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Anthony
March 17th, 2003, 07:49 PM
the_wingman
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Posts: 48
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Registered: JAN 2001
posted February 11, 2001 03:40 AM
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Has anyone tried this?
KNO3 : K2CO3 : S = 3:2:1.
It's supposed to work better than common black powder!?


ALENGOSVIG1
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Posts: 766
From: Vancouver, Canada
Registered: NOV 2000
posted February 11, 2001 03:56 AM
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"Fulminating powder" or "yellow powder". detonates with 3 times as much force as the best commercial black powder when melted.
If you plan on making this, melt the kno3 and K2CO3 together then powder it very finely. Then add the sulfur. This is said to explode with 8 times as much power as the best Black powder. This has been discussed before. You should have conducted a search.

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Explosives Archive


wantsomfet
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Posts: 233
From: EU
Registered: JAN 2001
posted February 11, 2001 07:07 AM
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It has to be mixed very, very good, otherwise it won't be useful. Be careful when melting it, not too high temperature...
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Anthony
Moderator
Posts: 2312
From: England
Registered: SEP 2000
posted February 11, 2001 08:16 AM
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So is it 3 or 8 times as powerful as the best black powder? I don't see how you can compare soemthing that detonates to someting that only deflagerates.


J
Moderator
Posts: 605
From: United Kingdom
Registered: SEP 2000
posted February 11, 2001 11:12 AM
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Yellow powder has been discussed before. The search feature is there for a reason.
J

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arm
May 2nd, 2003, 10:56 AM
Hi,

Yes, well, i just attempted to melt together the three ingreadients of fulminating powder and now i am deaf. I had it coming i suppose - i should have melted the carbonate and sulfur together first and then dry mixed it with the KNO3. I would say that this mixture is extremely powerful, unpredictable and not to be mixed in this way. It is easily 8x more powerfull than BP. Approx 1/2 teaspoon full 'detonated' and it utterly destroyed the tin can i was heating in. Luckily this was in a large iron pot for shrapnel protection.

Also, has anyone lost hearing from a pyro experiment gone wrong? I was a 4m away at the time of the blast! I think i may have perforated an eardrum but am not sure. My hearing is diminished and my ears are singing a bit. The left one feels like it is clogged up.

Advice would be good right now (i have searched), so:

1. Does this mixture still work as well if the produced Polysulfide is dry/cool mixed with the KNO3?
2. Whats does it sound like ive done to my poor ears, lol?

This post seems to have been put in high explosives, dunno if it belongs here.


arm

Anthony
May 2nd, 2003, 02:50 PM
If it was only 1/2tsp and you were 4m away, don't worry, you'll be fine.

arm
May 2nd, 2003, 03:18 PM
Cheers Anthony,

Yeah my hearing is now almost back to normal. Next time, hearing protection!!!

Ive been conducting i little more research into this stuff. The text by Samuel Guthrie suggests that the Potassium Nitrate should be melted together with the Potassium Carbonate and then dry combined with the sulfur. But previous posts say that the S should be melted together with the K2CO3 to produce polysulfides. Has anyone got any experience of which method is best? It would seem that the latter method would be a little safer since no hot oxidiser is used. But inferior in quality since the oxidiser + reducer/fuel intimacy is less.

cheers,
arm

xyz
May 2nd, 2003, 10:03 PM
I think that melting together the carbonate/sulfur would be the better option. That way all the polysulphides are produced. Does the polysulphide dissolve in water? You could dissolve the KNO3 and the polysulphide in boiling water and then recrystalyse it so that the two are nicely mixed.

nbk2000
May 3rd, 2003, 02:09 AM
You wouldn't want to add water to it, because the polysulphides could react to form various sulphurous acids, degrading or destroying explosive power. It has to be anhydrous to work, just like golden powder.

xyz
May 3rd, 2003, 04:00 AM
Errr... Golden Powder (if you are referring to KNO3/Ascorbic Acid) is usually made by dissolving the two components and recrystalysing, that is why I thought that this method may work for yellow powder as well.

Are you referring to a different comp. other than KNO3/Ascorbic Acid?

jfk
May 3rd, 2003, 04:41 AM
Whats a good source for potassium carbonate? (its brobably infront of my nose, but i just cant think of it right now)

personaly, i wouldnt waste time with golden powder, the stuff ive made wasnt that powerfull and stunk so bad......

arm
May 3rd, 2003, 05:50 AM
hi all,

Ceramics supplies shops sometimes sell Potassium Carbonate. I was infact using Sodium Carbonate sold as Washing Soda. This is actually Na2CO3.10H2O so you will need to heat it separately to drive out the water.

Guerilla
May 3rd, 2003, 12:04 PM
I've been wanting to try fulminating powder but I'm lack of potassium carbonate too. I have tried with barium carbonate without success, if it really works with Na2CO3 then I gotta give it a try.

The reaction between polysulphides and nitrate takes place easier when there's a small amount of moisture present, thus the hygroscopity of polysulphides can make the mix even more sensitive.

Does anybody know the solubility properties of these polysulphides? Apparently water can't be used but maybe some organic solvent could be used to dissolve KNO3 and polysulphides as xyz is referring. It would suffice even if only the other dissolved, they would intimately mix together after rapid recrystallisation, like black powder is made with CIA method. The most important thing is of course that the solvent wont cause any unwanted reactions.

Probably the safest way is still to put the dry mixed ingredients in foil bag, throw it on embers and take cover.

arm
May 3rd, 2003, 01:00 PM
Hi,

I actually sucessufully managed to melt a very small quantity of yellow powder together not long ago and let it cool without detonation. I then gingerly tested the mix, the amount was very small (still got the previous detonation ringing in my ears!), a lump 2mm in diameter. Even cool the solidified mass burst with a loud pop sending hot liquid reaction products through the air. I have yet to test dry mixing the polysulfide with the nitrate but will do within the next few days.

Ive tried mixing the three compounds together without melting and quite frankly the results are a bit lame. Without the polysulfide this stuff is (logically) pretty crap.

If your gonna try melting all three ingreadients together guerilla go real easy on the temperature used and the amounts. I'll try and get some pics up some time of whats left of the tin can i used. It wouldnt hold many baked beans now, lol....

arm

Sparky
May 3rd, 2003, 02:08 PM
My friend has experimented with this mix before. He heated the potassium carbonate and sulfur together first, before mixing and melting with the potassium nitrate. I don't want to be a downer but this mix seems useless for most things. It burns very fast when melted and dry, but it is very hygroscopic (more than ammonium nitrate). Then when it gets wet it burns slowly of course. Hopefully you will have better luck, possibly melting the two salts together first, but I have seen that it is not useful for anything.

arm, you are right it is very loud. About an eighth of a teaspoon damaged my friends hearing for a day when it exploded (he overheated it on purpose and didn't know it would be so loud) as he was about 1 meter away. It was not contained in any way, simply melted on a spoon. Anyone experimenting with this stuff should deffinetly wear hearing protection and of course only work in small amounts.

arm
May 3rd, 2003, 05:02 PM
Hi

mmm, interesting. Perhaps the mixture could be water proofed by the slight addition of a water resistant compound (wax, grease, oil, NC lacquer etc). The stuff is very brisant, i wonder how it compares with flash.

Also, in which way is it useless? Surely it could find use as a pyrotechnic report formulation if it can be proofed against water ingress. Ive read that it was used in 19th century firearms for a while. Also i wonder if its power is increased further by confinement. I will have to experiment further.

I am still unsure as to whether this mixture belongs in high explosives. It is a mixture after all. But then again 'burning' does not seem a fitting description of the reaction that takes place, especially since such a loud report is generated without confinement.

arm

xyz
May 3rd, 2003, 10:41 PM
Potassium Carbonate can be bought at agricultural and garden supply shops where it is sold as "Potash" or "Carbonate of Potash". You can buy 2.5Kg bags of it from hardware shops and plant nurseries around here.

I have not made yellow powder yet but I will probably try pretty soon. When you are using the melting method, what tempertature does it melt at (approx.)? Do you have to finely grind the ingredients if you are using the melting method?

I will only be melting about 0.1g or less and I will be wearing hearing protection.

Sparky
May 4th, 2003, 12:48 AM
I consider it useless because it is so hygroscopic and dangerous to make. If you could make it waterproof easily then it would be useful, though maybe still unpractical to make. On the other hand the ingredients are easy to get.

Good luck trying to waterproof it. Wrapping in alumnium foil right after making it could be useful.

My friend bought his potassium carbonate from a ceramics store. It is very hygroscopic so it's probably a good idea to dry it out in the oven first. I suppose as you melt the potassium carbonate the water would leave and not cause a problem.

It certainly burns much faster than your normal everyday flash, at least when melted and probably when dry and cool too. As I said, it is easy to get a loud report with no confinement and very small amounts.

I don't have any good idea at what temperature it melts. My friend used an alcohol flame. I think you will find that it turns black and bubbles before going off, just to let you know.

xyz
May 4th, 2003, 03:51 AM
Thanks for telling me about the turning black thing.

It is probably best to dry the K2CO3 first so that the weight of the water in it doesn't screw up your ratios when you weigh it.

arm
May 4th, 2003, 06:42 AM
Hi,

xyz, yeah before i melted i ground the three components together in a ball mill - but only for 30mins. My sulfur was coarse so it probably could have done with being longer.

I do not know of the exact temperature at which to heat the stuff. But here are the melting points of a few of the constituents.

Sulfur(monoclinic) 115C
Potassium Carbonate 891C
Sodium Carbonate 851C
Potassium Nitrate 334C

Its interesting that the Carbonate melts at such a high temp. Especially compared to the sulfur. I dont think when i melted the temp got that hot. Even if it had the KNO3 would have decomposed long before. Would the Carbonate somehow dissolve in the molten sulfur to produce the polysulfides?? Or does the sulfur react on contact with the carbonate?

xyz
May 4th, 2003, 06:51 AM
The K2CO3 and the sulfur would react on cantact when heated, the polysulphide that is produced thn melts.

kurtti
May 4th, 2003, 10:12 AM
if i remember right, sulfur + potassium hydroxide - reaction forms various potassium polysulfides... no need for dangerous melting operation. :)

xyz
May 5th, 2003, 08:02 AM
The melting of the sulfur/carbonate to produce the polysulphide is not dangerous. It only becomes dangerous once the nitrate is added.

Potassium Hydroxide would also probably have to be heated before it would react with sulfur. This reaction would produce water as a byproduct and wet/decompose your polysulphide. The reaction with carbonate/sulfur only produces carbon dioxide as a byproduct.

arm
May 5th, 2003, 09:14 AM
Hi,

While melting the sulfur/carbonate ive also dectected strongish sulfur smelling fumes. What could this be due too? I attributed it to maybe sulfur vapours or some of the sulfur decomposing. Mind due, my sulfur is gardening grade so it could be due to sulfur based impurities decomposing.

Wouldnt there be a possibility of H2S when using NaOH? Ive read on materials safety data sheets that H2S is a possibility when using Polysulfides in various reactions - especially aqueous ones.

Finally, are polysulfides with higher amounts of sulfur stronger reducing agents? And, if so, is there a way to tailor the heating reaction to produce these more highly sulfurated forms? Ive noticed that the final product is more powerful if heated for longer. I beleive that NaOH would only produce the polysulfides with lower sulfur content.

the arm

Guerilla
May 5th, 2003, 09:29 AM
It produces also sulfur dioxide, as follows

2 K2CO3 + 8 S --> K2S3 + K2S4 + 2 CO2 + SO2

I would be interested in what does the reaction between polysulphides and nitrate looks like..

Mr Cool
May 5th, 2003, 09:38 AM
The sulphurous smell is due to side reactions.

As Guerilla said, 2 K2CO3 + S8 --> K2S3 + K2S4 + 2 CO2 + SO2 (<-- smelly SO2)

Also, if water is present (which is likely) then hydrolysis of sulphides can lead to the formation of H2S.

Going off on a tangent here:

Can anyone guess why Na2Sx (formed by mixing dry NaOH and S, and adding a few drops of water to start the reaction) turns acetone blue? I was extracting the polysulphides from the other products/left over reactants with the acetone. As more polysulphides dissolved, it turned green and brown, then red, which is the colour that you might expect. But initially, it went a clear blue. Strange. Also, there's a funny smell to it, but I can't decide if this is just acetone with SO2 and H2S, or a new compound :confused:.

The only thing I can think of would be CH3-CO-CH3 <=> CH2=COH-CH3, + H2S (formed by hydrolysis) --> CH2=CSH-CH3 + H2O
I have no idea if this would actually happen, but it's the only thing I can think of.

arm
May 5th, 2003, 12:13 PM
Interesting, i havent heard of H2S or SO2 turning acetone blue, so it may be a new compound. But then again its been a couple of years since i ditched BSc chemistry for BSc Computer Science, lol. Are your reactants completely pure?

Going off on a tangent myself, i recently did a UK google search for some chemicals and found a site called gardenchemicals.co.uk. Now what strikes me as odd about this site is that it only sells KNO3, NaNO3, S, and NH4NO3. You would think being a fertilizer site they would have your more usual ferts such as "Blood, Fish and Bone Meal" and "MiracleGrow". Anybody know anything more about this site??? Its either a dodgy site to get credit card numbers, a police setup or someone who just wants to sell pyro chems to his mates. I did a WHOIS search on the url and it came up with a pretty normal looking address, not a company address.

I notice there are a few other chaps from the UK here, where on earth do you get your chems from???

Sorry about getting sidetracked there...

arm

zaibatsu
May 5th, 2003, 01:06 PM
For me at least, getting chemicals in the UK is annoying, but can be done. The main problem being that you have to buy from lots of different places as the chemicals are usually sold as a product, not the specific chemical, IE NaClO<sub>3</sub> from weedkiller.

Yowza, that place is expensive! AN in the uk shouldn't cost more than about £3 a kilo, much less in bulk.

arm
May 5th, 2003, 01:49 PM
Yeah, im constantly reading package increadients/contents, i get my KNO3 from an unspecific shop, its a little pricey but its fairly pure (although the bloody website's down at the moment). Whenever NaClO3 is sold, its 53% fire suppressent and has to be removed via double decomposition.

(Getting very off topic now...ill shut up)

Editted to protect source...

Anthony
May 5th, 2003, 03:12 PM
Double decomposition isn't necessary, only a fine mesh sieve is - NaClO3 crytsals are caught, fire depressant falls through.

BTW, please be careful with the GD source, it is important that it doesn't dry up from kewl abuse, so please don't publish it!

arm
May 5th, 2003, 05:20 PM
Apologies, wont happen again Anthony. But i wouldnt worry too much about them drying up, they are part of a much larger company.

Anthony
May 5th, 2003, 06:07 PM
No need to aplogise, you weren't to know. It is doubtful that they'd stop selling the particular products we're interested in, but they might stop processing "suspicious" orders, or even reporting them.

Ollie Snowie
November 6th, 2003, 04:07 PM
Well, I have just tried this and I am quite impressed. I just mixed KNO3, Na2CO3 and S together in spatula measured quantities. Then I just ground them up in the mortar and pestle - unwise for trying something new, but no, there was no accidental explosion. Then I held a small pinch over a candle flame on some aluminium foil. It made SO2 and then caught fire like not very good BP does. Then I wrapped some of it up in foil and heated it over the candle. It waited to get hot and then went "puut". I decided that there was too much S so I added a bit of KNO3 - confined test "bssssss". Then I added a bit of NaHCO3 just to see if it could substitute Na2CO3 - confined test "crack!" Yippee!
Then I decided to make an impact sensitive explosive with it (The pure stuff just sat there when hit with a hammer.). I diluted it with BP, mixed in a bit of NaClO3 and a bit of sand to make sure it would go off (Even with NaClO3 it the whole pile would not explode from a hammer blow.). About 1mm cubed of this hit with a hammer made me a bit deaf and my sister started complaining of the "bang whenever you go outside" :). I told her it was going to be small because I thought it was going to be small too!
I'm overjoyed because this is the only flame ignited "bang" I have made except the pathetic TACN (and the weedkiller'd BP I made when I was a kewl :().
I'd certainly recommend this to anyone getting fed up with nothing working and just wants to hear a bang.

[PS - I forgot to mention - the first time a did the confined test I was sure I felt a shockwave go over me (I think it could have detonated). On second thoughts I used about 2mm cubed so unless it was very well wrapped up I don't think it is possible for unincorporated powder.
Unless you think it's a definite no, I well try making blasting caps with this. erm...?

xyz
November 7th, 2003, 05:39 AM
You can try it but I don't think that detonators made with this will be very reliable. If they do work then they will probably have to be fairly large.

But try anyway, I am interested to see if it would work.

Marvin
November 9th, 2003, 02:18 AM
Yeah xyz, thats a sensible thing to suggest to someone who when the experiment didnt work added chlorates to the sulphur mixture until it did work.

Ollie, fulminating powder only detonates when hot and molten, you cant make caps with it. The problems with sulphur or particulally sulphides and chlorates are well known and if you're serious about coming out of the kewl stage, you'll learn about these and probably end up dumping one of the two completely. Detonators made with sulphur or sulphides and chlorates are only going to cause accidents.

skatastamoutra
January 1st, 2004, 03:54 PM
I recently tried to manufacture some Na2Sx for use in yellow powder but always my problem was the high hydroscopic nature of the final product.
In my last attempt I added a slight amount of oil in the powder to waterproof it as “arm” mentioned, which worked well, and the powdered composition didn’t absorb any water from air. The main problem is that it lost deflagrating speed making it useless as a pyro compo.
After this failure I searched in google for polysulfides that probably someone could buy and contain some sort of waterproof and found this pdf file http://www.aartdevos.dk/web600/datablad/ta65_000.pdf
Scroll down and check the blue/violet pastel colors. They seem containing sodium polysulfide aluminosilicate (I don’t know what exactly is aluminosilicate, could someone with knowledge help) and also other colors, anyone believes that these polysulfides could be used in fulminating powder? At least they must be waterproofed although I don’t know what is the concentration of polysulfide in the pastels.
I know it sounds kewl “polysulfide from pastels” but where I live I can’t find this material pure and making it close to neighbors is pain in the ass, every body complains for the bad smell. Btw the smell when using as a fusion mix NaHCO3 + S8 is SO2 or H2S? It could be both though.

Ollie Snowie
January 6th, 2004, 02:46 AM
Wellll, I can't see the pastel polysilfude working, because it's probably not very pure.
Sodium hydroxide can be reacted with alumina and silica to make aluminosilicates, and apparently these pastels have a polysulfide of these molecules as the colouring. That's it - the colouring - so it's probably less than 50% polysulfide.
The smell is probably SO2 because you get that whenever you burn sulfur. It is choking or does it smell of rotten eggs? The only hydrogen around is in the NaHCO3 but I do sometimes notice a smell of rotten eggs after the SO2 goes away. Perhaps it reacts with water and reducing agents to make H2S.

skatastamoutra
January 6th, 2004, 07:25 AM
The smell with NaHCO3 + S8 has a dense smell of rotten eggs, is this H2S. I breath some of these fumes but i am not sure what it is.

gliper
January 9th, 2004, 02:49 AM
I think its more likaly sulfer dioxide, ether way try not to breath those fumes.

Rhadon
January 9th, 2004, 02:56 AM
The smell of rotten eggs is an indication for H2S.

skatastamoutra
January 11th, 2004, 08:04 AM
Would it be more wise to heat the soda bicarbonate to remoove water before melting with sulfur?

vulture
January 11th, 2004, 07:24 PM
Yes, If you heat it strong enough you'll convert it to soda:

2NaHCO3 --> Na2CO3 + H2O + CO2

Note though that NaHCO3 is much less hygroscopic than Na2CO3.

skatastamoutra
January 12th, 2004, 11:03 AM
when you say strong enough in what temp. and for how long.
Could a stove for 5 minutes for example do the work?

vulture
January 12th, 2004, 04:56 PM
Decomposition begins at 65C, at 300C the conversion is nearly quantitative.

Someone
January 13th, 2004, 01:23 PM
Hi,
i think 200°C should be enough...if my chemists-database does not lie.

skatastamoutra
January 13th, 2004, 03:16 PM
Yeah thats right... But could also someone tell me for how long i should heat it. 5 min? 10min???

xyz
January 13th, 2004, 10:18 PM
The time taken will obviously depend on the amount of heat that your heat source creates (I'm not talking about degrees here, I'm talking about the amount, as in BTUs). It will also depend on how much NaHCO3 you are heating.

Marvin
January 14th, 2004, 01:21 PM
skatastamoutra,

Its giving off CO2 and water vapour, it should be very easy to tell when furthur heating produces no more and accidental over heating even to well over red hot wont hurt the product in this case.