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Author: Subject: Picric acid: different instructions
grndpndr
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[*] posted on 27-7-2010 at 14:44


Quote: Originally posted by Hennig Brand  
I always sort of wondered if putting Al powder in AN based explosives was kind of a waste because of the low heat of detonation. Maybe the ones with high concentrations of Nitric Esters or Nitrated Aromatics would get much more potential out of the Al powder.

Anyway here is a close(r) up picture of the hole the 2g of TNP made(2g TNP compound cap #1). Does anyone know if this seems like a reasonable amount of damage for 2g of TNP? It seems a little wimpy. Anyone with first hand experience, your opinion would be valued.




[Edited on 26-7-2010 by Hennig Brand]


If your cap was sitting with its end against the sheet metal it should have made a clean cut similar to a hole punch slightly larger in dia. than the det. Looks like the TNP failed to detonate.Pressing the primarys properly?

[Edited on 27-7-2010 by grndpndr]

[Edited on 27-7-2010 by grndpndr]
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[*] posted on 27-7-2010 at 16:08


Quote: Originally posted by quicksilver  

An impact test would be the easiest. A track for a weight (it's also been 1Kg TTBoMK) to slide down - could be rigged up pretty easily; the only challenge would be the actual impact surface....Too small or too spread out & you tweak the results. There would need to be one standardized contact surface area & I have not read what that is exactly. Pictures do not come close enough to the base area to make a determination.

Wizard - if you ever get any info on the above I would seriously appreciate it. I have not found contact surface area (size) for impact testing nor have I found contact design for friction (I have found that it was one cm however). I checked U.S. Bureau of Mines, Weaver, Federoff, Urbanski,etc (the usual).




Here is something to keep you busy while I compile some
better info.



Title: Evaluation of Test Methods for Pyrotechnic Hazard Classification.
Personal Author: Wilcox, Wayne R
Corporate Author: GENERAL ELECTRIC CO BAY SAINT LOUIS MS ENGINEERING AND SCIEN...
Source Code: 409145
Page Count: 160 page(s)
AD Number: ADB004208
Report Date: 01 MAR 1975
Distribution Code: 01 - APPROVED FOR PUBLIC RELEASE
Report Classification: U - Unclassified
Collection: Technical Reports

http://tinyurl.com/2b6t9dc
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[*] posted on 27-7-2010 at 16:32


@Grndpndr
All caps where laid on their side on the barrel. Not a proper test probably, just for fun really. My endcaps are wood and epoxy so the end test wouldn't work right I don't think. The second comp cap with 2g TNP went high order for sure. It was a hell of alot of noise for only 2g of explosive, and the damage to the steel was not too far behind what the 1.5g of ErTeN did. I am pressing with a vice and dowel, just like you. I measured/estimated that I am getting compaction to ~1.5g/cc. I saw figures for Lead Azide and Mercury Fulminate and for best performance I think the densities were much higher. Honestly it is a little hard to tell exactly how densely the Lead Azide was pressed. I used about the same amount of pressure as I did for the TNP if that tells you anything. Both MF and LA are very dense materials anyway I guess, must be a lot easier to press I would think.

Oh yeah, I think I used "concussion" where I should have used "percussion" a few posts ago.

BTW, does anyone here have any personal experience with Basic Lead Picrate, in particular its sensitivity to percussion. Any experiences or info welcome. All I know is the stuff I made makes great firecrackers, but I don't know if I'd trust it to initiate dynamite.

[Edited on 28-7-2010 by Hennig Brand]
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[*] posted on 27-7-2010 at 16:35


Quote: Originally posted by quicksilver  

Wizard - if you ever get any info on the above I would seriously appreciate it. I have not found contact surface area (size) for impact testing nor have I found contact design for friction (I have found that it was one cm however). I checked U.S. Bureau of Mines, Weaver, Federoff, Urbanski,etc (the usual).



Muhamed Sudc'eska
Test Methods for Explosives
Springer 1995

Mentions and has a drawing of the BAM (FDR) apparatus.
You can read parts of the book @ google.books.com,
however, the drawing is missing (I own a hard copy).
La machine is made by Julius Peters KH, Berlin. Google
them.

He sez that the American US Bureau of Mines and ERL apparatus
are covered by MIL-STD-650, methods T 511.1 and T 505.1.
I have not been able to find this Military Standard in the usual
places. Google it.

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[*] posted on 27-7-2010 at 16:51


Quote: Originally posted by quicksilver  

Wizard - if you ever get any info on the above I would seriously appreciate it. I have not found contact surface area (size) for impact testing nor have I found contact design for friction (I have found that it was one cm however). I checked U.S. Bureau of Mines, Weaver, Federoff, Urbanski,etc (the usual).



Have stumbled upon the attached PDF

LLNL Small Scale Friction Sensitivity (BAM) Test
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[*] posted on 27-7-2010 at 16:56


Wizard, thanks for pointing out that book, "Compressed Gun Cotton for Military use". I just downloaded it, going to give it a read. I have been playing with Guncotton a bit lately. Wrapped up tight in some tin foil it makes a pretty good bang on an anvil. A lot easier to set off this way than my TNP.

BTW just Google "Picric Acid and low order detonation" and lots of stuff comes up. Apparently even in large shells if not properly overdriven you will often get a low order detonation of the entire shell. Were you just messing with me a little bit Quicksilver? It must be nice to have a good memory though, one of these days I am going to forget how to get home(ok, not that bad maybe).

[Edited on 28-7-2010 by Hennig Brand]
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[*] posted on 28-7-2010 at 05:13


Quote: Originally posted by The WiZard is In  



Have stumbled upon the attached PDF

LLNL Small Scale Friction Sensitivity (BAM) Test



There was an attachment but (?) It didn't hook up.

However: thank you for checking into this. It's not easy to find this info. I usually can get a great deal of material but this has been a tough one.




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[*] posted on 28-7-2010 at 05:19


Quote: Originally posted by Hennig Brand  
BTW, does anyone here have any personal experience with Basic Lead Picrate, in particular its sensitivity to percussion. Any experiences or info welcome. All I know is the stuff I made makes great firecrackers, but I don't know if I'd trust it to initiate dynamite.


By themselves picrates probably would not be reliable initiators of dynamites (mind you, apparently even black powder charges have been used successfully to detonate some types of dynamite, but not reliably.) However, mixtures of picrates with potassium chlorate and other chemicals have apparently been used to detonate dynamites reliably (according to the inventor's claims.) The earliest proposer of such a method seems to have been Prudencio Castellanos, who used such mixtures to detonate both commercial dynamites as well as those of his own invention:

http://www.google.com/patents?id=2C9tAAAAEBAJ&printsec=a...

This is an interesting topic for which there appears to be rather little information. As Castellanos points out, his preferred percussive mixture was that of Designoble & Casthelaz:

http://www.google.com/patents?id=oqoAAAAAEBAJ&printsec=a...

The problem facing anyone who wants to put Castellanos' claims to the test is that his patent (or that of Designoble and Casthelaz, for that matter) does not address the issue of how are these chemicals mixed without blowing up in your face. Mixing potassium chlorate and potassium ferrocyanide is already scary enough, needless to say adding a picrate to the mix. According to the Designoble & Casthelaz patent, these mixtures are made pretty much like black powder, but no further details are given. It goes without saying that the chemicals must have been worked wet, then granulated and allowed to dry.



[Edited on 28-7-2010 by Blasty]
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[*] posted on 28-7-2010 at 05:21


Quote: Originally posted by Hennig Brand  


BTW just Google "Picric Acid and low order detonation" and lots of stuff comes up. Apparently even in large shells if not properly overdriven you will often get a low order detonation of the entire shell. Were you just messing with me a little bit Quicksilver? It must be nice to have a good memory though, one of these days I am going to forget how to get home(ok, not that bad maybe).

[Edited on 28-7-2010 by Hennig Brand]


No: honestly I haven't googled it. Just from reading, I simply thought of NC (w/ low order det) and frankly was curious.

I was thinking back when or if I did use TNP and was confusing it with TATB & TNA. It was an error on my part of not searching (& maybe having a senior moment there).




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[*] posted on 28-7-2010 at 06:27


Quote: Originally posted by quicksilver  
Quote: Originally posted by The WiZard is In  



There was an attachment but (?) It didn't hook up.

However: thank you for checking into this. It's not easy to find this info. I usually can get a great deal of material but this has been a tough one.



Yes 3X.

Try this

http://www.osti.gov/bridge/purl.cover.jsp?purl=/273797-vzcRJ...

The most interesting thing in it is that when
diaminepropane diperchlorate was tested it broke the ceramic plate.

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[*] posted on 28-7-2010 at 07:28


Excellent, Thank you.



"when diaminepropane diperchlorate was tested it broke the ceramic plate."

I think an "unknown" was: did this occur from a gradual weakening; a progressive deterioration or from the energy of the material itself?




edit:

Testing is such a detailed oriented aspect of science that (IMO) it takes a very detailed oriented mind to produce a paper with all bases covered. ...And then the reader is occasionally overwhelmed by the detail that unless acute organization is inherent within the design, some elements of the tests can be hidden from all but the most intricate search.

ps:
....need a paid subscription (of course...sigh) to snag MIL-STD-650. I once has access to the Library of Congress and didn't take advantage of it when I had it. That was a serious blunder I deeply regret. I could have gotten some of the most unique items imaginable & I took it for granted.....



[Edited on 28-7-2010 by quicksilver]




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[*] posted on 28-7-2010 at 07:42


Quote: Originally posted by quicksilver  


The Trauzl blocks I have seen appeared to be 1Kg as a 4"x4" cube with a 6mm hole. I hefted it and it seemed like 2lbs +. However I once saw a picture of one with a larger hole (it did appear 4x4 however). The lead should be pure; if it has tin or other elements the results will be thrown off & I don't know if it will expand without tearing or fragmenting. Making a mold for one would be pretty simple with 5 plates, some "C" clamps, and some "mold release" from hand swedging home-made bullets.



It could be any size, however, it dobe required that it is
large enough that the effect of the primer is not obvious.
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[*] posted on 28-7-2010 at 11:20


Quote: Originally posted by Hennig Brand  


BTW, does anyone here have any personal experience with Basic Lead Picrate, in particular its sensitivity to percussion. Any experiences or info welcome. All I know is the stuff I made makes great firecrackers, but I don't know if I'd trust it to initiate dynamite.



I believe the last person to have any personal experience with
basic lead picrate was killed in an accidental explosion last week.

I do have a copy of Capt. E. de W. S. Colver's 1918, 830 page
opus High Explosives.

He notes —

Lead picrate. Lead picrate exist both as a neutral and basic salt.
Neutral lead picrate, [C6H2(NO2)3O]2 Pb.H2O is obtained by
double decomposition of an alkaline picrate with lead acetate
in dilute solution. Of all the picrates, this salt is the most
explosive and most sensitive to percussion.

[C6H2(NO2)3O]2 Pb.H2O This yellow powder
explodes violently at 270o. This salt is, further, extremely
sensitive to friction and percussion in contradistinction to the
other picrates.

Captain Colver cites Will [Zeitschr. F. Schiess. U. Sprengst. 1906,
page 212] column 1. **
Urbanski column 2. Provide the following falling weight test values:


Picric acid 35 to 90 cm. ——-
Lead picrate 5 cm. 2 cm. 2 kg.
Fe III anhydrous —— 40 cm. 2 kg.
Iron 7 cm.
Copper 7 cm. 30 cm.
Zink 60 cm. no explosion
Sodium 80 cm.
anhydrous —- 19 cm.
Ammonium 80 cm.
Manganese —- 60 cm. 10 kg.
Chromium — 28 cm. 2 kg.
Nickel —- 40 cm. 10 kg.
Strontium — 17 cm. 2 kg.
Barium —- 2.5 cm. 2 kg.


Guttmann notes that the French ca. 1869 used potassium picrate and potassium
nitrate in powders for use in torpedoes, shells, as cannon and rifle powder.
“Designolle powders.” He notes (his book was published 1895) that “Designolle
powders have been abandoned.”

1894 VJ Feeny patented a mixture of:

ammonium chromate
potassium or sodium picrate &
ammonium picrate

As an explosive!!

There are a number of other picrates:
Aluminum
Cadmium
Cobalt
Lithium
Mercury
Potassium
Silver
Double salts

Esters of picric acid:
Trinitroanisol
Trinitrophenetol (ethyl picrate)
Phenyl picrate
Nitrophenyl picrate
Acetyl picrate

Other picrates/compounds of picric acid:
Guanidine picrate
Sodium peroxide derivative of picric acid
Benzene picrate
Napthalene picrate
Aniline picrate
Antracene picrate
Phenanthrene picrate
Phenol picrate
Acetophenone picrate
Picramic acid

Other than picric acid and ammonium picrate none of the others has found use.
Indeed even picric acid has been replaced by TNT &c. Ammonium picrate
“Explosive D” is used in armor piercing shells for ships gunnery. However, as
“guns” on ships are rapidly disappearing I would think the number of shells in
stock is adequate to meet demand.


** I own 3-volumes of this publication, however, not this year.
It dobe in German - bad. Script - terrible!


An Explosion Of An Appalling Character.

Report on the Circumstances attending a Fire and Explosion at
Messrs. Roberts, Dale & Co.'s Chemical Works, Cornbrook, Manchester,.
Gov. Rep. No. lxxxi.
Colonel V. D. Majendie, C.B.
In:—The Journal of the Society of Chemical Industry. Vol. VI. No. 12. December
31, 1887

THIS exhaustive report shows that the articles manufactured on the side of the
works where the explosion occurred, were picric acid, nitrate of lead, nitric acid,
hydrochloric acid (nitre cake and salt cake), tin crystals, tin solutions, nitrate of
iron, nitrate of copper, aurin, Manchester brown, Manchester yellow, lakes for
paper stainers and emerald green. Such raw materials as carbolic acid, sulphuric
acid and litharge, the litharge being used for making nitrate of lead, were all
present, the latter salt in very considerable quantity; some nitrate of strontium
was also present.

A fire commenced the catastrophe, this breaking out at or near the stove used
for drying the picric acid. The fire spread quickly, and in five or six minutes an
explosion followed, but not one of an alarming character. This explosion came
from the site of the picric acid stove as nearly as it can be located. It was
followed in something under a minute by a second explosion of an appalling
character, and attended with disastrous results in the shape of damage. One life
was lost.

There is little doubt that the fire was caused by the carelessness of a workman,
who was smoking. Several theories are advanced to explain the first and lesser
explosion, but the second, which was so disastrous, was in all probability due to
the blazing and molten picric acid coming in contact with the litharge placed in
close proximity and with the nitrate of lead and nitrate of strontium. It would at
once combine with these and form fearful explosives. Picric acid alone can
scarcely be called an explosive, but if it comes in contact even with plaster or
lime, it forms a picrate of high explosive character, and it is shown that picric acid
mixed with a little litharge in the cold, produces a mixture which explodes much
more readily than picric acid alone.

Finally, the precaution is urged, that in the manufacture of picric acid the
separation of the acid from all other substances or ingredients, contact with
which would be likely to produce under favorable conditions a picrate or
explosive mixture should be carefully seen to.

"At present picric acid and picrates appear to fall within the category of
'explosives,' and to be subject to the Explosives Act, 1875, only when they are '
used ' or manufactured with a view to produce a practical effect by explosion or
pyrotechnic effect. "

" In view of the present disaster," Colonel Majendie proceeds, "and of the results
of my experiments it will be a matter for careful consideration whether it is not
necessary in the interests of public safety to take advantage of the powers
conferred by the 104th section of the Explosives Act, 1875, and to extend the
definition of explosive to picric acid and all picrates, for whatever purposes
manufactured, and to apply the same provisions of the Act, subject to such
exceptions, limitations and restrictions as may appear reasonable. This point,
however, is one which, in the interests of the trade, as of the public, demands
the fullest and most careful consideration."

As to the storage together and in close proximity of the several substances which
resulted in the formation of such fearful explosives, Colonel Majendie stigmatises
it as the result of negligence.—W. S.


Curious —

By the action of ammonium sulphide on picric acid, salts of
picraminic acid are formed, and these are explosive if heated
rapidly. Lead picrate, one of the most dangerous salts of the
picrate series, is used in the silk industry; it renders the fabric
liable to spontaneous ignition.

[Weighted silk - the heaver silk was felt to be - the higher its
selling price. Though it may have been a dye.]
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[*] posted on 28-7-2010 at 13:20


-={ Please excuse OT remarks}=-


Wizard:

Those were the size I actually saw and held. When I saw a picture in a technical paper it looked the same as well. But that's not a big deal....

What I did find was hard copy of frictional (& impact) studies from the US Bureau of Mines (if you have a source on the web please let me know because I have looked and looked and never found the real collection. I always had to send away for the paper copies.) The one that's pretty interesting is USBoM "Frictional Studies" Tech. Paper 234, 1919. In it there are studies on friction testing, chlorates/perchlorates, and sensitivities to copper. MANY of the tech papers in the 200's are interesting from an energetic materials perspective.
The copper stuff is very intriguing. There is also an attachment of the commercial production of Cuprous acetylide and Cupric acetylide! The latter being usable in electric dets; the former being a curiosity that just too sensitive to make more than about 100mg. Pointed was a supposed agenda of not being forced to use copper (I) salts (CuO2) but yet copper (II) salts (like copper sulfate. Therefore it would be damn simple to make with copper sulfate, ammonia, acetylene & normal caution.

The correct material will be a deep orange-red: the cuprous material will be a black sludge which is just too sensitive. They use both chlorate and the copper example to demonstrate sensitivity. Cupric (or copper acetylide) is the old fashion bridge-wire coating and the friction ignition, "pull wire" used in various pull ignitors. The cuprous acetylide is not a touch explosive but not predictable enough to have a great deal of use aside from "throw-down popper toys.
If I had a way to scan it I would have posted it. I really enjoy the "Mines" papers. It's worthy of trying to find the USBoM collection.
NOTE: I checked the US Dept. of the Interior and they DO have some USBoM material (they did a few years back) but none of the old stuff.




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[*] posted on 28-7-2010 at 16:36


Quote: Originally posted by quicksilver  


What I did find was hard copy of frictional (& impact) studies from the US Bureau of Mines (if you have a source on the web please let me know because I have looked and looked and never found the real collection. I always had to send away for the paper copies.) The one that's pretty interesting is USBoM "Frictional Studies" Tech. Paper 234, 1919. In it there are studies on friction testing, chlorates/perchlorates, and sensitivities to copper. MANY of the tech papers in the 200's are interesting from an energetic materials perspective.



I have a not very good photocopy I made years ago. If you are
in the US of A, Depository Libraries have copies of Bureau
of Mines and other publications supplied to them by the Gov.,
assuming they have not de-acquisitioned them!

Or ask the Inter-library Loan librarian at your library to obtain a copy for you.

I recommend Bureau of Mines publication Bulletin 346,
Physical Testing of Explosives. 1931 146 pages.

I have a photocopy. Try this

http://digital.library.unt.edu/ark:/67531/metadc12516/

You maybe able to DL it as PDF, my request is pending.
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[*] posted on 28-7-2010 at 17:58


Thanks for all the info guys.

Didn't mean to give you a hard time Quicksilver, I am well aware that many of you guys know more than I, which is one of the reasons I really thought you were messing with me alittle(I was not upset by it though). You say you may of had a senior moment, I had you pegged as a smart younger adult, not a smart older adult(I assume you are implying that you are older with the senior moment thing). I'm not a kid, but I'm not old either, young adult I guess. As you can see I do have an adolescent enthusiasm for anything related to fire.

I made what I think is Basic Lead Picrate with the method in "the preparatory manual of explosives", I know it is not the best reference but it does have some interesting things in it. First put TNP in solution, use NaOH to convert to sodium picrate in basic solution, then add Pb(NO3)2 solution gradually+heat and stir, filter, wash, etc.(general summary I think) I wonder what I may have done wrong, mine is explosive as hell to a flame, but pretty damn insensitive to percussion. Maybe being the monohydrate makes it alot more insensitive? What would be the result if my TNP was alittle less than pure? I thought(not knowing for sure) that I might have been giving the impurities the slip when making the Picrate, but maybe not.
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[*] posted on 28-7-2010 at 21:38


Quote: Originally posted by Hennig Brand  

I made what I think is Basic Lead Picrate with the method in "the preparatory manual of explosives", I know it is not the best reference but it does have some interesting things in it. First put TNP in solution, use NaOH to convert to sodium picrate in basic solution, then add Pb(NO3)2 solution gradually+heat and stir, filter, wash, etc.(general summary I think) I wonder what I may have done wrong, mine is explosive as hell to a flame, but pretty damn insensitive to percussion. Maybe being the monohydrate makes it alot more insensitive? What would be the result if my TNP was alittle less than pure? I thought(not knowing for sure) that I might have been giving the impurities the slip when making the Picrate, but maybe not.


At the bottom of that same page where the preparation of lead picrate is given, there's a section entitled "Lead picrate initiating mixture". It is similar in general composition to the ones used by Castellanos to detonate dynamites back in the 1870s (picrate + chlorate + other chemicals.) The procedure looks fairly simple: the materials are worked wet, packed into "pellets" and allowed to dry (however, Castellanos says that such mixtures work better in loose granules, not pressed.) Since you seem to be able to perform such "noisy" experiments without much trouble, have you thought about trying it? (in a smaller scale than stated in the book would be wise) The author of that book claims it can work with RDX (yes, we all know he's not always reliable, but maybe he actually tested this.)
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[*] posted on 29-7-2010 at 05:32


Quote: Originally posted by The WiZard is In  

I recommend Bureau of Mines publication Bulletin 346,
Physical Testing of Explosives. 1931 146 pages.

I have a photocopy. Try this

http://digital.library.unt.edu/ark:/67531/metadc12516/

You maybe able to DL it as PDF, my request is pending.



Yea: I'm in the US. And that was a good tip. (I snagged it as a PDF) - Thank you.
Usually universities are tough to access. I had a damn hard time with our "local" one.
When my wife was working on her degree I was able to get a library card & it was "kid in a candy store" time.
I would love to see a thread in "REFERENCES" on sources people use to find materials. Because some people come up with obscure sources that I would NEVER have thought of.




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[*] posted on 29-7-2010 at 05:56


Quote: Originally posted by Hennig Brand  
Thanks for all the info guys.

Didn't mean to give you a hard time Quicksilver, I am well aware that many of you guys know more than I, which is one of the reasons I really thought you were messing with me alittle(I was not upset by it though). You say you may of had a senior moment, I had you pegged as a smart younger adult, not a smart older adult(I assume you are implying that you are older with the senior moment thing). I'm not a kid, but I'm not old either, young adult I guess. As you can see I do have an adolescent enthusiasm for anything related to fire.

I made what I think is Basic Lead Picrate with the method in "the preparatory manual of explosives", I know it is not the best reference but it does have some interesting things in it. First put TNP in solution, use NaOH to convert to sodium picrate in basic solution, then add Pb(NO3)2 solution gradually+heat and stir, filter, wash, etc.(general summary I think) I wonder what I may have done wrong, mine is explosive as hell to a flame, but pretty damn insensitive to percussion. Maybe being the monohydrate makes it alot more insensitive? What would be the result if my TNP was alittle less than pure? I thought(not knowing for sure) that I might have been giving the impurities the slip when making the Picrate, but maybe not.



HA.....I'm on the deeper side of 50! - getting close to social security age (which God willing I will see a few dimes from). I have had a very eclectic career in diverse vocations. I also was one of those guys who "lived in school". And honestly, I wouldn't fuck with you; it's too serious a subject. I just made an honest boo-boo. When you get a bit older, the second thing that goes is the memory.....

There were some in depth discussions (back about '06) about Normal & Basic Lead Picrate & most people pretty much agree that unless certain steps are taken, it's not a quality initiator: but it could be workable.

Legard (Preparatory Manual of Explos) does have some interesting stuff, it's just his citations suck. And therein lies the problem. If something interests you; you're generally stuck because his damn patent numbers are often incorrect.

Remember that many materials have a place in commercial production. Primers for firearms need to produce a strong flame spit, fuse-caps need to have a flame sensitive contact material, stab detonators need to have a very friction sensitive primary, & on and on.... Too often we examine a primary from the standpoint of "will it drive an explosive train?" when in fact, it may have more utility than just that alone.
Both Lead Picrate & lead styphnate will initiate a secondary; they just need a bit more mass than an azide but they certainly have utility.
If I could have found that old thread, the contributors had a great deal to say about the flexibility of picrates. It's worth hunting for but it's way back there.



edit:

And thank you for the complement but remember, anyone can make a mistake - so it's always a good idea to check info from internet conversations for veracity, accuracy in detail, & any omission.
I remember long discussions on alt.engineering explosives (UseNet) and some of the truly professional folks there occasionally made a typo or forgot something; even those who were truly gifted professionals. This is much too dangerous a hobby not to take anything with a grain of salt. If the guy gives citations for his perspective or has a reprint of an article, you're on much stronger ground but he could still misinterpret the idiosyncrasies of the subject. Some of the people I most respect have made an occasional omission or honest mistake.
I have really studied Legard's 2nd & 3rd edition & as much as I get down his case about the material, he's certainly someone who put some work into his books. ...But I would always double check the lab prior to getting into anything. It could have been his editor or he could have basically made a mistake which went over the heads of his proof-readers. Either way, his stuff isn't worthless, it's just a potential minefield - IF you don't double check. Remember he had the "copper fulminate" entry which was totally incorrect (& which I have always wondered about).
I believe it's vital that we as a group care that the information be as accurate as possible and honestly care for the safety of the other contributors.



[Edited on 29-7-2010 by quicksilver]




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[*] posted on 29-7-2010 at 09:43


Thanks for all the good advice, and information. I am going to try and track down some of the older picrate thread stuff.

Your still a young fellow yet, my Dad is getting close to 70.

Different peoples comprehension and interpretation of what they read or saw, even in a good reference, can vary greatly can't it. I'm always getting new, or expanded meaning from things I am reading again for more than the second time sometimes.
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[*] posted on 29-7-2010 at 11:27


Quote: Originally posted by Blasty  

The problem facing anyone who wants to put Castellanos' claims to the test is that his patent (or that of Designoble and Casthelaz, for that matter) does not address the issue of how are these chemicals mixed without blowing up in your face. Mixing potassium chlorate and potassium ferrocyanide is already scary enough, needless to say adding a picrate to the mix. According to the Designoble & Casthelaz patent, these mixtures are made pretty much like black powder, but no further details are given. It goes without saying that the chemicals must have been worked wet, then granulated and allowed to dry.



potassium chlorate and potassium ferrocyanide is already scary

Best mixed the same way porcupines make love....

Augrendre's White Powder [White Gunpowder]

K ferrocyanide - K chlorate - Sugar

...The respective quantities of the ingredients are then weighed
off, poured upon a sheet of paper, and intimately mixed with
the fingers or a feather......

Brannt-Wahl
Techno-Chemical Receipt Book
Henry Carey Baird & CO
Philadelphia 1917

{Maybe available from Google books.}



A Dictionary of Explosives
(Second Edition)
Lieut.-Col J. P. Cundill, R.A.
Entirely Re-arranged and Brought Up To Date
by Captain J. H. Thomson, R.A.
London HMSO 1895

I own an original it has been reprinted, or can be DL'd
from Google Books. Also Daniel's Dictionaire Des
Matières Explosives

9. IV2 Acme Powder, invented by Mr. Liardet, consists of a mixture of
picric acid, chlorate of potash, nitrate of potash, and tar. This explosive
proved fatal to its inventor. (Spec. No. 19,391, 23.10.1893)

[Mr. Liardet's powder is gon'a be a tough sell!]
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[*] posted on 29-7-2010 at 12:37


Sorry for my sort of gratuitous use of pictures, but I think this is maybe more the picture Quicksilver was looking for when he asked for a picture of the metal tears. Shot taken down the end of the barrel with the top off(barrel stood up).

Blasty, thanks for pointing out the Lead Picrate composition stuff, and the Wizard for elaborating. Porcupines in coitus, that is funny to think about.



[Edited on 29-7-2010 by Hennig Brand]

Barrel blasting (interior shot).jpg - 169kB
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[*] posted on 30-7-2010 at 01:59
Three Basic Igniters


Igniters based on derivatives of lead picrate

US1478429 See example 1 for synthesis of basic lead picrate which is the parent compound for the two more advanced derivative compounds below. IIRC this compound is a brick red orange color and extremely fine granulation crystals.

US2175249 See example 2 for one of the best "first fire"
low order detonating flash igniters , a superbly useful
and easily made compound , lead nitrato-bis basic lead picrate. The color of this one is bright yellow a bit coarser crystals.

US3293091 See example 4 for a similarly useful different compound, basic lead picrate - lead nitrate - lead chlorate tertiary clathrate, bright yellow crystals. As an interesting further note, a 4/16 azo-clathrate derivative can be made from this parent compound, and is a more powerful azo-clathrate than the 4/12 non-chlorate variant already described. The 4/16 azo-clathrate is experimental but a sample appears stable after several years of adverse storage conditions.

All of these compounds are excellent flash igniters for use as "first fire" compositions as a loose powder priming for fuse or electric ignition and readily undergo DDT low order in sub tenth gram amounts. All these materials are free flowing dense fine mesh crystals, not hygroscopic, and appear to be perfectly storage stable even at moderately elevated temperatures.



Attachment: US1478429_US2175249_US3293091.pdf (1.4MB)
This file has been downloaded 1077 times

In my opinion Legards books are trash. Caveat emptor.

[Edited on 30-7-2010 by Rosco Bodine]
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[*] posted on 30-7-2010 at 05:42


Quote: Originally posted by quicksilver  

Wizard:

Those were the size I actually saw and held. When I saw a picture in a technical paper it looked the same as well. But that's not a big deal.....



Your memory works, they were Small Trauzel Lead Blocks.

These blocks are used for testing detonators and are cylindrical
100mm. in height, and 100mm, in diameter. A hole is bored
in the block the exact diameter of the detonator and of such
depth that the top of the detonator is flush with the top of
the block. The tests are reported on the same form as that
used for reporting Trauzel lead blocks.


Munroe and Tiffany
Physical Testing of Explosives at the Bureau of Mines Explosives
Experiment Station Bruceton, PA.
Bulletin 346
1931
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[*] posted on 30-7-2010 at 05:55


The "flower-petal" tear in the metal has a certain significance re: the proximity. power, and speed of the det. I really have to find the information related to this as it's tucked away but aside from a forensics aspect, there is a variety of information that witness-plate punctures provide (the barrel's a damn big witness plate).

For those who do not have it, Roscoe posted the classic Dec 20 "Clathrate" patent, which may have enormous value to anyone who is seriously interested in primaries (US329091), It's this patent that is the basis of some great work & extremely interesting material.

US1478429 makes reference to nitrated cresol as a building block. Cresol is (IMO) much easier to nitrate than phenol but very difficult to obtain, which is a shame because there are quite a few things that employ it. The reagent-grade material is quite expensive & unnecessary, yet I have not found a source for anything but high-end cresol. I would really appreciate it if anyone who does know more about where to obtain same would post their experiences. {TNC is very close to TMP in a variety of tests.}



EDIT:
Re: those lead blocks, I wish I could post a picture because the one that I had looked like it fit a detonator. but I've read about ones that could be used for free materiel w/ tamping so the hole HAD to be bigger than 6mm.
I'm fairly sure a really accurate example could be home-made for just a few dollars.

[Edited on 30-7-2010 by quicksilver]




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