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RogueRose
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[*] posted on 7-6-2016 at 12:13
SIMPLE Distillation setup with parts on-hand


All that was available was a 1L Erlynmyer flask and a 12" Liebig condenser. An aquarium pump was aquired to cool the condenser and used an old metal stand (like a music stand) to hold up the apparatus.

So, how to get a distillation unit out of this? Take the outer case of a 35ml syringe (the hard plastic case that the syringe comes in). The wide part of the neck, near the end of the plunger fit PERFECTLY inside the neck of the flask!!!

1/2" OD, 3/8" ID vinyl tubing (food grade) was used to connect the syringe case to the condenser. To ensure it stuck together RTV silicone was added as a "bung/stopper" at the flare of the syringe case to make a seal and keep it from falling down if it could even happen.

A hole was drilled in the needle end (no needle here though) of the syringe case to put the tubing through. A bulb of RTV silicone was applied to the end of the 1/2" tubing (heated with hot air gun to speed sealing outer layer) then pulled up through the syringe case from the inside and then filled the rest with RTV to keep it from moving. Used long screwdriver to ensure tubing was clear of silicone.

On the outside of the syringe case, 3 layers of RTV to stick/glue the tubing to the syringe casing ensuing there is no leaking from the vapors.

After each use of RTV a 1500 watt heat gun was used to seal the outer layer so it wasn't sticky. This takes about 30 seconds. Be careful to continually rotate/move so it doesn't melt the syringe case.

The vinyl tubing terminated inside the condenser with a perfect fit and used double wide electrical tape first wrapped around the tubing and then around the condenser (2 wraps) and then back to the tubing for a number of wraps. This has held for a LONG time with NO leaks of failure.

Normal vinyl tubing was used to cool the condenser - no big thing here. MAKE SURE YOU CHECK THE CONNECTION often as they can slide off, especially when the water gets warmer. small pipe clamps will be very helpful.

a 15" lenght of vinyl tubing finished the run from the end of the condenser. Many benefits to this as it can provide extra cooling and can be moved to different containers when possible.

Total expenditure: $2.62 for the tubing & RTV usage - all else was on hand.

Hypothetically. This is able to take alcohol wash of 5% to about 40-50% after one run and after a second run 92-93% was measured!!!



Pleas no rude comments about the adapter to the erlynmyere flask. I know it looks like one of those "male enhancement" vacuum attachments that is leaking from the end:D:o

[Edited on 7-6-2016 by RogueRose]

[Edited on 7-6-2016 by RogueRose]

still.jpg - 439kB

[Edited on 7-6-2016 by RogueRose]
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Firmware21
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[*] posted on 7-6-2016 at 13:40


Well at least you've got a condenser :P. My first "distillation apparatus" was roughly the same, except there was no condenser or stative to hold the whole thing.

I hope there is good ventilation where you work with it, as it looks like a big fire hazard to me. Honestly, I'd be afraid to work with it in my lab.
I might just be a scaredy cat though...

You might want to get the adapter someday, they make your life easier IMO :cool: .
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RogueRose
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[*] posted on 7-6-2016 at 14:16


Quote: Originally posted by Firmware21  
Well at least you've got a condenser :P. My first "distillation apparatus" was roughly the same, except there was no condenser or stative to hold the whole thing.

I hope there is good ventilation where you work with it, as it looks like a big fire hazard to me. Honestly, I'd be afraid to work with it in my lab.
I might just be a scaredy cat though...

You might want to get the adapter someday, they make your life easier IMO :cool: .


Well a lit flame next to the erlynmyer junction and at the end of the condenser hose posed no fire risk. Keeping the condenser at 55F or so and running slow, so very little vapor this way.


What I coulnd't get over was the fact that I could get almost 95% with this cheap setup while my $500 essential oil still can't get past about 50% This is what makes me so mad when people say that they have the best b/c it is most expensive.

Kind of like a $2,000 space pen (writes in zero G) vs a pencil, lol:mad::(:(;):P

[Edited on 7-6-2016 by RogueRose]
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The Volatile Chemist
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[*] posted on 23-6-2016 at 10:52


I was just using a still apparatus with a 500mL sep funnel replacing the thermometer through the top rubber stopper, to make Acetic acid from sodium acetate and sulfuric acid. Didn't work too well, lots of fumes and very little condinsation in my tiny 100mm liebig...



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[*] posted on 8-7-2016 at 18:50


I built this little DIY centrifuge out of an empty spool, some microfuge tubes, nuts and bolts, hot glue, and a rubber band. It's powered by an electric drill - my cordless didn't quite have the muscle to do what I wanted in a timely manner, but my neighbor lent me a higher power drill, which worked :cool:

centrifuge1.jpg - 241kBcentrifuge2.jpg - 200kB




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thumbup.gif posted on 14-7-2016 at 03:15
Making filters from PVC pipe & removable lids on pipes



I needed a way to change the material in my filters made of PVC pipe and the PVC screw-on end pieces were really expensive (comparatively for what I needed), were a little awkward in size and needed Teflon or plumbers tape to ensure seal each time it was opened.

What I did was find some plastic jars and gallon juice containers that had the size mouths (large/wide mouths) that would allow the pipe to fit inside. I then cut the plastic containers threaded neck off and then used an epoxy/resin to glue it to the PVC. I then put whatever attachment/barb onto the container lid & glue/epoxy/JB weld it to the lid. Now I have a water tight removable lid and it can be made if your local hardware store doesn't have the size PVC threaded cap you need (at my store, one 3" cap costs almost as much as 10' of SCH40 pipe!)


As for filters, I like using square cotton swabs over-layed out one on top of the next and so on. Then roll it up in a tight bundle (very tight if you want high filtration) and squish it into the PVC pipe. If you try this you MUST "charge" the cotton with water (or some liquid) before attaching to the holding vessel with the solution to be filtered. It may not be possible to have the liquid penetrate the cotton if you pack it tight enough, but if you soak the cotton (once in the PVC) on both sides of the filter it will help IMMENSELY!

Also, I have needed to attach small diameter tubing to garden hose and it was difficult to find anything that would allow this. This can be great for running a condenser.

Also, if you need an inexpensive ball valve for vinyl tubing I found using one of the garden hose shut-off valves works great all you need to do is get the hose ball valve (the yellow ones below) and either buy the garden hose cap or a 3/4" pvc pipe cap and cut it to fir the valve - then attach the proper hose barb.


*Note all the threaded "necks" are glued with an epoxy and have one on both sides of the pipe
**the picture of the grey PVC filter, it is open-ended and that is fine if you just hang it over the receiving container. If you do this the cotton needs to packed tightly enough to not allow the pressure to push it out (I hang the holding tank 5-12' above receiving vessel. Placing a drywall screw at the bottom - near outlet - works well to keep them all in there.
PVCscrewcap1.jpg - 104kB PVCscrewcap2.jpg - 80kB filtermaterial1.jpg - 45kB filtermaterial2.jpg - 100kB PVCfilter1.jpg - 248kB

pipe end cap1.jpg - 164kB pipe end cap2.jpg - 173kB Hose Attachments.jpg - 154kB
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arkoma
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[*] posted on 14-7-2016 at 16:26


Quote: Originally posted by RogueRose  
All that was available was a 1L Erlynmyer flask and a 12" Liebig condenser. An aquarium pump was aquired to cool the condenser and used an old metal stand (like a music stand) to hold up the apparatus.

So, how to get a distillation unit out of this? Take the outer case of a 35ml syringe (the hard plastic case that the syringe comes in). The wide part of the neck, near the end of the plunger fit PERFECTLY inside the neck of the flask!!!

1/2" OD, 3/8" ID vinyl tubing (food grade) was used to connect the syringe case to the condenser. To ensure it stuck together RTV silicone was added as a "bung/stopper" at the flare of the syringe case to make a seal and keep it from falling down if it could even happen.

A hole was drilled in the needle end (no needle here though) of the syringe case to put the tubing through. A bulb of RTV silicone was applied to the end of the 1/2" tubing (heated with hot air gun to speed sealing outer layer) then pulled up through the syringe case from the inside and then filled the rest with RTV to keep it from moving. Used long screwdriver to ensure tubing was clear of silicone.

On the outside of the syringe case, 3 layers of RTV to stick/glue the tubing to the syringe casing ensuing there is no leaking from the vapors.

After each use of RTV a 1500 watt heat gun was used to seal the outer layer so it wasn't sticky. This takes about 30 seconds. Be careful to continually rotate/move so it doesn't melt the syringe case.

The vinyl tubing terminated inside the condenser with a perfect fit and used double wide electrical tape first wrapped around the tubing and then around the condenser (2 wraps) and then back to the tubing for a number of wraps. This has held for a LONG time with NO leaks of failure.

Normal vinyl tubing was used to cool the condenser - no big thing here. MAKE SURE YOU CHECK THE CONNECTION often as they can slide off, especially when the water gets warmer. small pipe clamps will be very helpful.

a 15" lenght of vinyl tubing finished the run from the end of the condenser. Many benefits to this as it can provide extra cooling and can be moved to different containers when possible.

Total expenditure: $2.62 for the tubing & RTV usage - all else was on hand.

Hypothetically. This is able to take alcohol wash of 5% to about 40-50% after one run and after a second run 92-93% was measured!!!



Pleas no rude comments about the adapter to the erlynmyere flask. I know it looks like one of those "male enhancement" vacuum attachments that is leaking from the end:D:o

[Edited on 7-6-2016 by RogueRose]

[Edited on 7-6-2016 by RogueRose]



[Edited on 7-6-2016 by RogueRose]



Good Job!!




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[*] posted on 3-8-2016 at 16:27


My woodworking skills fall somewhere below "carpenter's apprentice", but I managed to finish and mount the shelves shown in the attached pictures. The short shelf on the left is 42 inches wide, and the one on the right is 48 inches wide. The shelves and ends are made from "1x4" pine.

Now to stock them with chemicals!:D


IMG_20160712_123952.jpg - 52kBIMG_20160801_143547.jpg - 41kBIMG_20160801_143706.jpg - 59kB
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[*] posted on 15-8-2016 at 13:56


Look nice! Especially with all the bottles on them.



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RogueRose
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[*] posted on 15-8-2016 at 21:52
Filter funnel from a 2L bottle


I used to use the spout of a cut off 2L bottle for holding filter paper (coffee filters) but found that the surface contact of the paper on the plastic restricted the flow significantly basically only allowing the small bottom opening as the sole area which liquid could flow out of.

So, I made some cuts to open up the sides and was going to cut the "vents" off when I realized that they could be used to hold the filter over the receiving vessel.



filterholder1.jpg - 149kB filterholder2.jpg - 88kB
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thumbup.gif posted on 16-8-2016 at 16:09


Isn't serendipity wonderful!:D

I forgot to add, that's clever, but I'm not sure the contact of filter paper with the "funnel" slows things down, at least for solvents that "wet" the "funnel". I need to try this.


[Edited on 8-17-2016 by CharlieA]
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[*] posted on 17-1-2017 at 12:26


Fractional distillation under (slowly fluctuating) vacuum with 2 pieces of glass. Homemade aspirator station next on the list.

Works a treat though...................



DSCN0013.JPG - 2.6MB

Comments and criticisms welcome.

If anyone wants a list of parts l will gladly post it.................

/CJ

[Edited on 17-1-2017 by Corrosive Joeseph]




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[*] posted on 18-1-2017 at 01:41


All I did was take a bit of 24 glass, it was a thermometer adapter I got far a couple of dollars but I took a file around the join and snapped it off. Next I put a Büchner funnel down the hole full of clear epoxy and there. No more need for a rubber gooch. Just a little vacuum grease and it works great. Kind of re- purposed I guess.

IMG_1109.JPG - 1.2MBIMG_1108.JPG - 1.4MB




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[*] posted on 18-1-2017 at 02:23


That IS a neat idea that I may copy,
have you tried hot water etc. yet?
I would be a little concerrned about differential thermal expansion
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