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MineMan
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[*] posted on 21-2-2016 at 19:16


I can only speak to number 3. If it is wet you should have no worries... even if it is dry... it should not be a big concern.
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[*] posted on 21-2-2016 at 22:40


It is safe to squeeze wet. But you will need to do more than that to ensure it is completely acid free. If it is not the product can be dangerous and will deteriorate fairly rapidly. Boiling in a carbonate solution for a while will ensure it is acid free. And as for 2 you can be fairly sure you have a good level of nitration if no carbon is left. To what nitrogen percentage exactly is difficult to tell without the right equipment. But it should be in the region of 12-13%Nitrogen for a nice fast clean burn with no residue and a nice whoomp sound.

[Edited on 22-2-2016 by NeonPulse]




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[*] posted on 22-2-2016 at 00:16


OK thanks,
Since I did not boil in NaHCO3 I guess it may deteriorate,
I'll 'test' it all tonight when I get home from work. ::D
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[*] posted on 22-2-2016 at 06:26
NC grain


And what use for neutralisation NC same process, as for ETN or PETN. Dry NC Dissolved in acetone, for example on 10% solution. And added NaHCO3 to neutral reaction on paper strip. Now written procedure for mechanical cracking nitrocellulose on grain 1x1mm. Or grain 2x2mm. Or grain 0,5 mm. You need some salt. Usually is possible used NaCl, or NH4NO3, because are cheap. On 10g NC-solution 10%, ( thus 1g NC dry) , is used 20g salt. Thus 5% mix NC in salt. Next step is drying and evaporate acetone, during process crushed. Almost dry mix is easy possible crushed through sieve 2x2, 1x1, 0,5 according fraction of using. We get defined dry grain of NC. Next step is total drying salt-NC. If is salt dry, all is pour to water. For example 100g salt to 1 liter of water. Boiled 1 minute. Or get water on 70 Celsia. Every salt remains in water. Separate grain of NC. Easy through fine sieve, for example 0,1. This process repeat again. Evaporate pure water, grain dry on hot plate by 70 Celsia. Stirring during evaporate. Important: total dry grain are very electro flying. This is my methode how to get nitrocellulose grain from nitrocellulose laquer, NC-glue or any liquid which contents NC. And you can filling to shotgun. Sieve determines the average grain size. ...:cool:...LL
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James Ikanov
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[*] posted on 22-2-2016 at 08:17


I believe that post was describing how to make grains of nitrocellulose, but honestly, it all went a bit over my head....


Well, anyway, aside from evaporation or the use of a saturated sodium chloride solution, how would one go about drying a sample of nitroglycerin?

Obviously, heating it seems like a rather poor course of action, but might mixing it with a quantity of something that evaporates rather quickly, such as 99% isopropyl, or Acetone or such, wait till it stratifies, and then separating it?

As an aside, I've read that one should expect about 2.5 units of nitroglycerin for each unit of glycerin that is used. Is this a theoretical yield, or a projected yield? I attempted such a nitration about thrice, and the third time yielded roughly 30% of what I was expecting at best.... the other two times, well, they had to be drowned, but they were quite adequate learning experiences for my purposes.

Finally, is there a combination of solvents that will dissolve nitrocellulose that does not require ether?




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[*] posted on 22-2-2016 at 09:34


I dry mine in a desiccator overnight but if you don't have one I'm sure sitting the beaker of NG in a sealed jar on a layer of moisture absorber (Damprid) would do just as well. Goes in cloudy and comes out crystal clear like the original glycerine.
Nitroglycerin dissolves in acetone which would be more handy for making dynamites once it is dried.

The yield for NG depends on the concentration of the acids (how much water is in the reaction) and the nitration time I would assume, you would probably be able to get 250% yields if the Nitric was above 90%. I usually get about 1.5 to 2 times original volume using 70% Nitric acid depending on how long it gets left before crashing into cold water.

Also, I am not aware of any mixtures of solvents that do not involve ether for dissolving NC.

[Edited on 22-2-2016 by greenlight]




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[*] posted on 23-2-2016 at 06:03
NG Theoretical Yield


Glycerol
C3H8O3
MW - 92.09382 g/mol
Density - 1.26 g/cc

Nitroglycerin
C3H5N3O9
MW - 227.09 g/mol
Density - 1.6 g/cc

Basis 1g Glycerol
Assume anhydrous glycerol

Theoretical Yield (100% conversion, no losses):

Mass
1g glycerol / 92.09382g/mol * 227.09g/mol = ca. 2.47g NG

Volume
(2.47g / 1.6g/cc) / (1g / 1.26g/cc) = ca. 1.95cc NG from 1cc glycerol




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[*] posted on 23-2-2016 at 23:18


Why would you want a more complex method for drying NG, when a simpler one would work at least as good? You could do it a number of ways, such as dissolving it in alcohol, adding anhydrous sodium sulfate or other drying agent, filtering and evaporating the alcohol. But there would be no point, since you could just use one of the ways you mentioned yourself. Personally, I use both: First saturated NaCl, then letting it stand in the open after separation; this also serves to separate a small amount of occluded NaCl from the NG. NG isn't hygroscopic so you really don't need a desiccator.

Acetone works very well for dissolving NC, and so does nitromethane.
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[*] posted on 24-2-2016 at 00:58


Quote: Originally posted by Deathunter88  
How can a chemical be above 100% pure? I have quite a few reagent bottles that state a purity upper value greater than 100%.

For example, my bottle of copper nitrate states a purity of 99-102% and my bottle of manganese dioxide states a purity of 98-101%.


Copper Nitrate is Cu(NO3)2.3H2O, MW = 241.6, Cu content = 26.3%
If during drying even if a very small part of "3H2O" gets evaporated leaving behind a small fraction of anhydrous or partially hydrated Cu(NO3)2, then the overall Cu content will go above 26.3 %.
Since 26.3 % Cu corresponds to 100 % Cu(NO3)2.3H2O, the purity of "overdried" crystals will be above 100%

Similarly in case of MnO2, which is either synthetically made or is a natural ore, contains some presene of "lower oxides of Manganese" such as MnO, Mn2O3 or Mn3O4. If they are estimated as MnO2, then you will get purity which exceeds 100%.

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[*] posted on 24-2-2016 at 14:09
nitrocellulose in blasting cap ???


HI! on youtube, i've seen some people using nitrocellulose in their blasting caps. For example, in one of these videos, the men put 200mg of lead azide and 1500mg of nitrocellulose. the lead azide is compressed but do you think it's sufficient to acieve the detonation of nitrocellulose?
sorry for my bad english :(
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[*] posted on 24-2-2016 at 15:22


I'd say it's likely enough, but depends on the grain size of the NC among other things... also depends greatly on the quality of the NC as well. Quality of the Azide would also be a big factor in whether it detonated. If either was poor quality I doubt the NC would really detonate, and if the grain size was wrong I also think that would cause a failure. It would be at best unreliable, based on your description....

I also can't imagine any real benefit over using it compared to a more reliable secondary explosive like loosely packed ETN, PETN, or Tetryl.... and if you can make NC, you can probably just as easily make ETN instead, which is more powerful anyway.

Your English is actually fairly good, by the way. Nothing to worry about. :)




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[*] posted on 24-2-2016 at 15:36


Ok thank you for the replie! yes i think it's better to use etn or another secondary. I just need to find erythritol :)
and thanks for my english ;)
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[*] posted on 24-2-2016 at 15:49


1500mg of NC in a blasting cap?
I'm also interested in the grain size and / or the size of the blasting cap.
That seems like a big volume of NC to stuff into a tiny blasting cap.
I totally agree with James Ikanov: if you can make NC, you'll be better of making ETN instead.
a) It's less costly in acid
b) I'll be a lot more efficient.

Though in my personal experiences (I should really make a post about it) "loosely" packed ETN doesnt give great results. Melting some, then adding some ETN powder on top (and finally you azide with a thin al foil separation) gives great results.
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[*] posted on 25-2-2016 at 11:31


Hey, does anybody have any tips on locations to do tests? I was planning to detonate a few grams of ETN, but am unsure of exactly how loud it will be, and how far I will need to be from other people to avoid attention.
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[*] posted on 25-2-2016 at 13:50


Quote: Originally posted by Abbott242  
Hey, does anybody have any tips on locations to do tests? I was planning to detonate a few grams of ETN, but am unsure of exactly how loud it will be, and how far I will need to be from other people to avoid attention.

Burried charge will do much less noise than open one...
Maybe if you have a large enough sand bucket...you could do it indoor for a few grams.




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[*] posted on 25-2-2016 at 14:07


Okay, thanks- I'll consider a buried charge instead.
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[*] posted on 27-2-2016 at 10:33


Hmm.

A quick browsing of wiki suggested that nitrous oxide could be reacted with oxygen to yield nitric oxides.

Given that nitrous oxide is virtually unregulated, and widely available, and oxygen easily created from electrolysis of water, I'm very curious to find out if it's plausible one could do this at any scale that would produce usable amounts of nitric oxides.




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[*] posted on 17-3-2016 at 07:34
Synthesis of dulcitoloctonitrate


Just before I try, would nitrating dulcitol in the same way as sorbitol of xylitol be able to form the octonitrate? I know that if it did, it would be potent...
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[*] posted on 17-3-2016 at 08:26


Not 8 nitrates but 6.
Dulcitol is a hexan-hexol just like sorbitol or mannitol...nitrodulcitol (dulcitol hexanitrate) power and sensitivity will be very close to those of SHN and MHN...




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[*] posted on 17-3-2016 at 18:22


I posted in the wrong place-sorry. Why does NaBH4 react with MeOH? Does it?



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[*] posted on 17-3-2016 at 18:26


It does react (forming hydrogen gas and borate esters/salts) but the reaction is slow at room temperature. This side reaction (among other reasons) means borohydride needs to be used in excess when methanol is used as the solvent.



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[*] posted on 19-3-2016 at 07:20


I have a rather stupid question in storage! ;)

'cause I need help with some comprehensibility problems I have, about the potassium dinitramide synthesis!!

The nitration part isn't clear for me. So how much of the potassium salt of the sulfamic acid do you actually use? 17g? or 17 on the beginning and the end so 34 or what???


Here are two ?opposing? quotes ?

Quote:

17g potassium sulfamate was added in small portions (0.5- 1 g ) to a mixture of 16mL 98% concentrated sulfuric acid and 45 mL fuming nitric acid, with continual stirring of the mixture. The mixture was kept between (minus) -35 and -45 degC, using an ice bath consisting of dry ice and methylene chloride. (The reaction temperature need only be below -25 degC, if care is taken to avoid overheating) The viscocity increased as the reaction proceeded, and potassium bisulfate precipitated. Dinitramidic acid is not stable under acidic conditions so the pH must subsequently be raised to avoid decomposition.


Quote:

45 ml fuming nitric acid and 16 ml sulphuric acid (95%) were mixed in a narrow, high bowl of a diameter of about 5 cm. The nitration mixture was cooled to about -30°C with a mixture of dry ice and dichloroethane. The reaction vessel (bowl) was fitted with a propeller agitator. The potassium salt of the sulfamic acid was now added in small portions of 0.5-1 g during very powerful agitation. The viscosity increased significantly as the reaction proceeded when KHSO4 precipitated. The amount of dinitramidic acid formed was checked by taking off 1 ml of the solution, diluting it to 1000 ml and examining it by means of a UV spectrometer. The acid has a maximum absorbance of 285 nm. Since the acid is not stable in acid environment, the acid content of the reaction mixture begins to decrease after a certain reaction time. By UV spectroscopy, a suitable point of time for interrupting the reaction so as to obtain an optimum yield of the acid can be determined. In this manner, 17 g of the potassium salt were added, and the reaction was interrupted after about 20 min. The reaction mixture was poured into a bath containing 150 g of crushed ice and 150 ml of water, and the neutralisation was immediately initiated.
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[*] posted on 19-3-2016 at 10:21


Quote: Originally posted by Mr.Greeenix  
I have a rather stupid question in storage! ;)

'cause I need help with some comprehensibility problems I have, about the potassium dinitramide synthesis!!

The nitration part isn't clear for me. So how much of the potassium salt of the sulfamic acid do you actually use? 17g? or 17 on the beginning and the end so 34 or what???


Here are two ?opposing? quotes ?

Quote:

17g potassium sulfamate was added in small portions (0.5- 1 g ) to a mixture of 16mL 98% concentrated sulfuric acid and 45 mL fuming nitric acid, with continual stirring of the mixture. The mixture was kept between (minus) -35 and -45 degC, using an ice bath consisting of dry ice and methylene chloride. (The reaction temperature need only be below -25 degC, if care is taken to avoid overheating) The viscocity increased as the reaction proceeded, and potassium bisulfate precipitated. Dinitramidic acid is not stable under acidic conditions so the pH must subsequently be raised to avoid decomposition.


Quote:

45 ml fuming nitric acid and 16 ml sulphuric acid (95%) were mixed in a narrow, high bowl of a diameter of about 5 cm. The nitration mixture was cooled to about -30°C with a mixture of dry ice and dichloroethane. The reaction vessel (bowl) was fitted with a propeller agitator. The potassium salt of the sulfamic acid was now added in small portions of 0.5-1 g during very powerful agitation. The viscosity increased significantly as the reaction proceeded when KHSO4 precipitated. The amount of dinitramidic acid formed was checked by taking off 1 ml of the solution, diluting it to 1000 ml and examining it by means of a UV spectrometer. The acid has a maximum absorbance of 285 nm. Since the acid is not stable in acid environment, the acid content of the reaction mixture begins to decrease after a certain reaction time. By UV spectroscopy, a suitable point of time for interrupting the reaction so as to obtain an optimum yield of the acid can be determined. In this manner, 17 g of the potassium salt were added, and the reaction was interrupted after about 20 min. The reaction mixture was poured into a bath containing 150 g of crushed ice and 150 ml of water, and the neutralisation was immediately initiated.

To me both quotes seems quite identical process except the % of H2SO4, the sligth T° difference and dichloroethane instead of dichloromethane...

So 17g is the way to go not 17g+17g= 34g!




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[*] posted on 19-3-2016 at 12:41
Making Nitrocellulose. How much cotton?


Ratio of Cellulose to HNO3 to H2SO4 while making Nitrocellulose?
ex. (3.1g Cellulose for every 10ml of 50/50 HNO3/H2SO4 acid mix.
more specifically I am using KNO3 as an acid bath, mixing 80g KNO3 for every 65ml H2SO4. Sorry if this is a bit long/confusing, but I haven't found an answer yet. Thanks.




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[*] posted on 19-3-2016 at 23:00


I made a spreadsheet in Excel a while back which is attached in the "Bullet Propellants" thread that should make life easier for you. It helps one determine quantities and strengths of acids needed for a particular percentage nitrogen NC. Often times acids of lower concentration can be used, for a particular %N, by adjusting the quantities used, but sometimes not. Keep in mind, the spreadsheet does not account for acid, cellulose or NC losses due to oxidation, acid losses due to evaporation, acid dilution due to absorption of water, etc, etc. Proper technique is still required!

http://www.sciencemadness.org/talk/viewthread.php?tid=22649&...

Attachment: Cellulose Nitration Diagram & Spreadsheet.xlsx (129kB)
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Attachment: Cellulose Nitration Diagram & Spreadsheet (compatibility mode).xls (143kB)
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