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Author: Subject: Diving Into the World of Fulminates
Lewis
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Diving Into the World of Fulminates

Hello everyone. This being my first thread here, I'm a little anxious, but I hope this doesn't rub anyone the wrong way as I'm pretty sure this hasn't been covered so far.

Let me first say that I'm not new to the world of energetics, but thusfar have used only organic peroxides as primaries. I've decided to experiment with Hg fulminate, and have everything prepped for a first run. I am, however, a little apprehensive...

My main concern stems from the source of my mercury, which was from the bowels of my ancient house. I was carting away the scrap cast iron from our ~110 year old heating system, when I inverted a section of piping and inadvertently sent a small deluge of elemental mercury onto the ground! Our furnace was a hulking beast-- a mass of clay, asbestos, and iron. God knows what sort of combustion products have been left in those pipes throughout the years (it once used coal, but had been retrofitted to burn natural gas somewhere down the line).

Back to mercury fulminate, I'm a little unsure as to what small contaminants of other heavy metals in the mercury could do to the reaction. Obviously silver, although it seems hugely unlikely, would cause a major problem. Past that I have no idea what else could screw up or make unsafe this reaction.

Visually, the mercury looks mostly pure, with a small amount of dark scum spread around in its mass. I have the equipment to distill it I suppose, but it seems wasteful, hazardous and frankly a waste of time. Another concern is what to do with the leftover reaction products after the Hg fulminate is made, most of which are very toxic.

I think I've gone on long enough here. I appreciate any thoughts.
Leander
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According to PATR and Urkanski small ammounts of other metals such as copper and zinc produce MF as a white participate of roughly 95% purity, while pure reagens grade Hg/HNO3/EtOH gives a sand couloured, brown or gray product wich has a higher purity of roughly 98%. Nowhere in both sources the possibility of other fulminates participating out of a one pot synthesis is mentioned.

I personally don't think its possible either, since other fulminate salts such as cadmium- copper- and sodium fulminate are always made by the action of amalgams, witch take hours if not days to produce a traceable ammount of corrosion on the other metals, leading to the possible formation of other fulminates. The synthesis of MF schould'nt take more than 20 min, so any intervention between free mercury, MF and other metals should have all taken place in a really short ammount of time, unsufficient to get that reaction going.

Though, starting with an amalgam in a MF synthesis could be dangerous, since the formation of other more sensitive fulminates is more likely to happen, because of the larger reaction surface beween mercury, mercury fulminate, and other metals. I think it can be done, but you should always consider en treat the reaction product as being contaminated and potentially dangerous.

[Edited on 30-8-2008 by Leander]
crazyboy
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Mercury fulminate is generally considered less powerful and less sensitive than other primaries such as AP. However there are some things you should take into consideration, do your research thoroughly. The reaction is quite violent and produces a lot of toxic gas. Mercury is also considered dangerous if you inhale fumes. I would suggest you get another source of mercury, that mercury could have been contaminated with any number of metals.

Lewis
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 Quote: Originally posted by crazyboy Mercury fulminate is generally considered less powerful and less sensitive than other primaries such as AP.

This is interesting... Acetone Peroxide never struck me as a powerful primary, but it's fine if MF is a little weak. It needs only to detonate ETN. I was thinking of an 80/20 chlorate mix as cited in various places.

I really doubt I'd go out of my way to find clean mercury, as my whole reason for choosing this primary was based on the fact that I had some mercury lying around.

By the way... I have the means to ventilate all fumes outside my workspace-- no worries there.
a_bab
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I don't think MF is less "powerful" than AP, nor it is less sensitive. It can dtn when scratched with a dried grass straw.
Lewis
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/\ Indeed.

And by the way, if anyone is interested, I didn't try the synthesis because I decided it wasn't worth the risk of forming some unstable compound I didn't predict.

[Edited on 8-9-2008 by Lewis]
grndpndr
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You may regret that particulaly if youve discarded the Mercury.My first fulminate synthesis and Its so much superior to PA in all ways as a detonator
including simplicity of synthesis and half the battle a source of Mercury. Free but questionable purity mercury I would have tried 1/2 a std batch or 2.5grs its being synthesised you have plenty of opportunity to remove yourself from the vicinity.Or place a barrier between you and the simple synthesis.If you notice unusual sensitivity det of its own accord or even as sensitive as AP you have the option of purifying the MF with instruction on both megolomanias website and powerlabs synthesis.MF is still a great Home primary despite its age,AP IMO poses a greater danger than possibly contaminated mercury.APs a finger eater IMO and unnescessary risk.
chemoleo
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I would seriously advise against AP - there are countless of threads as to why - for starters it is unpredictable, different batches have different sensitivities unless conditions are fiercely controlled. There are many better primaries, I've even heard of silver acetylide nitrate being used for ETN. HMTD springs to mind too, much safer than AP. MF should be perfectly adequate. After all it was (is) also used commercially. ETN does not need much initiating power to detonate.

As to your Hg- as you have to work it up as the nitrate salt anyway, perhaps you can think of a purification scheme that weeds out most other metals... i.e. AgCl is insoluble, while Hg2Cl2 is not, based on this you can remove the silver. You can use various other anions to remove other metals this way.

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magneet
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 Quote: I've even heard of silver acetylide nitrate being used for ETN
Silveracetylide-nitrate is alot more underestimated about its ability to initiate insensitive secundairy’s in its practical primairy function.
The reason is simple, when research into its practical function exceeds someone’s ability to make more advanced primairy’s like lead azide for example, nothing feeds the need to make it work anymore.

Hi,
Lewis
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 Quote: Originally posted by grndpndr You may regret that particulaly if youve discarded the Mercury.

Not a chance! That stuff is way to cool to throw out (not to mention I don't know how I'd get rid of it).

Perhaps I'll synthesize about a gram in the standard fashion. After washing and decanting, I'll gingerly transfer some wet crystals to some sort of drop-rig, and leave them there until dry.

COPAE sites Hg(CNO)2 as having a drop test sensitivity of 2-4 cm for a 2kg weight.

If it was going off from a significantly weaker impact, I'd know something was up.

[Edited on 17-9-2008 by Lewis]
grndpndr
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If your mercury is satisfactory i would be willing to bet you'll be pleasantly suprised with the results from what ive always felt to be a more sympathetic primary (than AP)particulrly if for some reason yor compelled to use a composite cap even TNP/FM if sufficient precautions agaisnst cross contamination.The destructive effect of even a small comp. cap; FM- w/1gr.of TNP/PETN/RDX etc quite likely to = #8 cap.

[Edited on 20-9-2008 by grndpndr]

[Edited on 20-9-2008 by grndpndr]
12AX7
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Re: subject,

I imagine an immense sea of mercury fulminate, beaches and dunes and ripples; and myself, as if jumping off a dreamland diving board, careening gracefully into the center. And then with a flash, this imaginary world... ceases to exist.

Tim

Seven Transistor Labs LLC http://seventransistorlabs.com/
Electronic Design, from Concept to Layout.
Need engineering assistance? Drop me a message!
grndpndr
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Poetry,how about bathed in the warm glow of nuclear fire?LOLEither way almost a religious experience assuming I did not end up a crispy critter.

[Edited on 16-10-2008 by grndpndr]
OWCHITBUURNS!!!
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cant seem to find it on the net now, but i used directions for synthisising picric acid , from from cheaply procured acetysallic and sulphuric acid,and potassium nitrate from a german site which i think was called LAMBDA synth ,it had about 4 synthesis methods,ill see if i cant find the pdf i made from that page

anyone can face a room full of zombies,true bravery is facing your own fears ,and weaknesses
grndpndr
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Do a site search on Picric acid should reveal so many synthesis youll be wondering which to use ?
OWCHITBUURNS!!!
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my bad , meant to post this on another board
and i have NO FREAKING CLUE how to DELETE posts on this fourm????, so moderators feel free to delete both .

seeing as i found it i thought id slap it up there anyway cause i
like the way it lists ALL the procedures ,with pictures between each intermediate step.all procedures ...except the one involving hot nitric acid ,and wood EEEK!! ,also seems less wastefull than most synthesis's.oh ja i meant Salicylic Acid in my last post

heres the link, its german so slap it into bablefish or gogle translations http://www.lambdasyn.org/synfiles/pikrinsaeure.htm

anyone can face a room full of zombies,true bravery is facing your own fears ,and weaknesses
grndpndr
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Though blessed with gift of a 1/4lb dist. merc from a friend,gold mining country still after all these years so its not uusual to find mercury for the purification process from the black sand bearing gold.And even caps now and then as privately owned mines still exist in the hills.MF would have still been a 1s choice primary due to simplicity of glasware and as well as all around suitability, sensitivity far from excessive still quite powerful but somewhat difficult to press to optimum
density.relatively easily procured precursors f whic only 2 are even of moderte difficulty obtaining and perhaps 10 min of Time from start to finish of good quality MF.Must be quite cautious of all fumes however the merury, heavy metal very painful poison.
quicksilver
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CLEAN UP YOUR Hg:

Obtain a large hypodermic of veterinary size (horse/cattle hypodermic: new) Place cotton in the bottom of the barrel of the syringe. Place the Hg that you want filtered on top of the cotton and place the plunger in the body and "squirt" the Hg into a container. Repeat w/ fresh cotton...
[Use cotton, it will work well. Courser filter material is unnecessary.]

This is obviously not the most complete method HOWEVER, it will pull all the external oxides and "crud" from the floor and - in fact - will function well for the purpose of obtaining clean elemental Hg for your purposes.
THIS DOES WORK! It also is a metal you are working with. That metal will not be contaminated without some effort. If it merely spills or is exposed to some superfluous junk; this is a well used method to clean it up quite well.

I obtained about a pound of Hg from switches at a junk-yard, using the same mechanism for cleaning up the material and the resultant Hg was fine for the purposes outlined & w/ no problems! In order to contaminate Hg on an elemental level you would need to do more than spill it.
If it's got "crud" in it: you have now a method to clean it up. I've used this technique & it works VERY well!

[Edited on 31-12-2008 by quicksilver]
Hennig Brand
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I like your mercury cleaning technique, it seems like it would be very effective. I am going to give it a try soon.
I have made a couple of small batches of MF in the last couple days. The first batch I used 90% nitric and didn' t wait for the nitrogen oxides to clear before adding ethanol, and it reacted very fast 1-2 seconds and when it did it nearly covered everything with mercury nitrate, HNO3 and ethanol. The last time (today) I used 5g mercury, about 40mL of ~70% HNO3 and 55mL 90% ethanol. This time I let the NO2 clear mostly after all mercury reacted and used a bigger beaker just in case. I added the ethanol and it took a good 5 minutes for the reaction to really start, and when it did it took about 15-20 minutes to complete. This was a hell of a lot more relaxing than starting in 1 second and over in 1 minute or so. What I want to know is, how much should I expect for a yeild from 5g mercury? Also most sources I have seen say that it doesn' t store very well. I think I have seen some say a few months to six months. How did industry make dynamite caps last for years, and the military make caps and rifle primers last for years. I have heard that people have shot old rifle shells with mercury fulminate in them that were maybe 50 years old. Is it just really good purification, or is it some kind of stabilizing chemical and/or technique?
Rich_Insane
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I don't think you guys see the advantages of AP and HMTD. They are just really easy to synthesize. I can't afford silver nitrate or an acetylene maker, so I'm restricted to explosives that are based simply off of nitration and organic peroxides (mercury is too expensive for me). Silver acetylide is way to expensive for me to produce. MF is promising, but mercury isn't very easy to obtain cheaply. I am talking under $15 for 10 g. Back to the topic: To purify mercury, just do what quicksilver did. No distillation needed. The main concern would be sensitive fulminates -- metal impurities shouldn't be too large, in fact there probably isn't enough to cause you any problem. What I'd worry about is not inhaling any of the byproduct gasses from MF detonation, because you produce mercury vapor, which is definitely something you do not want to breath. ammonium isocyanate Hazard to Others Posts: 124 Registered: 13-7-2009 Location: USA - Midwest Member Is Offline Mood: sick The Science Company has 3x distilled mercury, 30 something bucks for 100g and fifty something for 250g IIRC. Rich_Insane National Hazard Posts: 371 Registered: 24-4-2009 Location: Portland, Oregon Member Is Offline Mood: alive Actually.... Daigger has 100 g 3x Distilled Mercury for$7.99
Hennig Brand
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Just got back from a week and a half work trip. While I was in an industrial park buying paint, I stopped in at a chemical supply place. I asked for their catalogue, and among the other things in there was mercury, for around \$11.50 an ounce IIRC.
Hennig Brand
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Does anyone know if mercury fulminate can be purified, recrystalized from boiling water? I know I have seen this described at least a couple times in old books, but was a little hesitant to try it. It seems like it could be done safely, but maybe I am missing something. Any input appreciated.

I was just reading from the thread "Picric Acid different instructions", and in the last post there on pg 14 is a description by Rosco Bodine on recrystalizing MF from water. I am glad to see it, because the couple times that I have seen it mentioned in books, it was described as common practice at the time (late 1800' s to early 1900' s), but didn' t describe how it was done at all. Thank you Mr. Bodine.

Does anyone know from either experience, or reading what the solubility of MF is in water? I guess I can experiment and see, but if someone knows I would appreciate it.

[Edited on 27-8-2009 by Hennig Brand]
grndpndr
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This is directly related to hennig's questions as to stability and storage time of HG fulminate.I have read that bakelite was a material used in the manufacture of hg fulminate detonators as it was inert to the HG fulminate.bakelite is obviously obsolete Is anyone aware of other materials that were used in the manufacture of hg fulminate caps, etc.HG fulminate was introduced in the early 18th cent long before the civil war for use in copper percussion caps for rifles .All iknow about the old percussion caps is they were filled with the appropriate amount of HG fulminate and a paper likely laquered disc pressed on top preventing the loss/contamination,water absorbtion of the HG fulminate.
Perhaps a laquer coating,parraffin,polyurethane coating of the interior of the detonator?Being wartime before modern transportation its easily concievable these rifle percussion caps werent issueed for often at least a year or more surely contained before issue in a vapor/water tight container.

[Edited on 28-8-2009 by grndpndr]
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 Sciencemadness Discussion Board » Special topics » Energetic Materials » Diving Into the World of Fulminates Select A Forum Fundamentals   » Chemistry in General   » Organic Chemistry   » Reagents and Apparatus Acquisition   » Beginnings   » Responsible Practices   » Miscellaneous   » The Wiki Special topics   » Technochemistry   » Energetic Materials   » Biochemistry   » Radiochemistry   » Computational Models and Techniques   » Prepublication Non-chemistry   » Forum Matters   » Legal and Societal Issues