Author Topic: cant get safrole? FREEZE IT!  (Read 31859 times)

0 Members and 1 Guest are viewing this topic.

DiMethyl

  • Guest
Got seed crystals---but....
« Reply #100 on: May 21, 2002, 12:06:00 PM »
A small amount of sassy oil in a baby food jar put in the freezer at -15c does "appear" to produce some crystals, or at least some white fluffy material on the bottom of the jar. But, when adding some of these supposed safrole crystals to the bulk of the sassy oil in the freezer, 300 ml, then nothing happens. From what I have read in this thread, you would expect an explosion of crystals in the 300 ml of sassy oil.
Not a particularly good sign.
Looks like I will be forced to do the non-vac fractional distill on some of the oil to see if there is any safrole in there.
Since I don't have a vacuum gauge, a vacuum distillation is out of the question. You really do have to know what is going on with your vacuum and without a gauge its all guesswork.
:(

DiMethyl

  • Guest
yes---but for this purpose
« Reply #101 on: May 21, 2002, 01:42:00 PM »
When attempting to determine safrole content or lack thereof, you have to know at exactly what temp the safrole will distill over. Unless you can get an exact measurement of the vacuum then you will not know that temp.
Without the vacuum then you know for sure what temp to look for.

wyndowlicker

  • Guest
well now!
« Reply #102 on: May 21, 2002, 03:52:00 PM »
well the pump is supposed to pull 15 microns right!the thats 28.4 "hg or whatever.Well when tested with a guage it delivered 30".Also bring safrole at 70-72c when it should  bee 114.4c Makes you go hmmmmm! :o

Society prepares the crimes,the criminal only commits one.

DiMethyl

  • Guest
Real Seed Crystals Work
« Reply #103 on: May 21, 2002, 03:57:00 PM »
Using a ~1/2 ml container produced one solid seed crystal in about 24 hours. Within 30 seconds after dropping this seed into 300 ml of sassy oil, massive crystallization was complete.
So---forget the baby food jar and its supposed seed crystals (they apparently were not) and go with a small/tiny container for creating the seed crystal.
For the seed generator was used one of thoes little brass screw together pet id containers. It's designed to hold a small note with the pets name and phone number on it, and then the barrel hangs on the pet's collar.
Worked over here.

foxy2

  • Guest
i wouldn't
« Reply #104 on: May 21, 2002, 06:41:00 PM »
"The unfreezable stuff is at least not safrole, as it doesn't freeze at sub-zero temperatures. Discard."

I wouldn't!

It still might have lots of sassy.  As terbium said, just because its cold doesn't mean the sassy will crystalize. And if it does crystalize that doesn't mean all of it HAS crystallized.

Those who give up essential liberties for temporary safety deserve neither liberty nor safety

Jubrail

  • Guest
Freezing instead of frac. dist.
« Reply #105 on: May 23, 2002, 07:08:00 PM »
Sorry to dig this up, but it's not too old and I was just utfse-ing.  Could someone use this same technique to get asarone out of calamus oil?  And, I am still new to this, why does this work?  If anyone can help, please do so, I'm just really curious and it's killing me to find out. 

Rainbows & Butterflies Forever :)

Rhodium

  • Guest
Asarone crystallization
« Reply #106 on: May 23, 2002, 07:37:00 PM »
The usual form of asarone (the asian variety) does not have an especially high melting point, so I'm afraid it wouldn't be as easy. However, if you are sure the oil contains alpha-asarone  (mp 62-63ºC) and not beta-asarone, it might be worth a try.

Possibly isomerization with KOH would transform the beta (cis) to the alpha (trans) form, and then the asarone could be crystallized from the solution. Please inform us if you try this and it works!

Suggested procedure: 100g (preferably distilled, but the crude oil may work, with lower yields) calamus oil (crude mixture of asarones) and 2g crushed KOH is vacuum refluxed (aspirator vacuum, 25 mmHg) for 6h with good stirring, distilled to remove the KOH, the distillate dissolved in an equal amount of petroleum ether and chilled (first in the fridge for 12h, and if that doesn't work in the freezer for another 12h). Scratching the inside of the beaker with a glass rod should help crystallization. The precipitated crude alpha(trans)-asarone is filtered off, washed with a small amount of freezer-cold pet ether and air dried. The product should consist of fairly pure alpha(trans)-asarone, mp 62-63°C.

baalchemist

  • Guest
ALL the bullshit that Baalchemist posted about
« Reply #107 on: January 17, 2003, 01:10:00 AM »
"ALL the bullshit that Baalchemist posted about 1 gallon jugs and seed crystals and putting the jugs upside down and draining off liquid is BULLSHIT.
I tried that.  The liquid is formed ON TOP of the crystals, not on the bottom.  If you turn the jug upside down and crystallize, none of the liquid will pour out--you will have to drill a hole in the bottom of the jug to drain the liquid and then cut the jug apart to get the crystals out.  There is NO WAY he actually did it the way he describes--he just made that bullshit up.  Not one bee posted it right.  It is SO FUCKING SIMPLE, I can't believe it.  The natent liquid is forced to the top and middle of the 20L bucket by the crystal growth on the bottom and sides of the bucket, so the most simple decantation by pouring off the liquid is all that needs to be done.  It is not necessary to check temperatures and do many decantations at 2 to 5 degree intervals, since the unwanted product does not crystallize at above -9 C, which is about as cold as a second hand deep freeze is going to get, in fact you DO NOT want a super-duper freezer, just an old one that can cool to -5 C.  Some other bee mentioned filtering the crystals--BULLSHIT!  All that is needed to achieve d20 of >1.099 is 3 times crystallization and simple decantation.  Nothing else.  For most people, 2x crystallization which gives d20 of >1.098 will be sufficient.

Fuck, it makes me mad to realize the amount of time I wasted on fractional distillation !
The only drawback to this method is that it takes a few days.  But shit, fuck, damn!  If I had known how simple it was, I would have done it already a long time ago.
And if I hadn't tried out Baalchemists' BULLSHIT post, I wouldn't have spilled crystalls all over the floor when I cut the jug open, so that now the whole fuckin place reaks of safrole!

ForYourInfo the density of 100% safrole is probably close to 1.100, because simple 3x crystallization gives me a clear liquid with d20 of 1.0994.  The d20 is definitely NOT 1.096 like has been posted by everyone on Hive, including you (LT/) and terbium.

All of this makes me wonder about the mentality of bees who inhabit Hive.  Baalchemist, for example. What was he thinking, what was his possible motive, when he posted that BULLSHIT about 1 gallon jugs and seed crystals and turning the jugs upside down overnight in freezer.  I tell you he NEVER actually did what he posted, because it is PHYSICALLY IMPOSSIBLE.  Who are these weirdos, who pose as cooks, but obviously make things up.  What is their fucking motivation?  And am I the only idiot who actually TRIES what others post?  Fuck, I'm mad.

If I were still posting, I would post a scathing write-up about separating safrole from sassy, and I would flame every single bee who ever once mentioned fractional distillation of sassy, then I would roast Baalchemist for being a blatant liar about those fucking upside down jugs, and then I would burn anybody who ever got the d20 of safrole wrong, and then probably call into the question the motivation of all those bees who post bullshit, and name them, one by one.  Baalchemist, youAxxxxx Mxxxxxxxxxx.  And I'm stone sober, btw."


Its quite interesting to stumble across a thread 6 months later such as this one. These are the type of people that blame all their inept behavior, stupidity & grossly undersized genitallia on anybody else other than their own inbred, downs-syndrome infested gene-pool. I bet he can type at least 70/wpm with one hand, while he's feverishly stroking his life-long inadequacy with the other. You should have just shoved the upside down jug up your ass, & then execute a handstand in your freezer, then you could've just spit out the non-safrole components along with all that other shit that seemed to be coming out of your mouth. If he was such the intellect he claims, why did his safrole end up all over the floor then?
(hint) because he's an idiot maybe, or possibly he could'nt perform the task one-handed..............


wyndowlicker

  • Guest
Hey now,
« Reply #108 on: January 17, 2003, 02:31:00 AM »
Hell,this is a blast from the past.Ill have to back BC on this one freezing works.You just have to know how its done. :P


gabd

  • Guest
Its freezing outside
« Reply #109 on: January 17, 2003, 05:07:00 PM »
right now , something like -25, -30 Celsius.
My oil deserves to be outside. I wonder if it will ever freeze. I cant do it at -14, but maybe that should be cold enough.

wyndowlicker

  • Guest
freezings fun!
« Reply #110 on: January 19, 2003, 11:18:00 AM »
Its fun and all but its a pain in the ass if you ask me.I still want to distill my final products just for good measure.If Im gonna do that I might as well distill it staight from oil.Its fun to see a whole gallon on oil crys up though. ;)


scram

  • Guest
Don't keep the temp so cold.
« Reply #111 on: January 19, 2003, 04:45:00 PM »
Don't keep the temp so cold. It never seems to freeze that way. Variate it from -10c to 11c over 1 to 2 hours and it should suddenly crystalize. Go to the local college and fill your hdpe cooler with some liquid N2. They have these tanks usually in the open. Drop some in the prechilled oil. Just be careful when handling the net. Dont drop it on your way out the door.

gabd

  • Guest
will try that
« Reply #112 on: January 19, 2003, 06:17:00 PM »
thanks for the tip!

pupilage

  • Guest
I found that
« Reply #113 on: January 21, 2003, 02:34:00 AM »
a very small piece of dry ice dropped into the cold sassy works also. Great to watch too. Only need to do that once then save a seed crystal to start any follow up freezings.

You still need to distill product latter but this does save on energy use and pump ware. Heck the fridge is on all the time why not use it.


RoundBottom

  • Guest
always on top
« Reply #114 on: January 21, 2003, 09:50:00 AM »
LT, in all the attempts at freezing, never once was any significant amount of impurities found at the bottom of, or inside, the crystal mass.  every time this method was used it was on a volume greater than 1L using 3 different batches of sassy oil. 

also, every time this was done a small depression formed at the top of the crystals, (a cup, if you will; it's evident in those pictures someone [Max?] posted a while back) that collects a pool of remainders.  also, keep in mind, DO NOT throw out the remainders, as there is probably a significant amount of safrole left.

i know SWIM has promised to do a comparison between a measure of oil distilled and an equal measure of oil frozen to compare which method is more efficient recovery wise.  if some other SWIM is willing to try this and report, it may finally put this debate to rest.  my theory is freezing does NOT get all the safrole out of the oil.

BOTTOM LINE: if you have a small amount of sassy (less than 1L), distil it; you probably need the experience anyway.  if you have, i don't know, say 20L, freeze it, and pool the remainders for later distillation.


scram

  • Guest
"a very small piece of dry ice dropped...
« Reply #115 on: January 21, 2003, 04:42:00 PM »
"a very small piece of dry ice dropped into the cold sassy works also."
Tried this once but it made the oil really opaque white. Was afraid as to the reason why it stayed like that.
Once your oil starts getting dark or amber it get increasing more difficult to crystalize the last amount out. The temps have to become even colder just to sustain a crystal that wont grow. Just save that nasty amber oil for the distillation rig and use that as practice oil. That what is planned to be done here. I think the average recovery rate of freezing is ~65% volume and that's without actually trying to salvage the amber stinky stuff. That takes more time and patience. Just the type of things I don't have right now until I feel comfortable.

pupilage

  • Guest
Perhaps i could have said that better.
« Reply #116 on: January 21, 2003, 09:32:00 PM »
a very small piece of dry ice dropped into the cold sassy works also. Great to watch too. Only need to do that once then save a seed crystal to start any follow up freezings. Take a seed crystal from the first freeze using dry ice save it. Then thaw out your oil. Place thawed oil back in fridge when the oil becomes cold again introduce the seed crystal back into it, should freeze into larger crystals and clearer.
Sorry for any confusion.


Arsenic

  • Guest
Seems to me...
« Reply #117 on: January 21, 2003, 10:38:00 PM »
It seems to this humble stranger that Baalchemist does Argox a dis-service.  Sure, we all love a good flame, but ARGOX (RIP) provided the Hive with useful posts.  Some well written, some less so, but he made a contribution and perhaps took the Hive more seriously than warranted.

What he wrote in the post Baal flames about safrole separation from sassy included never-before-mentioned-on-the-Hive data regarding the density of pure safrole (d20--1100g/l), which should have garnered him kudos, not flames.  Perhaps he was too emphatic in his language regarding what he percieved as a BS post by Baal, but what he posted had merit, and should have been enough to change the sticky threads that have persisted since the dawn of time that tell newbees to extract safrole from sassy by fractional distillation, a chore that is actually impossible using the equipment most clan labs have on hand.

ARGOX had his faults, like us all, but he seemed proud to have never posted bullshit, unlike others.

Baal--some respect for the fallen would be more appropriate than your flame.  Some of us have paid a heavy price for the knowledge given away freely to others.

Think about it.


goiterjoe

  • Guest
you lazy bitch
« Reply #118 on: January 22, 2003, 05:40:00 PM »
extract safrole from sassy by fractional distillation, a chore that is actually impossible using the equipment most clan labs have on hand.

Well then get off your lazy ass and go buy the fucking equipment you need to do this with.  It's not like you're going to freeze the ketone out of a post performic reaction, now is it?  I've personally never gotten safrole to freeze before, so I'm not going to recommend it to anyone.  On the other hand, I have fractionally distilled safrole from sassafras oil a few times and didn't find it to be much of a chore.  It would take less time to do than freezing the safrole out unless you're talking about doing over a litre at a time, and then it would just be a matter of getting the appropriate equipment to do so.  You're going to have to scale up everything else at some point.

The purpose of the hive is to discuss the chemistry of mind altering substances, not to teach morons with no chemical experience how to make X in their bathtub.  Keep that in mind before you go about asking for methods that don't require real equipment or proper cleaning techniques.


Arsenic

  • Guest
You don't have a clue, do you?
« Reply #119 on: January 22, 2003, 10:19:00 PM »
Goiter:

Don't call me a lazy bitch.  You have no idea.  Show some respect.

Why do I say that fractional distillation of safrole from sassy is impossible with equipment most clan chemists have?  Because it is.

Fractional distillation REQUIRES a packed column, not just a vigreux.  You need to understand the word "fractional" and what it implies in distillation.  Until then, you only demonstrate your ignorance.  To properly separate safrole from the other ingredients in brazilian sassafras you must use a long packed column, maybe even four to five feet long.  Who the fuck wants to invest in one of those?  When, as was pointed out in the beginning of this thread, that you can separate 20liters of safrole in a day with NO effort, by using fractional crystallization, i.e. freezing.  This is a fact.  You cannot separate pure safrole by simple vacuum distillation as expounded in the sticky threads, or as you say.  This is also a fact.  Have you ever checked your distilled product, safrole, for purity?  Do you even know how?  Check the d20 of distilled safrole from sassy against safrole obtained by freezing sassy and you will see that a higher purity product with MUCH higher yield is obtained by freezing.  The MP of safrole is -11C exactly.  Bees should take advantage of that high MP to separate safrole from all the other oils in sassy, which have MPs much, much lower.

But why do I even bother explaining this to you?  You come off as a complete moron from your post, and first impressions are generally correct.

Learn some manners, while you're at it.  You have no idea who a Stranger might be.  Some have more fucking knowledge about this subject than you could imagine.