09-18-03 08:45
No 459710
SWIM stuck a container with approx 500ml sassafras oil in the freezer for a few hours to see a whitish-yellow crystalline mass that reeked of sassafras oil; SWIM was curious if it would be way to easy to simply turn upside down the narrow rimmed 800mL Jar that has 500mL frozen sassafras in it and decanted excess oil to retrieve the frozen safrole (hopefully)
'A Helpful Bee, is a Friend Indeed'
(Hive Bee)
09-18-03 09:48
No 459721
This is what SWIM did,
I does not really matter what you freeze sassafras in, preferably a beaker or jar or container of simular nature. SWIM put 500ml in an let it freeze, when crystals appreared SWIM removed and placed another 500ml in the freezer also, but, placed some of the crystals formed from the 1st freeze in the second batch of oil.
leave in for a couple of hours, SWIM found that with in 2 hours~ it was full of crystals both beakers, dont let the whole thing freeze wait till there are a big heap of crystals and then pour the excess of and then repeat, by placing a few in crystals in the run off..
just another point that SWIM would like to mention, just let the crystals defrost in the beaker that they formed in, depending on purity level of safrole in your oil it may vary slightly for you.
SWIM has explained it simple cause it really is that simple
all the best.
(Hive Addict)
09-19-03 04:26
No 459845
(Rated as: excellent)
Do not put Sassafras Oil in the freezer!
If you read the information provided by LT Post 294426 (LaBTop: "Sassafras components data", Methods Discourse) it tells you that Eugenol has a MP of -7.4 . Celcius.
So, if you place your Sassafras oil in the freezer then you may freeze Eugenol along with it.
Here is what has worked well
You will need:
Container of Sassafras oil
Dry Ice (frozen CO2)
Solid safety gloves
Solid plastic Ice cube tray
Solid Glass Bottle with cap
Refridgerator/Freezer
Now:
1. Get some dry ice
2. place some sassafras oil in 2 of the cube spaces in an ice cube tray (2-3 mls in each space)
3. Sit ice cube tray on dry ice for 15 minutes (wear gloves)
4. After 15 minutes place (now) frozen Sassafras oil in ice cube tray into freezer.
5. Chill empty glass bottle and container of Sassafras oil in refridgerator for 6 or more hours.
6. Pour chilled Sassafras Oil into chilled glass bottle.
7. Drop in one of the frozen crystals of Sassafras oil, from ice cube rack in the freezer, into the chilled bottle containing chilled Sassafras oil, then return remaining crystal to the freezer.
8. Place bottle back into the refridgerator and leave for a couple of days to slowly crystallise your Safrole.
9. After 2 days, pour off remaining solution and store (it contains small amounts of Safrole)
10.Place bottle with crystallised Sassafras oil into a cold water bath, then warm water, them hot water, in order to melt crystals. (Don't heat up the cold bottle too quickly and crack your bottle because of thermal shock, or you will be a very sad bee.
)11.Place Safrole laden Sassafras oil back into the refridgerator and chill for 6 or so hours and repeat steps 7-10.
12. You now have a suitably pure batch of Safrole.
P.S. You would then keep some of the double frozen safrole crystals, and place them in the freezer to use as future "seed crystals"
Read and learn: http://www.polyarchy.org/
(Hive Bee)
09-19-03 08:23
No 459893
Its amazing another day passes and another BEE learns something... thanks for the pointer as well, SWIM will try this and see what happens
Also ABOLT i understand what you are saying.. what you mentioned is good if you just wish to freeze to obtain safrole, but SWIM thinks all should distil anyway, which would counter the Eugonol prob/concern.
thanks anyway SWIM now knows something that SWIM did not know before.
Cheers
(Hive Addict)
09-19-03 23:30
No 459993
Just out of curiosity which is the correct melting point for eugenol: Chemfinders 15.44C, My chem dictionarys' 9.2C, IPPDs' -7.5C or Merck Indexs' -9.2C?
And if you google eugenol melting point you'll get at least 3 more alternatives.
Why such a range?
(Chief Bee)
09-19-03 23:52
No 459996
Because different researchers have managed to purify their eugenol to different degrees before measuring the melting point.
Also, literature melting points which are reported to be below room temperature tend to vary more than those which are considerably higher, because of the increased difficulties inherent when working below RT.
(Hive Addict)
09-20-03 00:10
No 459998
Thanks Rhodium! Suspected purity was coming into play but wasn't sure.
(Hive Bee)
10-02-03 04:22
No 462202
wondering if a kind bee could help me determine the problem. Everything goes fine with freezing the seed crystals and placing them into the pre-chilled sassy oil. Once I drop the crystal into the jar, the entire jar immediately forms crystals all over, just as predicted. here is where the luck runs out. I place the jar of crystallized sassy into the refrigerator, but instead of slowly growing, the crystals slowly shrink. eventually all of them melt away. what could be the problem? I put a thermometer in there and it reads between 6-8 deg C. Is that too warm for them to grow? It must be noted that when i put it in the freezer, the crystals grow rapidly. but the initial post in this thread says not to freeze as it will freeze the eugenol as well. suggestions?
Theres nothing to be afraid of, just concentrate, and trust the music.
(Hive Bee)
10-02-03 06:50
No 462225
The pre-cooled Sassafras is to chilled, SWIM did not have to adjust fridge as the temp seemed right..
Once you have seeds cool the sassafras in the fridge only for a little while then place seeds and then it will crystalize the lower you can get your fridge the slower and purer the safrole..
Trust SWIM, SWIM thought that it was pure as pure can be, unitl done in fridge the color was piss, and whoha in the fridge clear, with faint smell.
cool slightly then seed try that, let us know how you go.
hope that helps
Eugonol will freeze in in the freezer try lifting the temp in fridge but not to much as you will get the same prob as the freezer the whole thing will crystalize..
just fuck around with fridge.. youll be right
(Newbee)
10-03-03 22:37
No 462431
SWIMs already distilled out the safrole from the sassy but swims wondering now about the purity of the safrole. Can swim do the procedure exactly as abolt describes just using his safrole instead of sassy?
(Hive Addict)
10-04-03 04:45
No 462476
If you cool down your distilled Safrole in the refridgerator for a couple of hours, then drop in a seed crystal then you should see the Safrole crystallise in front of your eyes. If it doesn't start crystallising straight away then I would question the purity of your Safrole.
Forget distilling, double or triple Freezing is the only way to go.
Read and learn: http://www.polyarchy.org/
(Stranger)
10-11-03 22:31
No 464060
pop swims sassy in the deep freeze and let the whole thing freeze then tip swims container upside down and let the shit melt and drip off till swim has pure safrole crystals. recycle if swims sassy is of hig enough safrole content. swim says pint jars (the kind for vodka) work good has long as you don't fill them all the way full.
(Hive Bee)
10-13-03 10:13
No 464363
pop swims sassy in the deep freeze and let the whole thing freeze then tip swims container upside down and let the shit melt and drip off till swim has pure safrole crystals.
That doesn't make sense? You are putting it in the deep freeze, which means you are freezing a hell of a lot of things that aren't Safrole. Eugenol would be the big one that someone pointed out here recently. And what is this let it melt to obtain pure safrole? Its not like the contaminants are going to be frozen on the outside of the safrole molecules, so you just shed the outer layer and are good to go. When you froze it quickly, a lot of crap became solid inside the safrole crystal matrices.
This is not a good way to purify safrole. Please do not post suggestions that refute everything everyone else says on this board w/o good ref's and theory to back up what you are saying. Otherwise, you just confuse more people who wouldn't know any better.
-Sifty
"...Come with us and leave your earth behind..." - Chem.Bros.
(Stranger)
10-13-03 17:06
No 464420
Cub has used deep freeze to purify his safrole and he has got a density of 1.096 at with 3 freezings.
(Newbee)
01-17-04 03:31
No 482941
Just out of curiosity, she placed a thermometer in her freezer and after several hours noticed that the tempurature was at -12°C. She tried to adjust the tempurature in the freezer to warm it up a but, but the tempurature only raised to about -2°C. She placed about 500ml of sassy for 8 hours. After 8 hours, the entire beaker was frozen. Does this mean the sassy does not contain any safrole?
According to what she read in LabTops posts, none of the constituints in sassy will freeze with the exception of the safrole. She was wondering if anyone else experienced a complete freeze but was able to adjust the temp in their freezer and ultimately achieved clear safrole crystal formation while the other crap did not freeze.
(Newbee)
01-17-04 04:06
No 482943
IN swim experience, swim had the same problem, what you have to do is, this: create a seed crystal in the freezer, as what you have done is right, if the sass you have is high in safrole then the majority of the liquid will freeze..
IMHO swim got a seed crystal from the freezer then put the sass in the fridge and then added a few seed crystals to the chilled oil in the fridge.. this way the safrole freezes out slower and you get bigger purer crystals instead of the hole thing just freezing...
do this once in the fridge as you get some crystal, for instance the whole bottom and the sides are blantantly covered in crystals drain of the piss color liquid, and you should have clear crystals remaining, then put them in a sink with luke warm water to melt, the you should have clear oily solution this is the safrole...
repeat the process, each time untill you have done all the sassafras... it is really that easy, hope that helped'
(Newbee)
01-17-04 05:12
No 482951
Thanks! She would like to know of the temperature in your refrigerator. Does it matter?
(Hive Addict)
01-17-04 05:27
No 482953
Thanks! She would like to know of the temperature in your refrigerator. Does it matter?
If your refrigerator is above 6 or 7 degrees celcius then you may have trouble crystallising your safrole (and your refridgerator is probably broken). Try to keep the temperature around 2-3 Celcius. Milk will curdle above 4 celcius so, unless this is happening, you can assume your refigerator is at a suitable temp.
The early bird may get the worm, but it's the second mouse that gets the cheese.
(Newbee)
01-17-04 17:40
No 483037
Ok, SWIM made some seed crystals and placed about 1 teaspoon worth of the crystals into a beaker with about 200ml of sassy that was in the refrigerator at 4°C. After about 20 minutes, the entire bottom of the beaker has these clear crystals that look just like minature octagon-shaped stir bars; is this safrole?
It's been about 1 hour and the temp of the refrigerator is at 7°C, and there appears to be slightly more crystals than before. How long should the beaker remain in the refrigerator at this temp? It appears as though the crystals are forming extremely slow.
(Hive Bee)
01-18-04 00:00
No 483087
d20 of 1.102 to 1.103 is more like it.
HA HA HA HA my evil plan is working.
(Newbee)
01-18-04 03:09
No 483114
SWIM has extracted the crystals for the third time, and contrary to other posts, after the melting the crystals, the oil still has a slight yellow tint, but much less yellow from the original sassy, that's for sure.
I'm sure SWIM can recrystallize the crystals again in order to get rid of more impurities.
(Newbee)
01-18-04 10:41
No 483152
YOURE on the right track SWIM didnt know the temp of his fridge but the crystals formed nice and slow, and were bigger then placing in the freezer... turn the fridge down slightly and try it again, as it is easy to do once you have it sorted.
(Hive Addict)
01-19-04 05:42
No 483263
is this safrole?
Yes, three recrystallisations is usually sufficient.
You can continue to recrystallise until all color is removed, if you are anal about purity.
The early bird may get the worm, but it's the second mouse that gets the cheese.