| Pages:
1
2 |
Actinium
Hazard to Self
Posts: 67
Registered: 2-9-2014
Member Is Offline
Mood: synthetic
|
|
Quote: Originally posted by aga  | | Quote: Originally posted by Actinium | | as a beginner seeing this in the Merck Report none the less you would think that it would hold some validity. Since its clear that it is wrong this
would be a perfect example to demonstrate that not all literature is accurate |
Definitely.
There is quite a lot of literature that Assumes that the information they have is True, and print it. Especially so on the Internet.
Hold everything you learn in the 'Might be right' box until you have experimented with it and proven it's validity for yourself.
Experimentation is how it all got discovered in the first place, and there is no substitute for sheer experience, so get distilling, fiddle with the
parameters and take load of measurements. |
That sums up what I'm trying to do. I think we are all here to
share in learning and fondness for Chemistry.
@ Arkoma that was my original intent was to recover the solvent, but when I started to smell pepper in the IPA it made me wonder, and was wondering if
you had a similar account and if so why? I don't have boiling chips I use my stirbar set on 300 rpm's.
@ S.C. Can you take a look at the link I had posted and give me your interpretation? The part I was talking about is one page back, right column
middle of the page.
I really want to invest in a soxlet extractor, Laboy has them fairly cheap, but for now would loading the pot and refluxing work the same?
|
|
|
S.C. Wack
bibliomaster
Posts: 2419
Registered: 7-5-2004
Location: Cornworld, Central USA
Member Is Offline
Mood: Enhanced
|
|
My interpretation is that it's a vague abstract of some observations on white pepper extracts. It's not about piperine extraction, it includes it, and
if I was going to go through the steps I'd just copy/paste them.
It's obvious that piperine is not distilled in any way.
There is a mention of using petroleum ether to remove oil from the piperine...this is the only part that really interested me; the recrystallization
in water would be interesting if it could be easily done on a large scale, but the filtration is too potentially horrible to contemplate.
In the oldest piperine thread IIRC I mentioned that if you leave denatured alcohol extracts to evaporate for a long time, the piperine crystallizes
out not badly, but then it gets crapped on by the oil suddenly precipitating, and like the Merck thingy said as well as I did then, it dissolves
piperine. So if you go that route it might be worthwhile to evaporate to whichever point and wash with pet. ether.
But I disavowed that later after trying base precipitation followed by washing with boiling hot water, instead of pet. ether, so it's moot...all I can
say is, after a couple IPA crystallizations, 3%, 134C.
Pepper does not float or stay suspended in alcohol without overhead stirring. Therefore, the Soxhlet.
|
|
|
aga
Forum Drunkard
Posts: 7030
Registered: 25-3-2014
Member Is Offline
|
|
White pepper ?!?!
Damn. I tried it with black pepper corns.
Got 1.38g of black pepper-smelling oil drying with some (what i hope is) CaCl2 in a bag.
Messing with the watery light brown top layer for a while, some of it dissolves in toluene.
It separated a little in NaCl and a bit more so in NaOH, but not much.
With Ammonia it went slightly darker, but nothing special.
Mixed all that together to see if it did anything, but no, so dumped it all.
Just the Black Oil and some residue from filtering.
OC smells a lot better than IC.
Edit:
Pepper corns being made by one of the most complex and amazing chemists ever living, strange and unexpected results when a monkey steals it's seeds
and 'extracts' things from said seeds should be expected, by the monkey.
[Edited on 22-9-2014 by aga]
|
|
|
Actinium
Hazard to Self
Posts: 67
Registered: 2-9-2014
Member Is Offline
Mood: synthetic
|
|
| Quote: Originally posted by S.C. Wack | My interpretation is that it's a vague abstract of some observations on white pepper extracts. It's not about piperine extraction, it includes it, and
if I was going to go through the steps I'd just copy/paste them.
It's obvious that piperine is not distilled in any way.
There is a mention of using petroleum ether to remove oil from the piperine...this is the only part that really interested me; the recrystallization
in water would be interesting if it could be easily done on a large scale, but the filtration is too potentially horrible to contemplate.
In the oldest piperine thread IIRC I mentioned that if you leave denatured alcohol extracts to evaporate for a long time, the piperine crystallizes
out not badly, but then it gets crapped on by the oil suddenly precipitating, and like the Merck thingy said as well as I did then, it dissolves
piperine. So if you go that route it might be worthwhile to evaporate to whichever point and wash with pet. ether.
But I disavowed that later after trying base precipitation followed by washing with boiling hot water, instead of pet. ether, so it's moot...all I can
say is, after a couple IPA crystallizations, 3%, 134C.
Pepper does not float or stay suspended in alcohol without overhead stirring. Therefore, the Soxhlet. |
thanks for taking the time to kindly answer. Is there anyway to makeshift a soxlet with a chromatography flask between the pot and the condenser?
@ aga Wiki pepper and it gives you the definition of white pepper. So no need to throw your project away.
so the left over gunk I had used to 70% IPA on to remove from the flask after my failed steam distillation, had formed plates which I believe to be
fats, i left the IPA in a beaker and have watched it evaporate very slowly over the course of a week. the bottom has the same plates, but in the oil
surface of the IPA are tons of sparkles, on further inspection revealed small clear needles.
[Edited on 23-9-2014 by Actinium]
|
|
|
S.C. Wack
bibliomaster
Posts: 2419
Registered: 7-5-2004
Location: Cornworld, Central USA
Member Is Offline
Mood: Enhanced
|
|
The only recommended improvised Soxhlet is the one attached to one of my posts in the thread my piperine posting is in.
[Edited on 24-9-2014 by S.C. Wack]
|
|
|
| Pages:
1
2 |
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
