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Author: Subject: Picric acid: different instructions
Rosco Bodine
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[*] posted on 6-7-2009 at 05:52


Quote: Originally posted by grndpndr  
Im sure you have far more experience here but are you sure a reinforced cap is really nescessary?

What I said about the need of reenforcing caps was qualified with regards to the quantity and properties of the initiator and base charge, and the geometry of the
device, ect. which are factors having bearing on whether or not a reenforcing cap is required or not.
You must have misunderstood or maybe I wasn't clear.
My own preference is to not use a reenforcing cap design. The quantities and materials which I report may then be presumed applicable to an unreenforced
configuration. I have tried to be specific about the
differences and how one configuration may be useful compared to another, without going so far into the
topic as would change this into a complete instructional step by step which would get this thread locked. When
you edit more than once, you can also edit out all your previous "edited notices" so that only one will appear.

You may be confusing the reenforcing cap configuration
with the laminated capsule design which I have described
having an aluminum liner. They are two entirely different things. A reenforced detonator can be made in any capsule
type laminated or not, where the reenforcement means
simply that the the initiating charge is itself mechanically
contained and retained in a pressed confinement against the base charge. The idea of a reenforced detonator is confinement of the initiator to intensify its impulse directed upon the base charge, and has nothing to do with the outer capsule which contains all of the inner elements assembled
in whatever sequence. Usually the reenforcing cap which
contains the initiator is a miniature capsule having a perforated closure disc, and the thimble like capsule is
filled with the initiator. Its diameter is a sliding telescoping
fit within the outer capsule, and when it is pressed against
the base charge in final loading, the expansion of the inner
walls of that thimble locks it into place holding the initiator
securely against the base charge. The perforations allow
for an igniter charge above the partition to commute fire to the initiator within the reenforcing cap. A laminated capsule is just a "stronger capsule" but a reenforced detonator references a specific configuration of containment for the
initiator itself being mechanically confined against the base charge, to greatly enhance the impulse of the initiator.


[Edited on 6-7-2009 by Rosco Bodine]
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grndpndr
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[*] posted on 7-7-2009 at 05:29
Reinforced detonators


Thank you sir for taking the time to clarify that for me.I believe I have the
basic idea now.I at first thought the reinforced cap was similar to a strongly confined hard to detonate energetic
in principle which didnt seem to make sense.If i understand the idea of the composite cap is to avoid the use of a metallic tubing avoiding its decomposition problems the metall tubing supplying the strenghth to withstand the pressing?

The pelletized detinators fascinate despite the drawbacks of I would suppose fragility,possible hygroscopic.Still i can evvision some great uses for such a devise,I suppose some rather exotic primarys are used.C an you recccomend some reading resourcesRosco, regarding primary sensitivities as wekk as pelletized detonator primaries/construction Regards. grndpndr
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Rosco Bodine
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[*] posted on 7-7-2009 at 11:26


Basically a reenforced detonator has extra confinement around the initiator so that the impulse of the initiator is focused more in the direction of the target base charge as opposed to three quarters of the energy of the initiator going off into space in different directions where
that energy is lost and never delivered to the base charge. Even in an unreenforced detonator you will find that the geometry of the initiator is important and the portion of the initiator having accelerated to maximum velocity should conform to the geometry of a ribbon charge , a platter charge which directs more efficiently
the impulse from that disc into the columnar section of base charge. When you get that effect then you are
getting what you need for maximum output. I'll have to get back on the rest later.
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grndpndr
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[*] posted on 9-7-2009 at 00:26


This must be the reasoning behind the concave end of a commercial cap.Focusing the energy very much like a SC.
The concave end like a platter charge or old fashioned monroe effect AP design.That effect would be simple to duplicate using hollow tubing
and copper/al end cap dimpled with a hammer and a properly sized ball bearing.Soldering the IMP sc end plate to the tubing of a composite cap and grinding the excess

I missed the primary reinforcement used to concentrate its shock helping detonate the composite caps secondary.It would be great to be able to buy a sized end cap to fit.Possibly in the copper fittings of a plumbing supply. To fabricate the reinforced primary cap/help initiate the secondary with a SC end cap?

Have thier been attempts to create detonators that are in fact minature CSCs? I have heard of military SCs maybe prior to piezoelectric CSCs that use a nose fused minature CSC to detonate the main CSCs detonator.Complex for sure but superior to some ideas ive seen floated elsewhere.

[Edited on 9-7-2009 by grndpndr]

[Edited on 9-7-2009 by grndpndr]
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Rosco Bodine
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[*] posted on 9-7-2009 at 05:47


Yes the shaped charge effect is exploited in some detonator designs for the initiator, the base charge, or both, but it is an added variable factor and a complexity which is not good to make an included aspect of an improvised cap except as an enhancement of redundant capability. For an improvised device you will likely be using components which were actually designed and manufactured for another purpose, instead of being precisely optimized for what they are being adapted.
That alone introduces enough complication and will generally increase the size of the device you are cobbling together. It is easier and better to put together
something basic and functional than it is to get elaborate when that isn't necessary.

[Edited on 9-7-2009 by Rosco Bodine]
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grndpndr
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[*] posted on 10-7-2009 at 04:32


KISS principle.:D

[Edited on 10-7-2009 by grndpndr]
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Rosco Bodine
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[*] posted on 18-7-2009 at 16:52


Something worth experimentation with regards to the lead salt of picric acid and the lead salt of styphnic acid
is making a determination if there is possible the formation of a double salt which is anhydrous, and could have improved properties as an initiator if it does exist. Ordinarily the normal picrate and the normal styphnate of lead are each monohydrate salts. However there is a double salt Lead Acetate Styphnate
which is anhydrous, I think :P, and a parallel circumstance may occur for the double salt which I hypothesize may exist similarly as Lead Picrate Styphnate. If it exists as anhydrous double salt,
by virtue of having less water and more nitrogen,
and being made from two parent compounds having
interesting properties, it could be worthwhile.

Formula for the hypothesized salt would be
Pb2[(C6H2(NO2)3O]2(C6HN3O8)
This may be novel and therefore unreported.

http://www.youtube.com/watch?v=1lleBP7Ai7Q&fmt=18


[Edited on 19-7-2009 by Rosco Bodine]
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[*] posted on 19-7-2009 at 11:21


Thanks for the lead Roscoe,I never cease to be suprised by how accomodating you are with those of us with lesser understanding /skills.Regards,grndpndr

In redards to the double salts/complex salts a quick check revealed several patents that may be useful though I havent
had time to look at them.
US patents 3293091 complex salts of basic lead picrates
2226391 man of basic lead trinitro-m-cresolate

2295104man of lead trinitroresorcinol and double salts
I havent seen the entire patents they may not apply at all to what you had in mind but in any event something learned isnt a waste.

[Edited on 19-7-2009 by grndpndr]
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Rosco Bodine
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[*] posted on 19-7-2009 at 11:57


No problem. My time for experiments has been non-existent, but I keep thinking about things and come up with virtual experiments in my mind. I share the ideas with anyone else who may have the time and the inclination to check out any of these possibilities where
the literature has nothing to say, but it would seem possible. It just leaves a head scratcher there for
not knowing. While I am speculating, if such a double salt does exist, it may also be a clathrate former if
the basic salt holds together as the double or multiple salt. There could be a synergistic multiple salt clathrate variant maybe with a chlorate or perchlorate component,
and possibly the azo-clathrate series as well. But the most immediate interest would be the formation of
the possible normal double salt to see what properties it might have and if it is a synergistic compound where
each enhances the other. Such things do happen sometimes, so it is definitely worth a look. If the normal double salt does exist and have a synergistic enhancement between the picrate and styphnate components, it would perhaps have enough initiating
ability that in a reenforced configuration it might be
usable for initiation of a styphnic acid base charge of
very fine mesh crystals, in a 5/16 to 3/8 in column
diameter base charge. A lot of unknowns there, but
that is what I was thinking.
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[*] posted on 19-7-2009 at 12:15


I most often do nothing with what ive learned or think ive learned actual experimentation the only way I would be assured what I had done was successful.Being of practical mind due to nescessity: skills not up to the task of interests
in many cases.Sometimes the 'simple' successful practical applications
require a suprising amount of effort which can be very satisfying.Attempting to improve ones understanding given limitations a slow process but quite engaging.Your help here is always appreciated.
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Rosco Bodine
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[*] posted on 19-7-2009 at 18:21


The method I was contemplating was to use a mixed hot solution containing sodium picrate 2 moles and sodium styphnate 1 mole, added dropwise at equal rate and simultaneously with an equal volume solution of lead nitrate 2 moles, slightly acidic with nitric or acetic acid, going into a starting lump of hot distilled water also acidified slightly with acetic acid. The presence of a slight acidity is useful to prevent the formation of the basic salts which lead is prone to do if the pH is too high.

http://www.youtube.com/watch?v=860HwEgSRhY&fmt=18 True Nature

Something with regards to improvising compound detonators of the reenforced type which I have seen described but have never tried, involves the use of cartridge brass of the straight wall variety or the blanks for what would later be
necked down using dies. Two different brasses are selected which are a close but easy telescoping slide fit for one inside the other and the intiating charge is placed in the smaller diameter and press loaded. The smaller shell casing is decapped and a fired primer or a drop of epoxy or solder closes the primer hole on the larger shell casing. A small increment of base charge is pressed loaded more lightly onto it. The main base charge is pressed in increments to nearly fill the larger shell and the shell filled the remaining way with a lightly pressed increment. Then the two shells are pressed firmly together, at a slightly maybe 10% reduced pressure as was originally used on the initiator. The soft brass of the inner casing expanded by the loading pressure locks everything into place. I forget which brasses are convenient for this. There are several which can be used this way.
.444 Marlin was one if I remember right. Just a little info
there for the scrounging around the gunsmiths shop sort of
thing. Coating the outside of the smaller casing with some epoxy just before final assembly would possibly help make sure there is no creep after pressing. Probably all gunsmiths know about this one and have known for a long, long time.

[Edited on 20-7-2009 by Rosco Bodine]
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[*] posted on 19-7-2009 at 21:56


Done a fair amount of reloading besides what youve mentioned a live primer in the primary side would make a fine stab or FP detonator.One would still want the interior to be of 5/16-3/8 if TNP were involved as a booster leaving pistol cartridge brass or carbine straight walled brass possibly .30carbine for the interior brass5/16 some .31hundreths actually .308 to accomodate the projectile if the brass were resized otherwise the projectile a drop in fit
likely near 2in long.The brass of course would be heavier at the primer end advantageous if ive been following the reinforced detonator posts correctly.
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Rosco Bodine
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[*] posted on 19-7-2009 at 22:44


You got it, the thickened brass at the base of the shell
acts as a reenforcing collar and confinement for the initiator and the extra mass there probably causes a
reflected wave additive to the main wave through the initiator in the direction of the base charge, so it is the
double whammy there which makes whatever initiator
is used have an amplified effect. It is similar to the situation if you were trying to crack a boulder with a stick of dynamite just laying against it, and it didn't work.
And then you put a five gallon bucket full of wet mud on top of another stick and tried it again and yep that'll
do it better. Pushing back against seventy five pounds
of mud gives the detonation wave a bit more traction
at the start, and it's the same deal with the reenforcing cap.
Anyway, I wouldn't do this or at least wouldn't make any habit of it using a regular press and dies. You need something where you can regulate the loading pressure
pretty well and know exactly what sort of pressure you are
delivering. And you need to use separable dies and have some sort of provision in safeguard for the what if one of
the things goes off during pressing....which can happen.
These things are not a trifling matter in terms of what they can do to press, dies, and operator if they should misbehave
and go unexpectedly. Think ahead, and be safe.

[Edited on 20-7-2009 by Rosco Bodine]
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[*] posted on 20-7-2009 at 05:48


Of course safety first,I would never confine a cap like that in a steel die!Basically,reinforced det. just tamping/stemming the primary charge not with mud/sandbags but metal.
The cap material ive seen used never required additional support to possibly create addittional shrapnel and careful is the word in measuring wgt/density for pressing to the correct gr/cc3 w/correct wood dowel and screw press.As well as sandbags covering the pressing op.and personal protection.In any event my interest is theoretical rather than practical application.Just as much fun, well....almost,but much safer in many respects.:

[Edited on 20-7-2009 by grndpndr]
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[*] posted on 16-8-2009 at 00:55


Another problem withn the HG fulminate/picric acid compund detonator would be the reactivity of the HG fulminate with the AL tubing or copper tubing.As well as storage stability of HG fulminate.
Given purified HG fuminate from powerlabs acetic acid ammonium hydroxide IIRC will give very good quality HG Fulminate with very good crystal shapes and density by itself increasing possible shelf life.
However im unaware of any material coating/tubing which is nonreactive with HG fulminate and TNP.SS possibly or a simple coating of the AL, steel,copper tubing?The basic Idea is successful in the extreme with just 1gr/2gr+ HG fulminate/TNPbut a storage stable cap with the material mentioned is out of the question.Ive yet to investigate the lead picrate /pottassium chlorate-TNP compound cap
90/10. AL would be suitable/nonreactive with this metal I assume but the safe storage life is still in question.
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Rosco Bodine
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[*] posted on 16-8-2009 at 21:43


Nobody but me that I know about ever reported it, but mercury fulminate can be purified quite easily from boiling water, so long as the process is carried out over a reasonably short time of exposure to the elevated temperature, the stability of mercury fulminate allows it.
Exactly how safe the process is I cannot guarantee, other than I did it and it went smoothly without any incident. I started a beaker of water boiling on a stirring hotplate and with rapid stirring sprinkled in
the amount of crude mercury fulminate to achieve about a 90% saturated solution at the b.p. of H2O, and then rapidly cooled or quenched the solution and out dropped snow white and pure mercury fulminate, pretty as you please. But truly this was just a curiosity and
mercury fulminate is not really a superior initiator.
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[*] posted on 28-8-2009 at 07:58


I have just tried to purify MF from water. I did get partial success, in the sense that I got a feel for it. I used 4.6g of MF from a batch I made two weeks ago, from 5g of mercury, and a 600mL beaker. I used a magnetic stirrer as you suggested, but mine is homemade and doesn' t have a heating function. I used a hotwater bath which I keep near boiling by replacing the water with water from a kettle kept at a boil nearby. I added 50mL of boiling water to the beaker then added the 4.6g of MF (your way is better I know as it keeps less MF crystals, undissolved floating around at one time), but I was trying to be quick. I soon found that I had filled my 600mL beaker with water from the kettle, and that the temp was only around 85C despite my best efforts, and I still hadn' t made all the MF go into solution. From a link that I have found this morning, if correct, it states that MF solubility in boiling water to be 1g to 130g of the water. So if 600mL of water was at the boil (100C), it should be about what was needed to put the 4.6g of MF in solution. I wish I had found this link before, oh well, live and learn. It sure takes a hell of a lot of water!
Link for wikianswers-MF solubility
http://wiki.answers.com/Q/Is_Mercury-II_Fulminate_Soluble_in...

[Edited on 28-8-2009 by Hennig Brand]
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[*] posted on 28-8-2009 at 16:03


Wtf has this 2 do with PA?

[Edited on 29-8-2009 by User]




What a fine day for chemistry this is.
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grndpndr
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[*] posted on 29-8-2009 at 11:45


Quote: Originally posted by User  
Wtf has this 2 do with PA?

[Edited on 29-8-2009 by User]


If youd have bothered to keep up with the thread it might be
it has to do with det PA ,picric salts etc..WTF does your post have to do with anything but whining?

[Edited on 30-8-2009 by grndpndr]
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[*] posted on 13-11-2009 at 03:13


Hey guys,

I just managed to purity about 56g of ASA, but it appears that it has saccharine traces in it.

My question is, will this effect the TNP synthesis, and would it be best to do my first TNP reaction with nitric acid and sulfuric? I've had bad experiences with solid nitrate and sulfuric acid, and nitric acid makes the stirring much easier.

Also been having trouble finding phenol(wow, that stuff is a bitch to find!) no industrial suppliers will give me any samples, even though I easily bought 99% sulfuric acid from a chemical company which is much worse. Do you guys buy it from lab suppliers? If so, at what price? Or do you find an industrial user and buy off them and what do they use it for? The cheapest I found from a supplier was 90USD for 500g, or 200L drums lol for god knows how much.

Any help is appreciated.

Cheers

Uchi

[Edited on 04-07-09 by uchiacon]
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[*] posted on 13-11-2009 at 11:27


Quote: Originally posted by uchiacon  
Also been having trouble finding phenol(wow, that stuff is a bitch to find!) no industrial suppliers will give me any samples, even though I easily bought 99% sulfuric acid from a chemical company which is much worse. Do you guys buy it from lab suppliers? If so, at what price? Or do you find an industrial user and buy off them and what do they use it for? The cheapest I found from a supplier was 90USD for 500g, or 200L drums lol for god knows how much.

I think 90 USD for 500 g is not a ripoff IMO, but others may know of cheaper suppliers. I paid just about that much to have a pharmacist in a mom & pop pharmacy order it for me. Don't try this at a chain pharmacy.

Several of the many chem suppliers that have been named on this very forum sell phenol. I don't know why you're having such a hard time, or are you not located in the US? Our overseas members have also mentioned a lot of suppliers as well. Go through the threads here and make a list of the companies that are mentioned. If they are discussed here, they will probably sell to individuals.

I sort of doubt that many of us are buying from industrial users, but I could be wrong. That would be my last resort, if that.

Finally, chemistry is just not a cheap hobby. I wish it were so.
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[*] posted on 13-11-2009 at 20:53


Well I live in New Zealand, which is why I can't order this stuff as easily as others...

Correction, the phenol is actually $100US/500g, which is a fucking ripoff. I know that when you buy these chemicals you're paying for A. the company name thats screwing you, and B. because they've taken a bit more time to refine it. I would also assume theres a HUGE markup on that, and they try to cover this by saying it's analytical reagent grade. Sure, but how much did that refinement actually cost?

Funny though, I might just skip DDNP and try to synthesise sodium azide from scratch with the hydrazine and nitrite method. In fact, it's probably actually the best route from here, and the best primary to date.

$100 US would easily cover all the chemicals (the apparatus I already have) for maufacturing sodium azide.
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[*] posted on 21-11-2009 at 02:32


Well, I managed to find a replacement for phenol; I'm fairly sure that sailicylic acid gives a higher yield of TNP than phenol too. I have a beaker full of yellow crystals, they stain like heck, and the volume is several times greater in TNP than what I had of salicylic acid. Now lets hope theres no crap in there. I'm buying my salicylic at $30 (21USD) for 500g, which is pretty crazy. And it's ridiculously fine.

When I figure out how to resize images I'll post some.

I'm looking into lead styphnate and lead azide, I'm sure I can track down some resorcinol to make the styphnic acid with. I don't think its particularly hazardous and it's widely used in parts of the industry that I phoned around looking for phenol.

Hydrazine hydrate will be a bit harder though, but if I can find a source of it then the lead azide manufacture should be quite straightforward from then on.

Is it used in narcotics manufacture at all?
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[*] posted on 23-11-2009 at 01:24


Ok, so I've been making TNP (or attempting to) using salicylic acid. I'm following the powerlabs procedure, but the four times I've done it (15g salicylic, 25ml sulf and 37.5mls of nitric) the salicylic acid has ALWAYS hardened into some crusty semi liquid brown reddish crap in the beaker. I heat the 99% sulfuric acid to about 60 degrees C, dissolve in the salicylic and turn up the heat to 100 degrees.

It then progressively turns into a dark brown/reddish solution. Then I take it off, give it a stir, and suddenly it just completely hardens into this crusty goop. Then I cool it in an ice bath, add the nitric at -20 and everything goes fine from there. Chuck it into cold water, precipates out the TNP and then I wash it and dry it.

But today as I was filtering out my first batches, I thought it was unnecessary to wash the crystals with about 1L of ice cold water as suggested by powerlabs. I used abotu half that, and when the TNP was sufficiently dry, I attempted to try and ignite it with hardly any success.

The pale yellow material stains my hands, is relatively insoluable in water but doesnt burn well at all. I did manage to get a large chunk to burn, but it only burned when I held the blowtorch on it for a while.

It also won't detonate from a hard hammer blow, what's wrong???
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[*] posted on 23-11-2009 at 04:30


What is the source for your salicylic acid?
Did you just buy it or is it purified/modified from aspirin?

It sounds like there is a percentage of TNP in your product.


[Edited on 23-11-2009 by User]




What a fine day for chemistry this is.
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