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Author: Subject: Preparation of nitrostarch
Laboratory of Liptakov
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[*] posted on 13-6-2023 at 11:36


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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[*] posted on 13-6-2023 at 21:08


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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[*] posted on 13-6-2023 at 21:41


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 LiptakovĀ“s container.



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[*] posted on 23-8-2023 at 18:50


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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[*] posted on 11-9-2023 at 03:06


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...:cool:

https://www.youtube.com/watch?v=oVZkPWxj5WE

[Edited on 11-9-2023 by Laboratory of Liptakov]




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[*] posted on 11-9-2023 at 23:25


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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[*] posted on 13-9-2023 at 03:47


Quote: Originally posted by Laboratory of Liptakov  
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...:cool:

https://www.youtube.com/watch?v=oVZkPWxj5WE

[Edited on 11-9-2023 by Laboratory of Liptakov]


Sounds like a much easier way than combustion analysis! :D 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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[*] posted on 13-9-2023 at 22:12


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.:cool:



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[*] posted on 14-9-2023 at 00:04



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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[*] posted on 14-9-2023 at 14:22


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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[*] posted on 14-9-2023 at 21:19


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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