FLchem10
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Weird PICRIC
Ok I have made TNP a good amount of times and after purification I get a very nice yellow crystals but I made a batch using the right ratios with the
ASA purified, H2SO4 , and Potassium Nitrate.......
Here's my issue my boiling flask I use for TNP isnt big enough for the amount I made to boil during purification at once so I split it......
The first batch came out a ver nice yellow as I said before but the second is very heavy and a DARK orange.....What might this be? It seems like I
should know whats going on but EVERYTHING and I meen EVERYTHING was done exactly the same and one came out with nice long yellow crystals and one is
very small crystals and a DARK ORANGE ( not the goo that has been talked about) actual crystals like the others and no metal contamination....
Please help Im stumped my brain is taking the day off
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quicksilver
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From the description you have a larger level of hydrogen in the 2nd synthesis; that often accounts for a darker orange. Test to make sure you have
fully nitrated to a genuine TNP; if so determine the issue wherein the one synthesis altered from the other. Always make sure you have a clean
trinitro product. Occasionally DNP exists within the synthesis. Hydrogen can occasionally be released by water re-crystallization obviously. Do the
math first, understand what is taking place. If genuine oddities exist then by study you will find not only what they are but why they are there.
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FLchem10
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I will check my math again but Hydrogen in the mix I not quite grasping that....how would one turn out fine with the same synthesis?
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FLchem10
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Well I re-purified the ORANGE filtrate and now it looks fine long crystals are forming and it is no longer orange????
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quicksilver
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OK water has what as part of the molecule? But that not my point.
There is a very quickly (and lazy) test for TNP. PURE TNP will pop if a tiny amount (mg level) like a match-head is placed in a aluminum foil square
and placed on a heavy steel (anvil) weight and struck with a hammer. -= For Heaven's sake just use a tiny bit and it will pop like a toy cap=-.
ALL too often completed nitrating leave undesired material in the synthesis. Most often this is DNP - simply a lower nitration. Nitrations are rather
gross in the sense they are a large often difficult to control reaction.
Your mp goes UP with the level of nitrations in picric acid. Single and di-nitrations have a mp of 114 and your THP should have a mp of 122-123.
The sulfonation of phenol slows the nitration & allows more control. some materials simply cannot be controlled without the sulfonation mechanism.
If you examine the process; it simply cannot take place without hydrogen but if control is lost at any point the hydrogen does not "get used" and
remains. This often results in two issues: more (or total DNP & a deeper coloration.
Pure picric acid is often SO light yellow it's almost white with just a bit of yellow. It's refined shape is mostly cubiod (commercial). I can't draw
a shape with a keyboard but the process looks something like similar to most benzene-family nitrations.
This leads to a portion of organic chemistry called the "Rule of Crum Brown": If an atom attached to the atomic nucleus is attached to some
other atom by unsaturated linkage through a bond which is commonly said to be "double or triple" then the next entering group takes a different
position in that molecule group. (this is where you hear the expressions meta, ortho, para. and is extremely important to get a grasp on what
taking place in a large activity such as a nitration.
This takes a lot of typing for someone like me to explain and you should do that reading yourself to get a good grasp on it. This also is what
balancing equations partially entails. I am a true hobbyist and have only had chemistry at the undergrad level.
Do a search for "picric acid, process of nitration" or "TNP, nitration" & someone has (most likely) posted it half a dozen times already. The
point is that a balanced equation of the nitration of phenol will show often enough a need to sulfanate to slow the process. Finding the REASONS why
this is important is actually very exciting once you "get it".
This also exists in analine.
The example of Dimethylanaline actually cannot be nitrated directly: it will oxidize immediately. Once that process gets started additional nitrations
cannot move forward. That why Toluene is generally nitrated separately as it bonds. So does napthaline. Most of the "yellow Orange" nitrations have
stopped at the di-nitration point.
This one reason why you do your math first: to see the balanced equation and proceed from there. The math is NOT the divisional aspect of materials
(the arithmetic of precursors, etc) but that of the equation.
Dividing a synthesis will not necessarily yield your synthesis just as multiplying the precursors / components in a synthesis will result in success.
In a sense I wish I could just drop the equation on the page and show you what exactly where I am headed. But honestly I don't have them memorized
& perhaps that's not in your best interests anyway as you will get more from hunting out the concept. The majority of these are referred to as
"CHNO" explosives. And one very good source is a search for "CHNO explosives, balanced equation".
I'm not a great teacher and there are some real chemists that could explain all this in 6-10 sentences. But you are at a juncture: either you will
choose to continue with "recipe-type" synthesis or you will start to begin all this mentally & explore other areas related to energetics that
illustrate the processes.
I totally such that some of the guys could do that but I sort of doubt they would want to do a one man TA blackboard presentation as it's much more
important to learn balanced equations by your own efforts: it's NOT that tough. And it WILL answer a great deal of questions; even if you have to look
up nuances every so often.
OK I DO remember one. It's from combustion reactions:
C25H52(S) + 30 O2 (G) -----> 25 Co2 (G) +26h2O (don't trust: verify. but I'm not too off)
Hydrocarbon in candle wax+Diatonic Oxygen Carbon dioxide water (it's probably incorrectly presented but it's something i remembered and should give
you a general idea. It's also important is many areas.
(the diatonic O is O squared); this is the math we're dealing with, not arithmetical constructs of divisional or multiplication in yield synths.
...throw that issue out. Dividing a synthesis in half is not a guarantee that you will get 1/2 the yield! But that's a whole other subject. A couple
of guys here helped me with remembering some things but (IMO) it's more important to know where to go to check your work especially before you begin.
--OK; I tried & I'm burnt out.
[Edited on 17-2-2011 by quicksilver]
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FLchem10
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Actually that makes perfect sense so thanks for the help
one question though....about something you said...Ive seen on here people doing the same process to make TNP but using napthaline....
Also I saw a video on youtube about make TNP and he used a crystal powdered phenol....I use ASA purified....where can I get this and which phenol is
the best....
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quicksilver
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I don't know any sources for chemicals. The best thing is to search the internet and find a deal. phenol is VERY common. Some folk like the smell some
hate it. but many of the ORIGINAL picric acid precursors are related by the slightest issues within the molecule. I once made picric acid from Indigo
(& it worked well) another gent made it from Oil of Wintergreen, and somebody tried making it from wool or horn but said it stunk too badly even
outdoors with a wind to continue. You do some real research on picric acid and it's fairly damn interesting. Some people enjoy the subject as it's a
jump-start to all sorts of interesting things.
There really is no "best"precursor. The (solid) phenol of the original nitration concept has a mp of 45C and has a unique smell. It's used in certain
anti-bacterial agents. You could find it on the net somewhere. But The easiest thing is to start an account at a chemical distributor that isn't too
costly and buy what you need as reagent-level material and buy some glassware to distill what you can't buy or afford.
Whenever gathering information on a subject that can be dangerous: always have a "double-level" authentication plan. Don't believe what anyone tells
you or you see - especially on the 'net till you have a book written by academics that substantiate that material. People will say all sorts of things
and it's always in your best interest to know if it can be substantiated.
Just a an aside: naphthalene is somewhat different! It CAN be nitrated by direct exposure to HNO3 in it's first position in nitration
(mono-nitro-nathaline) and is easily obtainable as mothballs (READ the ingredients!). There is a lot to learn as to WHY this is. READ and understand
the balancing of the equation 1st: then do your lab. Study the basics IF you have trouble with it and ask questions. Someone WILL help you understand
the elements of chemistry in so far as the concepts and notation. That's the proper way to learn this subject. It's NOT difficult IF you really want
to learn it.
[Edited on 17-2-2011 by quicksilver]
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