| Pages:
1
2 |
ScienceNoob
Harmless
Posts: 19
Registered: 3-6-2012
Member Is Offline
Mood: No Mood
|
|
I am 19... lack of maturity? I can tighten up if need be... 
|
|
|
Hexavalent
International Hazard
Posts: 1564
Registered: 29-12-2011
Location: Wales, UK
Member Is Offline
Mood: Pericyclic
|
|
No, just lack of confidence and effort mainly.
Look up the terms to make sure you use them correctly and avoid ambiguity . . .how long have you been doing chemistry BTW?? Why don't your family
trust you? With some dedicated space to keep your stuff, a fire extinguisher, a regulated hotplate, safety gear and common sense most experiments can
be done safely.
Again, try insulating the column even more and supply additional heating if necessary to it. Make SURE the liquid itself is actually boiling in the
flask, and be sure that a vacuum is actually coming out of the aspirator . . .answer some of my questions and then I can help answer yours much
better
I'm 14 BTW and my family trust me
"Success is going from failure to failure without loss of enthusiasm." Winston Churchill
|
|
|
ScienceNoob
Harmless
Posts: 19
Registered: 3-6-2012
Member Is Offline
Mood: No Mood
|
|
I feel ashamed, so bad right now... I actually just started last week I am doing this as a hobby. I am majoring in Computer Science with strong
emphasis on software application development. I would like to say I am impressed with your level of maturity for your age and your intellect in this
area I have a feeling you will do great things one day. Also the place where I live is an apartment complex so I do not wish to endanger others with
my stupidity god forbid something goes wrong. I am however pretty careful and paranoid about almost every move that I make while carrying out my
procedure. Here are some of the pics as requested. Also I am not getting a temp of 51C at the adapter...
     
|
|
|
ScienceNoob
Harmless
Posts: 19
Registered: 3-6-2012
Member Is Offline
Mood: No Mood
|
|
Oh to add I did as instructed it is boiling without stirring I tested it for 60 secs and I would like to correct the typo in the last post I am now
getting a temp in the three way of 51 C I am about to try heating with a blow dryer for a while as instructed. I thank you for your help and I do plan
on studying the terminology from now on before using it in a sentence xD
|
|
|
ScienceNoob
Harmless
Posts: 19
Registered: 3-6-2012
Member Is Offline
Mood: No Mood
|
|
I shut it down for the day should not have taken this long.
|
|
|
Nicodem
|
Thread Moved
3-6-2012 at 22:25 |
Paddywhacker
Hazard to Others
Posts: 478
Registered: 28-2-2009
Member Is Offline
Mood: No Mood
|
|
Great work Hexavalent, you have a nice tutorial talent.
Noob, you do realise that the vacuum has to be applied to the opening marked '9' in Hexavalent's diagrams on page 1, don't you?
It is difficult to make out exactly what your setup is from your photographs. Maybe you could draw your setup, either in a paint program or on a
sheet of paper and then scan or photograph that.
Once we are on the same wavelength about your setup then things will go more smoothly. A thought before I hand you back to Hex ... if you have
already distilled off the low boiling fractions in an earlier experiment then your oil will boil at a higher temperature than you expect.
|
|
|
Hexavalent
International Hazard
Posts: 1564
Registered: 29-12-2011
Location: Wales, UK
Member Is Offline
Mood: Pericyclic
|
|
Thanks, Paddywhacker!
ScienceNoob ~ are you using the same oil now as when it worked for you the first time? If so, then as Paddy stated, all of the lower boiling fractions
(those with a lower molcular weight) will have come off in that first run, leaving you with higher boiling fractions (those with a higher molecular
weight) this time around.
I can only second what he also says about the diagrams; the images you have posted so far are 'incomplete' and make it very hard to see precisely
what's going on and what you are doing and how your apparatus is actually setup.
Additionally, are you sure that the aspirator can generate a sufficient vacuum for a long distillation? IME short filtrations are fine with them but
long distillations are a no-no. For the lower boiling fractions, it is probable that a vacuum is not necessary to boil them under a reasonable
temperature, but the longer-chain ones, thusly those with higher boiling points - probably do need it to lower their BP to make it a more easily
attained temperature for your heating apparatus.
Supplu us with details, and we shall supply you with answers. I still don't believe, though, that fractional distillation under vacuum is a good place
to start for a beginner, hence the ambiguity we get from the array of factors that could be causing your problem and you not using the proper terms
correctly without even bothering to research them and their definition first.
I should point out, however, that with vacuum distillation you were corret to use a stir bar and not boiling stones to avoid bumping or superheating
(sudden, violent burts of boiling that can cause the original mixture to splash up into the stillhead, damage apparatus and cause injury) - under
negative pressure, I recall reading somewhere that standard boiling chips do not work as, because of the pressure differences, they cannot release
their little bubbles of air when heated that rise to the top and promote smooth boiling.
[Edited on 4-6-2012 by Hexavalent]
"Success is going from failure to failure without loss of enthusiasm." Winston Churchill
|
|
|
mr.crow
National Hazard
Posts: 884
Registered: 9-9-2009
Location: Canada
Member Is Offline
Mood: 0xFF
|
|
What are you distilling from camphor oil?
We are happy to help, but distilling safrole on your apartment balcony isn't the best way to get into it or represent amateur science
Double, double toil and trouble; Fire burn, and caldron bubble
|
|
|
| Pages:
1
2 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
