Author Topic: Sassy distillation, total disaster.. Solved!!  (Read 7951 times)

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NeoSynthesis

  • Guest
Sassy distillation @ 1 ATM - "Take 2"
« Reply #20 on: September 07, 2003, 02:13:00 AM »
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

  • Guest
..
« Reply #21 on: September 07, 2003, 02:24:00 AM »
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

  • Guest
Tap water to cool condenser - 1 ATM Sassy Dist
« Reply #22 on: September 07, 2003, 02:33:00 AM »
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

  • Guest
Just a side observation...
« Reply #23 on: September 07, 2003, 02:44:00 AM »
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

  • Guest
..
« Reply #24 on: September 07, 2003, 02:53:00 AM »
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...!!!!) :P

Vitus_Verdegast

  • Guest
not wise
« Reply #25 on: September 07, 2003, 02:55:00 AM »
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

  • Guest
You might want to look at this thread
« Reply #26 on: September 07, 2003, 03:26:00 AM »
or at least that post by Chromic,

Post 399083 (missing)

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

NeoSynthesis

  • Guest
Sassy distillation @ 1 ATM - A Broadway Hit!!!!
« Reply #27 on: September 07, 2003, 04:59:00 AM »
***  :)  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

  • Guest
Well done NEO
« Reply #28 on: September 07, 2003, 09:20:00 AM »
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

  • Guest
!!!!!
« Reply #29 on: September 07, 2003, 03:17:00 PM »

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


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


OcoteaCymbarum

  • Guest
Can I offer you a little piece of advice
« Reply #30 on: September 07, 2003, 03:58:00 PM »
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

  • Guest
Whoah! Heating mantle = Windows XP!!!!!
« Reply #31 on: September 07, 2003, 06:24:00 PM »
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

  • Guest
So,
« Reply #32 on: September 07, 2003, 06:44:00 PM »
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

  • Guest
PLEASE NOTE !
« Reply #33 on: September 08, 2003, 05:58:00 PM »
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

  • Guest
Ok Neo, heres what you needed
« Reply #34 on: September 08, 2003, 10:53:00 PM »
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

  • Guest
Time to speak up
« Reply #35 on: September 09, 2003, 07:11:00 AM »
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)