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Laboratory of Liptakov
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It's just a suggestion of a reaction to neutralize nitro starch. The method is not tested for nitro starch. The basis of everything is that the nitro
starch is completely dissolved in acetone. Afterwards, nitro starch can be acted upon by various basic substances. For example, NaHCO3. And even
without the water content in the solution. The basic preparation is on the wiki: https://en.wikipedia.org/wiki/Nitrostarch
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ManyInterests
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They did mention ethanol and acetone in that article. This is where I got the idea of refluxing it in ethanol, but the bumping I got when trying to
boil it in carbonate solution made me not want to do that.
BTW, on a slightly off-topic note. I spent the last 24 hours making a lot of ammonia. I ended up with 1000ml of 24% ammonia solution! Is this
concentration sufficient to make CHP and other stuff you make that calls for ammonia?
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Laboratory of Liptakov
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Yes, 24 % is ideal concentration for any purpose with relatively low evaporation at 20 C (or lab. temp.) And of course ideal for preparation TACP in
rolling Liptakov´s container.
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ManyInterests
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I'm bumping up this thread again for one more question:
How does one determine the nitrogen content of the nitrostarch? I am away that lower-nitrogen nitrostarch has a weak detonation velocity (only around
1000 m/s) while high nitrogen content (around 14%) is around 6200 m/s, which is close to TNT.
What needs to be done in order to make sure you have higher nitrogen nitrostarch? More nitric acid and higher concentration nitric acid to sulfuric
acid?
Is there any uses for nitrostarch in a lower nitrogen content than a higher one? For example I did read that nitrostarch is used as a binder for some
liquid explosives, such as methyl nitrate, would lower nitrogen content nitrostarch be better for that or not?
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Laboratory of Liptakov
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Because nitrostarch is insoluble in water, but soluble in ethanol and acetone, is possible after nitration (with unknown %N) use the methode PLM.
Starch stay in solution, but all others with high % of N will be precipitated...
https://www.youtube.com/watch?v=oVZkPWxj5WE
[Edited on 11-9-2023 by Laboratory of Liptakov]
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Microtek
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You could also do a classical combustion analysis:
A sample of precisely known mass is mixed with CuO in excess and taken to red heat. This converts the sample into CO2, NOx, N2 and H2O (and possibly
O2). A known volume of nitrogen gas (or dry air) from a syringe is used as a carrier to lead the combustion products through heated copper gauze (to
reduce NOx and O2), alkaline solution to absorb the CO2 and a strong drying agent to absorb the water. All that remains is nitrogen and this gas is
lead into an inverted measuring cylinder filled with water to measure the volume of dinitrogen. Now you can calculate the nitrogen content of the
sample (but you have to do a control run without sample to find out the displacement from the carrier gas).
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ManyInterests
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Sounds like a much easier way than combustion analysis!  Also afterward, I can
let the ethanol and acetone solution evaporate and I can still keep the lower N% stuff. Will this work as a recrystalization, too?
For the ethanol, I assume it is best to use 95% ethanol, correct? Absolute if possible.
edit: Also this is exactly what I need to make gun cotton into double base smokeless powder... I need it in fine powder form and I always wondered how
it is done.
[Edited on 13-9-2023 by ManyInterests]
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Laboratory of Liptakov
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Each precipitation requires multiple tests of its own. The PLM method may not always work perfectly and exactly according to the instructions. The
basis is a test of 1g (dry weight) of nitro substance + different ratios of acetone and alcohol. (before adding H2O) During the process, it is
possible to carry out neutralization at the molecular level with NaHCO3. Even before precipitation. It's all about playing with liquids. Is possible
use any ethanol and any acetone.
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Microtek
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| Quote: |
Sounds like a much easier way than combustion analysis! |
Certainly. But the accuracy of your analysis will be lower. It all depends on what you are trying to achieve...
Solubility of nitrocellulose (and probably nitrostarch as well) is not a simple linear function of the degree of nitration. Very highly nitrated NC
has a lower solubility in acetone than NC with a somewhat lower N%. There could also be assorted types of entrainment issues to contend with.
[Edited on 14-9-2023 by Microtek]
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ManyInterests
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What I am trying to achieve, ultimately, is to make sure that the nitrocellulose and nitrostarch that I make is of sufficiently high nitrogen content.
I'm sure that in one of Urbanski's books they have some information on making high vs. low nitrogen NC.
I assume that making smokeless double base gunpowder will require high nitrogen NC (can nitrostarch be used for that as well?). I'm specifically
looking to make powders that are appropriate to use with pistols, such as 9mm rounds.
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DennyDevHE77
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The ability of nitrostarch to form solid colloidal solutions with nitroesters is much less than that of NC. Therefore, nitrostarch in its independent
form is not suitable for the production of smokeless powder, only as an additive to nitrocellulose.
In general, all nitrocellulose is divided into colloxylin (10.7 - 12.2% N), pyroxylin No. 2 (12.2 - 12.5% N), pyroxylin No. 1 (13.0 -
13.5% N). And colloxylin is excellent for gunpowder, it is more easily plasticized with nitroesters, and it generally contains a fairly large number
of compounds.
And yes, in the fourth volume of Urbanski (pages 577-599) it is briefly written about gunpowder
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