the cooling loop pump. Something like this, with caster wheels under the corners:

    I want to make it out of leftover pieces of wood. I would need:

    • 4x 44x44x400mm horizontal
    • 4x 44x44x338mm vertical
    • 2x 69x44x362mm horizontal, at the bottom
    • 2x ~12x150x412mm sides
    • 1x 12x312x450 bottom
    • 1x 12×150+x450 backplate

    I can get all of that out of scraps, yay! Let’s get building!

    Edit: done! I don’t remember the last time I went from conceptualisation to finishing a project in one afternoon. It’s nice to finish something for a change.

    Next up: figuring out all the connections on my random collection of glassware that I want to build a distillation setup from.

  • Essential oil distillation

    Another thinking-out-loud post.

    I have inherited a 500mL round bottom flask and heating mantle from my lab. I’m trying to see what I would need to make it into an essential oil still.

    Option 1a: simple distillation, 250 mL capacity – 29/32

    Option 1 is the cheapest

    • Round bottom flask 500 mL 29/32 €0
    • Elbow 75 degrees 29/32 €8.34
    • 14/32 stopper €0
    • Jacketed straight condenser 200 mm 29/32 €16.85
    • Receiving adapter 29/32 €8.60
    • Separatory funnel 250 mL €13.18

    Total: €46.97

    Option 1b: simple distillation, 250 mL capacity – 24/29

    Same but 1 size down

    • Round bottom flask 500 mL 29/32 €0
    • Elbow 75 degrees 29/32m to 24/29m €8.14
    • 14/32 stopper €0
    • Jacketed straight condenser 200 mm 24/29 €6.86
    • Receiving adapter 24/29 €8.87
    • Separatory funnel 250 mL €13.18

    Total: €37.05

    Option 1c: simple distillation, 250 mL capacity – 19/26

    Same but 2 sizes down again, needs adapter

    • Round bottom flask 500 mL 29/32 €0
    • Adapter 29/32m – 19/26f €6.80
    • Elbow 75 degrees 29/32 €6.45
    • 14/32 stopper €0
    • Jacketed straight condenser 200 mm 19/26 €12.67
    • Receiving adapter 19/26 €8.60
    • Separatory funnel 250 mL €13.18

    Total: €47.40

    Option 2a: reflux distillation, 250 mL capacity – 29/32

    This one is the most simple option; a reflux separator with a condenser, straight onto the flask.

    • Round bottom flask 500 mL 29/32 €0
    • Reflux separator 29/32 €28.99
    • Jacketed Dimroth condenser 300 mm E.L. 29/32 €30.36

    Total:

    Option 2b: reflux distillation, 250 mL capacity – 24/29

    Same as before but reduced to 24/29, i.e. thinner separator & column

    Total: €56.60 (200 mm) / €65.67 (300 mm) / €67.76 (400 mm)

    Option 2c: reflux distillation, 250 mL capacity – 19/26

    Same as before but reduced to 19/26, i.e. thinner separator & column

    • Round bottom flask 500 mL 29/32 €0
    • Adapter 29/32m – 19/26f €6.70
    • Reflux separator 19/26 €29.61
    • Jacketed Dimroth condenser 300 mm 19/26 €30.42

    Total: €66.73

    Option 3a: reflux steam distillation, 500-2000 mL capacity – 24/29

    This one is the maximum I can do with my 500 mL heating mantle, although I could possibly fit a 2L chromatography flask too. Reduced to 24/29 better to keep 29/32 for easier filling/emptying? Reduce reflux separator and Dimroth condenser?

    • Round bottom flask 500 mL 24/29 €12.86
    • Some sort of reservoir
      • 500 mL round 24/29 €19.63
      • 1000 mL round 24/29 €27.78
      • 2000 mL round 24/29 €41.14
      • 500 mL globe separator €18.11
      • 1000 mL globe separator €26.66
      • 500 mL globe separator 29/32 €21.51
      • 500 mL straight column separator 24/29 €25.61
      • 500 mL straight column separator 29/32 €29.40
      • ~500 mL straight column 24/? (50×300 mm) €32.59
      • ~1000 mL straight column 24/? (70×300 mm) €41.00
      • Wait a minute, I have an awesome big ~1.8L glass reservoir that is the perfect shape! It’s just missing the DN100? lid. The lid on its own is more expensive than all the other options though. Maybe use a temperature resistant funnel? Print a PETG lid and line it with PTFE baking sheet?
    • Reflux separator 24/29 €27.92 €32.90
    • Jacketed Dimroth condenser 300 mm 24/29 €29.43

    Total:

    Option 3b: as above, but I’ve put more thought into it

    Putting a stopcock between the boiling flask and the reservoir is a bad idea. It’ll clog up with plant material. Also, I want the biggest diameter reservoir opening possible, to make it easier to fill/empty/clean.

    • Round bottom flask 500 mL 29/32 €0
    • Reservoir
    • 29/32 option (€68.05)
      • Clevenger apparatus 5mL 29/32 €37.76 don’t trust
      • Jacketed Dimroth condenser 300 mm E.L. 29/32 €30.29
    • 24/29 option (€69.60)
      • Adapter M29/32 F24/29 €7.33
      • Clevenger apparatus 5mL 24/29 €32.90
      • Jacketed Dimroth condenser 300 mm E.L. 24/29 €29.37
    • 24/29 option with thermometer adapter (€80.86)
      • Y adapter M29/32 2*F24/29 €14.80
      • Thermometer adapter 24/40 €3.79 (probably fits)
      • Clevenger apparatus 5mL 24/29 €32.90
      • Jacketed Dimroth condenser 300 mm E.L. 24/29 €29.37

    Things to figure out

    • Can a Clevenger device even be used with steam distillation (refluxing through the biomass flask)?
      • Yes, e.g. 1 2 3
    • How on earth am I going to clamp such a tall installation
    • Do I want to use my jacketed column? Perhaps upside down, but how would I connect the little screw adapter into the 24/29 Clevenger? Maybe just get the cheaper shorter 200 mm Dimroth for €21.27?
    • Could I perhaps use my condenser as part of a DIY Clevenger? It has an extra port at the bottom. Would need to improvise a stopcock at the spout. This would make for a much less tall setup; it would sit next to the boiling flask / biomass vessel stack, with hydrosol overflow going up diagonally back into the boiling flask or biomass flask. Would need some sort of splitter adapter there, a hydrosol hose, a lid for my reactor (biomass) vessel, possibly an insulated metal pipe from the vessel to the condenser.. Maybe if I want a big volume, I should just hook up the Clevenger & Dimroth to a pressure cooker or other metal pot.
    • Do I need to put some sort of restriction at the top of the Dimroth condenser to limit flow/vapor loss?
    • Would a Vigreux column do something? I’m already refluxing

    Option 3c

    Ok I’ve decided I want the 5mL graduated 24/29 Clevenger and a Dimroth on top of it, but I think I can get away with a shorter 200mm one because of the low heating power and high efficiency of the condenser. I can ramp up the coolant pump if needed, or just add another condenser on top if it turns out to be too short.

    Total: €109.80 (dual with stopper) or €107.37 (single, no stopper)

    Option 3d

    What would a 2L biomass flask cost?

    Total: €126.56

    Option 3e

    What about the one with a bigger mouth?

    • Round bottom flask 500 mL 24/29 €12.84
    • Biomass flask: 2000 mL round 50/40 & 24/40 €49.24
    • Adapter M50/40 F24/29 €14.45
    • Clevenger apparatus 5 mL 24/29 €32.90
    • Dimroth condenser 200 mm 24/29 €21.27

    Total: €130.70

    Things to figure out

    • Will my 200W heater provide enough heat for a 2 L biomass flask?
      • 500 g plant material: 1 kW for 4.5 h, 6 kg of water -> 200W can do 100 g?
      • ~1 kWh/kg -> at 4.5 h, 200 W can do ~1 kg?
      • ~1.9 kWh/kg -> at 4.5 h, 200 W can do ~500 g?
      • 0.3-4.0 kWh/kg, best results at 1.2-4.0 kWh/kg -> at 4.5 h, 200 W can do ~250-750 g?
      • 250 g per liter biomass
      • Ergo, 200W might just keep up with 500 g / 2 L flask? Otherwise, just run for longer?
    • Will my 500 mL boiling flask provide enough water for the process?
      • Fill to max 50%
      • Water is refluxed
      • 2.8 L/kg -> water must be refluxed at least 6 times
      • If not enough, just add through condenser? And pre-wet biomass?
    • Do I want to spend the extra €20 on a flask twice the size?
    • Do I want to spend €100+ on new glassware when I already have used stuff? It might be toxic and I’d have to figure out connections, especially both sides of the 1.8L reactor that has no lid.. The condenser I could probably figure out now that I know the screw connections. I still want a Clevenger in any case.
    • Microwave assisted extraction or microwave pretreatment

    What I have bought

    I’ve bought a Clevenger (5mL graduated, 24/29 connections).

    I’ll try to connect everything I already have up first. But none of those things are made to connect. There are 4 places that I’d like to be mostly “steam tight”:

    • 500 mL round bottom flask to biomass flask: 29/32 ground glass to glass hose connection. Maybe drill out a rubber stopper?
    • Biomass flask to biomass flask lid: custom clamp? Or maybe make a new lid from stainless steel or old pot lid?
    • Biomass flask lid to Clevenger: GL25 (or was it GL32?) screw connection to 24/29 ground glass – maybe a 24/29 to hose adapter, and then stick it in a screw cap with teflon ring?
    • Clevenger to condenser: put the glass hose connection of the condenser into a drilled out 24/29 rubber stopper again?

    To be continued.

  • Idea: extracting volatile oils

    I’ve saved some lab ware and equipment from the dumpster. I wonder if I can use some of it to make a distillation setup for essential oils.

    Some things I want to try extracting oil from:

    • Banana peel
    • Mandarine peel
    • Ginger
    • Cherry tree petals
    • Rhododendron petals
    • Monarda didyma
    • Mentha aquatica
    • Pine/fir/spruce needles
    • Green walnut peel

    I could start with putting the material straight into my 500mL round bottom flask, which is incidentally the largest still size I can use legally. However it would only fit about 250mL, so adding a biomass chamber with it would be very nice. It would be great if I could somehow use my ~1.8L reactor, it is the perfect shape, however it is missing a lid. I think my jacketed chromatography column could make a decent condenser. However none of them have matching glass fittings..

    Thinking of buying a oil/hydrosol separator, or a Clevenger apparatus, to separate and reintroduce the hydrosol to the boiling flask.

    Lots of things to figure out still.