greenivan
Harmless
Posts: 9
Registered: 1-7-2012
Member Is Offline
Mood: No Mood
|
|
An accident in my "lab"
I modified my basement as my private and simple lab.... yesterday i tried to make phenylacetone from dry distillation of lead acetate and phenylacetic
acid. I have ever tried similiar method using calcium acetate and it worked well except there's cement like residue that couldnt be removed in my
boiling RBF. yesterday, I used graham condenser + vigreux condensor (fract column) and "condenser" using large pipe filled by dry ice. After set my
heating mantle on maximum heating, i went back to my diningroom for just 10 minutes to get some tea, and i heard strange voices from my basement. OMG.
i ran there and found that the reactant was burned vigorously... the "plastic lid + thermometer" throwed away and the fire went out like a butane
torch lighter. After that, under panic I threw water and stopped the reaction. All my condenser burned so bad and my RBF broke off... no phenyacetone
distilled. Maybe can someone tell me what is my fault?
sorry for my bad english..
|
|
|
kavu
Hazard to Others
Posts: 207
Registered: 11-9-2011
Location: Scandinavia
Member Is Offline
Mood: To understand is to synthesize
|
|
Lesson learned: Never leave a setup running unless you have first made sure it has stabilized.
It might well be that the dry ice condenser got blocked by moisture/etc. freezing in it. Pressure built up and pop goes the thermometer adapter. Hot
gases of organic stuff are allowed to evaporate and can catch on fire quite easily.
[Edited on 5-7-2012 by kavu]
|
|
|
greenivan
Harmless
Posts: 9
Registered: 1-7-2012
Member Is Offline
Mood: No Mood
|
|
Quote: Originally posted by kavu  | Lesson learned: Never leave a setup running unless you have first made sure it has stabilized.
[Edited on 5-7-2012 by kavu] |
yes, I really shocked with the accident and I'm really sure that I will learn from it... But what parts are not stabilized in my setup? Where the fire
came from?
|
|
|
Hexavalent
International Hazard
Posts: 1564
Registered: 29-12-2011
Location: Wales, UK
Member Is Offline
Mood: Pericyclic
|
|
This is highly irresponsible; as kavu said, never leave a setup on its own until you are certain it is going smoothly at a good rate, all apparatus is
working correctly, set to the correct mode/setting etc.
How were you heating the reaction vessel? It is also possible that the dry ice condenser became blocked by moisture/water vapour etc. freezing in it,
building up pressure and popping the thermometer joint, being a comparatively weak connection on many ground glass setups. The organic vapour could
then have escaped and maybe caught fire that way.
Do you have a proper extinguisher (ABC or AB + C) for your lab?
"Success is going from failure to failure without loss of enthusiasm." Winston Churchill
|
|
|
woelen
Super Administrator
Posts: 8012
Registered: 20-8-2005
Location: Netherlands
Member Is Offline
Mood: interested
|
|
| Quote: Originally posted by Hexavalent | | This is highly irresponsible; as kavu said, never leave a setup on its own until you are certain it is going smoothly at a good rate, all apparatus is
working correctly, set to the correct mode/setting etc. |
I'm even more restictive on this. I never let a
powered setup on its own. As long as power is supplied to the setup and for quite some time after power off I babysit the setup. NEVER leave a running
reaction alone, not even if it seems to run smoothly and seems to be stable. What now looks stable may be unstable after 5 minutes (e.g. due to
evaporation to dryness of your setup). If you need to go to the toilet, then do that before the reaction starts or ask someone else to keep an eye on
the setup while you are away.
|
|
|
Nicodem
|
Thread Moved
5-7-2012 at 12:30 |
greenivan
Harmless
Posts: 9
Registered: 1-7-2012
Member Is Offline
Mood: No Mood
|
|
| Quote: Originally posted by Hexavalent | This is highly irresponsible; as kavu said, never leave a setup on its own until you are certain it is going smoothly at a good rate, all apparatus is
working correctly, set to the correct mode/setting etc.
How were you heating the reaction vessel? It is also possible that the dry ice condenser became blocked by moisture/water vapour etc. freezing in it,
building up pressure and popping the thermometer joint, being a comparatively weak connection on many ground glass setups. The organic vapour could
then have escaped and maybe caught fire that way.
Do you have a proper extinguisher (ABC or AB + C) for your lab? |
I heated my vessel using a heating mantle. My heating flask is 2000 ml one necked RBF, the condenser is 1 graham + 1 vigreoux, cooled by dry ice in a
pipe wrapped around it.
|
|
|
greenivan
Harmless
Posts: 9
Registered: 1-7-2012
Member Is Offline
Mood: No Mood
|
|
I just really wondered if the lead (II) acetate + phenylacetic acid is actually really easy to burned ?
|
|
|
kavu
Hazard to Others
Posts: 207
Registered: 11-9-2011
Location: Scandinavia
Member Is Offline
Mood: To understand is to synthesize
|
|
Not as such, but when heated strongly organic compounds tend to decompose to smaller readily volatile molecules.
|
|
|
edgecase
Hazard to Self
Posts: 65
Registered: 4-11-2011
Location: Ontario, Canada
Member Is Offline
Mood: Viscous
|
|
| Quote: Originally posted by greenivan |
I heated my vessel using a heating mantle. My heating flask is 2000 ml one necked RBF, the condenser is 1 graham + 1 vigreoux, cooled by dry ice in a
pipe wrapped around it. |
2000ml is a *very* large scale, especially for something you are trying for the first time. You mentioned that you did a *similar* reaction before...
how about using say 250ml when trying something for the first time? I have gotten in trouble by having too large a scale; when things get away, it
can get ugly really fast. Now I think smaller, at first.
|
|
|
greenivan
Harmless
Posts: 9
Registered: 1-7-2012
Member Is Offline
Mood: No Mood
|
|
| Quote: Originally posted by edgecase | | Quote: Originally posted by greenivan |
I heated my vessel using a heating mantle. My heating flask is 2000 ml one necked RBF, the condenser is 1 graham + 1 vigreoux, cooled by dry ice in a
pipe wrapped around it. |
2000ml is a *very* large scale, especially for something you are trying for the first time. You mentioned that you did a *similar* reaction before...
how about using say 250ml when trying something for the first time? I have gotten in trouble by having too large a scale; when things get away, it
can get ugly really fast. Now I think smaller, at first. |
If I have the stuffs more than enough, I prefer do large scale so the product is in larger amount and easy to identified.
Anyone know how to recognize the vapour of phenylacetone? I mean how is the colour, etc...
|
|
|
Hexavalent
International Hazard
Posts: 1564
Registered: 29-12-2011
Location: Wales, UK
Member Is Offline
Mood: Pericyclic
|
|
Pay a little more attention, greenivan.
When we say do a reaction on a small scale first, we mean to try it using <250ml, possibly <100ml amounts, just to test how it goes, if the
reaction goes smoothly, any unexpected results etc. If a reaction is unexpectedly vigorous, it's better if it occurs with 2ml or even 20ml of
chemicals in a small flask or test tube as opposed to 2L in a large flask. If nothing unusual is noted and the reaction proceeds fine, THEN you can
scale-up if you want.
It is not a waste of time, just an important safety consideration. Professional labs never experiment with 2L of chemicals the first time, usually
under 500ml: when they stumble across something they like, then they scale it up.
"Success is going from failure to failure without loss of enthusiasm." Winston Churchill
|
|
|
maxpayne
Hazard to Self
Posts: 78
Registered: 15-11-2011
Member Is Offline
Mood: No Mood
|
|
Can I ask you how you made phenylacetic acid?
|
|
|
woelen
Super Administrator
Posts: 8012
Registered: 20-8-2005
Location: Netherlands
Member Is Offline
Mood: interested
|
|
| Quote: Originally posted by greenivan | If I have the stuffs more than enough, I prefer do large scale so the product is in larger amount and easy to identified.
Anyone know how to recognize the vapour of phenylacetone? I mean how is the colour, etc... |
This is bullshit,
even if you have hundreds of liter of "the stuffs" then still you don't want to start an unknown reaction on a liter scale. This kind of posts makes
me pissed off. Why are you here? You want some advice? Then at least try to listen to the people who respond to your questions.
Test tubes and small scale glassware exist for a good reason. They allow you to test things on a relatievely safe and small scale and I strongly urge
you to use that option before proceeding to larger scale. This is important from a safety point of view, but it also can safe you a lot of losses.
What if the reaction does not work at all and you have 2 liters of mixed crap? What are you going to do with all the waste?
|
|
|
hissingnoise
International Hazard
Posts: 3940
Registered: 26-12-2002
Member Is Offline
Mood: Pulverulescent!
|
|
| Quote: | | What are you going to do with all the waste? |
Not to mention the product, if he actually gets it, that is?
|
|
|
maxpayne
Hazard to Self
Posts: 78
Registered: 15-11-2011
Member Is Offline
Mood: No Mood
|
|
I also agree with scaling up, but only AFTER trying small/test scale in chemistry as everyone here said.
Here greenivan claims that he want to go large scale because of the massive product for easier identification, he gets fire only, but he do not
specify what is the amount expected from his try. So, if this reaction produce so little product from 2000ml flask it is not worth discussing.
Another question is the nature of the product and how he (if) made the reagents. Maybe the source of fire lies in the impurity of the reagents.
|
|
|
Hexavalent
International Hazard
Posts: 1564
Registered: 29-12-2011
Location: Wales, UK
Member Is Offline
Mood: Pericyclic
|
|
Maybe, that is certainly a possibility.
Why are we even still discussing this topic now?
"Success is going from failure to failure without loss of enthusiasm." Winston Churchill
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
