04-04-02 17:34
No 292562
still having problems from the begining it went like this.
Simple distillation of 250ml sassy
got silocone grease
got ice water running threw the condenser
first start stirring on 5
attach vacuum already running
then turn on heat to 1 out of a possible 10
first thing to come over was 64c 30ml of very clear watery oil that doesnt sink when dropped in water.Bath temp 110c.
then temp raised to 74c held there gave 10ml or so.then raised up to 84 holds there 1dp per 13 sec or so.bath temp 145.
when nothing came over for 2 min took off emptied put back on.
then it skyrockets to 114c then slowly raises to 120c oil temp 167.stays there for a while then nothing.
So now total swiw has maybee 50ml.
took it up slowly till it hit 130 then it gave off a slightly clear yellow oil with what looks like rainbows its like what a puddle looks like when oils in it.It didnt give alot maybee 10ml and it stopped took it up to 140c and nothing so swiw stopped never got the bath temp past 200c to keep from frying the oil till swiw figures this out.think possibly the oils bad.
Now keep in mind swiw has raised the temp no more than 1/2 click every hour and still nothing.
I will choke untill I swallow!Who are you to judge or strike me down!Miss you Kerra!
04-04-02 18:53
(Rated as: redundant)
(Greenhorn)
04-04-02 18:59
No 292612
Sounds like u might have some none safrole containing sassy oil. Is it essential oil of sassafras?
We'll soon find out if I'm a chemist or not!
(Hive Bee)
04-04-02 19:00
No 292615
Either your vacuum source is not strong enough or you have bad oil.
Leonard Cohen cheers me up !
(Stranger)
04-04-02 19:39
No 292629
Try distilling ATM up to Safrole's BP (234*C) it should withstand that temp. Later
(Hive Bee)
04-04-02 19:51
No 292636
yes its essential oil Swiw knows what hes looking for no internal use external use.sasafrass albidum.And swiws pump is supposed to be prime for this yelowjacket 15 microns.
I will choke untill I swallow!Who are you to judge or strike me down!bye bye red bee.
(Hive Addict)
04-04-02 21:10
No 292687
LOSE THE VACCUUM
I think it's been suggested 5 times, in several thread on this subject. TRY IT. I seriously believe the vaccuum is way to strong for this. Safrole doesn't scorch at its boiling point. There is no need for you to be afraid of it. There is no need for you to post over and over about how you can't get safrole while refusing to try the suggestions the bees here give you.
So if you want to keep trying to get safrole with your yellowjacket pump, and won't try to do a simple distillation to verify that there is any safrole in the sassafras to start with, maybe you should try a new hobby.
I'm sorry for being rude. Maybe it will wake you up.
MDP2P is when you need to be careful about the high heat.
Mastery is based on the understanding and practice of technique.
(One Man Show)
04-04-02 21:11
No 292688
Was this portion of sass oil one that you tried to distill previously? Or was it a fresh/new sample?
Describe the sass oil, its appearance, color, odor.
"Have we descended to the level of dumb beasts?" Fear & Loathing
Be loved and blessed hp and cg!!
(Hive Addict)
04-04-02 23:36
No 292726
freeze it and be done with it.
i learned a thing or two from charlie dontcha know.
(Stranger)
04-05-02 05:22
No 292805
I may be so that your sassy doesn't contain any safrol(like said before) because some distributors sell sassafras oil that contains no safrole.Try 232C without vacuum or just freeze it to -14C(safrole melting point) like Strike wrote in his/her book
(Hive Addict)
04-05-02 06:49
No 292832
11.2°C is the mp of safrole according to Merck and chemfinder.
Mastery is based on the understanding and practice of technique.
(Stranger)
04-05-02 11:50
No 292909
You may not see safrole crystals form without agitation in the freezing method, though, right? Or at least crystal formation will be slow.
(In a dream, I saw a beautiful maiden place some sassafras in a small glass container, and put in a freezer. Tiny white crystals formed on top. The beautiful maiden then blew on the sassafras. More crystals appeared. Afterwards, she shook the container for further agitation. The maiden put the sassafras back in the freezer. Unfortunately, I woke up before the dream finished. Perhaps the dream can finish in the next few weeks.)
(Stranger)
04-05-02 13:00
No 292942
Buy an aspirator and see if there's a differnce, then try no vacuum at all, as noj and a bunch of other people have already told you, in this thread and others. If you get the saffrole, then it's your pump. If not, it's your oil. Right?
"No...why would I need a fire extinguisher?"
(Hive Bee)
04-05-02 14:17
No 292979
Try again with an aspirator, buy a GOOD one ( for instance, NALGENE, plastic, very good even with low water flow ) and use it also for filtering, evaporating solvents, etc. Save your vacuum pump for serious work, like ketone.
Also, your oil might be dirty again. I have this problem with my vacuum pump, is a good one, single stage rotary vane, but everytime I use the vacuum degrades, I have to replace the oil. How do I know ? I measure the vacuum with my vacuum gauge. I am planning to add a trap, but I can't do it right now, so I just distill fast, start with aspirator to get out a bit of H2O vapor and other stuff that degrades the vacuum when absorbed in the oil.
Repeat, get an aspirator. Also test your oil, use the FSE.
(Hive Bee)
04-07-02 13:13
No 293792
Alright here is swiws reason for not taking it to atm tep.
the oil smokes out my space and there is not sufficent ventalation.as far as freezing goes the oil swiw has been in the freezer for some time now without freezing swiw will try turning up the freezer and see if this works.doesnt anyone else have problems with there peanut oil smoking?
I will choke untill I swallow!Who are you to judge or strike me down!Miss you Kerra!
(Greenhorn)
04-07-02 14:40
No 293836
your oil will smoke if it's old and used. try fresh oil.
We'll soon find out if I'm a chemist or not!
(Hive Bee)
04-07-02 15:20
No 293852
Smoke and fumes sometimes cannot be avoided. the smoke from peanut oil, although being slightly irritating to the eyes, it really not all that bad. A friend of mine has the same pump that you are using, and it is pretty strong. If you have never done an ATM distillation you might want to try this first. Make sure that the container your oil bath is in has good contact surface on the plate, and sometimes insulating the oil bath is neccessary. You should see the safrole vapors come up almost like smoke if you put a black peice of paper behind you apparatus. The higher the temp, the higher the vapors rise. Make sure they are flowing into the condenser consistently, this will be visible. Use a small flask, as often there is a lot of reflux on the walls of large flasks which slows things down. A tip that I read here and tried, and can vouch works well, is to completely immerse the flask in the oil bath. A good drip rate (at ATM) would be a drop about every 3-4 sec. Sometimes atmospheric distillations take forever, especially if you have a lot to distill, but you should probably try this if you are having difficulty with your vacuum.
Flip
_flip_@hushmail.com
(Hive Addict)
04-07-02 15:49
No 293866
(Rated as: excellent)
take a small amount of your oil, about 4mL, and put it in a small glass vial (like the kind you get GHB in). stick this in the freezer, and it should crystalize. scrape a small amount of the crystals and put in pre-chilled flask/jar of oil. put the oil back in the fridge (not the freezer). crystals should be noticable in 5 minutes.
pre-chill the oil, as if you put the crystals in warm oil, they will just melt. replace the small vial of frozen oil into the freezer to keep it crystalized.
i learned a thing or two from charlie dontcha know.
(Hive Bee)
04-07-02 18:20
No 293923
Please be careful, I think if your oil is starting to make smoke it is also close to igniting. I have never tried to distill sassy oil at normal pressure, is is very easy with an aspirator. If you would like to try it at normal presure, could you use a heating mantle ? Boiling stones might be OK in this case.
(Stranger)
04-07-02 18:31
No 293931
Do what roundbottom says!
You've been dealing with this since our mutual friend
talked w/me about it!
Do exactly what RB says, htis is in fact as good a method of purifying as distilling at least for 1 alkene > 2 alkene
Ketone is gonna bee exstremely problematic if ya can't
get this one ouy of the way, and freezing won't help in
that area!
This is humid by the way.
Also this is the preferred method >safrole for some respected bees here1 (madmax for one)
(Daddy)
04-07-02 22:50
No 294073
(Rated as: excellent)
YES YES and YES!
This is the one and only no bullshit way to purify sassafras, also confirmed already to me by another well respected member, who couldn't believe his eyes reading all the rantings about distilling, refluxing and smoking stillpots after he simply freezed out in 2 subsequent freezings all impurities, and obtained a clear slightly yellow 1-alkene oil (safrole) with a density of 1.0982 at 20C, which is sufficient pure (ideal is 1.1000 density at 20C for Safrole) to proceed with an overnight full vacuum isomerization with 5% 99%KOH to 2-alkene (iso-safrole).
Thanks, MadMax, Roundbottom, Argox. There should be a whole lot more of -- no-bullshit, I wanna see it with my own eyes -- members like MadMax, Roundbottom and Argox.
I must admit I have tried to assist in the endeavours of so many, by describing how to fractionally distill sassafras. However, I never needed to do that, Safrole could be get at bottom prices in my times. MDP2P also, by the way. Nobody even thought about buying sassafras oil, redundant then.
Times have changed, so this is my new stance on Sassafras oil purification:
FORGET DISTILLING SASSAFRAS, FREEZE IT slowly 2 TIMES, decant the unfrozen oil, freeze the melted Safrole slowly again to collect a next crop of impure non frozen oil, and decant the non frozen oil again, this will not freeze at all, especially near the temperatures where the safrole freezes out!
Congealing point of safrole is according to Rhodium table +11.2 C, which was observed as the exact same congealing point for the 1-alkene.
You get rid of Eugenol, alpha and beta-Phellandrenes, various Sesquiterpenes, Pinenes and Camphor and other traces of different oils in a few relaxing hours by the TV set. LT/
PS: see also thread Post 220835 (menthol_man: "Safrole Crystals", Methods Discourse) with beautifull pics of MaDMAx, or his pics at:
http://www.geocities.com/marktsas/saf4.j
http://www.geocities.com/marktsas/saf2.j
http://www.geocities.com/marktsas/saf3.j
See also Baalchemists easy method for freezing Sassafras: Post 253681 (baalchemist: "Re: Safrole Crystals", Methods Discourse),
and Osmium who gives wise advice in Post 223146 (Osmium: "Re: Safrole Crystals", Methods Discourse).
WISDOMwillWIN
(Daddy)
04-07-02 23:13
No 294087
Damm, now I remember who the guy was with those damm nice pictures, I wrote the above post in a hurry, ofcourse the same gratitude goes to MadMax ! Thanks for the inventive work.
Let's also not forget Eleusis and Strike who also already indicated that this was the easiest way to proceed many years ago! LT/
WISDOMwillWIN
(Hive Addict)
04-08-02 02:21
No 294162
(Rated as: excellent)
yeah, that's the post i was looking for a couple weeks ago.
ok, here are a couple additions...
1. don't use a freezer. everything will freeze and you'll just have to let it thaw out again. use the fridge. slow and low, that is the tempo. the slower the better.
2. leave it for at least three days. SWIM uses 1L apothacry jars (don't ask, small fridge), and let's them crystalize for a minimum of three days. pour off the remainder after three days into a collecting jug/jar. keep this for further distillation.
3. repeat at least one more time. let it thaw out overnight or put the jar in a pot of warm water. once it's completely liquid, put it in the fridge again to cool. then, add a seed crystal and do it over. you will find another bit of impurity to add to the collecting jar.
4. don't forget to periodically add some more safrole to the small vial to ensure your ability to continue this simple method.
SWIM gets between 70%-80% asfrole (EDIT: ok, safrole, not asfrole) from the oil. SWIM doesn't know the exact content, but it seems there might be more safrole, so don't throw anything out. SWIM will attempt to distill out any remaining safrole. does anyone know if this get's all the safrole out or just most?
look kids, it does not get any simpler than this. SWIMs a lazy fuck and used this method because SWIM didn't want to distill for hours. it works, it's easy, it's effiecient, and there's no long distillation to watch.
i learned a thing or two from charlie dontcha know.
(Hive Addict)
04-08-02 02:33
No 294167
ok, i'm 100% certain you don't need liquid nitrogen or dry ice to make seed crystals. i believe you when you say it will work, but it strikes me as duck huntin' with a SAM missile.
the trick, i believe, is to use a narrow vial, like the 5mL screwtop borosilicate vials you get GHB in (i'm sure they have other uses).
someone mentioned vibrations, another mentioned dead chickens, again... sound like voodoo. just put some oil, or even better, some distilled safrole, in the vial, stick it in the freezer until it comes out solid. pull it out once in a while. tilt it back and forth, stick it under your arm, whatever. SWIMs fridge was encrusted in glacial freezer floes, maybe that had something to do with it.
i learned a thing or two from charlie dontcha know.
(Hive Bee)
04-08-02 03:04
No 294179
Well although freezing safrole would be the simplest, no hassle way to get safrole from sass, I might also point out for the newbee's reading that there is something to be said for the good old fashioned art of distillation. This is a skill to be mastered for all chemists, and without the experience of simple and fractional distillation your options as far as synthesis become extremely limited. For window, I would go ahead and freeze your sass, but also do not give up in your efforts of distillation. I think you will find that your flaw is with the equipment, but it is also a necessary skill to know what will work and what will not. Now freezing safrole is pretty much equivalent to distilling in the sense that differences in temperature are used to seperate the fractions of a substance, but freezing will not always be a viable option. So do not give up in your efforts, and even if this method should become more common than distillation, let's all keep 'the old fashioned way' in our minds, and even after all of our current methods become far far obselete, we will have something to tell our grandkids when they are cooking drugs.
Flip
_flip_@hushmail.com
(Sector G)
04-08-02 03:18
No 294181
Freezing and boiling have been known since the dawn of time, both of them. They are both viable means of chemical seperation, and there are even more methods to accomplish the same.
There are other situations directly involved with clandestine chemistry where distillation reappears, such as the purification of ketones and freebase amines. Tradition plays little role in this at all IMO; it is much more of an efficiency and resource issue, and each situation has many factors such as the user's equipment, skill, the compounds being seperated, etc.
I do agree with your statement that one should not think they can avoid all distillations simply by freezing. If that is what some of you think, heh, be prepared to have a surprise in the future.
PrimoPyro
Vivent Longtemps La Ruche!
(Hive Bee)
04-08-02 05:00
No 294193
Ahhhhhhhh Primo.... I love you man, youre always one to chime in with a perfectly analytical and well phrased contradiction. Of course i'm just up late rambling, and my post was more of a facetious remark towards the process becoming obselete due to all of this praise. As if distillations would ever be out of date? Just to re-emphasize for future readers of this thread, the easy way is not always the best way, take the hard road before you find the shortcuts.
Flip
_flip_@hushmail.com
(Daddy)
04-08-02 11:33
No 294290
The hard way was taken at first:
A very professional fractional distillation (with a glassbeads packed vigreux reflux column) of sassafras oil at first, taking ages, and resulting in a product with a density of 1.088 , much too far off from the 1.1000 density of pure safrole.
Then the 2x freezing method was applied, and the ONLY conclusion of that can be:
All distillation threads and posts regarding sassafras purification can be forgotten.
Totally REDUNDANT.
Very simple, just keep checking your densities untill you reach that magical 1.1000 mark.
And believe me, Argox is a researcher who --only accept the maximum possible, and take NOTHING for granted--, like you all should have written on your first page of your Labnotes journal. LT/
WISDOMwillWIN
(Hive Bee)
04-08-02 11:57
No 294297
The safrole faq on Rhodium's page lists the density of safrole as 1.096g/ml ... anyone have a copy of the Merck handy that can verify this or corroborate LaBTop's claim?
(Daddy)
04-08-02 14:26
No 294340
Merck: 1.1000
. That safroleFAQ data is wrong. LT/WISDOMwillWIN
(Hive Addict)
04-08-02 15:18
No 294352
The 1999 CD version of Merck has "Density: d 20 1.096"
Mastery is based on the understanding and practice of technique.
(Daddy)
04-08-02 16:37
No 294375
I referenced that same 1.096 data to him, and he answered he found Merck referenced it as 1.1000 , and also lugh posted that same 1.1000, so now I am confused. Chemfinder states it as 1.095.
I just worked 3 hours on a very extensive post, was nearly ready, and then Chemfinder came up with a nasty popup window, which I thought I clicked away, but it was the whole fuckin browser I clicked away. Why the fuck do I do all this? I should get a live again!
I hope the webmaster at Chemfinder and the others from those popup ads all will burn in hell in eternity for this.
Now I have to construct that post again, se you in 3 hours. LT/
WISDOMwillWIN
(Daddy)
04-08-02 20:16
No 294426
(Rated as: excellent)
Ingredients of sassafras oil with CAS nrs, so you can look data up in Chemfinder, Interactive Physical Properties Database or the Merck Index,
Especially the densities and melting points are interesting for the 2x freezing method:
Usual components 0f Sassafras Oil,
From Guenther, E.,"The Essential Oils", vol II and IV:
pinene.......... 2-10% Bp= 154C at 1 atm
phellandrene. 2-10% Bp= 175C at 1 atm
d-camphor.... 0- 5% Bp= 204C at 1 atm
safrole.......... 80-90% Bp= 234C at 1 atm
eugenol........ 0-10% Bp= 252C at 1 atm
CHEMFINDER data:
( http://chemfinder.cambridgesoft.com/ )
==============================
(1S)-(-)-alpha-PINENE [7785-26-4]
Colorless to pale yellow liquid.
Mp= -64C Density= 0.874 g/cm3 at 20C
Bp= +155 - 156C
==============================
alpha-PHELLANDRENE [99-83-2]
Pale yellow liquid.
Density= 0.843 g/cm3 at 20C
===============================
CAMPHOR [76-22-2] also known as (±)-CAMPHOR, d-CAMPHOR:
But note: is has a different CAS nr than the IPP data! A solid, not the oil!
Colorless, glassy solid with a penetrating, characteristic odor.
Mp= +177C Density= 0.99 g/cm3 at 20C
Bp= 207C Water Solubility= 0.12 g/100mL
IPP data:
CAS Number : 000076-22-2
Chem Name : CAMPHOR
Mol Formula: C10H16O
Mol Weight : 152.24
Melting Pt : +180 deg C
Boiling Pt : 204 deg C
Water Solubility:
Value : 1600 mg/L
Temp : 25 deg C
Type : EXPerimental data
Ref : YALKOWSKY,SH & DANNENFELSER,RM (1992)
=================================
CAMPHOR oil (light) [8008-51-3] :
Colorless liquid.
Density= 0.89 g/cm3 at 20C
No IPP data!
=================================
SAFROLE [94-59-7]
Colorless or slightly yellow liquid
Mp= +11.2C Density= 1.095 g/cm3 at 20C
Bp= +232 Water Solubility= Insoluble. <0.1 g/100 mL at 18 C
=================================
EUGENOL [97-53-0]
Clear, colorless or pale yellow liquid. AIR SENSITIVE.
Mp= +15.44C Density= 1.066 g/cm3 at 20C
Bp= +487 at 0 mm Water Solubility= <0.1 g/100 mL at 20 C
These data are totally different from the IPP data!
=================================
+ + + + + + + + + + + + + + + + + + + + + + + + + + + +
Interactive Physical Properties Database:
( http://esc.syrres.com/interkow/physdemo.
==================================
CAS Number : 001330-16-1
Chem Name : PINENE
Mol Formula: C22H32
Mol Weight : 296.50
Melting Pt : not given
Boiling Pt : not given
Water Solubility:
Value : 7.36 mg/L
Temp : 25 deg C
Type : EST
Ref : MEYLAN,WM ET AL. (1996)
==================================
CAS Number : 000099-83-2
Chem Name : alpha-PHELLANDRENE
Mol Formula: C10H16
Mol Weight : 136.24
Melting Pt : < +25 deg C (that's vague, we need a more precise value!)
Boiling Pt : 172 deg C
Water Solubility:
Value : 2.86 mg/L
Temp : 25 deg C
Type : ESTimated data
Ref : MEYLAN,WM ET AL. (1996)
==================================
CAS Number : 000464-49-3
Chem Name : (1R,4R)-(+)-CAMPHOR, d-CAMPHOR
Mol Formula: C10H16O
Mol Weight : 152.24
Melting Pt : +178.8 deg C
Boiling Pt : 207.4 deg C
Water Solubility:
Value : 100 mg/L
Temp : 25 deg C
Type : EXPerimental data
Ref : RIDDICK,JA ET AL. (1986)
===================================
CAS Number : 000094-59-7
Chem Name : SAFROLE
Mol Formula: C10H10O2
Mol Weight : 162.19
Melting Pt : +11.2 deg C
Boiling Pt : 234.5 deg C
Water Solubility:
Value : 121 mg/L
Temp : 25 deg C
Type : ESTimated data
Ref : MEYLAN,WM ET AL. (1996)
===================================
CAS Number : 000097-53-0
Chem Name : EUGENOL
Mol Formula: C10H12O2
Mol Weight : 164.21
Melting Pt : -7.5 deg C
Boiling Pt : 253.2 deg C
Water Solubility:
Value : 2460 mg/L
Temp : 25 deg C
Type : EXPerimental data
Ref : YALKOWSKY,SH & DANNENFELSER,RM (1992)
===================================
What do we learn by this? You can not TRUST BLINDLY any online data, check always the BOOKS! LT/
WISDOMwillWIN
(Daddy)
04-08-02 21:02
No 294437
As Strike already outlined in TSII, page 33, Brazilian Sassafras or Brown Camphor contains normally no Eugenol.
Thus a 3-5% NaOH solution wash before freezing the oil is redundant in most cases.
Let's look at what he had to say about purifying by freezing of Sassafras oil, page 34 :
It will be a little tricky, but one can also try to purify by freezing!
The sassafras oil is thrown into the freezer to chill. Safrole itself freezes at -14C, so anything that starts to freeze before that can be cold filtered in a prechilled vacuum setup. Thefiltrate goes back in the freezer until -14C is reached and the motherload of safrole freezes up. This again is filtered cold but this time the frozen mass of safrole crystals are washed with some icecold methanol or ethanol (preferably beeing -14C also), to wash away the unfrozen high-boiling constituents.
As you can see in the above posts, there are much better procedures described now, to purify by freezing.
= = = = =
LT/: Editted 08May2002.
Proceed with your now mainly pure 1-alkene (safrole) to a:
5% weight/weight (99%pure) KOH + Safrole overnight vacuum reflux:
Setup:
1.---Highly adviced: (when you have one!) an air cooled 20 or 40 cm vigreux column vertically set on your distillationflask,
2.---(flask placed in an aluminum oilbath, [filled with peanut oil or silicone oil and a STIRBAR], which stands on a stirrer/hotplate, flask for 3/4 or nearly totally submerged in the oil, just the neck free),
this will keep the refluxtemp of the MANY constantly condensing and falling back safrole/isosafrole drops much higher than by using just simply a watercooled condenser, thus avoiding a too fast cooling down of the main safrole/isosafrole/KOH body in your distillationflask at full vacuum reflux all those hours overnight and perhaps slow down the reflux rate and lower flask-temperature,
3.--- PLUS on top of that a vertical set watercooled-condenser setup,
(which will trap and forcefully cool all eventual vapours which eventually still escaped the vigreux column).
4.---On top of the condenser you place a vacuum adapter and vacuum tubing to your vacuum pump.
This gives conversion from 1-alkene (safrole) to 2-alkene (isosafrole), under full vacuum, OVERNIGHT, while first removing all traces of water which would wreck your isomerization results.
A.---To remove all water traces FIRST, you begin the procedure with a different simple setup, with the vacuum adapter connected directly to the distillation flask, put on the full vacuum for 30 minutes, while the hotplate is switched on for the first time. In that time the mix will not heat up very much, thus avoiding sucking off too much volatile oils, but the high vacuum will remove all water traces at that temperature.
After those 30 minutes you put the vigreux column + watercooled condenser back on the distillation flask, put the vacuum adapter back on top of the watercooled condenser, and switch the vacuum on again.
(Already in the first 15 minutes after switching on the vacuum pump and the stirrer/hotplate and adding a egg-shaped stirrbar to the contents of your distillation flask, before your safrole/KOH even reaches near its boiling point under your specific vacuum, depending on what pump you use, you will -perhaps, when traces of water are present- see some light boiling in your flask, that is the eventual water boiling and evaporating to your pump, after that time all that water will be gone into your pump; leave the GAS BALLAST of your pump full open!, in case of an oil-filled vacuumpump, this will allow the watertraces to be washed out of the pump by the air washed through the vacuum oil when that gasballast is full open. You should leave that one always fully screwed open, it will influence your maximum vacuum very minimal, no more than half a mbar, but will keep your vacuumoil as clean as possible).
B.---After those first 30 minutes, you replace the whole setup as in 1-2-3-4 above, and continue the heating and stirring under full vacuum again.
Then when your safrole + KOH starts steadily boiling and full refluxing back from the vigreux column, fix your temperature setting at that specific temperature scale point of your hotplate,
(I can't give a precise temperature, because it will differ for everyones specific vacuum obtained by different pumps and setups),
and leave it OVERNIGHT full refluxing. No need to crank up the heat further, don't do it.
C.---The next morning you switch off the vacuum temporarily, to insert a T-piece with thermometer sticked in, on top of the (ev., but highly adviced) vigreux column, attach your watercooled condenser now on the T-piece's sidearm under a ~30° downward angle, put a vacuum alonge on the other end of the condenser, and hang a receiving flask on the vacuum alonge, put the vacuumtube on the alonge outlet, switch the vacuumpump and mixer on again, and just increase the heating untill the vapours of your boiling --now 95-98% isosafrole/3-5% safrole mix-- reaches the top of the (ev.) vigreux and the sidearm of the still head (it still refluxes back partially, that's good, you now have the purests vapours at that temp reaching the top of your vigreux and still head side arm) and starts condensing in the condenser and drips in the receiving flask.
C2.---The first small portion coming over will be the 5 to 2% safrole+?impurities? -left after the isomerization process.
When at that temp setting and vacuum nothing more comes over, remove the receiving flask and discard this portion in a "Fore-run Safrole" labeled glass bottle for use in the next isomerization batch again! Check its DENSITY (and total weight of this fraction compared to the starting weight of your safrole!) and compare it to my density data in Post 294426 (LaBTop: "Sassafras components data", Methods Discourse) in this thread.
Note this fore-run temp setting and density and total fraction weight in your labnotes (handy for your next batch).
C3.---Hang your receiving flask on the alonge again, switch the vacuum on again, and proceed to heat further untill you reach a new higher temp where as good as all fluid (isosafrole) at that temperature will come over. Inbetween you will have to check at intervals your (now) isosafrole vapour temperature in the still head (T-piece), if that goes up suddenly FAST more than 5-10°C, your done, all what comes next is not isosafrole and should be thrown away. Better don't use the leftovers from your distilling flask (KOH + Whatever carbonized shit?) in a next batch, just use then fresh KOH in your distilled and freezed-out safrole again!
Check the density of your obtained isosafrole against the density data in my Post 294426 (LaBTop: "Sassafras components data", Methods Discourse) in this thread.
If not sufficient precise, repeat the whole procedure again, until you got it RIGHT.
A PURE isosafrole will give you the highests REAL KETONE yields in a performic, peracetic or other method, ALWAYS! LT/
WISDOMwillWIN
(Hive Addict)
04-08-02 21:21
No 294444
1. get popup ad filter from meaya software (www.meaya.com). it's excellent. doesn't always work, but there is other software like it, i just prefer this one.
2. if i'm going to write a long post i usually type in notepad and copy and paste. it's a better interface than the usualy web text field.
i learned a thing or two from charlie dontcha know.
(Daddy)
04-08-02 21:59
No 294452
That's what I saw also, so again, like I showed you, data gathered on the Net, and god knows where else, should always be concidered as at least questionable. Practice proofs.
I begin to understand now why there was such a heap of contradictionary info gathering lately, lots of people believe they have found in one quick websearch some solid data, post it in full honesty, and then we see that ALL that data is questionable. What a mess. LT/
PS: I don't give a shit what Merck says, the density of pure safrole is definitely 1.1000.
3x freezer crystallizing gives a d20 of 1.099 !!!
WISDOMwillWIN
(Daddy)
04-08-02 23:19
No 294480
(Rated as: excellent)
A VERY angry Argox has this to say:
I can't believe that nobody ever posted this:
Foolproof way to separate safrole from sassy oil, any volume.
1. Pour 18L sassy into clean 20L white plastic bucket from Home Depot, cover bucket with plastic top.
2. Put bucket in horizontal deep freezer (buy for $100 from second hand appliance store) for 8 hours.
3. Pour off natent liquid on top of crystals into 2L glass beaker.
4. Melt crytals by immersing covered 20L bucket into hot water bath.
5. Repeat steps 2,3,4, using same 2L glass beaker to collect all liquid that doesn't crystallize.
6. Repeat steps 2,3,4, using same 2L glass beaker to collect all liquid that doesn't crystallize.
7. Measure specific gravity of liquid from melted crystals (safrole). If less than 1.099, then repeat steps 2,3,4, but HIGHLY unlikely that you will need more than 3 crystallizations to acheive goal of d20 >1.099.
8. Place 2L glass beaker in freezer for 2 hours, decant liquid from any crystals into a second 2L beaker.
9. Melt any crystals in first 2L beaker on hotplate at 40 C.
10. Repeat steps 8 and 9, until liquid from melted crystals has d20 of >1.099.
11. Discard approx. 2 liters of yellow oil, which is probably eugenol and phellandrene.
12. Result of above steps: about 16 liters of crystal clear 99% safrole. D20 >1.099. And about 2 liters of yellow liquid, not safrole, and who the fuck cares what it is.
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.
Sorry for the angry tone, just blowing off steam. It just pisses me off, that after so many years, the Hive doesn't have a definitive step-by-step guide to this process, and I have to learn by figuring it out for myself, through trial and error.
Regards, Argox.
I fully understand the rage this guy is feeling, after all these years of blatantly wrong posts, and I have to blame myself also, to have let myself slowly suck into that kind of theorizing, while not taking the time to research these simple data a lot deeper.
The overall tendency on the Hive is leaning to posting proposals as concrete hard evidence or even first hand experience, while not having done anything constructive.
It is concidered by me that this kind of work is dangerous, but why the fuck do you come here then?
I will not allow any posts anymore which claim sincerity, who are not doublechecked first by at least 2 known exact operating Hivers, any other posts must contain a disclaimer:
This procedure, only tried, and truely, by me, member xxxxxxxxx.
Any responsibility is for the next experimenter, to see if this works as advertised.
After 2 confirmations from reliable wellknown honest Hivers, you can give me, member xxxxxxxx, the well earned congratulations.
I'm also getting sincerely pissed off. Not in the least on myself. LT/
WISDOMwillWIN
(Hive Addict)
04-09-02 00:40
No 294527
SWIM has never had a container in the freeze fail to completely freeze... but, SWIM has had a contianer sit in the fridge for over a week WITHOUT freezing. SWIM has also had a container sit in the fridge and spontaneously freeze after a few hours (only once or twice). SWIM has never had a cool container of oil not freeze when a seed crystal is used.
other info: only 2 different batches of oil have been used. the first completely froze when a seed crystal was used first time this was after distilling half of it (a good exercise, but glad it doesn't need to be repeated). the second had the varying results above.
i learned a thing or two from charlie dontcha know.
(Hive Addict)
04-09-02 00:47
No 294530
that system sounds a lot like the eBay feedback system. if we have the mods decide who are the trusted bees to confirm any claims, then this system will be as secure as it's gonna get.
but... who watches the watchers?
i learned a thing or two from charlie dontcha know.
(Daddy)
04-09-02 01:20
No 294548
Let me tell you something, it's strange that only two of the ones I should trust to give me a counter expertise on a proposed "tried" method answer this nightly ranting.
And even stranger that they seem to doubt their own professionalism, clearly proven by their valuable postings in the near past, and think that THEY get attacked. Get some selfesteme!
I don't take it anymore, it's getting so fuckin annoying, btw, if you should have noticed, Osmium is nearly not answering any posts anymore, I slowly start to FUCKIN UNDERSTAND WHY!
And ofcourse I know that it is totally needless to even try to think to implement something like that 3x screening rule on a highly clandestine board like this, but I really get fed up with the literally THOUSANDS of TOTALLY bullshit posts about the trillionth time some obviously absolute idiot who can't spell, use punctuation or whatever, comes back to explain what he did wrong again, which utterly important fact he now again discovered tonight, FUCK, the books and the Net is full of the answers.
No they need spoon feeding.
YOU know what?
Stick the fuckin spoon in your asses! LT/
WISDOMwillWIN
(Sector G)
04-09-02 08:23
No 294627
(Rated as: excellent)
LaBTop: You are far too cranky. Go to bed, or at least lay off the stimulants for a few days; might want to take a handful of downers while you're at it...
You guys are setting up a fucking government here with all these checks and balances and watching everyone and rating. Fucking calm down. No wonder so many bees only read the couch.
(I bet I could hold my breathe and count until this post gets rated, and I wouldn't even hit 100. So be it.)
PrimoPyro
EDIT After Rating:
Who's doing that!? That's just to "prove" to me that I can't predict everything you do, isn't it? I say I expect a negative rating, so I get a positive one as an "oh yeah?" instead? That is hilarious. Who did that??Vivent Longtemps La Ruche!
(Hive Bee)
04-09-02 11:04
No 294669
(Distinctive Doe)
04-09-02 11:56
No 294689
(Rated as: excellent)
Quick to judge.
How many types of sassafras essential oil are there?
At least 3 common ones and others
Chinese, American, brazillian.
How many people make sassafras essential oil?
Hundreds of companies most likely.
How can you say one method works the same for all the oils?
YOU CAN'T
If you have 70% oil it sure in the hell is going to behave much differently than 95% oil. So all this talk of foolproof one and only methods is a bit arrogant IMHO. We are dealing with natural products from many different sources and even different plants. I'm sure that 10-20% eugenol would have a huge affect on any crystallization, what about water content, ect ect ect.
Don't say somethings foolproof until you do GC analysis of your oil so everyone knows exactly what is in the oil your using.
Hey LabTop
"I will not allow any posts anymore which claim sincerity, who are not doublechecked first by at least 2 known exact
operating Hivers, any other posts must contain a disclaimer:"
LOL, thats funny.
Your starting to worry me here. Anyone would have to bee an idiot to take what one person posts as a "tried and true" method. The disclaimer is INHERANT in every post I read, IMHO. Shit you have to look at patents and journal articles the same way!!! See the recent information on nitroethane for your example. Anyone who really cares will take the time and search for someone who verified a procedure. I do admire your catologing and attempting to do this for everyone, however I think reading many different accounts of the same procedure is much more valuable than one "tried and true" method. Maybe this is because I am always looking to optimize what I do and reading multiple experiences is the best way to get a jump start on innovation.
Thoughts and ramblings
Foxy
Those who give up essential liberties for temporary safety deserve neither liberty nor safety
(Stranger)
04-09-02 19:37
No 294836
I can tell you from lots of experience only using this method with no distillation apparatus has worked well to get mdmx mdex and mdx.
BTW, when I saw the voluem 5 Guenther it stated safrole had a density of 1.70 to 1.09. Maybe it mean sassafras oil. not sure
Re: "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."
I think baalchemist meant to do it the same way I have which is the best method I've found to date, pretty much what is already discussed here:
Place in jars, make sure you got at least 1/2 volume of air in the container in the fridge at the coldest setting (use coldest setting first for practicing). place seed in there if it doesn't already spontaniously crystalize. Full crystallization can be complete in anywhere from 2 minutes to 6 days depending on temp. Slowest is the only way to go. But first practice on getting the shit to crystalize a few times before tweaking it to a warmer temp.
Best length for crystalizing is at least 3 to 6 days. The crystals form from bottom up pushing the impurities away from the lattice in a slow gradual manner. Once about 66% has crystlized, YOU THEN TURN THE JAR UPSIDE DOWN and let it drain off at ~12c for 1 day to get a opaque clear liquid. Melt it and Repeat once more. Works very simply and on the second run you'll get fat crystals that have virtually no yellow impurities locked into the crystal lattice. Check the old hive for information I posted about this method nearly 2 years ago when I still tweaking this method. PEACE OUT!
(Daddy)
04-10-02 02:49
No 294961
Post 294426 (LaBTop: "Sassafras components data", Methods Discourse), and look at all the densities from the sassafras constituents according to Guenther, then you see not ONE which nears 1.1000, only safrole. So there is nothing mentioned more dense than safrole, which could interfere with the reported 1.0992 density of the purified frozen safrole from Argox, and lifting it's density above the Merck ref of 1.096 . (Merck=most reliable imho)
Ofcourse there could be something dense there at forehand which we don't know.
But the sassafras was FIRST distilled with a very good fractionating column, so the freezing was tested with already quite pure "sassafras"/safrole.
How can someone who has calibrated exactly a one liter erlenmeyer with 20C water, and uses a calibrated official one liter vessel, and a precise digital balance, leveled with a waterbubble, checked with calibrated weights, come then to a density at 20C of 1.0992 , for the frozen part (safrole), after 3 x freezing?
You see also that 3 different companies give 3 different densities for safrole.
Scram, I think I found the confusion, found 2 posts from Baalchemist,
1. "could" be interpreted wrong, because it doesn't state that the liquid is ALREADY frozen before turning it upside down, (btw, he states also a d20 of ~ 1.1)
2. is more clear:
1. =========================
baalchemist (Chef d'Equippe)
01-07-02 15:13
No 253681
Re: Safrole Crystals
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.
2. =========================
baalchemist (Hive Bee / Eraser)
04-15-01 03:16
No 184267
Re: Sassafras oil --> Safrole??
Freezing is the easiest if you got the good chinese shit, that 60-70% shit needs a seed crystal most of the time. Once its frozen, turn the bottle upside down in the freezer for a day or two. All your crap will settle away from the goods for easy disposal.
============================
In 2. he also states to wait for 2 days before draining.
Argox prolly didn't wait that long, and/or his sassafras was purer. And he stated that he fractional distilled the sassafras first, so got a MUCH cleaner product to freeze! That can explain the observed anomaly, that the impure oil constituents where located UNDER the crystals at the bottom of the pail, even after turning the pail upside down, and were NOT leaked through the crystal matrix, and therefore he had to puncture the bottom of the pail to drain it away. And he prolly did not wait 2 days to see if it leak through.
Still I can see his reasoning: whatever you do, if you have to wait a long time before freezing proceeds, the impure oils will form in a "hole" on top of the crystals. That means if you turn your pail upside down, your impure oil will still form in the same hole, but NOW facing the bottom.
And he saw NO oil leaking through the crystal mass at all. So unscrewing a lid or removing a lid will show you ONLY a dry mass of crystals, while the impure oil is locked between the bottom and the crystalmass.
I would like to ask MadMax and Roundbottom if they ever found impure oil leaked through the crystal mass, at the BOTTOM. Because when it leaks through from bottom to top if upside down, it should also leak through from top to bottom prolly when used in normal position.
If they never found any bottom sludge, then "leaking through" seems strange.
Or if they ever used that upside down method long enough (2 days) and can confirm it too.
And don't mind anyones reputations when the truth is at risk, look at my sticky threads where I proposed fractional distillation of sassafras for so long, and it turns out that a simple test done for a few days proofs that it is totally redundant and a waste of time prolly in most cases.
However, the fanatical purist should fractionally distill the sassafras first, and THEN freeze it 3x, to get near quantitative amounts of pure safrole oil!
But that's for real scientists who seek reliable data of ONE component, and cooks can skip that step. LT/
PS: Primo Pyro, as stated in my later post, I saw no practical possibility to implement such a basic scientific standard of contra expertising here.
PSII: My opinion is that the rating system should be used with care, so we don't wreck it's potential value to indicate real good posts, and the bad ratings should be used to dam the sinflood of unnescessary multiple posts about one test, which could be posted after the tester has tried everything possible, and searched extensively for answers while in the process of testing, and THEN, when all his tests went wrong, he comes here to ask for help.
Now hundreds of posts are dumped here every half hour into the process of the testing ITSELF.
Stupid, you can see clearly that the dumfuck has his IP connection beside his workbench!
When I can conclude this, LawEnforcement can see that clearly too.
WISDOMwillWIN
(Stranger)
04-10-02 06:17
No 294987
Just to put to rest (somewhat) the question that Foxy
brought up about oils with a higher % of crap in them,
swim placed the eugenol etc, extracted from 1 liter of
natural Albidium into about 800 ML of the same unexstracted
oil and used an amount of this adulterated oil in a
simple freezing technique using a seed crystal.
The safrole crystalized out with the expected additional
amount of crap oil floating on top.
So it seems that safrole will crystalize despite being
present in an excess of the other natural constituents
of sassafras oil.
(Hive Bee)
04-10-02 10:24
No 295050
Ok now I think there are some comunication disturbences. Well What I make of it is this:
1:Too succesfully purify your safrole you need a sassafras oil that already has been vacuüm distilled ones so you have a somewhat cleaner oil.
2:you need seed crystalls
3:It's good to do the procedure three times.
4:Unfrozen liquid forms above the frozen safrole crystalls.
5:You will get 99% pure safrole with a density of 1,1 g/cm³
questions
Ok is this correct or not?
How do I get seed crystalls??
You've gotta love me.
(Hive Addict)
04-10-02 12:59
No 295110
> if they ever found impure oil leaked through the crystal mass, at the BOTTOM
in my unscientific, anecdotal experience, i have not seen any impurities resting at the bottom below the crystals. they do seem to be 'pushed' up and i always seem to have a little 'well' at the top where the impurities sit. it's noticable in max's pix, too.
my thought is, the crystals are pure safrole. if you start the freezing process and then stop while there is still safrole to be frozen, your crystals should be pretty pure. unless the impurities are trapped in the crystals. this is beyond my expertise, maybe i'm just talking out the side of my mouth.
i learned a thing or two from charlie dontcha know.
(Daddy)
04-10-02 14:34
No 295166
Flipper:
Ok now I think there are some comunication disturbences. Well What I make of it is this:
1:Too succesfully purify your safrole you need a sassafras oil that already has been vacuüm distilled ones so you have a somewhat cleaner oil.
LT: I just explained it is NOT needed! Only if the institution where you would ever work as a research analytical chemist wants to be sure and let's you check about the compounds EXACT data!
2:you need seed crystalls
I doubt it, if a deep freezer is used first.LT/
3:It's good to do the procedure three times.
You'r good in repeating. LT/
4:Unfrozen liquid forms above the frozen safrole crystalls.
Dito. LT/[red]
5:You will get 99% pure safrole with a density of 1,1 g/cm³
[red]Dito! Btw, you will only be sure when you have access to complicated analytical instruments, so "probably ~99%" and "nearly 1.100 g/cm3". And that's no nitpicking, that's everydays logic for "cooks", who have to live with certain insecurities, due to oppression. LT/
questions
Ok is this correct or not?
How do I get seed crystalls??
"You've gotta love me."
Where do you see communication disturbances? I think I made it perfectly clear that I doubt you will see any impure oils filter or leak through the main bulk of safrole crystals, if performed like Argox says. And his data empirically found indicate that the whole "upside-down" thingy is redundant, if not at all impossible when you want to reach his data results.
"1. Ok is this correct or not? 2. How do I get seed crystalls??"
Now here (1.) you start really annoying me, THAT's the whole basic principle we are looking for, you don't need to pop in and repeat everything.
And (2.) how to get seed crystals is made perfectly clear by a few people already. UTFSE! or reread this thread. LT/
WISDOMwillWIN
(Stranger)
04-10-02 15:17
No 295185
LT, just to clairify, you can get it to freeze w/o a
seed crystal, but when it does it'll all go at once,
trapping unwanted gunk in the matrix.
By using seed and chilled (not supercooled) oil, the
lattice grows slowly, pushing the impurities away,
just like recrystalization does with bisolvent solutions
at the right temp
And as gump says "that's all I'm gonna say about that.
(Daddy)
04-10-02 15:48
No 295212
Both Humid and Roundbottom indicate already also that the impurities in different "species" of sassafras don't make a flying fart difference, as I expected.
Especially Humids method of re-introducing a big amount of Eugenol + other impurities, into his original sassafras oil, to check if that would interfere with the freezing, proofs it right, it doesn't! I like prompt returns on insecurities that way. Thanks, Humid.
And Roundbottoms observations indicate the same as we already heard, the impurities form in in hole on TOP of the freezing crystal mass. Just like you could see in MadMax pics, as I did also already.
Any water can be removed in a preliminary step first, however as you can see in the water solubility data I handed over on a silver platter, these eventual water contents are neglectible for all compounds of sassafras oil, and btw, if you unfreeze purified safrole, the next isomerization step asks FIRST for a water removal, to not interfere with the KOH complex while isomerizing.
If unsure what to do, throw in your new sassafras oil, a buttload of dried silicagel first, and decant after a night standing.
That thought of many different percentages in sassafras oil ofcourse came directly to my mind also, that's why I searched 6 hours on the Net to dig up those data from the main constituents of Sassafras oil. And that's why I gave the Guenther list of those VARIABLE percentages.
And gave you all the MAIN constituents data for sassafras oil, from the bible of Essential oils, Guenther again. And I am SURE the ranges he found in percentages for every constituent found, reflected the bulk of available sassafras species and suppliers.
He's a German scientist, FAMOUS for their precise and reliable data mining. (Proof: PolytheneSam, only partly German, but mainly PRECISE
, you Foxy, however, have never indicated your roots, so I can't give you credit on that, but there must have been some german precursor in your family too)And again, review those main data, there's not one except Eugenol, which could propose a threat while freezing.
The intention of posting that list, was mainly to make clear to the investigative mind, that Eugenol has a Mp of -7.5C, and Safrole a Mp of + 11.2 which means there is such an immens difference in melting points, that you can forget the possibility of Eugenol interfering with the freezing process.
Btw, I indicated in red already that the data from the Chemfinder website is UNRELIABLE, at least for this compound. But there are many more flaws in other compound data from them also. They should get a burning message to review their whole online data asap.
Eugenol is the only impurity I would even worry about, caused by its close relation chemically spoken, to Safrole, and we know that it, if carried along into the next isomerization annex next steps, will respond to these treatments in the same manner as Safrole, thus severely wrecking the posted YIELD results of far too many members.
All the other impurities form no serious threat to interfere in the freezing technique, they all stay liquid within the set freezing range of your deep freezer (-5).
Why a deep freezer? Because those work much faster, and fast freezing is a wellknown technique in many procedures.
Now, to conclude, may I say that your (reasonable, but not deeply thought over) reply:
""If you have 70% oil it sure in the hell is going to behave much differently than 95% oil. So all this talk of foolproof one and only methods is a bit arrogant IMHO. We are dealing with natural products from many different sources and even different plants. I'm sure that 10-20% eugenol would have a huge affect on any crystallization, what about water content, ect ect ect.
Don't say somethings foolproof until you do GC analysis of your oil so everyone knows exactly what is in the oil your using."",
is reasonably profen to be not appliable for as good as all cases of members, buying industrial sassafras oils.
Do not feel offended, this is an ongoing discussion and in the process everybody introduces new bits of theory and/or knowledge, and so it should be, always. LT/
PS: Foxy, let's not call it arrogant, but Wonder, wonder why such a simple method was overshadowed for so long by much too complicated theory and practice, while a simple check of the densities after a fractional distillation could have indicated that there was something terribly wrong with all those posters who believed truely they had pure safrole in hand, but in fact had their sassafras nearly unchanged back. Just lately freezing came back to this board again, before it was just shortly mentioned now and then, but never really propogated as the one and only reliable fast and clean method.
And THAT's why I get so upset, not having access to a lab for so long already, and having to rely on postings from amateurs, who don't CHECK their products data after each conversion step. You will understand that too, being in the same situation.
Non lab owners should be very carefull with what they post, leave always room for cooks to proof you wrong. See myself, I really never expected such a bad result from sassafras fractional distillation, a technique what comes to mind as the first option in most purifying procedures.
WISDOMwillWIN
(Hive Addict)
04-10-02 16:22
No 295232
also of note, i previously posted about an isomerization attempt using crystalized safrole, Post 278285 (RoundBottom: "Re: vacuum refluxing", Chemistry Discourse). labtop mentioned it was the best result he had seen (which still surpises the heck outta me, SWIMs lab technique is nothing if not amaturish, and leans more to comical
).> - measured 2400mL of safrole double crystalized from sassy oil (brazillian)
this safrole was not 'dried' in any way before use.
SWIM is having a heck of a time with the Os AlHg, though; the learning process never ends. babybees, keep at it, you can get it. SWIM knew zip about chemistry before ariving on the HIVEs doorstep. </rant class="tony robbins">
i learned a thing or two from charlie dontcha know.
(Stranger)
04-10-02 16:41
No 295238
Cool, RB, and let swim say that upon observing the rest
of the adulterated oil (should be around 40% bad, 60% good)
which was placed in the fridge and seeded with crystals
from batch number one, that time seems to be factor.
Way more crystals should be present than are.
Cold sinks, and as the safrole becomes cold it also
becomes more dense (unlike water), and swims thinks it's
just the fact that the denser safrole is just held up
a little, by the increased shit it has to go through
before reaching the lattice where it can bond.
Usually goes MUCH quicker than this.
(swim just left the first sit in overnight with no
observation)
So the only difference between safrole content where
freezing is concerned is rate.
(or so it looks)
EDIT So it seems that a weird side effect of using
adulterated oil, is that the slowing of the rate at which
the lattice grows may actually create purer crystals!
(chemical irony, i'm stoned)
04-10-02 20:10
(Rated as: insignificant)
(Hive Addict)
04-11-02 00:14
No 295401
shammy, i thought it was a cute post. i wonder if someone could make a rap record out of that or something.
i learned a thing or two from charlie dontcha know.
(Sector G)
04-11-02 00:21
No 295402
I liked that post, too.
You got my vote.
Vivent Longtemps La Ruche!
(Distinctive Doe)
04-11-02 04:46
No 295455
Damn LT
Your good!
you Foxy, however, have never indicated your roots, so I can't give you credit on that, but there must have been some german precursor in your family too
Well I can tell ya this much
I am 1/4 Nazi, got a tiny bit of Napolean and a small slice a Sven, and the rest on me likes a good Sauna,
I really like Saunas
Now your Hypothesis is verified and ego inflated
Foxy
FUCK!!!!!!!!!!!!!
I had like 10 different journal articles open(not saved) and fucking Dr Watson happened when I open google, aarrrrrrrrrrrr fukin
Those who give up essential liberties for temporary safety deserve neither liberty nor safety
(Distinctive Doe)
04-11-02 04:57
No 295458
Ok arrogant was overstated
But being so critical of baalchemist seemed a bit rediculous. Especially after reading his posts on the subject. He didn't exaclty post a step by step guide, just some bs from memory.
I just tought getting all hot and bothered when something posted here doesn't work was rather stupid and I didn't like the bitching attitude. That colored my reply a bit.
But I guess I can understand the bitching if you just spilled a bunch of sassy all over.
That might smell a LITTLE
Foxy
Those who give up essential liberties for temporary safety deserve neither liberty nor safety
(Daddy)
04-11-02 10:01
No 295519
The main purpose of this thread will be reached when everybody starts getting the basic idea:
Be as PRECISE as possible, don't take shortcuts, and especially when you report your findings in our forums, be VERY exact, controll as many different data from your supposed product as you can, and include them in your reports.
There are too many, if not nearly all, reports, where a very messy report is quickly delivered, and no confirmation is given at all if the product obtained was bio assayed by anybody, and confirmed to be the desired product.
But everybody hops on that bandwagon, starts experimenting, and then 2 month later we find out that the originator never made the desired product, and was too embarressed or just lazy, or deliberately did not report back to tell us he/she failed in the most important conclusion:
Did it work or not!
LT/
PS: this thread will be moved in a week to the Methods forum, so don't panic when it's gone here.
WISDOMwillWIN
(Can't SWIM)
04-11-02 13:09
No 295615
You should see the SIZE of the crystals that resulted
from the slow freezing in the adulterated oil.
Great big ones about an inch square. Sorry can't
eyeball too well in metric.
CG I miss you sweety, I really do.
(Hive Addict)
04-11-02 13:50
No 295635
way to go. looks awesome, doesn't it? the trick is the slow freezing. fast freezing results in more of a crysteline mush. hard to desribe, like a chunky slushie, i guess.
i learned a thing or two from charlie dontcha know.
(Can't SWIM)
04-11-02 15:36
No 295672
Yeah, but it's fun to drop a crystal in supercooled oil
and watch the stuff "bloom" like a mandelbrot painting.
CG I miss you sweety, I really do.
(Hive Bee)
04-11-02 16:07
No 295686
please go to this post and help with SWIM's problems
Post 294100 (chem_123: "steam distillation!?", Newbee Forum)
My schwartz is bigger than yours!
(Old P2P Cook)
04-12-02 00:06
No 295926
Yeah, but it's fun to drop a crystal in supercooled oil
I actually once had a beaker of supercooled water crystallize on me like that. I was extracting mescaline from peyote buttons and wanted ice cold water to wash the mescaline sulfate.
There was no freezer in the apartment over a garage where I was working so I had someone stick a liter beaker of water in the freezer in the main house. Later they retrieved the beaker and carried it all the way from the main house and up the stairs to the apartment still in a liquid state. When I put a thermometer in it and gave it a quick stir it suddenly all crystallized in a matter of seconds.
(Hive Addict)
04-12-02 01:29
No 295945
ok, does someone want to try this? take an amount of sassy oil, shake it up for a bit, and split it into two equal portions.
take one portion and vac distill it. measure the amount of safrole.
take the second portion, and freeze crystalize it. measure the amount of safrole.
write a post with the two numbers.
this should answer the question.
i learned a thing or two from charlie dontcha know.
(Hive Bee)
04-12-02 10:00
No 296062
very scientific of roundbottom to suggest that...SWIM'll be eagerly awaiting the results as well!
My schwartz is bigger than yours!
(Hive Addict)
04-12-02 11:07
No 296087
bastardo :)
obviously someone didn't take to heart my statement that SWIM is a lazy bastard. SWIM would love to do it, but, as above, SWIM is a lazy bastard and doesn't want to run that noisy pump in SWIMs apartment when SWIM doesn't have to.
unless a karma reduction is heading my way, that's where SWIM stands. :p ptttffftttt!!!!
i learned a thing or two from charlie dontcha know.
(Daddy)
04-12-02 14:24
No 296150
It was already stated that the sassafras was FIRST professionally fractionally distilled, and gave a product with a FAR off density of 1.088.
Then 3x freezing gave safrole with nearly the right density of 1.0994.
So yeah, it would be nice if someone who knows what he's doing, and not the occasional garage chemist, would repeat that, and checks the densities folowing my posted procedure about calibrating a 1 liter erlenmeyer, or has a calibrated professional 1 liter density testing bottle. LT/
WISDOMwillWIN
(Hive Addict)
04-12-02 16:11
No 296198
guess that means you have to do it hydro!
oh, he means me. ok, but i won't be able to until next week. can anyone do it this weekend? *sigh* i thought my sassy distillin' days were over.
i learned a thing or two from charlie dontcha know.
(Can't SWIM)
04-28-02 16:47
No 302761
Here are a couple pics of slow grown safrole crystals,
that were obtained from an adulterated soultion of
non safrole components, from natural oil.
http://WWW.rhodium.ws/archive/picture108
http://WWW.rhodium.ws/archive/picture110
Those are rods are half inch thick and 3/4 inch long.
CG I miss you sweety, I really do.
(Stranger)
04-29-02 06:58
No 302980
Did the safrole from those crystals oxidize and aminate, like safrole from non-adulterated oil?
(Hive Prodigy)
04-30-02 13:32
No 303455
Of course they did.
Vivent Longtemps La Ruche!
(Newbee)
04-30-02 14:54
No 303496
Uh, that was directed to humidbeing. I guess your point is that safrole can be purified from (if it even exists) adulterated/denatured sassy. This safrole will oxidize and aminate. VL posted how hsi wouldn't. Not only that, but the only physical properties that difffered between iso that resulted in honey and iso that didn't were forming pseudonitrite cake without any tan polymer and (one other property which I forgot). My impetus for posting to this thread is to try to determine where my error lies. And, I am considering the denatured sassy theory. I sure hope that I am barking up the wrong tree!
(Hive Prodigy)
04-30-02 15:00
No 303498
I had mistakenly written my answer with the assumption of your question being if safrole purified by freezing would react the same as safrole purified by distilling: they would.
If that was not your question, then I apologize for the intrusion.
PrimoPyro
Vivent Longtemps La Ruche!
(Newbee)
04-30-02 15:08
No 303501
Yeah, just wanted to know if that safrole isolated from the adultered sassy worked. No foul dude. Any help you can give me would be much appreciated. See my thread "Amination Failure". Thanks.
(Can't SWIM)
05-01-02 01:18
No 303708
Swim doesn't know, but has heard yes.
The term adulterated means only that more non-safrole
constiutuents of natural oil were added before freezing took
place.
The actual brand of oil has been known to be authentic.
CG I miss you sweety, I really do.
(Chief Bee)
05-01-02 12:32
No 303882
Safrole is safrole as long as it has been purified. It doesn't matter how it has been purified or what it has been purified from - it is still the same molecule.
(Daddy)
05-01-02 13:35
No 303906
The question here seems to be if an addition is invented that can't be circumvented by our normal lab techniques. It is mentioned already since 1998 in these forums, and it seems to me that it's not a hoax, i've once seen it myself, all goes perfectly well untill the end, then your crystals melt in 5 minutes exposed to the air, or you don't get them at all.
Simplest solution: buy from non US sources, it is definitely contained to the US suppliers only, ...yet. LT/
WISDOMwillWIN
(Stranger)
05-03-02 10:56
No 304621
How come I never got credit for this shit!
Post 107751 (smokemouth: "DP Harma's Sassafras Freezing technique Modified - scwam", Methods Discourse)
Post 107782 (smokemouth: "Determining Safrole content thru congealing point - scwam", Methods Discourse)
(Daddy)
05-03-02 11:31
No 304631
Dammit, already so early posted all that good info, from scwam, DPharma and Osmium and some more, why tend so much info to sip away over the years and get forgotten?
I'm glad dormouse did all that recovery work that time, thus saving all this hours of typing in invaluable info by so many former and recent members. LT/
WISDOMwillWIN
(Chief Bee)
05-03-02 14:21
No 304662
why tend so much info to sip away over the years and get forgotten?
Because I haven't yet gotten my T3 broadband brain implant yet and still have to rely on manual information data gathering which is relatively error-prone. Hopefully cybernetics has evolved enough for that stage before I reach your age LT - I want to be able to use it for as many years as possible...
(Daddy)
05-06-02 23:50
No 305703
This thread is now moved to Methods forum.
Lili has at last made a reminder when a thread is Moved to another forum. Thanks, Lilienthal! LT/
WISDOMwillWIN
(Hive Bee)
05-13-02 12:32
No 308051
Swim has had about 2 ml of sassy sitting in his freezer for 4 days in a 5 inch test tube and nothing has frozen. swim knows it has safrole, it has the right smell, swim has distilled it before, etc. it is chinese. swim has tried putting the test tube in ice, scratching the inside of the test tube with a screwdriver, swirling the contents, putting the freezer setting on coldest, everything! and still, no seed crystals
. anyone got any suggestions?
(Hive Addict)
05-13-02 13:09
No 308066
if you can stick a screwdriver in the tube, it's too wide. my theory is that the narrowness of the vial is paramount. try a perfume sample vial (but clean it with alcohol first).
i learned a thing or two from charlie dontcha know.
(Hive Bee)
05-13-02 13:15
No 308072
This has got to bee swiws longest thread.Swiw has had this bunk sassy in the freezer for months as in multiple.Its not freezing even in a purfume vial.Cant wait for more sassy!
Keep it going.A more complex post or wright up on freezing would bee nice does anyone have a real good post number for swiw?I will choke untill I swallow!Who are you to judge or strike me down!Miss you Kerra!
(Hive Bee)
05-15-02 18:38
No 309041
anyone off hand know what temp dry ice gets down too?
I will choke untill I swallow!Who are you to judge or strike me down!Miss you Kerra!
(irritable and cranky)
05-16-02 05:29
No 309333
How about spraying butane gas from a lighter refill can on a few drops on a plate?
Bored...
(Chief Bee)
05-16-02 06:38
No 309350
Butane has a boiling point of -5°C, that's much warmer than in the freezer. Perhaps nitrous oxide (from whippits), with a bp of -89.5°C?
(Hive Bee)
05-16-02 14:38
No 309570
Very interested in that one Rhodium.How does it work?
I will choke untill I swallow!Who are you to judge or strike me down!Miss you Kerra!
(irritable and cranky)
05-17-02 03:13
No 309879
Good thinking boss! I shall try it out!
Bored...
(Chief Bee)
05-17-02 10:59
No 310012
wyndow: How does what work? I haven't tried using it myself, I was just giving an example of a non-toxic OTC liquified gas with a low bp.
(Hive Bee)
05-19-02 14:17
No 310933
Well, swim was about to follow max's advice on liquid N2 or dry ice, but the next morning he had a solid chunk of frozen sassy in the test tube! so swim took that and put it into about 500 mL of sassy, blah blah, you know. the stuff that did not freeze was dark brown, the stuff that did was light yellow. did that four times, and tried freezing the decanted junk in a separate, smaller beaker. got a few extra mLs to crystallize from the decanted stuff. anyways, from 1000 mL was obtained about 90 mL of unfreezable junk. swim's freezer/fridge has thermometers. the freezer fluctuates between -10 to -20 C, while the fridge won't get colder than about 12 C. So, swim cannot freeze in the fridge. should swim's shit be pure enough anywayz?? or should swim buy a new fridge that gets colder? Also, swim took the unfreezable shit and mixed it with 5% NaOH to see if it had eugenol in it. what happened is that there was a tiny bit of even darker oil on the bottom and about 80 mL of "cafe con leche" colored stuff floating on top. what does this mean? thanks for the advice everyone, any more feedback would bee appreciated. laaaaate
(Chief Bee)
05-19-02 15:52
No 310959
The unfreezable stuff is at least not safrole, as it doesn't freeze at sub-zero temperatures. Discard.
(Hive Bee)
05-20-02 00:55
No 311193
well its clear now after a distillation it just may have been a little fast its slightly cloudy white clear with rainbows.
I will choke untill I swallow!Who are you to judge or strike me down!Miss you Kerra!
(Hive Bee)
05-20-02 16:41
No 311521
Ok, I've just read this whole post in its entirety almost, but I can't help but wonder why eugenol would ever be in sassafras oil in the first place provided that the oil was obtained from steam distillation. Doesn't that hydroxy group on eugenol make the compound water soluble? Furthermore, 10% to 20% or whatever eugenol in sassafras oil would make the shit smell completely different. Also, say the rest of your oil is 20% random (i.e., non-essential oil) hydrocarbons, what does it matter? Can't they just be considered a form of a solvent to be later separated out in the manufacturing process?
Anyway, I can't wait to try out this simple and elegant method later on for the experience (props to scram, MaDMAx, LT etc...), but I would be willing to be that my clear oil doesn't really need it. I think LaBTop must have been trying to invoke Ockham's razor in some kind of oblique way, and I wonder why Baalchemist didn't post any reply. And who is Argox? Is he like Strike or something?
(Hive Bee)
05-20-02 20:17
No 311644
I once had a quart jar of yellow phenylnitroproplyene cyrstalize in about 3 seconds and it was a sight I will never forget. The jar had been sitting for a week while the rxn took place and every day it got more and more yellow. After one week I wonder--hmmm--where are the damm crystals? I pick up the jar and stick a glass rod into it and rub the rod on the bottom of the jar and----damm---I think I actually heard it crystallize. It produced alot of heat.
Very interesting stuff.
(Hive Bee)
05-20-02 20:57
No 311662
Pour a very small amount of the oil into a small beaker or baby food jar and put in the freezer. After taking the jar out 2 or 3 times to look at it you should notice crystals on the bottom of the beaker and also mixed in with the oil.
I would expect all of the safrole to eventually freeze.
Really, at the point where you can see the little seed crystals forming, you should be able to just pour some of the oil/crystals into the motherload of chilled sassy oil to get the safrole there to crystallize as well.
If problems still persist then try to create seed crystals with dry ice and acetone.
(Newbee)
05-21-02 11:04
No 311975
would this work with a seed and all with other oils
that contain safrole say ylang and camphor
remeber its not about the drugs mate its about the music
ye right :)
(Old P2P Cook)
05-21-02 11:28
No 311989
But for a counterexample consider a solution of 3% salt in water. Even if the water is cooled to near its freezing point and a seed crystal of salt added, the dissolved salt is not going to crystallize out. Similarly with safrole, just because you cool a safrole containing solution below the freezing point of safrole and add a safrole seed crystal does not insure that the safrole will crystallize out.
(Newbee)
05-21-02 11:42
No 312002
yes terbium that is what I have found with ylang
GOD also found this (actual he found it out first I tried
it becouse im a prat)
I found with ylang you get a few snow like crystals
mixed in the oil and a heap of milky white stuff that
kind of takes the shape of a spiral.
dont know if the snow is water vapor from me trying it
in singapore and opening the jar before freezing
(singapore can have up to 80% humidity) or if it
was safrole.
remeber its not about the drugs mate its about the music
ye right :)
(Hive Bee)
05-21-02 12:06
No 312021
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.
(Hive Bee)
05-21-02 13:42
No 312079
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.
(Hive Bee)
05-21-02 15:52
No 312153
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!
Society prepares the crimes,the criminal only commits one.
(Hive Bee)
05-21-02 15:57
No 312155
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.
(Distinctive Doe)
05-21-02 18:41
No 312255
"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
(Hive Bee)
05-23-02 19:08
No 313406
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 :)
(Chief Bee)
05-23-02 19:37
No 313417
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.
(Chef d'Equippe)
01-17-03 01:10
No 398991
"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..............
GODISNOWHERE
Shoot Narcs, Not Drugs
(tourbee)
01-17-03 02:31
No 398998
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.
The wisest man is deep insane.-GD
(Hive Bee)
01-17-03 17:07
No 399237
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.
(tourbee)
01-19-03 11:18
No 399738
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.
The wisest man is deep insane.-GD
(Hive Bee)
01-19-03 16:45
No 399789
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.
(Hive Bee)
01-19-03 18:17
No 399797
thanks for the tip!
(Hive Bee)
01-21-03 02:34
No 400153
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.
"Sometimes I sits and thinks, and sometimes I just sits." Satchel Paige
(Hive Addict)
01-21-03 09:50
No 400216
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.
Now with 12% more Bottom!
Nymphomania is not a disease, its a goal! (Methadist)
(Hive Bee)
01-21-03 16:42
No 400300
"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.
(Hive Bee)
01-21-03 21:32
No 400358
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.
"Sometimes I sits and thinks, and sometimes I just sits." Satchel Paige
(Stranger)
01-21-03 22:38
No 400366
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.
From the ashes...a new beginning
(Title on BackOrder)
01-22-03 17:40
No 400587
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.
If at first you don't succeed, try, try again. Then give up. There's no use being a fool about it.
(Stranger)
01-22-03 22:19
No 400671
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.
From the ashes...a new beginning
(Title on BackOrder)
01-22-03 23:37
No 400704
The stranger title fits you very well, as you definitely know nothing about what you're talking about. You make fractional distillation sound like an impossibility and a density check appear to be labor intensive. You're going to have your work cut out for you then.
So how many bees do you think here are working with 20L of safrole at a time? A couple of dutch cooks maybe that weren't lucky enough to come across MDP2P? Most of the bees here wouldn't even dream of ordering that much at one time, let alone trying to work it all up at the same time.
If you're too cheap to buy equipment, then shut the fuck up about it already. When you're bitching about low yeilds on your aminations because you're not properly distilling your isosafrole or MDP2P, you'll hear this all over again from everyone else here.
If at first you don't succeed, try, try again. Then give up. There's no use being a fool about it.
(not quite as irritable lately)
01-23-03 02:06
No 400752
I would just like to state that both my new 2003 13th ed. Merck hardcover and CD both list safrole as "Density: d 20 1.096".
Intelligence is not the recall of knowledge, but the ability to use it. (Rainman was a retard)
(Daddy)
01-23-03 05:30
No 400805
Placebo, and which is only 0.004 off from 1.100 found by Argox last year. He mentioned to use a self prepared density equipment which indicates to me that with that (still rough, compared to what Merck can come up with) homemade thingy, he managed to come very close to the Merck value.
Hey, old grumpy friend, they still glue the beerbottlelabels upsidedown downunder?
LT\
WISDOMwillWIN
(Hive Addict)
01-23-03 07:00
No 400826
Arsenic stop bitching. The purity of disilled sassafras, i.e. safrole does not need to be 99.999999999999% It will work for isomerization and after simple vacuum distillation of the isosafrole you are left with isosafrole of atleast 95% purity. Most bees do not care if its 95% or 99.9999999999999% because frankly the yields will still be the same!
Sink or SWIM
01-23-03 07:45
(Rated as: off-topic)
01-23-03 09:14
(Rated as: off-topic)
(Chef d'Equippe)
01-24-03 00:55
No 401070
Baal uses a Mettler/Paar Digital Densitymeter-DMA35 for density measurements on liquids. It certainly takes alot of the guesswork out of determining purity of most liquids Baal deals with. On my meter I get these readings;
Safrole 1.1
Iso-safrole 1.122
Ketone 1.188-1.191 This reflects a ketone that is not 100%, never seen it @ 1.195 as 100% purity is supposed to be, but close enough to run.
GODISNOWHERE
Shoot Narcs, Not Drugs
(Hive Bee)
01-26-03 08:08
No 401613
RB: Only problem when you distill the pooled contaminants is that you may get foaming (up through column, three-way and condensor down into receiving flask. SWIDR guesses that contaminants act as surfactants, so if you have 20 liters and freeze down to 15-16 liters, then just toss the riemaining 4-5 lters instead of attempting to distill that last liter out.
TRISMUS!!!
(I'm Yust a Typo)
01-26-03 09:33
No 401625
???
I've never seen foaming sassafras oil or ditto distillations. I do have seen distillations where the temperature was too high, and where an occasional bump to the table resulted in the distillation flask puking all its contents into the receiving flask. But that's bad technique, not bad chemicals.
Of course, if you have bad technique, you might as well throw away the remaining 'difficult' oil, even if it is 5 l....
(Stranger)
09-05-03 08:08
No 457337
(Rated as: The only thing lacking was your home address.)
I've read some conflicting posts about distilling sassy @ 1 ATM. Some read that shit might "polymerize" @ heat that high and that is why the vacuum distillation is recommended. Seeing as so many bees are saying that it's safe to distill sassy @ 1 atm i'm going to try it. I'm wondering if the 232 C is constant regardless of where you live? I'm a Canadian bee... XXXX to be specific. I'm wondering if there's anything I should know (or could check) about 1 ATM in XXXX, Canada that would affect the temp @ which the sassy would come over, at 1 ATM?
Thanks....
NOT cool, it's plain stupid to tell where you live in such an incriminating post! LT/
(Hive Bee)
09-05-03 08:14
No 457338
the only thing that would affect your distillation would bee how far above sea level you are. If your town is less than 500meters or so above sea level, I would just proceed as normal. good luck peace
D.A.R.E. = Drugs Are Really Exciting
(Hive Bee)
11-21-03 02:15
No 472216
I think I may have been successful in freezing asarone out of calamus oil.
First I poured about 10ml of nepalese calamus oil into a shotglass and put it in the freezer on its coldest setting. A day later, it was still unfrozen, at which point I abandoned the experiment and completely forgot about it.
A few weeks later I noticed it while getting some biscuits (mmmm, tasty frozen biscuits!) and checked on it. Interestingly, I saw whitish wartlike crystals awash in a darker yellow mass of crystallized oil. Cool, I thought, so I put it in my fridge. Two days later, it was still frozen solid, so I set it on my fridge to melt a bit, hoping to get a seed crystal. Later that day I came back and there were lots of chunky clear crystals soaking in the now liquid yellow oil (considerably more crystals than oil). I carve a few chunks out and throw them into a chilled shotglass and put it in the freezer, putting the larger crystal mass on the fridge to melt. I noticed when I came back later that as they melted they had separated into layers, the bottom clearish one having that peculiar irridescent sheen we all know and love. Anyhow, I poured this into an emptied soy sauce bottle and added the rest of the amount I had purchased (225ml), then put it into the fridge. After it was good and cold (8hrs) I threw in a seed crystal and went to work. When I got home, the bottle was full of white crystals but it had obviously trapped much yellow oil in the many crevices, not to mention the thick skin at the interface of oil.
So, onto the fridge it goes to melt. When it had melted down to the last few xtals (shaking helps) I put my fridge on "2" (it was on "5" previously) and put it back in there. It kept forming skins on top and trapping the yellow in crevices, so I crystallized and melted until I had huge crystals (~4 times) then turned the thing upside down over another container and collected about 75ml of nasty, stinky, pee-yellow oil.
Thirty percent (most asarone bearing oils being 60-70% asarone) of 225ml is 67.5ml.
After washing the crystals with ice-cold etoh, I let them melt into a very mildly yellow irridescent liquid.
Maybe I should have recorded the temperatures...
This begs the question... What in "Bob"'s name am I gonna do with this nasty stinky not-asarone stuff?
over and under, then back to the start
this sidewalk's bottom is the same as its top
(Chief Bee)
11-21-03 02:51
No 472226
What you have left is probably an 1:1 mixture of asarone and [unusable crap] so just vacuum distill it with a column to retrieve the other half of the asarone. You will probably not be able to crystallize out all of it in pure form from the impure matrix.
(Stranger)
12-01-03 12:15
No 474120
After SWIM tried for 3 days to create a seed crystal with no luck, tried small test tube, small perfume vial, freezer was at -18 and still no luck, so today SWIM decided to take a small amount <100ml> of oil that was in the freezer and dropped in a small cube of dry ice <1cm cube> and instantly it bubbled and a film of white fine crystals grew around the dry ice. SWIM removed the dry ice cube and the film simply fell off the cube. SWIM took the 1L bottle of oil from the freezer and dropped in the film of crystals and put the bottle back in the freezer. 15 min later the bottle was full of large white crystals. This made creating a seed crystal super easy. Followed all the other suggestion for freezing the contents 3 times <Ended up moving it to a 1L beaker as it was really hard to get everything out of the bottle.> Ended up with ~750ml of really white crystals that melted to really clear colour liquid that refracted light nicely.
(Hive Bee)
12-01-03 19:27
No 474210
you got a good yield with 75% v/v if its completely clear.
(Stranger)
12-01-03 19:41
No 474214
MIGHT I SUGGEST:
IMHO i would freeze or, slow freeze in the fridge, it may take time but FUCk around with the fridge as to find the a low enough temp to freeze slowly as the freezer does it to fast and you get other crap in with the safrole.
IMHO get the crystal from freezing in the freezer then, crystalize in the fridge as the lower temp freezes slower and you get BIGGER purer crystals.. then repeat this process and just drain of the yellow piss color and distil. Do this process 2 to 3 times then distil, though some may argue this, purtiy is the main convern not time'.
(Hive Bee)
12-02-03 21:44
No 474431
Biger crystals that for 6 to 8 sides are more pure. Also, make sure your d20 is 1.098 to 1.1 and you'll know if it's really pure.