06-13-03 06:25
No 439745
befor i go and do it i wanted to run some last min checks with some bees more experanced them me.
?#1 when distilling my sassy is it 100% nessesary to have to add some buffer oil to it towards the end or just stop befor it burns in the flask and loose my last bit?
?#2. one of my hot plate/stirrers has been modified to stay one all the time so it only stays on high heat. am i correct to assume it don't matter sence the oil wont get heated past its BP? or should i use anouter plate?
?#3. if doing say 250ml of sassy is an oil bath 100% nessisary or can a fbf be used instead. as long as it don't implode from the vac. i took my whole rig down to 15 torr. with noting in it to see if it could handle the vac and it din't implode on me.
?#4. when doing the methanol wacker. witch alc is the best to use? i have acsess to ethanol,anhydrous methanol. and anhydrous isp.alc. wich is best and why?
?#5 when i am done wacking my oil in the wacker. can i just vac filter it a few times. then throw it in a flask and fractinaly distill off the alc. then collect my fraction containing my p2p?
?#6 when doing the Nitromethane Al/Hg reduction will an indented 2,000 ml flask be ok to use? thats all i have.
?$7 what condenser should i use? i have a 4 bulb allin seems the easiest to clean after. but dont seem like it will be big enought to contain every thing if it gets out of hand. i have a 500mm liebig also. and a fredric but the freddi seems like it would be a bitch to clean should any thing puke up in to it. shit what to use what to use?? should i just go ineny meany miney mo? or rock paper scissors?
?#8 how smelly is the Nitromethane Al/Hg resuction? if my condenser is good enought will it stink up the lab? will a ballon over the end of the condenser be ok or not ok to do?
?#9 i have a few gallons of nice distilled pet ether. can that be used for my NP when extracting my goods? also could distilled turpentine or turpinoid be used at all?
?#10 do i HAVE to gas my finel product? can i just titrate it from my NP in to DH20 and evap my water? the only reason i don't want to gas is i dont have any H2SO4 right now. inless i take it out of an old car battery i have out in the barn. would lead in the battery cause any problums? could i do it using foil and hydrochloric as long as i dry the cock out if it?
and one last one that should of been closer to the top. when doing my Al/Hg would it be ok to add a few mg more HgCl2. and if not whats the reason not to.
thanks in avance for any help/advice any bees my have to offer. hopefully it don't seem like i am asking any one to holf my hand threw this. tho i would not mind if any one was willing :-) feel free to flame me if you want as long as its a good for me type flaming. and last but not least forgive my spelling i aready know i suck ass at spelling.
(Hive Addict)
06-13-03 07:12
No 439757
feel free to flame me if you want as long as its a good for me type flaming.
you suck. you are SO stupid and ugly. you smell funny.
UTFSE!
Every question you asked can bee awnsered by using the search engine. Swiy will learn a heck of alot more by doing this research, as he/she will have to read through TONS and TONS of worthwhile, relivant information in the process-
information that will:
-increase yeilds
-prevent forest fires and lab explosions
-protect breakage of glass
-preserve swiy from legal difficulties
-increase general knowledge of how to bee a good 'hack'
-prevent 2nd and 3rd degree burns
-increase libido
-avoid smelling like your grandma's underpants
-save swiy time and money
It will not, however, make swiy a better speller or prevent teen pregnancy.
shit...I found out it was all just one big manic episode!
(Hive Addict)
06-13-03 07:13
No 439758
?#1 when distilling my sassy is it 100% nessesary to have to add some buffer oil to it towards the end or just stop befor it burns in the flask and loose my last bit?
Forget distilling,freeze!!!Distilling you won't get it even nearly as pure as with freezing.Freezing is lot easier also.
?#2. one of my hot plate/stirrers has been modified to stay one all the time so it only stays on high heat. am i correct to assume it don't matter sence the oil wont get heated past its BP? or should i use anouter plate?
Use another plate,you need that to distill your ketone.
?#3. if doing say 250ml of sassy is an oil bath 100% nessisary or can a fbf be used instead. as long as it don't implode from the vac. i took my whole rig down to 15 torr. with noting in it to see if it could handle the vac and it din't implode on me.
See question 1
when doing the methanol wacker. witch alc is the best to use? i have acsess to ethanol,anhydrous methanol. and anhydrous isp.alc. wich is best and why?
Doesn't really matter,but use methanol,it's easier to get rid of it later as has lowest bp of em all.
when i am done wacking my oil in the wacker. can i just vac filter it a few times. then throw it in a flask and fractinaly distill off the alc. then collect my fraction containing my p2p?
Probably yes,but i'm not familiar with this rx so i can't tell for sure.
?#6 when doing the Nitromethane Al/Hg reduction will an indented 2,000 ml flask be ok to use? thats all i have.
Depends how large rx you are planning to dream
?$7 what condenser should i use? i have a 4 bulb allin seems the easiest to clean after. but dont seem like it will be big enought to contain every thing if it gets out of hand. i have a 500mm liebig also. and a fredric but the freddi seems like it would be a bitch to clean should any thing puke up in to it. shit what to use what to use?? should i just go ineny meany miney mo? or rock paper scissors?
See previous question.Your condenser won't get filled with shit.
?#8 how smelly is the Nitromethane Al/Hg resuction? if my condenser is good enought will it stink up the lab? will a ballon over the end of the condenser be ok or not ok to do?
Doesn't really depend which condenser you use,methyamine bp is below zero C so it'll get out anyway.Depends how hot is you rx mix.
?#9 i have a few gallons of nice distilled pet ether. can that be used for my NP when extracting my goods? also could distilled turpentine or turpinoid be used at all?
Pet ether will probably work.
?#10 do i HAVE to gas my finel product? can i just titrate it from my NP in to DH20 and evap my water? the only reason i don't want to gas is i dont have any H2SO4 right now. inless i take it out of an old car battery i have out in the barn. would lead in the battery cause any problums? could i do it using foil and hydrochloric as long as i dry the cock out if it?
and one last one that should of been closer to the top. when doing my Al/Hg would it be ok to add a few mg more HgCl2. and if not whats the reason not to.
Battery acid doesn't work,you could also titrate freebase in acetone and it'll will precipate if you 3-base was pure,if otherwise,you won't probably see any nice crystals at all and may just titrate in water and evapp.Rxtal would be nice.You may add as much HgCl2 as you want but emptying 100 gram HgCl2 bottle to amalgamate 25 grams of foil is not right thing to do,however,cuz it costs pretty much.
For those about to synth,we salute you
(Daddy)
06-13-03 08:51
No 439777
Raffike, for taking the time to answer all these valid questions, the way he putted them indicated already a lot of UTFSE, mr GOD, however I also like some witty remarks from time to time to lighten up the forum.
LT/
WISDOMwillWIN
(One Man Show)
06-13-03 09:31
No 439784
Forget distilling,freeze!!!Distilling you won't get it even nearly as pure as with freezing.Freezing is lot easier also.
I am not disagreeing, as I know Raf has solid skills, but it just doesn't seem that it could be easier than:
1) dumping the oil into your boiler, along with a stirbar
2) setting up your vacuum distillation rig properly with greased joints, etc.
3) filling a pan with peanut oil, and placing it on a hotplate
4) submerging the boiler into the peanut oil
5) turn on the heat and stirrer
6) turn on the vacuum
7) turn on the recirculating water pump for the condenser
sit back and wait... Time wise, it seems much more efficient.
What ever floats your boat I guess...
"...somebody is feeding these damn animals booze." Fear & Loathing
(Hive Addict)
06-13-03 09:37
No 439786
I am not disagreeing, as I know Raf has solid skills, but it just doesn't seem that it could be easier than:
If it was that easy i(and LaBTop here and other bees) would reccommend simple distillation but swiraf distilled his sassy like that w/o fractionating column and ended up with safrole of sg of 1.083,doesn't sound very pure.Freezing left safrole with density of 1.097
PS what could be easier than putting your safrole in a jug and then putting it to freezer,coming back tomorrow and pouring away impurities and repeating same procedure 2 times?We are not in hurry anyway.
Distillation probably work also but you need very good packed column to achieve acceptable purity but it still won't beat purity got with freezing.
For those about to synth,we salute you
(One Man Show)
06-13-03 10:12
No 439795
True, it does sound just as easy. And no, we are not typically in a rush.
SWIM just found that simple vacuum distillation of the oil was a good foundation builder.
Maybe a good exercise (disregarding time as an element) would be to vacuum distill, and then place the receiver flask in the freezer and follow up as you suggest. Thereby giving a good experience in both procedures, and ensuring good quality.
Seems plausible to me...
"...somebody is feeding these damn animals booze." Fear & Loathing
(Hive Addict)
06-13-03 10:52
No 439809
Yes,this sounds ok to me.One can also see how much his pump pulls if he distills oil.
For those about to synth,we salute you
(Hive Addict)
06-13-03 13:23
No 439841
...and that will certainly bee nessisary (to have bp of saf under his vac) for later when it comes time to distil (and verify) ketone- so for a first time run, its definatly nessisary.
LT- OK, I admit it...I was origionally going to awnser his questions, but when I realised how much work it was going to bee -going back and forth (ADD)- I said 'fuck-it' and took the easy road.
Story of my life.
shit...I found out it was all just one big manic episode!
(Hive Addict)
06-13-03 13:27
No 439843
a few things i feel are worth mentioning on the topic.
1. i am not convinced that freezing, while very labour saving (no keeping an eye on an operating still) and clean (very little mess or smell associated with the procedure) is as efficient as distilling. anecdotal evidence suggests that freezing will get 80%-85% safrole from a oil reported to be 90%+ safrole. NEVER throw away your remainders. collect and retain them. once you have enough, distill them for the remaining safrole.
2. one big merit freezing has over vacuum distilling, especially at the larger scale, is less wear and tear on equipment. running a vacuum pump for (roughly) 10 hours per litre just doesn't make sense when you can freeze it out. that's just me, though. save the distilling for the remainders.
3. i'm still stunned by everyone's inability to generate seed crystals. i have never had a 5mL vial of safrole fail to freeze. most jugs of sass i've seen have never failed to spontaneously freeze in the freezer. most will do so spontaneously in a fridge as well. just leave it alone, set the temp to the lowest and come back in a week, it WILL be frozen. if it was feasable, i would gladly mail a frozen vial in dry ice to everyone who wanted it... sadly it isn't, so don't even think of asking.
i AM NOT saying there is never a reason to distill. i AM saying don't give up on freezing.
if someone wants to take the time to split a 500mL into two equal parts and distill one and freeze the other, they will tell us the efficiency once and for all.
AND NEVER, EVER throw away your remainders.
Now with 12% more Bottom!
Nymphomania is not a disease, its a goal! (Methadist)
(Hive Bee)
06-13-03 16:08
No 439878
It has been mentioned before that a good way to get a seed crystal if you are having trouble is repeated temperature changes. Put about 5-10 ml in a small container and put it in the freezer. Come back several hours later, if it hasn't frozen take it out and let it warm up to room temp then put it back. Do this a few times on stubborn safrole and it should give.
(Hive Addict)
06-13-03 18:45
No 439890
Once Swim had some sassy in the freezer that, after 5-6 days, wouldn't start freezing.
He read up on some posts on the hive and one in particular mentioned rubbing the bottom of the beaker with a glass rod to "Induce crystallisation".
So swim scratched the bottom of his beaker full of sassy for about ten minutes and put it back into the freezer.
Next morning, VOILA!, a beaker full of crystals.
Don't ask swim as to the mechanics of this phenomena as he wouldn't have a clue. But it did work.
Heavens just a rumor she'll dispel
As she walks me through the nicest parts of hell
(Hive Addict)
06-13-03 23:06
No 439929
Post 436454 (GOD: "If you distil a small amount, it (the small...", Chemistry Discourse)
shit...I found out it was all just one big manic episode!
(Hive Addict)
06-13-03 23:37
No 439934
For raf it takes about 2 hours and first crystals start to appear.In 10 hours,whole flask is frozen and some liquid may be poured away.That drained stuff when put into freezer,doesn't freeze which indicates low <50% safrole content and smells bad.Pure safrole has little smell,impurities make sassasfras oil smell hard.
Safrole itself is slightly yellow or green but color is very faint.sg at 20 is over 1.096.If i could get a digicam somewhere i could post a pic but at the moment i don't have one.
For those about to synth,we salute you
(Hive Addict)
06-14-03 09:28
No 440001
(Rated as: excellent argument)
raff- if you leave it in the fridge, it should continue to freeze, just exponentially slower.
Swim used to keep his fridge just one or two degrees lower than the melting point (the slower, the better, the cleaner). It'd take ~4 days for it to finish freezing (400-800ml's in a mason jar). By that point, the unfrozen liquid would have gone from a pale-yellow, to a concentrated-yellow-dehydrated-piss color. Swim would then repeat 2 more times, saving the 'waste' (and combining). The 'waste' could then bee innoculated with another seed crystal and so on.
shit...I found out it was all just one big manic episode!
(Hive Bee)
06-16-03 07:22
No 440295
every one thanks for helping out.
i'll let yas all know the results of my dream if it come out right.
i ended up going with distilling my sass. so i would know my rig better.
i just wish the wacker was easier. 18 hours total so far and only biginging to see red. my hands are like rocks now. i think a few runs like that and i'll have some pythons for arms.
(Newbee)
06-16-03 09:21
No 440315
I think it's a better idea to turn on your stirrer, then turn on your vacuum, then turn on your heat. If you do it in this order: Stirrer, heat, vacuum...you could have some serious burping into your previously clean column and receiving flask.
D.A.R.E. = Drugs Are Really Exciting