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..