menthol_man (Stranger)
10-05-01 20:21
No 220835
      Safrole Crystals  Bookmark   

Ok bees... I have been able to initiate the crystilization
of safrole in my freezer.  You can get pure safrole via
freezing for you low budget bees.  The down side... it's
kinda hard to do and you better not need it quickly...

Here's what Menthol man did...  I threw the safrole in
the freezer for 10 hours... I noticed a few crystals...
very small ones.  Then I noticed that there was a very very
thin seperation... less than a layer really... when i would
blow in it to get a ripple there was a difference in the way
the light refracted... it looked a little different.  When
the ripple returned the layer swirled together slowly and
crystalized... very small crystals mind you.  I blew into
it again.. and after the ripple a SMALL crystal appeared.
SO im at the right temp for crystalization BUT safrole
needs a little help until it can get together enough to
work on its own.  So do this a couple of times and close up
the freezer... dont let me un freeze... it can take a time
or two to get it going but once the crystals get big enough
it will slowly grow on its own.  I rebember another post a
bee swirled a couple of time and got crystals... just blow..
so I will keep this thread updated on safrole purification
via thermal process.  Good luck bees

Gott Mit Uns!
 
 
 
 
    menthol_man
(Newbee)
10-05-01 23:34
No 220861
      Re: Safrole Crystals  Bookmark   

And wouldn't you know it... 6 Hours later there was
a MASSIVE amount of the PUREST safrole crystals I have
ever seen.  And I did it with NO GLASS!

laughlaughlaughlaughlaughlaughlaugh

Gott Mit Uns!
 
 
 
 
    spric
(Hive Addict)
10-10-01 21:51
No 223048
      Re: Safrole Crystals  Bookmark   

Aren't menthol cigarettes used to smoke PCP on?wink

4:20
 
 
 
 
    zooligan
(Hive Addict)
10-11-01 05:35
No 223137
      Re: Safrole Crystals  Bookmark   

Slapping a super-chilled container of sas or saf can sometimes cause nearly instantaneous crystallization.  Pretty fucking cool to watch...

"And if we don't get some cool rules ourselves, pronto, then we'll just be bogus too!"
 
 
 
 
    Osmium
(Stoni's sexual toy)
10-11-01 06:03
No 223146
      Re: Safrole Crystals  Bookmark   

If you want purity you want those crystals to grow slowly. The slower the better. I suggest you
1) find out what temp a semi-crystallized batch of your sassy has
2) fiddle around with your fridge until it produces that temperature, or 1-2 degrees lower
3) have some seed crystals ready
4) let a batch of sassy cool down close to the temp you recorded in 1)
5) seed that sassy with a few crystals
6) give it whatever time it takes to crystallise 60-70% of the sassy
7) decant the uncrystallized oil, save it for some future rainly day
8) repeat all of the above
 
 
 
 
    zooligan
(Hive Addict)
10-11-01 08:20
No 223192
      Re: Safrole Crystals  Bookmark   

While it is cool to watch the crystals grow rapidly right in front of your eyes, you are right, it should be melted and re-crystallized.  After pouring off the dark oil from a rapid crystallization, the melted remains usually have no problem spontaneously crystallizing very slowly (over a couple of days) at fridge (not freezer) temps.

z


"And if we don't get some cool rules ourselves, pronto, then we'll just be bogus too!"
 
 
 
 
    Scooby_Doo
(Hive Bee)
10-12-01 17:08
No 223839
      Re: Safrole Crystals  Bookmark   

Not so long ago I ran across a ref which used Pet ether to recrystallize safrole. I have even seen safrole crystallize in cold THF.
 
 
 
 
    kdog_x
(Stranger)
01-06-02 02:19
No 253184
      Re: Safrole Crystals  Bookmark   

This procedure sounds very nice, but what kind of purity should be expected in the final product. Anyone ever Distill afterwards to check it?
 
 
 
 
    Rhodium
(Chief Bee)
01-06-02 02:46
No 253189
      Re: Safrole Crystals  Bookmark   

Has anyone been able to grow large (1-3 cm) crystals of safrole or isosafrole and taken a digital picture of them? I have begun collecting precursor pictures.
 
 
 
 
    ChemicalSolution
(Newbee)
01-06-02 23:43
No 253465
      Re: Safrole Crystals  Bookmark   

You don't need seed crystals at all.

If you place you sassy in the fridge for 1hr then scratch the flask with a glass stirr rod, you will find a load of crystals in your flask in another hour. 

Now melt (most) of these crystals by running the flask under warm water.  Place the flask back in the fridge (8-9C) and the orange crud will form on top of the safrole crystals.  Pour this crud off then run the flask under warm water again to melt 90% of the crystals and then put in the fridge again.  Repeat until desired purity is obtained.  This is a heck of a lot less laborsome than a distillation.

Ch
 
 
 
 
    baalchemist
(Chef d'Equippe)
01-07-02 12:13
No 253681
      Re: Safrole Crystals  Bookmark   

Baal takes 1 gallon jugs of Chinese sassy and tosses them in the freezer for about 30-40 mins. Then a seed crystal is tossed in and the jug is put back into the freezer, but this time turn it upside down and leave it overnight. The next day the jug will be completely crystallized and the residual crap has found its way to the bottom(which is actually the jug top) and can be removed easily. Baal will let this 'drain' upside down over a beaker for a few mins and is left with clear white safrole w/S.D.~1.1 . This is then vac. isomerized with KOH 'as is'. Been doing it that way for a couple years now without a problem, of course Baal
has been fortunate enough to have only acquired that 95%+ stuff in recent years.

GODISNOWHERE
 
 
 
 
    RoundBottom
(Hive Bee)
01-08-02 11:59
No 254090
      Re: Safrole Crystals  Bookmark   

exceded transfer alottment, i think.  too popular :(
 
 
 
 
    PoohBear4Ever
(Junior Service Representative)
01-09-02 16:20
No 254553
      Re: Safrole Crystals  Bookmark   

Beautiful crystals smile! I have a pair of tweezers that look exactly as those the pictured above cool.

PB
 
 
 
 
    Sektor7G
(Stranger)
01-09-02 19:38
No 254619
      Re: Safrole Crystals  Bookmark   

Wow, those are very nice looking crystals!!! Id like to be on the receveing end of that batch, when the time comes.

[quote]Life is like a box of chocolates, short n sweet!shocked
 
 
 
 
    Goodtimes
(Hive Addict)
01-12-02 06:35
No 255601
      Re: Safrole Crystals  Bookmark   

Very nice mad...


"The gods are too fond of a joke."  (Aristotle)

 
 
 
 
    acid_egg
(Hive Bee)
07-13-02 06:54
No 332060
      pretty pictures  Bookmark   

Wowcool  these crystal pics are so pretty.Stick them on your hard drive for a dreary day.smile

(rated as:eggsellent)
 
 
 
 
    raffike
(Hive Bee)
07-13-02 09:21
No 332090
      The last one is good for desktop wallpaper.  Bookmark   

The last one is good for desktop wallpaper.Anyway seems like you have good digicam.

A friend with speed is a friend indeed
 
 
 
 
    humidbeing
(Can't SWIM)
07-13-02 17:20
No 332236
      as  Bookmark   

Well. I know mine sucked, but I tried!
 Actually Swim has found that the larger % of non-safrole constituents the oils has, the longer and more symetrical
the crystals will be.
 Swim wasted quite alot of gold before finding this out.frown

CG I miss you sweety, I really do.
 
 
 
 
    spectralmagic
(Hive Bee)
07-28-02 16:23
No 338232
      SWISM would like to report that this technique ...  Bookmark   

SWISM would like to report that this technique appears to work with Virginian Cedarwood (Juniper Virginiana) oil as well...

For a week or so the oil remained liquid in his freezer, but just now he's noticed little tiny crystals forming, with thin "blades" starting to grow at various points at the bottom of the beaker.  This is a self-defrosting freezer so he doubts this is water contamination freezing out.  Now, this oil is supposedly 11% safrole and 6% isosafrole, so most of it will remain liquid, hopefully easily poured off the safrole crystals (and isosafrole?)... good enough for SWISM!

One concern is that there might be other oils in J. Virginiana that freeze at a similar or higher temperature...  well, melting point & boiling point tests on the collected crystals should tell him something...

Add your thread to the rich tapestry of conspiracy...
... and wave hello at the satellites!
 
 
 
 
    scram
(Stranger)
07-29-02 09:32
No 338564
      "Actually Swim has found that the larger % of ...  Bookmark   

"Actually Swim has found that the larger % of non-safrole constituents the oils has, the longer and more symetrical
the crystals will be"

I also have noticed this.

I got sick and tired of trying to start a crystal, especially during these hot months. So I decided to try using "Duster" brand computer canned air sprayer. It's 1,1,1, 2-tetrafluroethane. I knew it had a low boiling pt solvent and figured it should disolve the oil and precipitate the frozen seeds as the solvent evaporates. I also figured that it would be best since there is no lubricating oils in it like freon R-12 cans avail at Wally world. Put it in the freezer to prechill it and the oil sample too. However once I got the solvent in the bottle and poured in about a 15ml oil sample, I found out it wan't miscible and floated on top of the solvent. I swirrled it and few times and sat it back in the freezer for 5 minutes. Nothing. This time I shook the open bottle a little and the whole thing turned into a weird white mass of trapped air bubbles, a helleva lot of frozen condensation (looked like 25ml water in it, now frozen) with the mass hold the oil. So I gues it worked, but the damn crystals a probably too small to sift out of the white mass. Maybe I can get the water to slowly melt leaving the crystals.