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otonel
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[*] posted on 4-9-2011 at 04:54
extract nitrocelulose from ping pong balls


"Ping-pong balls are made of nitrocellulose [pyroxylin] (cellulose dinitrate), specifically celluloid that consists of roughly 75% cellulose dinitrate and 25% camphor"
When I read this I thinking if I can make a rocket motor using nitrocellulose from ping pong balls
The problem in to find a solvent for camphor but not to disolve nitrocellulose
I try alcohol and acetone to separate nc. without any result
If you can help me with some suggestion I will be grateful
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[*] posted on 4-9-2011 at 06:45


I don't think the cellulose dinitrate will work well for what you have in mind. Just make some hexanitrate. It is probably the easiest nitration ever. It can be done with KNO<sub>3</sub> and H<sub>2</sub>SO<sub>4</sub> drain opener. Just allow for complete nitration by letting it nitrate for 12 hours and agitate often. Then wash, neutralize, dry, and then repeat the nitration again. Make sure the finished product is free of all acid and very dry. Then either press, or dissolve in acetone for casting.



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[*] posted on 4-9-2011 at 08:00


I understood what you say and you have right but I`m afraid about hexanitrate to be more powerful and to explosive for my purpose
May be if I mix some cellulose hexanitrate with some ping pong balls to stabilize burning speed
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[*] posted on 4-9-2011 at 08:34


Its hard to detonate cellulose hexanitrate. Good to keep safety in the front of your mind though.



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[*] posted on 4-9-2011 at 10:33


Ok but I want to try to extract nitrocellulose from ping pong balls and what I need is some advice about what solvent to use
Tomorrow I will try to use acetic acid like a solvent for camphor and I hope to have a good result
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[*] posted on 4-9-2011 at 19:13


If you dissolve the cellulose hexanitrate in acetone it should be safe and burn instead of explode. I'd add stabilizer to it in case I didn't use it right away.

As far as the ping pong balls go, I've worked with them some. I've had reasonable results in this area without worrying about removing the the camphor, but I've also at least added 10% KNO3 to it. The camphor works as a stabilizer so some of it is desirable, but 25% is more than is needed for that. A mix of ping pong ball, KNO3, NH4NO3 & ammonium dichromate is better as far as power, is cheaper, etc.

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[*] posted on 5-9-2011 at 04:46


Quote: Originally posted by bearcreek  
A mix of ping pong ball, KNO3, NH4NO3 & ammonium dichromate is better as far as power, is cheaper, etc.


You have luck with this mix in rocket propulsion? In what ratios? That is very interesting to me. I do a lot of small rockets and I am really into trying different propulsion compositions in my small scale design. I have had good luck using cellulose haxanitrate as a monopropellant but have never adulterated it. As far as detonation risk, I have never had trouble in my rockets, and I imagine as long as the scale is not ridiculous it is a pretty safe fuel.
I have achieved detonation of cellulose nitrate before, but I had to employ a fair sized TNP booster. Albeit, I am sure my density was not optimal.

Good luck friend, and be safe.:)

P.S. I camp at bearcreek every summer. In the cohutta wilderness preserve.




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[*] posted on 5-9-2011 at 07:29


I make a mix with acetone, alcohol and dissolve some balls piece , when that was dissolved I add some acetic acid and wait to obtain o separation

Bot0nist you have right, is hard and expensive to obtain nitrocellulose in this way, can you send me exact recipe for making cellulose hexanitrate with details about your monopropellant and rocket dimensions

bearcreek please post exact recipe for your mix
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[*] posted on 5-9-2011 at 10:45


Even though the cellulose nitrate synthesis is a relatively safe nitration it is not without its dangers. The biggest of which is the inhalation of the evolved oxides of nitrogen. Do you have access to concentrated sulfuric acid? Even SA drain cleaner will work for this simple nitration. Let me know and I'll u2u you a quick workup. In the mean time please read up on nitrations and their dangers.



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[*] posted on 5-9-2011 at 11:46


Bot0nist I read and know nitration process and his danger, I have some concentrated H2SO4 making by boiling H2SO4 used for batteries filling
I nitrated cotton along time ago and make some nitrocellulose for fun so I know some chemistry and safety rules
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[*] posted on 5-9-2011 at 13:32
Simple synthesis of cellulose hexanitrate.


I am sure you could have found this by searching a bit, but I'm feeling generous. This is a fun synth that I loved to do when just starting out in the hobby.

*Safety*
This synthesis uses concentrated acid which can cause severe burns and blindness. It also produces some fumes. Mainly NO2 and some H2SO4 mist. These fumes will really hurt you and can kill you. Do not run this reaction indoors unless it is in a fume-hood, and make sure it's a windy day or use a fan for ventilation outside.


What you'll need:

Equipment:
1.) glass beaker at least 250ml
2.) glass stir rod
3.) non-open flame heat source
4.) Large glass bowl or beaker at least 500ml

Chemicals:
1.) 55ml 98% sulfuric acid
2.) 32grams of KNO<sub>3</sub>, NaNO<sub>3</sub>, or NH<sub>4</sub>NO<sub>3</sub>
3.) about 50grams of sodium bicarbonate
4.) 5grams of cotton balls (100% pure cotton)
5.) a couple liters of fresh (preferably distilled) water and some ice.

Procedure:

1.) Prepare your materials;

Sulfuric acid
- Assure that your H<sub>2</sub>SO<sub>4</sub> is concentrated as much as it can be by heating it to >110C or until white fumes are emitted. Allow the sulfuric acid to cool to room temperature before proceeding

Nitrate salt
- Ammonium nitrate is the best nitrate salt to use because of its higher solubility, but the others (KNO<sub>3</sub>, NaNO<sub>3</sub>;) will work fine. Make sure the nitrate salt of choice is dry and thoroughly sifted of all clumps. Weigh it accurately to 32 grams.

Cotton balls
- Take 5 grams of cotton balls (about 5 balls) and carefully unroll them into long thin sheets of cotton. Try and separate any clumps or knots in the fibers.

Bicarb wash
- Make a saturated solution of sodium bicarbonate (baking soda). At least 500ml or more.

2.) Preparation of the nitrating bath;

Begin adding you nitrate salt to the 55ml of room temperature sulfuric acid. Add the nitrate salt in 5grams increments and insure that it is fully dissolved after each addition by stirring with the glass stir rod. If you are using KNO<sub>3</sub> you will have some trouble getting the last few additions of the salt to dissolve. This can be solved by gently heating the acid to about 75-80C by placing the beaker with the acid in it into a boiling water bath during the additions of the KNO<sub>3</sub>. After all the nitrate salt has been dissolved allow the acid/nitrate mix to cool to room temperature.

3.) Nitration of the cotton.

Add your cotton sheets, one at a time to the acid/nitrate salt mix. Using the stir rod, make sure that each piece gets thoroughly saturated and submerged in the nitration bath. Once all of the cotton is added, let the mix nitrate for no less than 12 hours. Using your glass stir rod, mix up and turn the cotton in the acid about every 2 hours.

4.) Rinsing and neutralization.

After 12 hours use you glass stir rod to press any acid out of the cotton and pour off the excess acid. You should now have a clump of acid soaked cellulose nitrate in your beaker. Add ~200ml of ice water to the beaker and swirl around. Then carefully pour off the water and leave the cotton behind. Repeat this rinse several time using cold water. The goal is to get as much of the acid off of the cotton as possible, so stir and press it with the stir rod while it's under the cold water. After several water rinses, place the nitrated cotton into the baking soda solution (Sodium Bicarbonate). It will bubble as any remaining acid is neutralized. Stir and separate the cotton in the baking soda water for several hours to assure all the acid is neutralized. Now drain the bicarbonate solution and thoroughly wash the cotton in hot water to remove any excess sodium bicarbonate. Spread out your cotton in a cool, dry place and let it dry thoroughly. It may take several days to really dry.

This cellulose nitrate will burn very fast, but if you want to assure that you have cellulose in its highest nitration state (hexanitrate) Just take the dry and ready cellulose nitrate and repeat the nitration procedure on it again with a fresh nitrating bath, as if it were just cotton. This will produce the best cellulose nitrate, it will rival the cellulose hexanitrate made with HNO<sub>3</sub> and H<sub>2</sub>SO<sub>4</sub>, albeit it's a lot slower and more work .

To make a gel, just drip some dry acetone onto the cellulose nitrate. Just enough to make a thick, clear gel. This can be pour casted into a rocket engine and allowed to dry for several days to a week. It can then be cored and fused if needed, depending on your rocket design

Good luck, and please be safe.:D


[Edited on 5-9-2011 by Bot0nist]




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[*] posted on 5-9-2011 at 15:50


Quote: Originally posted by Bot0nist  

2.) 32grams of KNO<sub>3</sub>, NaNO<sub>3</sub>, or NH<sub>4</sub>NO<sub>3</sub>


Wouldn't the amount of nitrate required depend on which nitrate was used? (i.e. KNO3 = 101g/mol, NH4NO3 = 80g/mol, NaNO3 = 85g/mol, etc.). Which nitrate is the 32 grams based on?

Very nice writeup, though!

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[*] posted on 5-9-2011 at 17:26


Yes, I suppose they would differ. I have always used NH<sub>4</sub>NO<sub>3</sub> because it makes a less viscous nitrating bath. This allows for proper agitation and stirring, which I think is really needed to get a thorough nitration when not using strong mixed acids. Of course, one could just distill some RFNA with the nitrate salt and H<sub>2</sub>SO<sub>4</sub> and get the same results in a few minutes, but I used this method a lot before I had the glassware or the confidence to distill HNO<sub>3</sub>. Also, letting the nitration happen at room temp or slightly above seems to be beneficial, both for the viscosity and solubility of the salt/acid mix, and a faster reaction. I imagine a runaway nitration is possible, but in the 5-10gram scale I often add the cotton slowly, and once it is all added I heat the mix gently to around 60-80C in a water bath for the duration.

The 32 grams is based on my trial and error when using ammonium nitrate as my nitrate salt.




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[*] posted on 6-9-2011 at 11:23


I've not had the properly designed glassware to test this however I would be interested in esterfications within a vacuum to possibly minimize "run-a-way" phenomenon. Does anyone have information on procedures of nitric ester synthesis within a vacuum?
A great deal of older information made a mantra of the "time, temp, addition speed" modality of keeping "run-a-ways" in check. To my understanding oxidation phenomenon is controllable beyond the above.

[Edited on 6-9-2011 by quicksilver]
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[*] posted on 6-9-2011 at 11:37


Be careful about generalizations with regards to nitrations because nitrations are specific to the thing being nitrated, as regards which nitrate is "best" or if any nitrate is best at all, as they are simply not interchangeable at will. There are specific combinations of acids, water content, temperature that definitely are governed by a kind of process curve and certain combinations are optimized while others simply are not optimized with regards to yield, safety, purity of product ect.
This is nitration process algebra....for sure not simple arithmetic. Actually the physical chemistry aspect is operative for most or many chemical processes, and nitrations are especially affected in ways where subtle changes can have substantial effect on how a nitration proceeds.

Microcrystalline cellulose is probably the substrate of most interest for nitration experiments. It has a less variable composition as a precursor and a more predictable response to the nitration which should lead to a more consistent product.

[Edited on 6-9-2011 by Rosco Bodine]
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[*] posted on 6-9-2011 at 14:30


This was a simple and quick write up using things you could get at WalMart in one trip, and is the way I often made guncotton by the handful years ago. I know this little writeup seems very recipe-ish but that is what was asked for. I am in no way advocating the use of a generalized ratio or recipe for any nitration. It was a bit of laziness on my part to include potassium and sodium nitrate in the same proportion as ammonium nitrate. I always use ammonium nitrate in this particular "improvised" nitration because it simply works better. Also, I know using such a crude substrate is not optimal, but again this was a fast and dirty run. In any case, the second nitration is a bit overkill and thus gives me a very consistent end product that preforms as expected.



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[*] posted on 6-9-2011 at 15:18


There is nothing wrong with using an ammonium nitrate sulfuric acid mix, it is just important to know that temperatures and nitrating mixture quantity and nitration times will likely change for alternate mixtures used to nitrate the same material. Rough stoichiometric equivalents are only a starting point for finding what works best and it may but more likely may not translate/convert directly when you use a different mix. Just making note that a direct stoichiometric conversion is not necessarily equivalent in nitrating effect and other process parameters. Nitrocellulose from cotton is going to have its preferred mixture and process and so is it likely true for other similar nitrations. There is often a surprising amount of difference in how well it goes for NaNO3, KNO3, NH4NO3 and there are probably others, even mixtures of salts that may work best. I haven't compared the nitrates with regards to nitrocellulose nitrations, but it holds true that way for nitrations of other materials, that one particular mix will work best, and it doesn't necessarily go by a simple ratio to substitute and adjust for another mix. The few times I have done a cellulose nitration was with mixed acids. I was thinking of the mixing difficulty for fibrous cotton versus a granular material, which caused my mention of microcrystalline cellulose as being a better substrate. Cotton is not easy to mix smoothly even with mixed acids.
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[*] posted on 7-9-2011 at 04:06


Quote: Originally posted by Rosco Bodine  
The few times I have done a cellulose nitration was with mixed acids. I was thinking of the mixing difficulty for fibrous cotton versus a granular material, which caused my mention of microcrystalline cellulose as being a better substrate. Cotton is not easy to mix smoothly even with mixed acids.


I have tried nitrating the cellulose powder that is sold as a dietary supplement, which is billed as pure cellulose. The one I tried was manufactured by Allergy Research Group:

http://www.acuatlanta.net/allergy-research-group-cellulose-2...

Which is said to be derived from pine trees. But using the same mixed acids, the results were inferior than when using plain cotton. The powder burns slower (though it does not leave much residue.) I think they do something to the cellulose, depolymerizing or some other chemical treatment, that prevents it from nitrating as well as cotton.

The nitrated cellulose powder seems very stable after being well washed. I kept a sample of it in an open porcelain dish for months, and it did not emit any acid smells or seem to lose its burning speed.

If you mix this nitrated cellulose powder (well washed to remove all acidity) with chlorates of barium or strontium, it burns faster and with a nice green or reddish-purple flame (though still slower than cotton nitrated the same way and treated with barium or strontium perchlorate solutions.) Strongly sealed in pyro tubes and provided with a fuse, these mixtures explode, but it's difficult to discern if the flash from the explosion is colored (so far I have only tested the one mixed with barium chlorate.) I suppose they would be detonated by a cap as well. Haven't been able to try it.
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[*] posted on 7-9-2011 at 04:43


That's not microcrystalline cellulose, that's wood powder, bleached sawdust. Avicel is a commercial product name for microcrystalline cellulose. The person
who patented the nitrated form, ordenblitz, is a member of this forum. You can look up the patent and see right that there "invented by ordenblitz" ;)

http://www.sciencemadness.org/talk/viewthread.php?tid=1007&a...

Just kidding, the nitration of microcellulose has been done and reported earlier, but ordenblitz did apply for patent on several compositions using the material to advantage.

What is the hexanitrate of cellulose I never have learned about, and that is probably wrong. The trinitrate is the fully nitrated form of cellulose.

3HNO3+ C6H10O5 → C6H7(NO2)3O5 + 3H2O


[Edited on 7-9-2011 by Rosco Bodine]
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[*] posted on 7-9-2011 at 05:41


Quote: Originally posted by Rosco Bodine  
That's not microcrystalline cellulose, that's wood powder, bleached sawdust. Avicel is a commercial product name for microcrystalline cellulose. The person
who patented the nitrated form, ordenblitz, is a member of this forum. You can look up the patent and see right that there "invented by ordenblitz" ;)

http://www.sciencemadness.org/talk/viewthread.php?tid=1007&a...


I have seen the word "depolymerized" associated with microcrystalline cellulose. Example:

http://www.fao.org/docrep/W6355E/w6355e0l.htm

I notice that ordenblitz also mentions the slower speed of this nitrated microcrystalline cellulose powder:

Quote:
All that being said, I don’t envision everyone falling in love with MCNC, especially this crowd. Anyone who has played with gun cotton is usually enamored by a small quantity burning with a pleasing thump when touched off with a flame. Compared to fibrous NC cotton, MCNC will burn much slower than a similar quantity of NC cotton. For use as a loose propellant, such as how gun cotton is employed in toy and novelty items, MCNC would be useless. However, if one wants to mix NC with other powders or liquids or if one aims to compress it or machine it… MCNC is a dream!


I also noticed the same in that cellulose powder (which leaves very little residue, so it seems to be considerably pure cellulose) I nitrated.

Ordenblitz does not appear to be interested in making nitro-cellulose derived from such cellulose powders detonate (at least not in his posts in that thread) so we are still without an answer as to how well they perform for such purposes. If you know of someone who has tried it (or if ordenblitz changed his mind since then and actually tried it), let me know. If they work well, it certainly would save one the trouble of having to come up with an improvised way of reducing the nitrated cotton to powder. The old literature on the subject speaks of "pulping" the nitrated cotton in specialized machinery, which is not available to the average Joe.

[Edited on 7-9-2011 by Blasty]
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[*] posted on 7-9-2011 at 06:14


If you want to make the material detonate, at particulate sizes of 100 mesh and moreso if mixed with a gritty oxidizer in small amount and compressed, it will initiate and detonate from shock, but there are better materials for such uses. If you are looking for a DDT sort of transition from ignition only then you are going to need an inconveniently large quantity of nitrocellulose and a lot of confinement to get it going high order, and something else that has a higher self acceleration would be way better for such use. The best nitrocellulose you can make really isn't like flashpowder, but has a progressive burning characteristic as its nature. You have to subject it to a pretty intense initiatory impulse to make it high order detonate. I really don't understand why anyone would want to make it detonate, when there are better alternative materials for that purpose. If novelty demonstration "flash paper" is the purpose, nitrating a paper towel or filter paper will give you what you want.

[Edited on 7-9-2011 by Rosco Bodine]
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[*] posted on 7-9-2011 at 07:20


Quote: Originally posted by Rosco Bodine  
If you want to make the material detonate, at particulate sizes of 100 mesh and moreso if mixed with a gritty oxidizer in small amount and compressed, it will initiate and detonate from shock, but there are better materials for such uses. If you are looking for a DDT sort of transition from ignition only then you are going to need an inconveniently large quantity of nitrocellulose and a lot of confinement to get it going high order, and something else that has a higher self acceleration would be way better for such use. The best nitrocellulose you can make really isn't like flashpowder, but has a progressive burning characteristic as its nature. You have to subject it to a pretty intense initiatory impulse to make it high order detonate. I really don't understand why anyone would want to make it detonate, when there are better alternative materials for that purpose. If novelty demonstration "flash paper" is the purpose, nitrating a paper towel or filter paper will give you what you want.


Pressed nitrocellulose was used as a main explosive charge (by itself, without even having to resort to an oxidizer.) For a time it was even nitroglycerin's main rival, and it was considered much safer (specially when damp) and about as powerful. Cellulose nitration is also relatively easy. All of this makes it a very interesting explosive. So if it could be produced from such commercially available cellulose powders, it would save one the trouble of having to do it the old fashioned way (i.e. nitrate the cotton first, then reduce it to powder.)
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[*] posted on 7-9-2011 at 07:53


Well yeah a lot of things compared to nitroglycerin are safer, dynamite for example is one of them even though the active ingredient is nitroglycerin.
Anyway, wet guncotton was used for naval mines and torpedoes but it
took a booster to set it off, IIRC. Nitrocellulose has more interest as a
component of other things than as an explosive itself. It has value for
use as smokeless powder more than anything else. If you consider the
difficulty in processing the nitrocellulose compared with the strightforward
manufacture of other materials for use as an explosive, its disadvantages
for use by itself as an explosive are apparent. Basically it is an insensitive
plastic material which only under very specific conditions can be detonated.
It also has some stability issues which must be addressed and even then
there is a shelf life for the stabilized material.
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[*] posted on 7-9-2011 at 08:11


Quote: Originally posted by Rosco Bodine  
Well yeah a lot of things compared to nitroglycerin are safer, dynamite for example is one of them even though the active ingredient is nitroglycerin.
Anyway, wet guncotton was used for naval mines and torpedoes but it
took a booster to set it off, IIRC. Nitrocellulose has more interest as a
component of other things than as an explosive itself. It has value for
use as smokeless powder more than anything else. If you consider the
difficulty in processing the nitrocellulose compared with the strightforward
manufacture of other materials for use as an explosive, its disadvantages
for use by itself as an explosive are apparent. Basically it is an insensitive
plastic material which only under very specific conditions can be detonated.
It also has some stability issues which must be addressed and even then
there is a shelf life for the stabilized material.


As you point out yourself, you need to have the nitroglycerin first in order to make the dynamite. That was one of the reasons why dynamite manufacture did not make it to England (at least for a time): nitroglycerin was condemned as too dangerous by Abel (if I remember correctly), and gun-cotton approved. I am sure that if you could make the dynamite directly without having to handle the nitroglycerin first, there wouldn't have been such issues.

If the cellulose powders deliver a good product, capable of detonation, equal or similar in performance to the nitrated cotton reduced to powder, then that would much simplify the process. It would be a direct nitration of the cellulose conveniently already in powder (microcrystalline or otherwise) form, then washing/stabilizing it and pressing into charges. No problematic & tedious (for the average Joe without access to specialized machinery) "pulping" process involved.
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[*] posted on 7-9-2011 at 08:37


You aren't making the distinction correctly for danger in manufacture of nitroglycerin versus nitrocellulose, or for the use of a dynamite compared with the use of nitrocellulose....nitroglycerin based dynamite wins that safety contest and probably wins on stability too. Nitroglycerin is safer, easier, and cheaper to manufacture commercially than nitrocellulose. But yeah given the easier processing if a person just insists that nitrocellulose is their preferred explosive, then it would make more sense to nitrate a particulate form of cellulose already in the mesh desired, to shortcut the otherwise tedious process. If you are looking for a practical explosive there are many better choices than nitrocellulose, just about anything else is better, less expensive and easier to make.
Probably the closest thing to any widespread use of an explosive containing nitrated cellulose was blasting gelatine, or gelatine based ammonia dynamites, or similarly a cheaper nitrostarch based dynamite.

A propylene glycol dinitrate based gelatin gelled with nitrocellulose and used as a dopant to form an OB mixture with an oxidizer would for example probably be a far more practical explosive than granular nitrocellulose used alone as an explosive. An uninvestigated material I found and posted about called glucose nitroureide tetranitrate is another possibility. What guncotton is mostly and best adapted to use for is in relation to "guns" as its name would suggest,
and it is only difficultly adaptable for use by itself as an explosive.

[Edited on 7-9-2011 by Rosco Bodine]
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