hi all.

right now, i am synthesizing TNP. i've only left it so it can cool down, before i add more KNO3.

but: when i add the KNO3, there should be red NOx fumes. but they aren't, there are WHITE fumes! what the heck are these? SO3 (sulfuric trioxide)? and if yes, how can that be?

There should be no nox fumes if the synth is done right, i had the same white fumes when adding my kno3 to the h2so4, it should be nitric acid.

~H

ah, okay, thanks



by the way, may you tell me please if this will yield pure HNO3 (pure enough for converting hexamine dinitrate to RDX):

quote:

To 182ml of 98% sulphuric acid (or the highest concentration you can get, the higher concentration of H2SO4 the higher concentration of nitric acid) 300 grams of sodium nitrate is added in small amounts so that it doesn’t clump up. If sodium nitrate is not available, yet ammonium nitrate is, you can supplement 150g (grams, not mls) of sulphuric acid and 120g of ammonium nitrate. When ammonium or sodium nitrate are used, put them in the oven on about60-70*C for 30 minutes to get rid of the water it may have absorbed (both are very hygroscopic). Other nitrates can be used also, you can work out the proper ratios by working out the molecular weight. 1 mole of nitrate for every mole of sulphuric acid.Heat this mixture gently in an oil bath, and stir till you get a clear or yellow liquid. Cool this liquid in the freezer for about an hour, possibly longer so that a lot of the sodium/ammonium hydrogen sulphate dissolved in the nitric acid will precipitate. It will also freeze any sulphuric acid that has not converted to nitric acid. Now the still liquid nitric acid can be poured off, but do it before it warms up so the sulphuric acid does not liquefy and the sodium hydrogensulphate does not dissolve.



so, will this be pure enough?

PS: it's from peace's chem lab, which isn't online anymore, but i've got a back-up

[Had 5 min at the hotel comp today - DTP]

[This message has been edited by DavidThePyro (edited 07-12-2003).]

I wouldn't really trust it to be pure enough to make RDX. I think RDX requires like no trace at all of sulfate ions. Distillation is probably the only way.

Dont ever use code tags unless you knowingly press enter after every space, now this page is wider than it is long, next time cut and paste, either edit this or a mod needs to...

No that isnt good enought you need pure white hno3 for rdx, and not to sound mean or anything but you need alot more practice before you try rdx, if your asking questions like you just did you need more time before you try to synth rdx, many people think its simple but the chance of a runaway is very high, so get you have to be very observent... get some practice and try rdx in the not so near future.

As for getting pure hno3, i sugest using brainfevers method, his site has description with lots of pics, however; the link has sliped my mind...

~H

i'm sorry that i didn't edit it myself, but i was in a hurry. sorry DTP

hey... what's so complicated about RDX? i've read a lot of synths about it, and everyone sounds very easy... just mix hexamine dinitrate & >95% HNO3. voilá. what might happen if a runaway occurs?

mmh, a TNP-related question:

it's sitting in an ice bath now, and the TNP is settling to the bottom. now, i've got two layers. one at the bottom, and one in the middle of the liquid, it's about as high as the layer to the bottom. the stuff in the 2nd layer is nothing crystalline, i guess, or... the crystals there look kinda big, is that ok? and, what's that 2nd layer in the middle of the liquid?

[edit]

alengg's syntheses are good ones, have a look at his page:

http://www.angelfire.com/linux/alengg/main.html

now, honestly, RDX doesn't sound that complicated...

[This message has been edited by FMShadow (edited 07-13-2003).]

I never said that RDX was complicated, i just said your not ready, when i was at your level a was about to try RDX luckily Smokey was there to talk me out of it, you can try it once youve completed and comprehend a collge level chem book.

As for the second layer im not sure but id say it is likely undernitrated phenols,

~H

mmh... what about purifying it, what's that good for? what sense does it make to remove remaining H2SO4-traces?

[edit]

i guess i won't purify it, brainfever also doesn't, and he's quite an intelligent person, he is, truly.

[This message has been edited by FMShadow (edited 07-13-2003).]

Are you still talking about tnp or are you talking about rdx? For TNP its pointless to remove the h2so4 because you will add it in again but for rdx you must have pure white hno3...

Lol this topic is just you and me, others should really talk a little more!

~H

You definately are not ready if you don't know what migth happen if a runaway occurs. When a run away occurs the reaction billows NO2 which is quite toxic. As to your question about removing traces of H2SO4, this must be done because if I'm not mistaken H2SO4 decomposes RDX although I'm not really sure if I'm accurate on that. I haven't really looked into RDX too much because I don't intend to make it in the near future. Why is it that RDX requires white nitric? How does dissolved NO2 affect the reaction?

If you have problems with TNP and don't understand most of what is happening in the reaction then you are not ready for nitration.

Man, the first time I made TNP I knew it was obviously caustic because of the chemicals involved but I didn't really know how bad it was. The stuff is very toxic and easy to get into your system. It lingers for a long time as well. I can't believe how careless I was with the stuff.

Hey FMShadow, what nitrations other than TNP have you done? I assume you have done some nitrations other than TNP. If you haven't you should go back a step and do the easier nitrations(nitric esters). The nitration of cellulose is really easy, the nitration of sucrose and starch are a little bit tougher. I myself have nitrated cellulose, sucrose, and more recently glycerin. I still don't feel like moving up to nitro-aromatics yet although maybe the results of my nitric still might change my mind on that.

quote:Originally posted by themagmasher:

If you have problems with TNP and don't understand most of what is happening in the reaction then you are not ready for nitration.

Man, the first time I made TNP I knew it was obviously caustic because of the chemicals involved but I didn't really know how bad it was. The stuff is very toxic and easy to get into your system. It lingers for a long time as well. I can't believe how careless I was with the stuff.

hm, what did you do?

well, i guess i will be fine if i wear gloves and never touch it, and also don't get too close to it. yep, i'll be alright, will i?

erm... this was my first nitration, but what's so bad about that? there wasn't even a vapor of NOx, so where's the problem?

by purifying, i meant TNP. what's it good for to dissolve it in water, cool the water and filter it again?

okay, remove the H2SO4 traces, but what's that good for? i mean, if this was AP or HMTD, i would understand, because they get damn sensitive with too much acid present. but TNP?

[edit]

i've read many synths and informations about TNP, and i know what can happen when runaway occurs. the temperature rises dramatically, and more, and more, and also, lots of red NOx fumes evolve.

[This message has been edited by FMShadow (edited 07-13-2003).]

In the synth of RDX, i also think that traces of sulphuric destroy the RDX fast and this is the main if not the only reason to use PURE nitric. As for white/red nitric i am unsure as to what excatly happens but there are obviously undesired side reactions, destruction of product or formation of other chemicals for example.

As for the neutralising of TNP (which i think you were talking about) i would only assume that it too is sensitised by the presence of H+ ions (like AP and MEKP are). If you are questioning this step, but with no idea what it's for (rather than having information on it and disagreeing) then ommitting this step would be foolish.

Edit: typo

[This message has been edited by 'Peach' (edited 07-13-2003).]

mmh, i know what it's for. to remove the sulfuric acid traces, and other stuff, for example the dye, if the H2SO4 was colored before, or so.

but i disagree with that, as you said, because TNP is a secondary, and i don't think that it will get even as sensitive as MEKP, if i don't purify it.

*smacks FMShadow*

It's true that TNP is a secondary that normally isn't sensitive but you still don't want to risk it becoming more sensitive when you don't know how much more sensitive it might become and prolonged exposure to H2SO4 might decompose it. Anyway, it really is a good idea to make cellulose nitrate, and one other nitric ester before making more complicated stuff stuch as TNP. Do you happen to know what it means when something is a nitric ester? or what it means when something is a nitroaromatic? If you don't know the answers to those questions off the top of your head then you haven't any business nitrating anything.

quote:Originally posted by a123x:

Do you happen to know what it means when something is a nitric ester? or what it means when something is a nitroaromatic? If you don't know the answers to those questions off the top of your head then you haven't any business nitrating anything.

Rather than not having any business nitrating anything, he has business learning them... you people these days.

Hmm we are just looking out for his safty and well being I think you may be jelous that the regular are talking over the head of you, a123x is just telling him to friggen studie before trying to make things that could cause him massive harm, whats wrong with that?

It is better to start with nitric esters; however, I would sugest TNP before NG...NG is an easyer synth, but i think the TNP synth is safer, not to mention the nasty headaches trinitrotolulene's experiance with them led me to stray away from NG.

~H

Yeah, you're right, NG is more dangerous to make than TNP. I've only made small amounts of NG for the experience, like just a gram. I did get a mild headache though. I intend to make a larger batch(8g) with my freshly distilled white nitric acid or else I'll make cellulose hexanitrate.

David the Pyro is right though, I was a little bit harsh in what I said. We need to keep the forums friendly.

no, i've heard the words "nitric ester" and "nitroaromatic" for the first time some days ago. maybe that's because english isn't my mother language, however.

well, i guess nitroaromatic compounds are compounds like TNP, TNT, NG... that's because they are all nitrated, and have a taste. TNP tastes bitter, NG sweet, and TNT... however.

am i right?

Yes NG is said to taste very sweet, but WTF the tasting of TNP will result in your death, its almost as smart as tasting sodium cyanide...

Nitro Aromatics are the nitro derivitives of any phenyl or simpley put any benzene ring with the -no2 group.

An ester is basicaly an:

code:<pre>

R

|

C=O

|

O

|

R'

</pre> Where R and R'are hydrocabons from the acid and alcohol groups, respectivly. Nitric esters are just as the name implys. ASA is an ester in some respect so well he is nitrating as ester, but well not really...

~H

The term nitric ester and nitroaromatic are chemistry terms refering to explosives made by nitration. It's something you should learn before doing any nitrations, not because you'll risk injury by not knowing but because it will allow you to understand the reaction that occurs in a nitration.

A nitric ester is where an organic compound with one or more OH groups has it's OH groups replaced with nitrate(NO3) ions. Nitroglycerin, properly named glycerin(or glycerol) trinitrate is a nitric ester. The formula for glycerin is C3H5(OH)3, the formula for glycerin trinitrate is C3H5(NO3)3. The OH group that is replaced by the nitrate ion combines with the H+ from the acid to form water. It is inaccurate to name these nitro(whatever), correctly they should be (whatever) nitrate.

A nitroaromatic is where nitric acid puts a nitro group(NO2) onto an aromatic compound. Aromatic compounds are organic compounds containing a benzene ring in some form. Benzene has the formula C6H6 and the molecule is in the form of a ring. Toulene is a benzene ring with one H replaced with a methyl group(CH3). Naphthalene is two benzene rings connected together. Phenol is a benzene ring that has one H replaced with an OH group. In nitration of aromatics hydrogens in the aromatic compound are replaced with NO2. These are properly named with nitro.

Hmm... Now thats odd; If you talking about sugars and starches that makes sence as they are esters but ive alway thought Ng was an aliphatic explosive...

Edit: added semicolon

~H

[This message has been edited by Halifax (edited 07-14-2003).]

You seem to know more about these explosives than I do so perhaps you're right about that. I don't even know what an aliphatic explosive is. I just thought NG was a nitric ester because it involves the replacing of the OH's with NO3. Perhaps if you could explain better I'd learn something new.

For all people intending to nitrate anything I suggest you look at this page: http://www.hpwt.de/Chemie6e.htm

From the parts I have read it gives a very good description of various things to do with organic chemistry such as what a benzene ring is and even talks about explosives some. Should give anyone who reads it a decent level of understanding as to what is going on when they are nitrating organic compounds.

quote:Originally posted by FMShadow:



well, i guess nitroaromatic compounds are compounds like TNP, TNT, NG... that's because they are all nitrated, and have a taste. TNP tastes bitter, NG sweet, and TNT... however.

am i right?



Wrong aromatic...

Please say you didn't taste the TNP.

quote:Originally posted by Halifax:

[B]Hmm we are just looking out for his safty and well being I think you may be jelous that the regular are talking over the head of you, a123x is just telling him to friggen studie before trying to make things that could cause him massive harm, whats wrong with that?

Being arrogant and looking out for someones safety are two differant things. I'm know you know more about chemistry than I do. I don't really care for chemistry, it's not my thing anyway. I don't so much care what goes on when I mix chemicals, as long as I know enough to keep it from doing something wrong, I won't give it too much thought. My interest is in the results.

Fair Enought, but the way i see it the more you know the more you can create... Take smokey for example, he is the reason liquid mekp is in our hands, he basicaly discoverd it, so keep that in mind. I know its been made as a fiberglass harderen but thats a soild disolved in a liqiud. Among that he has invented several other explosives, its chemist like him , and me one day, that are the reason that you can even read about things that go boom...

~H

quote:Originally posted by Halifax:

Fair Enought, but the way i see it the more you know the more you can create... Take smokey for example, he is the reason liquid mekp is in our hands, he basicaly discoverd it, so keep that in mind. I know its been made as a fiberglass harderen but thats a soild disolved in a liqiud. Among that he has invented several other explosives, its chemist like him , and me one day, that are the reason that you can even read about things that go boom...

~H

And thats why you got me unending respect... Love those booms.... almost as good as tacos, sweet sweet tacos...

err... you're joking, are you?

smokey didn't really invent MEKP... or did he?!

No im not fucking with you, he basically discoverd it, thats is liquid mekp, mekp has been around since before we were born but he is basicaly soley responcible for bringing liqiud mekp into backyard chemistry...

~H

quote:Originally posted by a123x:

You seem to know more about these explosives than I do so perhaps you're right about that. I don't even know what an aliphatic explosive is. I just thought NG was a nitric ester because it involves the replacing of the OH's with NO3. Perhaps if you could explain better I'd learn something new.

For all people intending to nitrate anything I suggest you look at this page: http://www.hpwt.de/Chemie6e.htm

From the parts I have read it gives a very good description of various things to do with organic chemistry such as what a benzene ring is and even talks about explosives some. Should give anyone who reads it a decent level of understanding as to what is going on when they are nitrating organic compounds.

Well a nitric ester is where -oh groups are replaced by -0-NO2 groups, but it tends to describe that by the reaction of an acid and alcohol... Others 'can' be conciderd nitric esters but it is not entirely correct.

An example of a nitric ester is:

CH3-OH + HNO3 --&gt; CH3-O-NO3 +....

~H