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Advice on a distillation kit/setup? Options
 
Uronam.345
#1 Posted : 11/23/2016 5:06:55 PM
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I've become interested in distillation, it looks like a really practical way for obtaining organic solvents that would otherwise be very expensive to obtain, DCM for example.

Ive seen videos online of certain distillations and honestly it looks like fun, ive also read some stuff on safety procedures, IE dont boil anything peroxide as it can BOOM. I would really like a lot more advice on safety, like things that you should do for all distillations, like not leaving the room while you have a solvent boiling or smoking in the vicinity, i know theres more and i would like to here about that. also what things i should avoid seperating even if they're in minute concentrations.

the only things i have interest in distilling would be simple alcohols, ethyl and IPA, as well as getting DCM from paint stripper. Ive also wondered if you could distill the lower carbon chains out of naphtha (pentane, hexane) in a ratio that would equate to pet ether.

Ive only taken one class in chemistry, that was during my senior year. are people without multiple years in chemistry shunned from getting or making distillation kits.

I saw a video where a guy took an old heptane can stabbed some copper tubing through the cap, bent it and swiveled it back on, that seemed kind of... sketch. no thermometer to check temp, also double boiling would be difficult, if your boiling hygroscopic compounds they'd just end up with water in them since its not under vaccuum.

my biggest concern is safety and maintaining my would be equipment.

If anyone could redirect me to a good overall sight that would be wonderful.

Thank you.
 

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benzyme
#2 Posted : 11/24/2016 1:40:14 AM

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scimadness is a good forum for things of that nature. alternatively, many universities have website pages
discussing common apparati used in organic chemistry, just search for organic chemistry lab procedures (distillation).

DCM isn't terribly expensive, as long as it is shipped by ground. it's very volatile (not flammable though).
the distillation app will be useful for recycling the dcm, as you never want to pour it down a drain.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of knowledge at our disposal. The rest is poetry, imagination." -Max Planck
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1ce
#3 Posted : 11/24/2016 11:46:37 PM

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Kubrick's organic lab survival manual is great for beginners learning simple lab techniques.
 
Ulim
#4 Posted : 11/25/2016 12:29:52 PM

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Theres nothing that can go wrong if you take care Smile

Just never ever use open flame heating or exposed heat coil. Also dont heat to much. Some solvents need to be distilled very carefully like ether for example.

Watch some of these videos https://www.youtube.com/user/TheRedNile
There you will get more tips and tricks.

 
entheogenic-gnosis
#5 Posted : 11/25/2016 1:04:55 PM
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in relation to distillation set ups...

You can find fractional distillation set-ups like the one pictured on Amazon for around $100.

-eg
entheogenic-gnosis attached the following image(s):
simpledistillation-1.jpg (24kb) downloaded 148 time(s).
 
benzyme
#6 Posted : 11/25/2016 2:25:06 PM

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I believe that one is a simple distillation app.a fractional distillation app would include a vigreux, oldershaw, spinning band, or other fractionating column, connected between the pot and distilling head. the most common, cost-effective one, is the vigreux.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of knowledge at our disposal. The rest is poetry, imagination." -Max Planck
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entheogenic-gnosis
#7 Posted : 11/25/2016 4:12:26 PM
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benzyme wrote:
I believe that one is a simple distillation app.a fractional distillation app would include a vigreux, oldershaw, spinning band, or other fractionating column, connected between the pot and distilling head. the most common, cost-effective one, is the vigreux.


You're right, my picture did not correspond correctly with the set up I mentioned... I selected the image in haste, and I apologize for the error, thank you for catching that benzyme.

(It was a Liebig condenser for simple distillation)

A Vigreux column or a packed fractioning column is what would be most common for fractional distillation...the only real difference between fractional and simple distillation is that with fractional distillation a fractional column is placed between the boiling flask and the condenser...

A "packed column" is a straight column (an air condenser) packed with stainless steel scouring pad or metal pieces such as Raschig rings (or glass helices/glass tubing sections or glass beads; glass packing material will have slightly better efficiency than steel scouring pad or metal packing material ) a column packed with stainless steel scouring pad (or glass material) is actually more effective as a fractioning column than a Vigreux column, but the margin of difference is fairly minimal...

Introduction to Organic Laboratory Techniques: A Small Scale Approach
By Donald L. Pavia ; page 752 goes into detail in this area, if you are interested in distillation it's actually a great read, very informative.

-eg


 
1ce
#8 Posted : 11/25/2016 11:24:28 PM

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entheogenic-gnosis wrote:
benzyme wrote:
I believe that one is a simple distillation app.a fractional distillation app would include a vigreux, oldershaw, spinning band, or other fractionating column, connected between the pot and distilling head. the most common, cost-effective one, is the vigreux.


You're right, my picture did not correspond correctly with the set up I mentioned... I selected the image in haste, and I apologize for the error, thank you for catching that benzyme.

(It was a Liebig condenser for simple distillation)

A Vigreux column or a packed fractioning column is what would be most common for fractional distillation...the only real difference between fractional and simple distillation is that with fractional distillation a fractional column is placed between the boiling flask and the condenser...

A "packed column" is a straight column (an air condenser) packed with stainless steel scouring pad or metal pieces such as Raschig rings (or glass helices/glass tubing sections or glass beads; glass packing material will have slightly better efficiency than steel scouring pad or metal packing material ) a column packed with stainless steel scouring pad (or glass material) is actually more effective as a fractioning column than a Vigreux column, but the margin of difference is fairly minimal...

Introduction to Organic Laboratory Techniques: A Small Scale Approach
By Donald L. Pavia ; page 752 goes into detail in this area, if you are interested in distillation it's actually a great read, very informative.

-eg




For volatile liquids I like a packed hempel column. Plugged with glass wool and filled with beads. For higher bp liquids I just use a spined vigreux.
 
downwardsfromzero
#9 Posted : 12/5/2016 1:46:39 AM

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Distillation is a great hobby, highly recommended (if you have the sense not to blow yourself up/poison yourself)!

People always snigger when I enthuse about my nicely packed column. For some reason.
Ora, lege, lege, lege, relege et labora

“To be GOVERNED is to be watched, inspected, spied upon, directed, law-driven, numbered, regulated, enrolled, indoctrinated, preached at, controlled, checked, estimated, valued, censured, commanded, by creatures who have neither the right nor the wisdom nor the virtue to do so. To be GOVERNED is to be at every operation, at every transaction noted, registered, counted, taxed, stamped, measured, numbered, assessed, licensed, authorized, admonished, prevented, forbidden, reformed, corrected, punished. It is, under pretext of public utility, and in the name of the general interest, to be place under contribution, drilled, fleeced, exploited, monopolized, extorted from, squeezed, hoaxed, robbed; then, at the slightest resistance, the first word of complaint, to be repressed, fined, vilified, harassed, hunted down, abused, clubbed, disarmed, bound, choked, imprisoned, judged, condemned, shot, deported, sacrificed, sold, betrayed; and to crown all, mocked, ridiculed, derided, outraged, dishonored. That is government; that is its justice; that is its morality."
― Pierre-Joseph Proudhon
 
entheogenic-gnosis
#10 Posted : 12/6/2016 2:32:09 PM
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I'm considering purchasing a LabTech EV311 rotovap.

Found a great deal....

-eg




 
downwardsfromzero
#11 Posted : 12/6/2016 8:48:25 PM

Eggnogstic - warning: Self-irony levels: high!


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Aargh... now I get Rotovap envy!!

Some say purchase of a Rotovap may lead to undesirable LE attention. Hope your story is straight.
Ora, lege, lege, lege, relege et labora

“To be GOVERNED is to be watched, inspected, spied upon, directed, law-driven, numbered, regulated, enrolled, indoctrinated, preached at, controlled, checked, estimated, valued, censured, commanded, by creatures who have neither the right nor the wisdom nor the virtue to do so. To be GOVERNED is to be at every operation, at every transaction noted, registered, counted, taxed, stamped, measured, numbered, assessed, licensed, authorized, admonished, prevented, forbidden, reformed, corrected, punished. It is, under pretext of public utility, and in the name of the general interest, to be place under contribution, drilled, fleeced, exploited, monopolized, extorted from, squeezed, hoaxed, robbed; then, at the slightest resistance, the first word of complaint, to be repressed, fined, vilified, harassed, hunted down, abused, clubbed, disarmed, bound, choked, imprisoned, judged, condemned, shot, deported, sacrificed, sold, betrayed; and to crown all, mocked, ridiculed, derided, outraged, dishonored. That is government; that is its justice; that is its morality."
― Pierre-Joseph Proudhon
 
benzyme
#12 Posted : 12/7/2016 2:37:28 AM

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love my Buchi R. it's like a vintage KitchenAid..it runs forever.
Pfeiffer Duo 2.5 provides the vacuum.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of knowledge at our disposal. The rest is poetry, imagination." -Max Planck
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entheogenic-gnosis
#13 Posted : 12/7/2016 2:26:07 PM
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downwardsfromzero wrote:
Aargh... now I get Rotovap envy!!

Some say purchase of a Rotovap may lead to undesirable LE attention. Hope your story is straight.



No worries on this end, no story needed either.

-eg

 
entheogenic-gnosis
#14 Posted : 12/7/2016 3:01:29 PM
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benzyme wrote:
love my Buchi R. it's like a vintage KitchenAid..it runs forever.
Pfeiffer Duo 2.5 provides the vacuum.




Sounds nice...

I've seen/used a Buchi R-210, it had a cold-finger (cold-trap) in place of a coil or Dimroth condenser, nice piece of equipment.

I've been looking into the labtech EV311VAC rotovap, over the labtech EV311 it's a little more expensive, but I think in the end it would be worth it

...A LabTech VC1000 Vacuum Controller and a VP18R Vacuum Pump with the labtech EV311 rotovap would actually cost a little bit more than just purchasing the labtech EV311VAC rotovap...

-eg

 
downwardsfromzero
#15 Posted : 12/8/2016 9:11:26 PM

Eggnogstic - warning: Self-irony levels: high!


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entheogenic-gnosis wrote:
downwardsfromzero wrote:
Aargh... now I get Rotovap envy!!

Some say purchase of a Rotovap may lead to undesirable LE attention. Hope your story is straight.



No worries on this end, no story needed either.

-eg


I am very relieved. And now even more envious Big grin
Ora, lege, lege, lege, relege et labora

“To be GOVERNED is to be watched, inspected, spied upon, directed, law-driven, numbered, regulated, enrolled, indoctrinated, preached at, controlled, checked, estimated, valued, censured, commanded, by creatures who have neither the right nor the wisdom nor the virtue to do so. To be GOVERNED is to be at every operation, at every transaction noted, registered, counted, taxed, stamped, measured, numbered, assessed, licensed, authorized, admonished, prevented, forbidden, reformed, corrected, punished. It is, under pretext of public utility, and in the name of the general interest, to be place under contribution, drilled, fleeced, exploited, monopolized, extorted from, squeezed, hoaxed, robbed; then, at the slightest resistance, the first word of complaint, to be repressed, fined, vilified, harassed, hunted down, abused, clubbed, disarmed, bound, choked, imprisoned, judged, condemned, shot, deported, sacrificed, sold, betrayed; and to crown all, mocked, ridiculed, derided, outraged, dishonored. That is government; that is its justice; that is its morality."
― Pierre-Joseph Proudhon
 
entheogenic-gnosis
#16 Posted : 12/9/2016 2:30:03 PM
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downwardsfromzero wrote:
entheogenic-gnosis wrote:
downwardsfromzero wrote:
Aargh... now I get Rotovap envy!!

Some say purchase of a Rotovap may lead to undesirable LE attention. Hope your story is straight.



No worries on this end, no story needed either.

-eg


I am very relieved. And now even more envious Big grin


never considered making the purchase yourself?

-eg
 
downwardsfromzero
#17 Posted : 12/11/2016 3:51:52 AM

Eggnogstic - warning: Self-irony levels: high!


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Very much considered, but multiple factors have been very realistic obstacles.
Ora, lege, lege, lege, relege et labora

“To be GOVERNED is to be watched, inspected, spied upon, directed, law-driven, numbered, regulated, enrolled, indoctrinated, preached at, controlled, checked, estimated, valued, censured, commanded, by creatures who have neither the right nor the wisdom nor the virtue to do so. To be GOVERNED is to be at every operation, at every transaction noted, registered, counted, taxed, stamped, measured, numbered, assessed, licensed, authorized, admonished, prevented, forbidden, reformed, corrected, punished. It is, under pretext of public utility, and in the name of the general interest, to be place under contribution, drilled, fleeced, exploited, monopolized, extorted from, squeezed, hoaxed, robbed; then, at the slightest resistance, the first word of complaint, to be repressed, fined, vilified, harassed, hunted down, abused, clubbed, disarmed, bound, choked, imprisoned, judged, condemned, shot, deported, sacrificed, sold, betrayed; and to crown all, mocked, ridiculed, derided, outraged, dishonored. That is government; that is its justice; that is its morality."
― Pierre-Joseph Proudhon
 
entheogenic-gnosis
#18 Posted : 12/11/2016 11:32:37 AM
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downwardsfromzero wrote:
Very much considered, but multiple factors have been very realistic obstacles.


Understandable.



-eg
 
pitubo
#19 Posted : 12/11/2016 1:15:22 PM

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Molecular gastronomy. Scroll down to see the rotovap.

When I bought my rotovap second hand, I asked the seller if he had been using it for "cooking". His look back seemed both perplexed and disturbed. Apparently, he took the term "cooking" in the Walter White "drug cook" sense. He had never heard of the gastronomical use.
 
DrSeltsam
#20 Posted : 12/12/2016 9:44:36 PM

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I do have a degree in chemistry and honestly I do not want to have DCM at home. It ist just too nasty and too toxic.

Please think about the environment when using this stuff. Never discard this in the drain or in an other way that is different from certified toxic waste. In my country there is the possibility to do this and even then I choose not to handle such chemicals.

Stay safe!
 
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