Sassy distillation, total disaster.. Solved!!

[NeoSynthesis]

Well SWIM went out & bought a liter of Sassy. The supplier seemed pretty legit and the Sassy seems to be 100% Chinese, smelled like it too. SWIM came home & set up his distillation apparatus (500ml RBF, 250ml RBF, 400mm Liebig, Fractionating Column, thermo's, etc). SWIM then poured about 100ml of Sassy into the 500ml RBF. SWIM used peanut oil to heat the Sassy on a hotplate/stirrer, and tap water to cool the condenser. What ensued was a sad failure. At first SWIM thought that nothing was happening because he was using the Vigreaux (fractionating) column so he got rid of it. Seeing as SWIM had no vacuum source (and seeing as he'd read that it was no problem to distill Sassy @ 1 ATM) swim was doing it @ 1 ATM.

Well.. What can SWIM say? The peanut oil heated (over time) to around 250 deg. Celcius. That's about it. There was some minor bumping (SWIM used a 2-inch teflon stir bar) but not much else. No forerun, no distillate, nada! at ANY temperature! Nothing ever came over! SWIM fucked up somewhere only he's got no clue where!??! Can someone please dang SWIM in the head with a saucepan?

[technology]

"Sassy distillation, total disaster.. Help!!"

if you are distilling at atmospheric pressure safrole comes over at ~254, and you said you heated to 250 perhaps that is your problem. i am unaware of your setup as it works different for everyone.

i say go back pull it all apart, clean, make sure you grease the joints and go for it, if you dont get anything than i would have to say you have been fuck over by the sassy person that sold you the sassy.

all the best.

[LaBTop]

Take a few ml of your sassafras oil, put it in a glass tube, put a thermometer in it, which scale goes to 300 C. Don't let the thermometer rest on the bottom, but 0.5 cm above where you heat it.
Heat the tubebottom with a torch.
Observe the thermometer. When at 255-260 C still no bubbling starts, and vapours don't rise up, you have found yourself an excellent source of heating bath oil. But no sassafras oil. LT/

[NeoSynthesis]

You mentioned that at 1 ATM Sassy comes over @ 254 C, are you reffering to the temp of the oil bath? or of the Sassy in the flask? I don't have a 2-neck rbf, so all's i got are 2 thermometers - 1 in the adapter, the other in the oil bath. How should i go about it?

Also, when cleaning the glassware can i use paint thinner? why do joints need to be lubbed @ 1 ATM distillation?

I know these questions are probably all on TFSE but i'm soooo depressed over this i'm hoping it'll be looked over just this once

Peace

[NeoSynthesis]

Just before I quite (temp of oil bath was @ around 248 C) I shut the stirring off, and I *did* notice some bubbling.. though very slight.. is this an indication of anything?

[technology]

Go to rhodiums home page an do a search on distillation of sassy..fuck here ill do it for you

https://www.thevespiary.org/rhodium/Rhodium/chemistry/safrole.distillation.html

check this for the temps.

also the temp of the oil bath is going to be different to that of the oil, dont worry aboout the oil you are heating concentrate on the temp of the pricless oil in the rxn flask..

[LaBTop]

It's Sassafras oil, not Sassy (sounds to me as slang for human seemen with mildew on it).
It's the temperature of your sassafras oil in the flask, at 254 C it should already bubble (boil) as hell (bp of Safrole = 234-234.5 C!), and giving off lots of Safrole vapours, rising up to your condenser, where they should be condensed nicely into your receiving flask.
You must grease all your joints, always!
You don't want to have to use a blowtorch on your joints, to unstick all the sticky stuff which will creap into the joints, after you thought it will only need grease when distilling under vacuum.
UTFSE: cleaning glassware .

Post 292562

(wyndowlicker: "cant get safrole? FREEZE IT!", Methods Discourse)
This thread I posted lots of boiling points of other constituents of Sassafras oil, and most of them lay far away from the Safrole bp. And it will also help you a lot with thinking over another method to clean your Safrole AFTER you distilled it, namely freezing the impurities out.
Btw, there are numerous threads in TFSE about freezing of Safrole, just a few already in the first 10 of this forum at this date!

Which means: Take your time to READ, READ and READ everything about the route of synthing you are willing to perform, before jumping into the deepest part of the SWIMming pool! LT/

[hypo]

to distill a 230° substance through a column, you need patience!
there's shitloads of heat losses, so heat stronger, insulate
your column and don't give up so easily. it takes time!

[LaBTop]

Post 457373

(slackdaddy: "Clean crystallized safrole for dumbies", Newbee Forum)
And the bp of pure Safrole is 234 to 234.5 Celsius, and NOT 254 C as stated in one of above posts, which is the bp of Eugenol. LT/

[NeoSynthesis]

Ok... just to clarify things out of consideration for all those helpful bees nice enough to answer my post, and in an effort to make better use of their time & effort...

1. My glassware setup consisted of the usual (all 24/40) borosilicate flasks (500ml & 250ml), 200mm Vigreaux (insulated top to bottom w/foam copper-pipe insulation, tie-wrapped), adapters (3-way, 105deg Vac, thermometer) 400mm liebig, metal pot, hotplate/stirrer (Corning), clamps, stands, etc. and 2 thermometers (1 in the adapter, 1 in the oil bath).

2. I measured out 100ml of Sassafras oil, weighing in @ 104.14g, heated in a peanut oil bath with high-speed stirring using an egg-shaped, 1 5/8 x 3/4" Teflon stirrbar, over about an hour, until i hit around 250C. (which is when I gave up). I used tap water to cool my condenser.

3. My observations were as follows:

11:37pm - Started full heat on oil bath, stirr on #8. As the Sassafras oil started to heat up the smell became less sharp, more "warm & diffuse", if i can call it that.

11:42pm - Bath temp @ 100 C, dropplets can be seen forming on the top (empty) half of the 500ml flask containing the Sassafras oil (I'm assuming this is water)

11:48pm - Bath temp @ 136 C, lots of dropplets can be seen forming on the top (empty) half of the 500ml flask containing the Sassafras oil

11:50pm - Temp in top thermometer (in the adapter) starts to rise, now @ 32 C

12:02am - Bath temp @ ~ 200 C, top thermometer @ around ~38 C, insulation on Vigreaux column is getting warm to the touch

12:06am - Bath temp @ 214 C, top temp @ 38 C, no more water dropplets forming, now a there are many steady streams of liquid running down all sides of the top of the 500ml flask containing the Sassafras oil

12:14am - Bath temp @ 232 C, top thermometer temp @ 40 C, heat reduced to #5 (since we've supposedly reached Safrole bp) no other changes.

12:24am - Bath temp @ 246 C, top temp seems steady @ 42 C, there's obvious condensation going on in the lower third of the Vigreaux column and streaming back down into the 500ml (Sassafras containing) rbf. I'm starting to wonder if using the Vigreaux column was such a good idea?

12:29am - Temps still climbing slowly, I'm gonna let the bath cool below 232C & get rid of the Vigreaux column. Heat set @ zero.

12:40am - Streaming in the flask is down to a barely-noticable minimum, I'm guessing that @ 232 the Safrole started to evaporate but for some reason couldn't make it through the Vigreaux column before condensing again. Vigreaux column is now removed so all i have is the 105deg adapter going directly into the Liebig, heating is cranked up to full blast on the oil bath.

12:50am - Bath temp climbing back to 196 C, top thermometer @ 50 C

1:01am - Bath @ 222 C, top unchanged at around 50 C, no streams observed in the top of the 500ml Rbf (containing the Sassafras oil)

1:03am - Bath temp climbs to 228 C, streams of liquid can be observed flowing down the sides of the top half of the 500ml flask containing the sassafras oil.

1:06am - Bath temp @ 233 C, more streaming, top temp unchanged,

1:10 - Bath temp @ 241, same deal.. no changes, I give up! where's my fuckup?

NOTE: Right before I gave up I shut the stirring down, temp was at around 240C, for the first time i DID observe a bit of bubbling, albeit not much. Thought I'd mention this for whatever it's worth.

There's a transcript of my lab notebook for this procedure. I read Rhodium's write up on distillation of Safrole as well as a few more, though most discuss vacuum distillation - and well, since I don't have a vacuum for the time being.. you can understand.

So far 2 bees have said that I should've pushed the bath temp to 254 C or thereabouts, I'm gonna try that. I will clean out all my glass, grease my joints & give it another shot. I'm gonna be using the same Sassafras that remained in the flask from last night - Hope that's okay. Circumstances surrounding the purchase of the Sassafras oil makes me pretty confident this is the real stuff.. I mean yea, it could be crap.. But then again I *could* be fucking up somewhere.. I'd hate to toast a really really really good source!

Some questions that come into my mind:

- Is a 500ml flask too big for only 100ml of Sassafras?
- I didn't grease my joints, could that have something to do with it?
- Should I heat the oil bath more slowly?
- I was stirring constantly at a setting of #8 all throughout. As I mentioned above, when I gave up I shut the stirring first & observed some (minor) bubbling @ around 240C. Should I perhaps be stirring differently?
- I know the Vigreax column was insulated, some bees have said I should be more patient, how long should this distillation take? what should I expect time-wise with, w/o a Vigreux column?

I'm gonna give this another shot tonight, advice, help, hints, suggestions and even prayers are GREATLY APPRECIATED! Will post results! Thanks to all you bees nice enough to help out!

Peace

[mindlib]

a) you need a "water pump" or other pump system, when you want to distill your ketone. Bright Star said, that the whole flask of ketone will polymerize, if heated over 220
b) as far I remember, it´s really necessary, if you are using a vigreux-column without glass-over, to wrap alu-foil around the column(for the first "insulation"), so that nada air will hit it.= no air under the alu-foil.
c) "metal pot"   alu or copper, right?..... but somewhere you said, your stirring works well.so all o.k./ALWAYS STRONG STIRRING
d) patience......
e) How much smelt that peanut-oil? I´ve heard, cannola oil will work well without smell.., but not self experienced..
f)SLOW heating, from the stand I would say, min. 3 hours to da boiling point(s).(see other threads/informations)
g) enjoy it   

[mindlib]

just to speculate for me and the others a little:

The advantage of the use of a vigreux-column (+glass-over)+insulation is, that it´s then just necessary to distill once to get a good result.

Simple distillation is necessary two times to get to the same result.

What´s with that?

[yinga]

Using a column with high temperature distillations like that is inefficient because of the heat losses.  Your column won't stay hot enough to keep the safrole in the vapor phase, and thus it will sit there refluxing all day unless you have really good insulation.  When using an oil bath to heat up a flask I find I need to have the oil bath temperature approximately 15C higher than my target temperature.  So heat your oil bath to atleast 250C, don't use a column, and freeze your distilled safrole to get a seed crystal and use that to freeze out the rest.  And don't cool your condenser with water when you're distilling at high temps like that.  The difference in temperature can crack the glass, blow air through the condenser instead.

[NeoSynthesis]

Okay well.. I've read the posts, done the math in my head, and have pretty much concluded that last night's failed attempt was such because I didn't keep the heat long enough. This happend for a few reasons: 1) I guess because I didn't realize how much heat is lost in the Vigreaux column (even though I insulated in with foam/copper-insulater). One suggestion that was made to me was to wrap the column in tin foil and THEN to apply the foam insulater. I'm wondering how to do that? I mean do I just wrap it in 1 or 2 layers of tin-foil and then wrap the foam around it? or many layers? anyways.. this'l be for next time. Tonight I just NEED TO KNOW that I didn't blow all my loot on donut oil!!!!

I'm gonna soak/clean my glass in Acetone, dry it all up & get distilling! I'm gonna fire up the hotplate w/max stirr, and bring the bath up to 250 C as quickly as possible. That's when I'll slow down the heating and try to hold it at around 255-260 C. I'll watch for bubbling in the rxn flask & post my results - WISH ME LUCK!!!!!!

Peace out

[calcium]

You ought to invest ten bucks in a simple water aspirator. It isn't ideal but at least you wouldn't be distilling at atmospheric pressure.

[mindlib]

"and bring the bath up to 250 C as quickly as possible"
NO, do it slow over a 3-hour period or longer, and look in da current thread about it.(DjTime-thread)

[mindlib]

Why you want to insulate your column? Because you want the heat from the hotplate in the apparatus, in the vigreux and etc. Air is a great transporter of heat, so you want no heat is going in the air "outside" of the apparatus(=heat losses), you must at least catch it around the column. No air should be on the surface of the column, so that the substances can go with the heat, at least into your receiving flask.
Until you not read about the whole insulation thing, you should make,
a)what yinga told: 1x simple distilling + freezing   or
b) 2x simple distilling
c)or, if you know the stuff     1x frac-distilling
Just buy that water aspirator.....!!

[mindlib]

"do I just wrap it in 1 or 2 layers of tin-foil and then wrap the foam around it?"
Hmmm, the problem is, that I cannot remember, where I read it, but as far I remember, it was 3 or 4 or 5 layers around the "column without a glass-over" and then the rest of the insulation. So, I didn´t experience that stuff, so it will be necessary for you to look in different information sources, like books and databases, libraries etc.
Important is, what I said in the posts before about the air-thing and that there should be no air on the surface.
But again, use vacuum and the stuff with the vigreux will go better...

[hypo]

> NO, do it slow over a 3-hour period or longer, and look in da current thread
> about it.(DjTime-thread)

look, last time the newbee tried it, nothing came at this temperature.
what the heck would it help to do it slowly? don't waste time, heat the
shit out of it, and when the first drops come regulate temperature
to about one drop per second. (but don't set yourself on fire!!)

also your "information" about insulation is pretty confusing (imho).

[mindlib]

First, Thanks for your input!
hypo, o.k, important is, not to overshoot the boiling point, and then just to collect it in small temp-ranges to get it at least, or ?

With that insulation thing, I read it and it sounds, if I´m thinking about it in a "nature way"(physical properties etc.), in that way, that it could be real.
What is wrong with it in particular?
The goal is to avoid heat losses, or? and to get a consistent temp in that vigreux, or ? and for that, we insulate..?
"also your "information" about insulation is pretty confusing (imho)."    or you meant my grammar...?
..and wasn´t da problem from da newbee, that he stopped short before it would come over ?
(I personally wouldn´t use a vigreux at atm, as yinga advised.)
"(but don't set yourself on fire!!)"  means that, to cool da receiving flask proper? or to be careful with the hot oils?

hypo, I believe serious, that you can distill at a very fast rate(for the whole distillation), because you are experienced with it and so you know all, what will happen, before you do it.
Through the problems, if you overshoot too much, it would be better for a newbee to increase the heating slow.(but here at this temps, it´s maybe not a matter..?)(and anyway, he chose the "middle-way")
Maybe it´s also so better, to collect better in small temp ranges good material?
Maybe I´m seeing some stuff wrong, but then, just help me to clear it up, if you want so..

[NeoSynthesis]

Whoah.. lol.. talk about a following!
I'm begining to feel like the fucking Sopranos! lmao!

Anyways.. here's the deal:

Just started my second attempt to distill Sassy @ ATM. I *AM* getting a 1/2 HP or 29" vac pump (in fact I got one on friday but had to ship it back same-day cuz it was fucked! damn). For the time being I NEED to know if this Sassy's good.. that's why I'm in such a fucking rush. I know that for all the next steps, (wacker, amination, etc) I'm gonna need a whole bunch of gear... I'm not worried about that tonight. All I need is to verify that the Sassy I bought is good so that I can hit this fucking source before it dries (which is like... Monday!).

Ok...

250ml RBF (rxn) plugged into a 3-way w/ a thermometer adapter & a 400mm Liebig, with another 250ml RBF (distillate). I'm not using a 105deg adapter this time because I don't have the space for it. Anyways.. I set the rxn flask into the peanut oil over the hotplate/stirrer, set stirring @ 8 & heat @ full blast. Also, last time I had the thermometer (the one measuring reaction temp) set a bit high, now it's right above the joint where the 3-way meets the rxn flask.

Bath temp climbed to around 158 C pretty quick, and rxn temp to around 40 C. I dropped the heat to around #7 simply because posts have been so damn conflicting about this part. I figured I'd kinda wing it by going in the middle! heh..

So that's it.. the Sassy's cookin.. I"m gonna let the heat rise to about 230 C (bath temp) before starting the condenser water.  In the future I'm damn set on buying a fountain pump & running it to/from a bucket of ice water.

I'll post the progress over the next few hours, imput HIGHLY VALUED!!!!

Thanks bees... Chill.. & Peace out

[mindlib]

yinga: "And don't cool your condenser with water when you're distilling at high temps like that.  The difference in temperature can crack the glass, blow air through the condenser instead."
But anyway, I have no experience with stuff like that. Decide for yourself.
If the water will heat up over the time, it will maybe go, but i don´t know..

and... you made that congealing-point test?

[NeoSynthesis]

Air? how do you blow air through a condenser? don't you need somekind of compressor or something? Anyways.. last night i survived and the rxn is already in full blow.. i'll take my chances with the tap water for this time. I appreciate the input though.. will research this issue further

[NeoSynthesis]

I'm working in a closed room with *some* albeit minor, ventilation. After a few minutes of being in there I started feeling a bit dizzy.. lightheaded so to speak. I'm wondering if it's just my paranoia or if there's something to this? I mean after all.. I'm just distilling safrole.. could fumes inhallation cause this? Could it be that it's the fumes from the acetone i used to wash the glassware? Safety first right? let me know bees....

peace

[mindlib]

please, safety first,
if you are collapsing there, is there anybody ?
let air in if possible
decide for yourself in a sane attitude
(And I´m sure you are wearing a protection for your face and your body, or?....or?...or?, but at the other hand, the oils are only at 230 and 250...!!!!)

[Vitus_Verdegast]

You should look for some kind of ventilation, even if it is a fan and a small window.

Also, make sure you attach a tube to the vac outlet of the recieving end, to lead the fumes outside.
You really don't want to stand for hours in a room that is constantly being filled with sassafras oil vapours.

[OcoteaCymbarum]

or at least that post by Chromic,

Post 399083 (missing)

(Chromic: "Didn't I write a document on this?", Newbee Forum)

[NeoSynthesis]

***    A Bee Iz Born    ***

Folks... That one says it all! The shit I bought (apparently) is the best Sassafras Albidium on this side of Texas! (even though I'm not in texas heh.. always wanted to say that!) Here's a synopsis of tonight's labwork:

- I'll reiterate what I posted earlier, setup consisted of (all 24/40) 250ml "still" RBF, 3-way adapter w/thermometer adapter, 400mm Liebig, and a 250ml "distillate" RBF. All joints were greased (thin layer @ the top of the male), used keck clamps on both sides of the Liebig condenser.

7:41 - Started cooking; Stirring set to #8, Heat set to full blast. Thermometer (rxn) was lowered this time so that the tip falls just below the point at which the 3-way adapter meets the rxn flask.

7:55 - Bath temp @ 158 C, rxn temp @ 40 C; Came back to read posts, it was suggested that slow heating would yeild better results.  Heat reduced to #7.

8:15 - Bath temp @ 180 C, rxn temp @ 55 C; not much more happening; Cranked temp back to #9.

8:50 - rxn temp now @ 74 C, some foaming can be observed in the rxn flask. Started (tap) water through the condenser.

9:00 - Bath temp @ 258 C, rxn temp @ 76 C, appears to be rising slowly. Lots of foaming/bubbling can be observed in the rxn flask. I'm starting to see miniscule (barely noticable) signs of condensation in the condenser-3wayAdapter area. Not much more happening.

9:01 - rxn temp starts climbing quicker, now @ 80 C, bath temp @ 259-260 C appears to be holding. Stirring raised to #9, VERY heavy bubbling & foaming can be observed in the rxn flask.

9:04 - rxn temp climbing steadily, now just above 92 C, bath temp seems to be holding at 260 C; Very heavy bubbling/foaming in the rxn flask. I can clearly see moisture condensing & streaking down the 3-way adapter.

9:07 - rxn temp just shot up to 130 C, VERY HEAVY condensation & streaming going on in the 3-way adapter. bath temp holding @ 260 C, nothing coming over yet.

9:08 - rxn temp sky rocketing! @ 158 C, bath temp holding @ 260 C, lots of bubbling & condensation in the 3-way adapter. I can see moisture condensing & dripping off the rxn thermometer.  Temp in rxn flask rising very fast.. now @ 174 C!

9:21 - [I left for a few minutes so I don't know if there were some observations missed] Woah! Bath temp @ 268 C, the room is filling up with smog.. it's not smoke.. but like a thick oily cloud.. looks like the bath oil starting to evap (thats just my guess). Rxn temp is 232 on the dot! Safrole is flowing through the condenser & into the receiving flask at about 2-3 drops per second. I drop the temp down to #9-9.5, have to walk out of the room.. can't fucking breath in here..

- I come back in a few moments later.. I kill the heat on the hotplate (shit.. i don't want to set off the sprinkler system!). I'm satisfied, I'm looking into the receiving flask & see a clear (somewhat thick.. maybe even a little misty) fluid. I smell it... Yep, smell's just like the Sassy did, only stronger. Is this my first date with Safrole??? you tell me!

Conclusions:

I'm guessing my sassy's good shit! Nothing came over before 232 C & at 232 C on the fucking dot it just started pooring over! I guess I didn't heat it enough last night, didn't have the rxn thermometer placed correctly, and concentrated way tooo much on the bath temp (instead of the rxn temp which is where i seemed to have gone right tonight).

I'm gonna have a vacuum pump by next week. I'm hoping that should solve my smoking-bath problem since the bath won't need to be heated more then (i'm guessing here) around 160 C, and last night I went to 250 C with practically no smog. Additionally, I plan to upgrade my vent system to something a bit more powefull. Right now I'm using a stove-type fan that vents right into the building's exhaust ducts that were intended for oven use. Should work. Do I need a respirator mask? Any words on this would be cool.

Lastly, my final concern for tonight's work is to see if there's a way to determine the safrole content (%) of my Sassy. Before starting tonight's cooking session I measured out exactly 98ml of sassafras oil. Is there a way to "interpolate" what percentage is Safrole based on comparison of what's left in the rxn flask & the safrole that came over? PLEASE let me know if you've got info on this.

Finaly, my heart & prayers, as well as immense grattitude goes out to all the bees out there that helped make this possible. Your insight and valued thoughts will surely encourage bees like myself & ravers.. heh all over the world! Next stop for me will most likely be vac distillation and damned-if-i'm-lying, careful insulation of my vigreaux col. to distill 1L of sassy! After that.. it's to the honey comb for me.... bzzzz...

Peace out Y'all!

[technology]

here is a link that you can check the purity of your safrole form your natural oil.

https://www.thevespiary.org/rhodium/Rhodium/chemistry/safrole.congealing.html

that should be able to help you..

all the best.

[LaBTop]

https://www.thevespiary.org/rhodium/Rhodium/chemistry/safrole.congealing.html

which is the 
SAFE SSL secured (128 bit https) connection to Rhodium!  LT/

[OcoteaCymbarum]

from my own experience.
You're getting a vacuum pump and thats good, absolutely necessary. If I were you, I would invest after in a heating mantle. A 2L one fits good for 2L, 1L and even 500 ml if you want. Of course getting more then one is the best option but I find a 2L one to be most versatile.

Heating control is much easier with a mantle, you can bring the temp up much faster once you know your mantle well. Also if you overshoot the temp, its easy to take your flask off the stirrer to let it cool down, less messy then with oil, no smoking ever... and a finer control. In the end, especially under vacuum, you will save a lot of time, effort, and there is no chance you spill hot oil when moving you bath around.
I started using an oil bath, then  bought a heating mantle and never looked back again...

[NeoSynthesis]

Ocotea - Wow! Heh.. I guess learning is a part of being a newbie! This heating mantle idea rocks! No more spending $$$ on expensive peanut oil which cannot be re-used! No more worries about setting off the sprinkler system, dangerous "boiling oil" pan, or smog!

I saw a pic of the heating mantle, looks like a "burner" with no flame. A few "newbie" questions for you... since you brought it up:

1. How do you stirr with this? Are there heating mantles that have magnetic stirring built in?

2. The base of it looks flat, how can you set a Round bottom flask onto it? Do you simply suspend the flask over the heating mantle from a stand?

3. Is there a pic anywhere of a heating mantle in use that I can reffer to for an idea of how this thing works?

Thanks Ocotea! Brilliant!


Peace Out..

[LaBTop]

you probably bought that precious Sassafras oil which caused such a hurried behavior.

NOW, you at last gonna READ!
This one:

https://www.thevespiary.org/rhodium/Rhodium/chemistry/equipment/distillation4dummies.html

  LT/

PS: and if I judge you right, you will spend a lot more time reading necessairy priceless info on that particular site! Before you spend again a lot of cash on worthless materials and equipment (in your case! An oil bath will allways be handy when you arrive at buying one of those digitally controlled Rotavaps).
And get a good exhaust fan, and NEVER blow the fumes into a building's pipes, they will come out all the neighbours kitchens, bathrooms and toilets. They are all interconnected by the same piping.
You're lucky you did not arrive yet at acetone or dichloromethane distillation!
That would have caused a fast visit to the next police precinct, for sure.

Never hurry, THINK first, then READ, then THINK again, then ASK QUESTIONS here about any UNCERTAINTIES, then WAIT, WAIT, WAIT until someone ANSWERS, then WAIT again untill MORE ANSWERS come, then THINK again, then say THANKyouALL, then

START COOKING!  LT/  

[mindlib]

The style of distillation of NeoSynthesis is DANGEROUS.
Don´t use water to cool your liebig.

Think about it, what can happen, if you are next to the apparatus to check the temp and then, cracking of your glass and then HOT oils and WATER will go their nature way.

Also it´s standard to use protection for your face and your body and, as Vitus told, don´t touch your skin with contaminated lab stuff.

Also it´s standard to have a good ventilation.


from Organikum p4:
"The Liebig-Cooler is mainly used as a product cooler (´til approx. 160°C).For the coolant, is used ´til approx. 120°C floating water, and from 120°C ´til 160°C standing water."
"Der Liebig-Kühler (c) wird vor allem als Produktkühler eingesetzt (bis etwa 160°C). Als Kühlmittel dient bis etwa 120 °C fließendes, von 120°C bis 160°C stehendes Wasser"



"e-book (German) Organikum 21st edition"   by Rhadon
available here at da hive

[OcoteaCymbarum]

But I swear man, its because I feel nice right now(seems to do that when I smoke a joint) that I'm giving you this link.

http://www.sigmaaldrich.com/Brands/Aldrich/Glassware_Catalog/Heating_Mantles.html

This isnt a source, since I know for a fact(well I dont but I'm so sure of myself) that 99.5% of bees here havent even had the idea about ordering from there. And no, if you work in a chemical company or at a university, then I dont count you in.

This is the first it when u use google and heating mantle as the search word.

This is one kind, use it with your hot plate(for stirring) and they are made for RB flasks. Stirring is no problem, but you have to install a dimmer to control the heat otherwise, its one setting.
For dimmers go to your local hardware store and figure it out yourself. All you have to do is match the wattage of your mantle and dimmer.

But please, you have to work for yourself if you want to get to the end.

[abolt]

The style of distillation of NeoSynthesis is DANGEROUS.
Don´t use water to cool your liebig.

Condenser temps are relative to distillation temps and the material that your distillation setup is made from. A long time ago I saw someone do a distillation with a 0.1 micron rotary vane vacuum pump.They were distilling Safrole @ ~120. Celcius. in a borosilicate glass rig and took the advice of some of the distilling posts on the Hive (some of these posts where from highly regarded bees) and ran only lukewarm water through their Leibig.

After they had finished their distillation, they were surprised to find about 50 mls of Safrole had gone straight through the condensing setup and collected in the condensation trap that they had in line on there vac pump. When the oil in the pump was changed, it also had a strong sassy smell and had to be stripped down and thoroughly cleaned.

MORAL OF THE STORY: Proper Condenser fluid temperatures are to be calculated, relative to the strength of your Vacuum.

or

The stronger the vacuum, the colder the condenser will need to be.


Think about it, what can happen, if you are next to the apparatus to check the temp and then, cracking of your glass and then HOT oils and WATER will go their nature way.

Once your vacuum distillation ratios have been taken into account, the next thing to take into account is the Thermal Shock Ratio of the material of your distilling apparatus, in this instance let's assume that is Pyrex.

As Pyrex has a maximum thermal shock ratio of 160.Celcius, it is probably good practice to have your distillate to condenser temperature ratios within a 140. Celcius range.
(e.g, if you're getting distillate at 150 Celcius, then it is advisable to have the condenser temperature at < 10 Celcius, and rest your collecting flask in ice water to enhance further condensation)