Bubbleplate (Hive Bee)
10-08-03 18:58
No 463385
      Sassafras Oil Questions     

A friend stored some Sassy Oil outdoors in a plastic gas can for a few weeks. (Temperature was in the 60's-70s).
Previously the Sassy Oil was a golden color and  95% would freeze solid when put in the freezer for an hour or two. (Had been previously "Freeze Purified")
However, when he retrieved it recently, the oil was now a deeper brownish color and will not freeze at refrigerator freezer temps, even overnight.
Any ideas about what could have happened, and ideas about salvaging this oil?
 
 
 
 
    hypo
(Hive Addict)
10-08-03 19:34
No 463389
      whoa!     

> Temperature was in the 60's-70s

what kind of hell do you live in!?

(har har...)

n'importe quoi
 
 
 
 
    cublium
(Stranger)
10-08-03 20:30
No 463394
      maybe a vac distillation could help?     

maybe a vac distillation could help?
 
 
 
 
    mindlib
(Hive Bee)
10-08-03 20:45
No 463395
      Read here:     

Post 459845 (abolt: "The last ever post on freezing out Safrole", Newbee Forum)
 
 
 
 
    Bubbleplate
(Hive Bee)
10-09-03 03:13
No 463469
      Thanks All For The Suggestions     

By the way, that was 60-70 degrees F. not C.
My friend was hoping not to have to look around for Dry Ice, but since he melted his "Seed Crystals" that he made in the Winter last year, guess he'll have to.
Thanks for the help guys.
 
 
 
 
    Midi
(Stranger)
10-09-03 04:32
No 463479
      !!     

Why was it you couldn't just vac distill??? I don't think any other method could give the same purity. With that being said, why even freeze as an option??
 
 
 
 
    DjTime
(Hive Bee)
10-09-03 08:54
No 463537
      SWIM says why not? SWIM thinks KNOWS that if...     

SWIM says why not? SWIM thinks KNOWS that if you
vac distill your sassy oil THEN freeze. SHIT FIRE! You
got some good ass safrole. SWIM did that and the yeilds
went up by 4.7 grams from distilled AND frozen vs. just
distilled. SWIM had an amazingley HARD time freezing
undistilled sassafras oil. He'd left his oil in the freezer for
over two months and not 1 crystal. Then SWIM phuc it
and vac distilled his oil and used that. Meanwhile he put
his distilled oil in the freezer and still for three weeks no
freezy. Until 1 magic moment when SWIM took his oil out
of the freezer and poured it into glass (from HPDE) and
OUT OF PHUCKIN no where the whole damn glass froze
SOLID!!! So then swim saw his chance and hasn't
looked back since. SWIM keeps seed crystals around for
the next freeze. Welp again long thread short style. Vac +
Freeze is much better then just one OR the other. Peace
 
 
 
 
    Midi
(Stranger)
10-09-03 09:17
No 463545
      uhh     

Welp again long thread short style. Vac +
Freeze is much better then just one OR the other.


What would be the point?! If you can perform a vacuum distillation then you are going to get very pure safrole the first time. Your just wasting time moving the shit all around from the jar, to the glass, to the HPDE thing, just distill the shit the right way, at the right pace, and be done with it.

With the time it's takin you to do all that, I could have distilled 20lbs with a rotovap and a decent pump, with the same purity.

NOTE: I would never distill ANY amount of safrole, for safrole is a listed chemical, but hypothetically speaking.

http://www.greenspun.com/bboard/q-and-a-fetch-msg.tcl?msg_id=00749A
 
 
 
 
    Bubbleplate
(Hive Bee)
10-09-03 14:46
No 463568
      Just To Throw Some Ether On This Threads Fire     

Yeah one could Distill the Oil, but its tedious to set up the equip, run the vac pump - and then the damn thing and the pump oil REEK of Sassy, and if one DOESN'T have a RotoVap, then how much can you do at a time? 1 Liter?
SWIM double froze his oil last Winter outside, and for 1 minutes worth of pouring between jars got 98%+ pure Safrole.
Now THATS the kind of easy lab work I like!
 
 
 
 
    mindlib
(Hive Bee)
10-09-03 14:58
No 463570
      ----     

As far as I see (e.g. for a oil), these are the ways to go:
(in no order)
1. 1x vac-frac distill
2. 2x simple-vac distill
3. double or tripping freezing
4. 1x simple-vac  +  1x freezing

Sure it depends also on the "seen" purity after the work,
 if someone should "repeat" it again to get a better purity.
( from a other bee:  " Garbage in - Garbage out : Good stuff in  - Good stuff out! " )


btw, a water aspirator is a very cheap vacuum source.
Itīs buyable or itīs possible to build one or more own.
Thereīs no need to distill in special cases without vacuum.
At least, for other substances a vacuum source is "required".

Post 462575 (mindlib: "OTC stirrer +  OTC heating mantle", Chemicals & Equipment)


Have a good day!

Feel free to comment....


EDIT:  Bubbleplate, you use "between" the vacuum-adapter (or whole piece condenser) and the vacuum pump a "condensation trap", e.g. a Woulfsche Bottle ?
 
 
 
 
    DjTime
10-09-03 22:01
      I Bet....
(Rated as: flaming)
    
 
 
 
    hypo
(Hive Addict)
10-09-03 22:16
No 463638
      what the fuck are you people talking about???     

you _do_ _not_ distill product with a rotavapor. a rotavapor is here to
evaporate solvents, not to distill product.

back to newbee forum!

(and quit the drama please - simply distill the shit.)

n'importe quoi
 
 
 
 
    Midi
(Stranger)
10-10-03 00:28
No 463672
      ignorance..     

Hypo, you may think you know what your talking about, but unfortunatly your wrong. You can distill kilo's upon kilo's of any of your 3 oils, safrole, ketone, and mdXX whatever using a rotovap. FAST, Excellent Qualtiy, and FAST!

You need to look into the R200 and R205 series with oil baths that go up to 180c

100g of freebase returns 105g of product. Please tell me again how you can't distill this shit with a rotovap! HA! Im all ears tongue

DjCheese: Whatever, your not worth the time it will take me to respond.

http://www.greenspun.com/bboard/q-and-a-fetch-msg.tcl?msg_id=00749A
 
 
 
 
    hypo
(Hive Addict)
10-10-03 16:42
No 463789
      get lost     

of course you _can_ distill with a rotovap. never said
you can't. but they are _not_ commonly used to distill products.
period. and you don't need one in order to do easy, fast
distillations.

your bragging is totally irrelevant to this thread and confusing newbees.

you can distill a liter of MDP2P in 5 minutes; nobody here gives
a flying fuck. so take your ego-boosting crap somewhere else.

n'importe quoi
 
 
 
 
    Midi
10-11-03 01:01
      heh
(Rated as: insignificant)
    
 
 
 
    yellium
(I'm Yust a Typo)
10-11-03 02:35
No 463888
      Aren't rotavaps way too lossy for ...     

Aren't rotavaps way too lossy for distillations? (too much surface area, bad separation..)
 
 
 
 
    mindlib
10-11-03 04:20
      -a little paranoia-
(Rated as: off-topic)
    
 
 
 
    Rhodium
(Chief Bee)
10-11-03 05:29
No 463906
      Rotovap - only useful for solvent removal/recovery     

Yellium: Most definitely - there is no question about the fact that you may be able to move MDP2P from one flask to the other using a rotovap, but you will have multiple grams coating the inside afterwards, as well as no useful separation between the various fractions of starting material, product and byproducts...
 
 
 
 
    Bubbleplate
(Hive Bee)
10-22-03 03:26
No 466050
      Well, As Usual, I Figured It Out Myself...     

Recalling a technique that a Brotherhood friend taught me...
I put some Sassy oil in a small glass vial, and then took  some glass tubing and crushed it up and and threw it into the oil. Then put the vial into a beaker full of crushed ice and 99% Isopropanol, and stuck that in the freezer. Next day vial was dumped into a liter of fridge cooled Sassy... and INSTANT Safrole crystals!!
Aint chemistry just GRAND?!!!
No distilling, No Dry Ice, No fuss, No muss!
2x times and 99% Safrole.