Takron
Harmless
Posts: 47
Registered: 19-5-2010
Member Is Offline
Mood: No Mood
|
|
Phthalic Anhydrid is red?
When I started heating my Phthalic acid to make anhydride, all it did was fog up inside the beaker and condensed on the flask as a very hard yellow
cake that I had to scrape off repeatedly through the process. After doing this and getting no anhydride crystal formation. The cloud turned red and
how there is an orange condensate forming inside the beaker and the crystals are red-orange. If I had to describe it, it looks like bromine when its
in the liquid phase. The crystals forming are equally red-orange.
|
|
Bot0nist
International Hazard
Posts: 1559
Registered: 15-2-2011
Location: Right behind you.
Member Is Offline
Mood: Streching my cotyledons.
|
|
Did you synthesize it? Which isomer?
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
|
|
Takron
Harmless
Posts: 47
Registered: 19-5-2010
Member Is Offline
Mood: No Mood
|
|
Yes I did. I believe it was ortho-phthalic acid.
|
|
woelen
Super Administrator
Posts: 8027
Registered: 20-8-2005
Location: Netherlands
Member Is Offline
Mood: interested
|
|
Phtalic anhydride is white. I have a commercial sample of this chemical.
Probably you heated too strongly and your material started charring somewhat.
[Edited on 4-11-11 by woelen]
|
|
DJF90
International Hazard
Posts: 2266
Registered: 15-12-2007
Location: At the bench
Member Is Offline
Mood: No Mood
|
|
Quote: | When I started heating my Phthalic acid to make anhydride, all it did was fog up inside the beaker and condensed on the flask as a very hard yellow
cake that I had to scrape off repeatedly through the process. After doing this and getting no anhydride crystal formation. |
The "condensate" is actually a sublimate, and is your product anhydride. Turn down the heat and it shouldn't char so much. I think Magpie has done the
phthalic acid -> anhydride prep here somewhere, look through his posts on the topic to find details that you need. What colour was your starting
phthalic acid? Did you follow a published procedure (e.g. journal or textbook)?
|
|
Takron
Harmless
Posts: 47
Registered: 19-5-2010
Member Is Offline
Mood: No Mood
|
|
I followed NurdRage's procedure for luminol and just was going to stop at the anhydride step. My phthalic acid was white and needly. When I heated it
there was a dense white fog inside the beaker for a time but it was comming out the beaker like smoke and I got a few tiny bits of anhydride forming
by the spout of the beaker but nothing ever looked like cotton candy inside the beaker. I am pretty sure it was some kind of condensate at the end
because very red liquid was running down the sides of the beaker on the inside and very red crystals formed on the cooler at the top and if I'm not
mistaken, sublimation is a solid to a gas.
|
|
Bot0nist
International Hazard
Posts: 1559
Registered: 15-2-2011
Location: Right behind you.
Member Is Offline
Mood: Streching my cotyledons.
|
|
Did you use a controlled method of heating, or did you use open flame? Maybe try using a tall narrow beaker. Put a little foil skirt around the bottom
1/4 of the beaker, then cool the upper 3/4 of the beaker with moving air, a wet tissue, or both.
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
|
|
Nicodem
|
Thread Moved 4-11-2011 at 10:08 |
DJF90
International Hazard
Posts: 2266
Registered: 15-12-2007
Location: At the bench
Member Is Offline
Mood: No Mood
|
|
You said it condensed as ahard yellow cake...
|
|
Takron
Harmless
Posts: 47
Registered: 19-5-2010
Member Is Offline
Mood: No Mood
|
|
semantics. The point of my question isnt' about the name of what happened its about why it was yellow and then turned red. it should have been white,
and I don't know what would have caused this to be dark red. There was only phthalic acid and sodium chloride in the mix.
|
|