nitrostarch

[Trinitrotoluene]

A week ago I had made nitrostarch. In a 150ml beaker I mixed 30ml of 93% H2SO4 and 20ml of yellow HNO3. Then let the mixture cool to 10*C. After that I slowly added 15 grams of corn starch and carefully monitering the temperature not letting rise above 15*C. After I was done adding the starch I let it nitrate for 1 hour at 10*C. Then dumped the soloution into 150ml of cold water the temperature rised u to 30*C but had no problems my nitrostarch percipitated. Over the rest of the day I waited for the nitrostarch to setting to the bottom and decented the acetic water above. I did that a few times aut it took me a day. Then I filtered it, added some sodium bicarbonate and NaOH to neutralized. I didin't feel my nitrostarch was neutralized enough so I added it to a soloution of urea. Then filtered and left out to dry. It is a long process. As its left out to dry in the air. Now its not 100% dry yet but perhaps like 95% dry and it weights 24 grams. As for now I will wait for it to dry then burn some of it. Most of it I will wait till the 4th of July to detonate it the background noise will cover me, hope its storage stable.Can't currently detonate anything in my backyard now neighbors will call the pigs.And in my town pigs are everywhere,too bad I live in a heavyly populated town. But who else had made nitrostarch?

<small>[ January 28, 2003, 01:08 AM: Message edited by: Trinitrotoluene ]</small>

[mongo blongo]

Made it! and in a word- CRAP!!. I suppose it's ok to mess around with a bit though. I mean it's crap compared with other HEs. It's a primary so you can mess about with it in very small amounts so that makes it a "fun" explosive for me. Is you wash it with very hot water you will be able to wash out the un-nitrated starch.
EDIT: I find it very similar to Nitrocellulose

<small>[ January 28, 2003, 10:45 PM: Message edited by: mongo blongo ]</small>

[aster]

why wait until 4 july,... :) i am usualy drive away from the town, in the night, :D and set off the bomb far from people or crowd populated area, i think nitrostarch won't explode by burn, they need primary to set off, am i right? <img border="0" title="" alt="[Wink]" src="wink.gif" />

[mongo blongo]

I don't think it will detonate without another primary but it does deflagrate.

[Trinitrotoluene]

Yes I am planning to take 1 gram and light it. And all the rest I will detonate it with 5 grams of HMTD.

[Resaca]

is there e method for making nitrostarch using 70% nitric acid.....all the methods i´ve found use concentrated nitric acid (95-98%)....except the one that use sulphuric acid and sodium nitrate.....
i´ve done nitrocellulose whith this concentration succesfully, but before doing nitrostarch i wanna be sure!....
thanks

[Boomer]

Nitrostarch used to be my favourite HE for making so called nitrostarch dynamite. It is 65% AN + 35% NS. The power + brisance are comparable to donarit (65% AN + 35% TNT, also at density 1.1) or a 30-40% straight dynamite, and it cannot be dead pressed like many other AN compositions. VoD is around 4500 m/s. Adding a few percent whole grain flour (no pure starch, the amines are needed!) makes it storage stable – I just found a pound jar from 1992 and it still works, though it starts to stink and must be used ASAP.

The AN must be dried in the oven at 80C and ground to flour-like meal in a coffee grinder or mixer for fruit shakes, and the NS can be processed in the mixer two, but as a slurry in water/bicarb before filtering and drying it. This makes it easier to get all acid out from between the particles. It can be detonated with a medium cap, I used 1g MHN + 25mg silver fulminate from ‘fun snaps’ (paper balls with gravel in them – extracted of course).

The main advantage is you need no HNO3, my method was 100ml SA (96%) + 90g AN mixed, starch added while still hand warm. Temp was held at 40-50C with hot water. At 65C it starts a runaway, but a harmless one (only fumes). After 30 minutes all was poured into a lot of water (a bucket), left to settle and decanted. Then re-washed, bicarb washed ….just as you described. If you use the mixer and then wash it warm with bicarb for an hour, the urea isn’t necessary.

Concerning the power: 10g in an OTC firecracker shell (makes it look legal if you use the original fuse for the cap) blow a hole into the sidewalk concrete plates. And a 100g stick splits a 15” x 6’ oak; I used it a lot for stumping and cutting timber (drilled holes 11/4“). Biggest charge used was 400g for a 4 foot diameter tree, but there I had to drill two more holes (300g) before it was completely split. The bastard was 14 foot long, weighing 4 tons!

[Bert]

25mg silver fulminate from ‘fun snaps’ (paper balls with gravel in them – extracted of course). Interesting- What's your extraction method? Ever had an accident handling after extraction? How do you load the det, pressed, loose...

[Boomer]

Man, that was a fast answer! There is mentioned somewhere in another threat the use of ammonia IIRC, but the easiest way is to open a few packs of these snaps into a glass of water, so the accumulated stuff does not explode – this happened once at the 50th from 50 snaps…HI Murphy. Then you stir it fast and decant it after a second when the gravel has settled but the fine fulminate is still suspended. If you do this three times you will see that nearly all stuff is ‘extracted’ (I know it is no real extraction using solvents). Then you let it settle, it takes a day, decant off the water (maybe re-use it, I do not know if it dissolves a little product) and scrape the grey crystals out while still wet. Mix wet with an equal amount of fine MHN (or PETN) and let dry. The MHN tends to ‘smear’ the fulminate crystals, and as you do not press them, they are not hazard (two packs give much lees than a gram anyway). The way to go is press a cap half full with MHN at high pressure, press it full at lower pressure, and press a 2mm hole into the upper centre. Into this hole go 25 mg of the primary mix, and the bridge wire or fuse. Then comes a layer of tissue and some epoxy. They store some month.

The right mix of fulminate / MHN can be found this way: add MHN and light in small piles (1x1mm) with a lighter. If it stops detonating, you have to add a little more fulminate. You could also omit this step, but it seems to make it safer, and you get at least twice the number of caps, as the intimate mix with a stronger HE increases the priming power per given amount of fulminate.

[Sahag]

I think the best way to detonate nitrostarch is using a primary explosive
also you can mix it with nitroglycerin to increase its sensitivity

[Bert]

I thought newbie posts were now moderated?

Sahag, go back and re-read the Forum FAQ (http://www.roguesci.org/theforum/misc.php?s=&action=faq), then go read Banned For Life! (http://www.roguesci.org/theforum/forumdisplay.php?s=&forumid=16&pagenumber=1&sortfield=lastpost&sortorder=desc&daysprune=1000&x=12&y=12).

[Resaca]

lood what i found on my computer....it´s a method for making nitrostarch, i don´t remember where i got it from, but uses 68% nitric acid (the one i have):

A solution of 65mL Sulphuric Acid (98%) and 35mL Nitric Acid (68%) are mixed in a 150mL beaker and allowed to cool (the dehydration of the nitric acid produces enough heat to warm the solution by as much as 60C, so it is very important to start off with the acids at no more than room temperature, and to cool the mixture down to 10C or so prior to the addition of starch.
Starch is than added slowly whilst the mixture is stirred vigorously until all of the 18cc have dissolved. During the addition the temperature rises and it is important that it does not go above 35C. Once all of the starch has dissolved the mixture is placed on a hot plate and heated to 40C for one and a half hours, with occasional stirring. It forms into a white precipitate with a consistency similar to honey.
Once the heating period is complete the nitro starch and acids mixture are added to 400mL of cold distilled water and stirred. Once stirring stops the nitro starch can be seen precipitating in the bottom of the beaker. As with nitrocellulose, the nitrated version of starch looks no different from what was started out with. Filtering this acid solution presents a special problem, however: It will weaken the filter paper and cause it to rip. Attempting to neutralize it with a carbonate will require very large amounts of it and cause everything to foam out of the beaker. Neutralizing it with ammonium hydroxide causes it to boil over and decomposes the nitrate. My solution was to use a micropore nylon filter which was not attacked by the acid, and filter the solution through it, with considerable loss of the final product. Decantation might prove worthwhile if one is willing to wait the long time required for all of the nitro starch to precipitate at the bottom.
The final product of any nitration will always contain some residual acid and oxides of nitrogen which can make it extremely unstable and prone to self decomposition when stored over time. It is thus necessary to neutralize this acidity. The industrial method calls for washing with Ammonium Hydroxide solution, however I found that my nitro starch decomposed when treated that way. I decided to boil it in sodium bicarbonate solution instead, and add some Urea to the final product so as to take up any nitrogen oxides produced (this is essentially what is done to nitrocellulose).
Here you see the final product, after 5 failed attempts. It consists in a fine powder that is mostly white but due to some decomposition during the acid neutralization phase (it seems as though nitro starch is highly temperature sensitive) acquired a brownish tint. It dissolves in acetone much in the same way nitrocellulose does.
------
what do you think?....is the final product as reliable as the one on megalomania´s?

[Hang-Man]

ya, what the hell? I lost 10 IQ points when I read that post. I'm adding this guy to the long list of people I owe a kick in the balls to.

[Mr Cool]

Well, he may not be Captain Clever, but at least what he said was true...
But Sahag, don't state the obvious again.

[K9]

Sorry for digging up an old thread, but I figured it's better than making a new one. I had made nitrostarch before and didn't quite like it, but I decided that I'd try it again. I'm using H2SO4/nitrate salt and I can't quite seem to figure out the optimal amount of starch to use. When making nitrocellulose with 60 ml H2SO4 and a nitrate, I can only usually fit about 4 grams of cotton into the nitrating mix. The last time I made nitrostarch I used 60 ml H2SO4, 40 grams NH4NO3, and 5 grams of starch. I've seen a few different syntheses where people use quite varying amounts of starch, and I don't really know what the best amount would be to use. Any help? Thanks in advance.

[The_Duke]

K9,
There are several factors one must take into account when nitrating starch, the main factors to be considered are; the type of starch used, the moisture present in the starch, and the concentration of the acids or the total available nitrogen content of the nitrate salt used for the reaction.

Ammonium nitrate has an available nitrogen content of around 34%, so you simply make a few small calculations to figure out the amount of starch you can nitrate with one mol of NH4NO3.Then you can toy with the amounts you use to create larger yeilds.

It is always good to use a slight excess of HNO3 or Xnitrate to avoid half nitrated starch.

[Boomer]

"So using Ammonium nitrate is like using 34%HNO3"

Trying to teach chemistry without having a clue yourself? :rolleyes:

One mol AN (80g) equals one mol of NA (63g). Starting with one glucose-rest in the starch (-C6H10O5- = 157 g/mol), you need 3 nitrate groups to form the trinitrate, which is 189g nitric or 240g AN. You also need 3 mol sulphuric to convert the AN, which is 3x98g = 294g. You need more SA to bind the reaction water, for high N content of the product there should not be more than 15% water in the final mix. This equals about one H2O to one H2SO4. With 3 mol water being generated above, this means 294g more SA. Summed up:

157g starch
588g SA (320ml)
240g AN

Because the SA will not be 100%, you should add a bit more, say 660g / 360ml.
This result is close to what was suggested here by several people, 2g AN for 3ml SA.
You need excess nitric in the mix because it is an equilibrium reaction, there must be at least as much nitric as water in the spent mix. Using 30-40% more nitric (or less starch) is OK. You will scale it down to 24g AN, 26ml SA and 10g starch.

Whatever you nitrate, calculate the moles nitric (which are equal to the moles water produced), use 1/3 excess and add one mol sulphuric for each mole water to bind it. Exceptions are PETN, MHN etc through the white nitric method, but most other things work well this way.

[K9]

Thank you very much for that. But isn't the molar mass for starch 162? Either way, when I was originally trying to calculate it I was coming up with numbers near those ratios and thought I had screwed something up because it seemed like too much starch (based on what I saw other people using). Just one more thing, I missed how you went from the original numbers to the scaled down ones? Would you mind showing? Thank you again.

[Boomer]

You are right of course. (I made this an extra post because it is so funy: the corrector stands corected!) At least the formula was right - it gives 162 g/mol.

We both know that the real mass is somewhere around 20000. But taking the smallest block is easier to calculate. And the10g per 24g/36ml will not change much anyway.

I took the 240g AN and 660g/360ml SA (slightly more as it is only 95%, see the sentence below the first amounts) and divided by ten. Taking off 1/3 of 16g starch gives 12g, but with a little water in both AN and starch I rounded downwards. BTW this is not too much starch: from 125ml of distilled NA I get 108ml NG, 92% of theory. That is 25% more nitric that theoretically needed BTW, distilled nitric allowes lower excess. The 15% water and 15% NA in the waste acid are still valid here, though in industry they go down to 17% water and 12% NA, but they use both acids fuming.

[K9]

Ah ok thank you, now it's clear. I just got confused because in your original post you wrote "24g AN, 26ml SA and 10g starch". I figured my calculations couldn't have been that far off and that people must just have been using less starch than they could have. Well now that's all cleared up :)