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Author: Subject: Picric acid: different instructions
quicksilver
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[*] posted on 8-8-2010 at 14:30


Quote: Originally posted by The WiZard is In  
This from a book I am not going to tell you the title
of as I own only 1 of its 2 (3?) volumes and I don't
need any competition looking for the missing volume(s).
However, I'll give you a hint - it is the book that
Fededoroff co-authored before he did PATR-2700.



Could that be.....
A Manual for Explosives Laboratories, 1943???




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Rosco Bodine
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[*] posted on 8-8-2010 at 15:15


Quote: Originally posted by grndpndr  
I cant ignore the respected forum voices any longer.I was evidently so invested in the now suspect data that I took as gospel what was printed in the data.Forum member Experience trumps paper/pencil in this case most others.How
badly underpowered is the plain PB picrate compared to simple HG fulminate approximately?
I regularly would use 1 gr of ful merc in these composite caps using PA.Mainly due to the abundance of mercury and nitric at the time not really based on need.Theoretically would a gram/gram and 1/2 pressed to 2.8 paper max density succeed in detonating PA pressed to less than max density '1.5 'to ease detonation somewhat and still reach 6500 mps
min.Experimentation may be in order unless theres experience willing to be shared, alothough as stubborn as I now appear...
Thanks for hanging in there fellas its appreciated.
Ive located some what seems to be dead soft lead metal that was used in a near century old home/more was salvage as new plumbing was installed.Seems to me the metal should be satisfactory its as soft softer than any lead ive ever encountered, far softer than even lead .22 bullets.I plan on imp a set of lead test blocks for detonator and the 10gr test of energetic det measuring the hole accurately w/water.Im also synthesising a few grams of K chlorate hoping to find some fine AL based paint to filter off the AL mesh.
One final question? In a gov interior dept paper where ww1 wartime PA was being surplussed I saw a eutectic mix with PA/Mononitronapthalene/Ammonium Nitrate.Aside from the basic energetics no further info was included.
No %,parts per, or wieghts were listed.Could it be Mononitronaphalene was used to initially coat the AN to prevent acid contacting the AN and causing damage or decomposition from the PA?No instructions were included for the composition at all nor were any time lenghths for storage mentioned.It sounds promising on the face of it but any advice would be appreciated.I would hope for a 6500 MPS det vel and higher with this energetic.Being cast it may require a booster of PA/ETN but the should be no problem. Thanks for all the help and patience.Pndr:D

That shrapnel shell is a trip,a holdover from the BP muzzleoader/breechloader era early 20th cent.Shrapnel was born in
late 17th cent and survived until the mid 18th cent.His initail design for muzzleloading artillery was basically a large riot gun.The original lead/iron ball contraption that held a # of large caliber balls at least the wieght of the rated cannon likely 2x the wieght of a normal Iron ball.Muzzleloaders of the era firing balls that wieghed from a light 6lber up to a med cal of 24 to 36 lber double that wieght in lead balls and thats a viscous mass killer a single large diameter ball passing through several ranks x 100 balls plus.Later shrapnel was considered as not being what it was originally named for but any piece of ballistic metal from most any source/size steel artillery shell or grenade splinter etc.

Synthesis notes like those of a snipers shot logbook detail almost every imaginable variable from weather to equipment.Down to humidity,mirage, cloud cover,pulse,respiration all can affect shot placement or synthesis results.Where I used to be a compulsive notetaker the only notes I make are those made prior to the start of the synthesis a habit I need to break.


With regards to the volume efficiency, and "critical mass" of initiators, there is a transition point for a given diameter, where the "self-accelleration" produces a
"bump" in the output that corresponds to the transition from low order to high order detonation. The difference between mercury fulminate and basic lead picrate, or normal lead picrate, or lead styphnate, or lead nitrato bis basic picrate, or basic lead picrate - lead nitrate - lead chlorate is a difference between about an order of magnitude roughly somewhere between 10 and 20 depending on diameter. By that I mean if the "bump" in output for mercury fulminate is around about a quarter gram quantity in self-accelleration, then the corresponding "bump" in the output for those other materials is in the range of two and a half to five grams depending on diameter. That's a ball park "guess" because I have not done a careful systematic study and charting of this transition based on self acceleration of materials which demonstrate low self-acceleration. My interest has been a whole lot more directed to materials which show an even better self-accelleration than mercury fulminate. There are ways you can improve the sluggish self accelleration of those primaries that are more generally useful as "primers" rather than initiators, by combining them with more rapid self-accellerating materials and / or using strong confinement, which helps "kick" them towards the transition to high order at an earlier point. Thereafter you still must have an additional charge quantity beyond the amount that is "burned off" during the "runup to high order", the additional quantity which will be the actual
"work performing portion" transferring its high order impulse to the target base charge to be initiated. I haven't seen this described anywhere in any literature, but this is simply my observation and interpretation of experiments. Some primaries are fine for primers, for "flash igniters" and they are dependable as "first fire" and low order compositions. Any "relative brisance" sort of figure would likely not reflect performance of such a material being used in its usual mode and quantity where brisance is not much of an aspect of that low order scheme. That "relative brisance" quantity is probably from a test where the material was not in small quantity undergoing self-accelleration, but was being used as a relatively large sample secondary charge and fired by a separate detonator. So the "relative brisance" of a material being tested under conditions different from its ordinary mode of operation does not provide useful information about the "unboosted" performance of the same material in smaller quantity.
Yeah if you put ten grams of basic lead picrate in a test block and detonate it with a compound detonator, the whole ten grams goes high order at once and has significant brisance. But if you simply stick a fuse in the sample, five of the ten grams may be burned off in the "runup" which was circumvented entirely by the
use of a cap to get it going. I hope this helps makes sense of how test data can be misleading unless you have all the details factored into interpreting the tests.


[Edited on 9-8-2010 by Rosco Bodine]
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[*] posted on 8-8-2010 at 18:23


Quote: Originally posted by Rosco Bodine  
" primaries that are more generally useful as "primers" rather than initiators "

You lost me there , if there be a semantic distinction in definition. I take it
from the implied context that " primer " you take to be what is set off by
fuze flame or heated wire, and " initiator " that subsequent part of the train
most proximately in contact with the main charge ( assuming no booster ).

Cap constituent formulation is very much an empirical art. Your layer cake
design will differ from another's jelly roll concoction. Field testing is the only
validation that matters.

.
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[*] posted on 8-8-2010 at 19:03


It is a bit of semantics, but generally a "primer" references a primary "explosive"
which would be used more as a pyrotechnic igniter composition involving an explosive combustion which is of lower order, as in the case of an ammunition primer, producing a sudden flame as for igniting gunpowder, but not directly producing a detonation.

On the other hand an "initiating explosive" or "initiator" in that context, would
be associated directly with only high order detonation, not a burning or pyrotechnic ignition effect, but only producing a detonation effect.

For some of the compositions which may be used for either purpose depending on quantity, composition, and what is the device operated upon, those other aspects will make the distinction whether the material is functioning as a primer
or as an initiating explosive. And to confound the semantics further, in some cases the same material may be both a primer and an initiating explosive,
so what is there to be confusing :D
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[*] posted on 8-8-2010 at 23:17



Thanks for your patience Roscoe.I understand your reasoning Roscoe and of course appreciate the help.layer cakes were mentioned.some are concerned with the finest ingredients, smallest size.If I make one my concern is it works well det difficult HE's uses OTC ingredients not nescessarily how big it is.Again thanks for your input,I particularly appreciate the OTC synthesis ofetn posted for common energetic secondarys.Sincerely pndr:)

[Edited on 9-8-2010 by grndpndr]

[Edited on 9-8-2010 by grndpndr]
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[*] posted on 9-8-2010 at 01:20
pentanitronaphthol (and possible salts ?)


Here's an off the beaten path material that may be of interest. I have never made this one and references on it are obscure to non-existent. Hey Axt ! Hey Philou ! Hey Engager ! Lookee here what I found :D

Attachment: US1419027 pentanitronaphthole.pdf (115kB)
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[*] posted on 9-8-2010 at 08:00


Interesting patent,thanks for bringing it to my/our attention.One of my first reactions upon reading its MP
and acidic nature was as a possible eutectic with PA.
Im sure it sounds as if Im near compulsive as regards PA but I assure you im also interested in other inexpensive OTC energetics.From those suitable for cutting steel to ditching dynamite.
And simple primary energetic materials capable of detonating even difficult secondarys.Simply put a main requirement is would this be relatively simple and inexpensive to synthesise using simple household and labaratory equipment and mainly OTC chemicals.:)

All theoreticall of course!:D

[Edited on 9-8-2010 by grndpndr]

[Edited on 9-8-2010 by grndpndr]
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Rosco Bodine
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[*] posted on 9-8-2010 at 09:30


It looks like a variation and extension upon the "catalytic process" of aromatic nitrations using mercuric nitrate to form an unstable addition compound as an intermediate in the nitration. Picric acid is made from benzene, and trinitrocresol is made from toluene via the "catalytic" process (not precisely catalytic although the mercuric nitrate is regenerated). Evidently naphthalene also forms a partially oxidized nitroaromatic compound more easily nitrated to a penta nitro derivative than is usual rigor of nitration required for the better known tetranitronaphthalene, and as a bonus the pentanitro compound is more powerful and has the acidity of a nitrophenol. Hmmmm, that's interesting because it may be something like tetryl in terms of power, while being thirsty for compounding with a metal like lead which should result in a primary having considerable impulse, probably greater than the impulse of styphnate or picrate salts. Such a "nitroaromatic acid" could be a useful substrate for various salts and double salts. PATR Vol.8 N-20 reports one research paper done by A.H. Blatt & F.C. Whitmore OSRD 1085, 74 (1942) , which was a WWII "scientists at war" kind of project having many branches one of which was the Manhattan project. And the fellow who invented and patented the compound is a recognizable name in the field, who wrote a little handbook we all know so well as COPE. So this is very intriguing. Is it a mono or di acid ? Googling the authors names for the OSRD reference turns up no hits for me, so that article must be buried in obscurity somewhere possibly hardcopy archived in a box and never yet digitized. We ought to fix that. :D Do we know any librarian types who are given to scavenger hunts for obscure historical material ?
Hmmmm, let me think .....any wizards around here ? Or just pretenders ? :D Now there's a document request, and I'll even add a pretty please with sugar on it.

[Edited on 9-8-2010 by Rosco Bodine]
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[*] posted on 9-8-2010 at 10:01


Quote: Originally posted by Rosco Bodine  
Googling the authors names for the OSRD reference turns up no hits for me, so that article must be buried in obscurity somewhere possibly hardcopy archived in a box and never yet digitized. We ought to fix that. :D Do we know any librarian types who are given to scavenger hunts for obscure historical material ?
Hmmmm, let me think .....any wizards around here ? Or just pretenders ? :D Now there's a document request, and I'll even add a pretty please with sugar on it.



A v/ very quick search turns up a reference to :—

A H Blatt Compilation of Data on Organic Explosives
O.S.R.D. 2014 (1944)

This evening I'll spend some time look for whatever turns up.
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[*] posted on 9-8-2010 at 10:08


Thanks Wiz ...I've been searching for two days. Evidently there was a declassification and reindexing of OSRD material under new PB numbers
so the catalog is required to cross reference original numbers which are
basically a "lost" filing system for the previously classified war related research. These research papers, there are about 600 odd thousand of them which were government funded research are now boxed in hard copy form in several historical archives. Whether or how much of it has ever been scanned is unknown. I think I read somewhere they spent nearly a trillion dollars to get those research findings.

[Edited on 9-8-2010 by Rosco Bodine]
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[*] posted on 9-8-2010 at 10:15


Quote: Originally posted by Rosco Bodine  
PATR Vol.10
N-20
reports one research paper done by A.H. Blatt & F.C.
Whitmore OSRD 1085, 74 (1942) ,




Vol. 8 N20 works for me.

I do not believe L Davis ever worked for the Gov. so you
are not going to find any OSRD &c. pubs w/ his name on
them.
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[*] posted on 9-8-2010 at 10:26


Yeah Vol.8 N-20 is correct. Right , Davis patented the material earlier, but the followup testing, review and research I would guess came later via OSRD.
There may be something in the journals subsequently or it may have fallen through the cracks and disappeared into obscurity.
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[*] posted on 9-8-2010 at 12:55


Quote: Originally posted by grndpndr  

And simple primary energetic materials capable of detonating even
difficult secondarys.Simply put a main requirement is would this be
relatively simple and inexpensive to synthesise using simple
household and labaratory equipment and mainly OTC chemicals.:)


WiZard-of-Id-Better-Off.jpg - 107kB
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[*] posted on 9-8-2010 at 13:12


Quote: Originally posted by Rosco Bodine  
IPATR Vol.8 N-20 reports one research paper done by A.H. Blatt & F.C. Whitmore OSRD 1085, 74 (1942)



Department of The Army Second Army-Navy Research Conference
of New High Explosives
1 November 1949

Byda AHB was editor of the 1 and 2nd Collective Volumes of
Organic Synthesis.

Blatt.jpg - 345kB
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[*] posted on 11-8-2010 at 22:43


Quote: Originally posted by Rosco Bodine  

As for detonating PA with basic lead picrate, the problem is scale. It can probably be done if you can accept a "cap" being 5/8" diameter and 6" long.

If a marginal primary is being considered for use, to attempt initiation of a nitrophenol type base charge, then probably it is better to use a base charge of styphnic acid because it is more sensitive to initiation and almost as powerful as picric acid. It is also possible that a small increment of the styphnic acid like a quarter gram, could be used as an intermediate between the initiator and a picric acid base charge, or a composite of styphnic and picric acid may have enhanced sensitivity, making it easier to initiate.


I was remiss in posting an example of the use of an "increment" of a more sensitive intermediate secondary to decrease the amount of initiator required. I found an example of this where a small charge of picric acid is used as a booster for a TNT base charge in a compound detonator.

US1502754 composite picric acid - TNT compound detonator

Also is attached another detonator configuration patent showing a general design that is readily adaptable for larger compound detonators for example as might use a test tube for a housing. There are available polypropylene test tubes of 5 or 6 ml capacity and approximately 3/8" ID which are adaptable for such use.

US2214721 DDNP-KClO3 75-25 PETN base detonator

US2842059 Special Capsule Design for Detonator


Attachment: US1502754 composite picric acid - TNT detonator.pdf (196kB)
This file has been downloaded 512 times

Attachment: US2214721 DDNP-KClO3 75-25 PETN base detonator.pdf (206kB)
This file has been downloaded 736 times

[Edited on 12-8-2010 by Rosco Bodine]

Attachment: US2842059 Special Capsule Design for Detonator.pdf (283kB)
This file has been downloaded 578 times

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[*] posted on 15-8-2010 at 06:56
efficiency of detonators


Here is a reference which may be useful for general information, even though it doesn't relate specifically to picric acid base charges, it does show the effect of some of the same variables as would tend to be generally true.

Attachment: Efficiency of detonators.pdf (759kB)
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[*] posted on 13-12-2010 at 01:55
The Sand Test Storm and Cope 1916


The sand test for determining the strength of detonators
Christian George Storm and Willard C. Cope 1916

http://sciencemadness.org/scipics/The_sand_test_for_determin...

Google books link
http://books.google.com/books?id=EdfHxMJtIBUC&printsec=f...

A bit of interesting history about Mr. Cope, is that he was an explosives expert who was involved in the construction of the Panama Canal. He was also an expert witness called by the official inquiry regarding the Halifax Explosion of Dec. 6, 1917. The Halifax Explosion was a result of a harbor collision between ships causing fire aboard one of the ships which was loaded with munitions and exploded less than an hour later, killing 2000 people and injuring 9000. Fragments of the munitions ship S.S. Mont Blanc were scattered for miles by the tremendous explosion.
2653 tons of munitions were involved in the explosion and most of that cargo was picric acid.

http://en.wikipedia.org/wiki/Halifax_Explosion

[Edited on 13-12-2010 by Rosco Bodine]
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[*] posted on 13-12-2010 at 13:05
K.I.S.S. extremus — The nail test for detonators


US Bureau of Mines 1915

http://tinyurl.com/266pkr5Text
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[*] posted on 13-12-2010 at 13:52


Aaahhhhh; beat me to it.


Personallly I have no problem with the idea of basic lead picrate initiating real reagent grade picric acid.




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[*] posted on 13-12-2010 at 14:48


It isn't impossible for basic lead picrate to initiate picric acid, it would just require
an inconveniently large amount and special confinement in a relatively large detonator in order for it to be possible. So it is not technically infeasible, it is simply an impractical and awkward arrangement compared to more efficient alternatives. It may well be that an increase of sensitivity to initiation can also be obtained depending upon the solvent and the method used for crystallization. It is not unusal for different crystal forms to be possible and some may be more sensitive than others.
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[*] posted on 14-12-2010 at 06:15


I had just recently bought a "add-on" for taking pictures via a microscope but it wasn't up to par. So I couldn't get what I really wanted, which were quality pictures (w/ sizing lens) of alteration in crystal structure (especially in the "picric-genre'"). Sometime back we had a discussion on the alteration of the crystal in Basic Lead Picrate (& some other materials as well) and there was some patent material in alteration of (IIRC) lead styohnate into granular cuboids. There are also growth procedures to lead picrate;normal & basic, that can make them substantially larger, well formed, & possibly more sensitive Testing their utility would be pretty interesting.



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[*] posted on 14-12-2010 at 06:19


Actually it was the picric acid and styphnic acid that I was more thinking about in recalling perhaps some reference that more sensitive crystals easier to initiate were possibly gotten from solvent crystallizations other than water,
alcohol may have been one of them. I never tested this
to see if there is any significant difference in sensitivity
for organic solvent crystallizations.
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[*] posted on 21-12-2010 at 11:15


Quote: Originally posted by Rosco Bodine  
Quote: Originally posted by grndpndr  
I cant ignore the respected forum voices any longer.I was evidently so invested in the now suspect data that I took as gospel what was printed in the data.Forum member Experience trumps paper/pencil in this case most others.How
badly underpowered is the plain PB picrate compared to simple HG fulminate approximately?
I regularly would use 1 gr of ful merc in these composite caps using PA.Mainly due to the abundance of mercury and nitric at the time not really based on need.Theoretically would a gram/gram and 1/2 pressed to 2.8 paper max density succeed in detonating PA pressed to less than max density '1.5 'to ease detonation somewhat and still reach 6500 mps
min.Experimentation may be in order unless theres experience willing to be shared, alothough as stubborn as I now appear...
Thanks for hanging in there fellas its appreciated.


I have deleted a majority of my own post for brevitys sake and keep this post somewhat on topic.
Roscoe's reply verbatim

"With regards to the volume efficiency, and "critical mass" of initiators, there is a transition point for a given diameter, where the "self-accelleration" produces a
"bump" in the output that corresponds to the transition from low order to high order detonation. The difference between mercury fulminate and basic lead picrate, or normal lead picrate, or lead styphnate, or lead nitrato bis basic picrate, or basic lead picrate - lead nitrate - lead chlorate is a difference between about an order of magnitude roughly somewhere between 10 and 20 depending on diameter. By that I mean if the "bump" in output for mercury fulminate is around about a quarter gram quantity in self-accelleration, then the corresponding "bump" in the output for those other materials is in the range of two and a half to five grams depending on diameter. That's a ball park "guess" because I have not done a careful systematic study and charting of this transition based on self acceleration of materials which demonstrate low self-acceleration. My interest has been a whole lot more directed to materials which show an even better self-accelleration than mercury fulminate. There are ways you can improve the sluggish self accelleration of those primaries that are more generally useful as "primers" rather than initiators, by combining them with more rapid self-accellerating materials and / or using strong confinement, which helps "kick" them towards the transition to high order at an earlier point. Thereafter you still must have an additional charge quantity beyond the amount that is "burned off" during the "runup to high order", the additional quantity which will be the actual
"work performing portion" transferring its high order impulse to the target base charge to be initiated. I haven't seen this described anywhere in any literature, but this is simply my observation and interpretation of experiments. Some primaries are fine for primers, for "flash igniters" and they are dependable as "first fire" and low order compositions. Any "relative brisance" sort of figure would likely not reflect performance of such a material being used in its usual mode and quantity where brisance is not much of an aspect of that low order scheme. That "relative brisance" quantity is probably from a test where the material was not in small quantity undergoing self-accelleration, but was being used as a relatively large sample secondary charge and fired by a separate detonator. So the "relative brisance" of a material being tested under conditions different from its ordinary mode of operation does not provide useful information about the "unboosted" performance of the same material in smaller quantity.
Yeah if you put ten grams of basic lead picrate in a test block and detonate it with a compound detonator, the whole ten grams goes high order at once and has significant brisance. But if you simply stick a fuse in the sample, five of the ten grams may be burned off in the "runup" which was circumvented entirely by the
use of a cap to get it going. I hope this helps makes sense of how test data can be misleading unless you have all the details factored into interpreting the tests.


[Edited on 9-8-2010 by Rosco Bodine]


With the above in mind 3.75grains of PB picrate was detonated in a layer of tin foil(enclosed) by means of heat from a hotplate with an aluminum plate .110 thick to protect the H/P element.The detonation was very energetic.Not having a method to measure decibels Id say it was equivalent to a .32 automatic pistol fired indoors.The Aluminum plate that absorbed the untamped detonation dented the approx 1/10in thick(unknown alloy) AL plate to a diameter of perhaps 3/4 in and using straightedge and feeler gauges,
as I dont have to hand a depth micrometer. A rough measurement indicates .080 thousandths dent depth.Wouldnt that indicate a detonation? And a detonation of 3.75grains (243 mg) Of 'KEWL' PB picrate.I prefix the PB picrate with KEWL as its made using a KEWL's recipe or synthesis along with some less than kind,mature observations(perhaps warranted)by some ,members.TNP/Methanol/Pb0,although an excess of TNP was used but no other additives such as nitrates / chlorates/Al were incorporated.Im curious as to the explanation for such a vigorous reaction.With respect . sincerely,grndpndr.

PS;In the interests of complete information, I strongly suspect this lead picrate was made using a poor quality TNP as the TNP itself doesnt det from a hammer blow.Steel on steel with the TNP enclosed with foil as well.
Also the alleged PB picrate isnt sensitive to friction or impact of the type described.Just a few sparks from a hammer blow!?

[Edited on 21-12-2010 by grndpndr]

[Edited on 21-12-2010 by grndpndr]
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[*] posted on 21-12-2010 at 13:02


You will get low order detonation even below 100 mg. Think of that as DDT for low order. It could take tens of times more to make the transition from low order to high order.
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[*] posted on 21-12-2010 at 18:54


I appreciate the insight Roscoe. Thanks!

PS; It would be interesting/enlightening to test a variety of primarys using the same test plate,duplicating the first test parameters.:D

[Edited on 22-12-2010 by grndpndr]
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