I did the nitration from DNT to TNT (so I think) I know that what I had before was DNT because the MP was right on point with the DNT melting point
(the common isomer). I didn't have oleum, so I used slightly higher temps, and excess concentrated sulfuric acid, I am not so sure what this top layer
is.. Maybe un-nitrated DNT? Although, that is the same amount roughly of DNT I started with, so is it possible no reaction occurred since there was no
sulfur trioxide present? I had thought TNT was a darker color
I kept the reaction between 112-120 Celsius.
My procedure was:
Starting with 30ml of DNT and 50ml of spent acid (from the nitration of MNT to DNT) I added 60ml sulfuric acid and brought the temp up to 95C. The
nitration mix was 30ml 99% HNO3 and 50ml 95% sulfuric acid, added slowly drop wise to the DNT mix keeping temps above 110C w/ hot plate.
BTW, in the picture, the temp is roughly 35C.
[Edited on 31-12-2013 by Turner]
[Edited on 31-12-2013 by Turner]Turner - 30-12-2013 at 18:23
Looks exactly the same, temp 30CTurner - 30-12-2013 at 19:31
Ok now the top layer has solidified and long crystals have began to precipitate throughout the mixture. I removed the top mass and now it is a
solution with what I presume to be TNT crystals and probably some DNT. I am wondering if the top mass was unreacted DNT? If so that would be a lot of
unreacted material. I will post a pic when I get a min.Turner - 30-12-2013 at 19:38
[Edited on 31-12-2013 by Turner]roXefeller - 30-12-2013 at 19:54
Now check it's purity and report yields. Make it a nice little lab write-up. Maybe the mod's will tack it onto the TNT thread. Did you get the
bisulfite? And next time you do a synthesis, don't make so many sequential posts that ask for spoonfeeding. You're only begging to have a thread
thrown to detritus. Try to have as many notes of the process before you start that you'll be able to re-read as its going along, and journal the work
while doing it. You can't expect to have someone holding your hand in realtime on the forum. Just do it... safely, and if you mess up, pour it out,
check your notes, correct and try again. Confidence and experience will come.
[Edited on 31-12-2013 by roXefeller]Turner - 30-12-2013 at 20:13
I guess you are right, but I've spent all day on this little project and was anxious to see others experience. Tommorow I will collect and wash
crystals and evaluate melting point.
I am keeping those chunks of unknown material, any clue what this May be? It separated right after final nitration as an oily layer, and the whole
mass stayed a liquid until the top began to solidify at which point long crystals began to form on this mass as seen in the picture.roXefeller - 31-12-2013 at 04:30
You can't be anxious around here. The sages will see it as an immaturity that begets accidents. Respect the chemistry, respect the fixed nitrogen.Fantasma4500 - 31-12-2013 at 04:50
''Respect the chemistry, respect the fixed nitrogen'' -roXefeller, 2013
straight up!
you could probably compare the burn with other videos of its burning..Turner - 31-12-2013 at 08:45
The milky green material has no crystals. I dumped everything in cool water and it is now just milky green, the other stuff on the top melted at 53C,
I assume this is DNT, and no DNT was nitrated to TNT.
[Edited on 31-12-2013 by Turner]roXefeller - 31-12-2013 at 16:07
''Respect the chemistry, respect the fixed nitrogen'' -roXefeller, 2013
straight up!
Don't repeat what he said, it'll go to his head.Turner - 31-12-2013 at 19:24
I guess only way to find out if I have any TNT is to detonate it. Here is a 15g cast TNT (?) charge. Will video.
Zyklon-A - 31-12-2013 at 19:32
Well that's what you made it for right? Do you have a blasting cap?DubaiAmateurRocketry - 1-1-2014 at 01:31
Well, congrats on your TNT, I hope you got there. Try purifying some more and do some burn test or detonation if you can I would like to see more.
What is the density of TNT ? I am pretty sure TNT is higher than DNT. So if you just add 10 ml of water. keep adding ur product until it reaches 1
extra, ml, see the weight inrease, and find some papers that says the density, and there you go.
I find testing density a good way of finding if ur product is what you want.
[Edited on 1-1-2014 by DubaiAmateurRocketry]Turner - 1-1-2014 at 21:06
I'll try and detonate it soon, I will have to base partially off sound to see if it detonates.roXefeller - 1-1-2014 at 21:29
You mean you let the new year's ball drop without detonating that charge. I thought for sure you were working on a schedule to get a midnight boom.Turner - 1-1-2014 at 21:48
Haha, we lit a standard blasting cap in the street and decided any more than that would be trouble.papaya - 2-1-2014 at 00:38
I bet it won't work.Ral123 - 2-1-2014 at 00:52
Don't these standard blast caps snap fingers and throw shrapnel? We aren't talking about flash and cardboard here.Turner - 2-1-2014 at 09:12
Papaya, do you care to explain why? You sound like you may know a bit about TNT and making it.
A metal industry blast cap probably would throw tiny pieces of shrapnel inside a small radius (3m?) but outside, there would be no worry.
[Edited on 2-1-2014 by Turner]simply RED - 2-1-2014 at 09:52
Cast TNT is notoriously difficult to detonate. In military munitions they put tetryl booster between the cap and the cast TNT. It may not work with
straight blasting cap.Zyklon-A - 2-1-2014 at 10:03
Make NI3.This is a bad idea, but you can put about half a gram of NI3 (while it's still wet) on top of you're TNT, when it dries, it will easily
set off the TNT.
The obvious downside is that you will never know when it's about to go off, and yes, WET NI3 is quite stable, I've hit it with a hammer and it didn't
go off, but when it's dry...
Edit: Actually, don't try this, it has been know to explode when wet, I guess mine was a bad batch. Still went off when it dried of course.
[Edited on 2-1-2014 by Zyklonb]Ral123 - 2-1-2014 at 10:27
Cast TNT is notoriously difficult to detonate. In military munitions they put tetryl booster between the cap and the cast TNT. It may not work with
straight blasting cap.
I guess 5g caseless pressed ETN would work. I've heard 7g of Tetryl and 20g Tetryl. But at what density, and what casing? I'm sure there's a huge
difference between heavily pressed 7g Tetryl caseless and hand pressed in PVC with thick epoxy layer on the bottom. papaya - 2-1-2014 at 14:45
Never prepared TNT, as I think it simply doesn't worth the trouble. I said it'll not, because I also think that in cast form it's too insensitive,
also critical diameter, etc..
Even if you wake up it with a huge initiator charge - it'll be somewhat hard do distinguish the effect from that 10gr of ETN for example or from your
TNT. But of course I don't want to stop you - try (safely) and report.
If you want I can tell you real story that happened with one of my friend - he found in the field a real military grenade (not hand one, but more like
small projectile). Of course he removed the cap somehow and when he showed me the stuff - it was that projectile with remainings of cast TNT inside
and the hole in place of detonator. Before that he even managed to SCRUB that TNT out with the use of wedge and hammer (stupid, but he had no
knowledge of the dangers and never asked me before starting), anyway we had a pile of about hundred grams of cast then crushed TNT flakes with no idea
what to do next.. I was familiar with TATP in that times and we decided to try to set off some part of it - 15grams were pressed into plastic tube
with 1cm or even more diameter, a gram of TATP above that, a fuse.. It went off with a very weak sound, not at all damage to underlaying objects(a
thin metal plate), but we didn't find any remaining TNT or plastic tube - just very weak explosion and disapperiance of 15gr TNT - must be partial
detonation of the finest powder only. We knew very little about theoretical things (that cast one is hard, diameter, etc) and started to think that
the material is not real TNT, so we just BURNED everything else we had, old good days...
Papaya, do you care to explain why? You sound like you may know a bit about TNT and making it.
A metal industry blast cap probably would throw tiny pieces of shrapnel inside a small radius (3m?) but outside, there would be no worry.
[Edited on 2-1-2014 by Turner]
Turner - 2-1-2014 at 16:02
it's not very reasonable to detonate cast TNT in amounts like 15g, I will probably use 5g ETN plastique booster, it may be hard to tell if it
detonates.
TNT (?) is the most tedious, and time consuming one I've ever done, though, also dangerous (hot sulfuric/nitric acids).
While melting some TNT (?) under water to clean it, some water boiled causing a tiny bit of molten material to splash out onto the hot plate which
caught fire instantly FWOOSH.
I got a bit impatient towards the end, I let the temperature rise to around 120C which caused some NO2 to form, I also didn't take 2hours of stirring
after addition. (Who stirs something for 2 hours straight?)
[Edited on 3-1-2014 by Turner]Turner - 3-1-2014 at 15:08
Charge failed, not enough primary used in cap!Zyklon-A - 3-1-2014 at 15:52
Try it again, with a stronger blasting cap of course.Turner - 3-1-2014 at 16:03
Yes, I tried w/ around 100mg of SADS in the cap and only a very small, weak pop was made, I got up and saw bits of TNT and pieces of plastic
scattered.
[Edited on 4-1-2014 by Turner]DubaiAmateurRocketry - 3-1-2014 at 16:28
try it again with a larger batch then. With a booster if you can. TNT is an insensitive explosive.Zyklon-A - 3-1-2014 at 16:40
Did you recover any TNT that was scattered from the blast?Turner - 3-1-2014 at 17:18
I need a 1000ml pyrex beakers, I might try a jar but how would this do on a hot plate? I had to dump some remaining acid for the TNT nitration because
my beaker got full.
I might try again, but it's so tedious, time consuming and complex making TNT and then worrying if your product is at the correct nitration level.
later this winter I'll do something more.Zyklon-A - 3-1-2014 at 17:59
I've had a household jar crack on a hot plate before, it wasn't a big deal for me, but I wasn't heating explosives. I think you should get a 1000ml
pyrex beaker, best to be safe then sorry, if the jar did crack and the TNT spilled on the hot plate it would just catch fire and burn, not explode
right? Here's something that you might want to read, an accident because of faulty glassware, be careful.
[Edited on 4-1-2014 by Zyklonb]Ral123 - 3-1-2014 at 20:19
I'm sorry for the fail bro, how was your blast cap made? Turner - 3-1-2014 at 20:31
.8g ETN pressed heavily into a plastic tube and .1g SADS pressed on top, fuse sits on this. Didn't get enough acetylide into the cap.Ral123 - 4-1-2014 at 02:19
If you've compressed the ETN with a wooden rod and a rubber hammer, that might have made it not go off from the pop of the SADS. I'm not sure if the
SADS detonated at all in such small amounts. Did you have tamping above it, like epoxy or some paper piece. Do you suspect lower nitrates in the ETN?Turner - 4-1-2014 at 08:25
I have used a cap with similar configuration before, the SADS is pressed firmly on top of the etn so there is like a pellet of etn and SADS stuck
together. I highly doubt lower nitrates of etn. I think there just wasn't enough primary to continue the explosive train. Ral123 - 4-1-2014 at 11:18
Bad luck bro.
"Make it strong enough and then make it twice as strong"
-John Moses BrowningZyklon-A - 4-1-2014 at 11:20
I would like to see more.