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quicksilver
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IF we are just talking about yield levels then phenol is your choice. If such is not available ASA is fine. But any route than direct nitration will
not get you what you may expect. This was the whole issue with R-Salt & RDX; the problem there being the precursors (acidic anhydride) being too
tough to obtain for the synthesis of choice.
Plant-level synths are MUCH more efficient than anything one can do in a lab. The recycling of acids being a major issue. That's why items like CL-20
are so expensive.....they can't be plant produced via the re-cycle of their expensive precursors. The military STILL pays top dollar for CL-20. IF we
were to deal with plant-level TNP one could even start with benzene. Plant-level TNT is so inexpensive that costs are ridiculous. That's why we still
use it today.
Most fellows interested in energetic materials skip the reading about plant production, thinking they could never emulate it or compose a lab that
would function in that medium. But actually, it can be done on a lab-dedicated level. It's a great hassle, yes. But IF the idea is to have enough TNP
to make sand castles with - it could be done. Most folks could experiment till boredom with a few ounces. 
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Rosco Bodine
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The possibility of using ammonium nitrate or sodium nitrate or magnesium nitrate, dissolved in azeotropic nitric acid and added dropwise to a sulfuric
acid solution of the sulfonated precursor derived from aspirin could be an improvement in terms of producing a lower viscosity nitration mixture. It
would be easier to make addition of the nitrating agent as a flow control of liquid, than to
use an auger type feeder for making addition of a solid nitrate. It also seems possible there could be catalysts for the nitration which would allow
for nitration in more aqueous systems where nitrosylsulfuric acid is not an
inherent byproduct or intermediate. IIRC one of the things I thought about but never tried was instead of using a sulfonated intermediate, to
alternately attempt a nitroso intermediate and then nitrate that, without any sulfuric acid involved at all.
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Hennig Brand
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I don' t completely understand the pros and cons of using solid nitrates dissolved in azeotropic nitric acid or any nitric acid which is less than
anhydros, But I do understand from experience the great advantages and facility of using a liquid nitrating agent instead of a solid nitrate. I have
also read the parts in Chemistry of powder and explosives and Urbanski relating to Picric Acid and they both talk of expedient methods by allied
governments to manufacture Picric Acid, and in them is talk of using weak nitric acid and nitrates(sodium nitrate usually), which was workable and got
results but was described as inferiour I believe to concentrated acids. This in no way means that it is not possibly very useful to the hobbiest, if
only as an expedient method. Rosco and others have pointed out, and proven that the methods using nitrates can be very fruitful and successful indeed.
I know this has been discussed here and elswhere at least a couple times, but if someone with some practical knowledge(actualy has done it) could
oblige me and explain a little about detonating Picric Acid say in a compound cap(or other), I would appreciate it. I have samples that can be set off
with quick snap of a hammer on an anvil, to give an idea of what I am working with.
I was also under the impression from reading other posts that AP was not all that great at setting off TNP, is this true? How much better would HMTD
be for this, if any? Or should I try for something else by way of a primary(I have been hoarding a bit of mercury which could be used I guess, but I
don' t think it will provide any performance enhancement). What does the hammer blow test tell about a TNP samples ability to be initiated by
primaries for example, and under what conditions.
From someone with experience, some detail of possible pitfalls would also be appreciated. I feel that I could make it work no problem now, or at least
"after a fashion", but words of experience would probably provide insite into things overlooked by me.
Here is something that may be of a little interest to some. It looked a little shoddy at first but it is supposed to be from a reputable company, and
labled as expedient proceedures(which can look less than professional by their very nature anyway).
http://www.dtic.mil/cgi-bin/GetTRDoc?AD=AD410390&Locatio...
[Edited on 22-6-2009 by Hennig Brand]
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Rosco Bodine
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Anhydrous acid is not needed for TNP. Use of solid nitrates is not just a hobbiest expedient method. Some solid nitrates have a greater nitrating
effect than nitric acid, in anybody's lab. Urbanski charts the nitrating activity of various nitrates and it is not a fixed rule but can vary also
with the thing being nitrated.
There is further I should share concerning the general "search for truth" by science or philosophy or religion with regards to intellectual honesty.
It has been observed by me that there is a measure of agnosticism found in the humility of honest religious people, honest scientists, and honest
philosophers, which is an intellectual honesty about the unknown, including things honestly recognized as probably being not knowable.
As an experienced observer who is familiar with analysis, mathematical proof, logical deduction, and reasonable conclusions, which are required for
valid thinking, I personally know that a measure of agnosticism must
be present to keep ones feet on solid ground with respect to the ethic of intellectual honesty. The pseudo-certainty which emboldens atheists to
proselytize a falsehood that science and religion are somehow at odds, venturing the false "belief" and proposition of atheism that science has
exclusive claim to reason and rational perception and other noble virtues, while religion does not or cannot, and is only "superstition" has always
been observed by me as lacking that reserve of agnosticism found to be always present with those who are intellectually honest. The certainty of
"belief" of atheists about something which no mortal could be certain, even to an extreme of their venturing to redefine history which may not fit
their belief so that history becomes more politically correct with regards to their biased view, is an indulgence not even allowable to science.
Ironically, for their lacking the humility of agnosticism
any atheist has a bias which is intellectually dishonest and
provides that false confidence of youth which emboldens their ridicule of their elders (and their betters) for being
superstitious. Scientifically speaking, how do any of us know
that the entire realm of things which we know is not itself a
"science experiment" on a cosmic scale in which we are
unwitting participants ? If there can be no certain and definitive answer to that question, then what intellectual superiority could actually exist
for anyone having the audacity to presume their own unproven knowledge or belief about any "meaning of life" kind of stuff is somehow an ignorance
which gives them license to chastise people of faith as being "superstitious" or "unscientific". There is an inherent non-sequitur there which must be
denied by all
irrational fanatics whether they are religious fanatics or
atheist fanatics or anything intermediate. Whether this same
rule also applies to any extra-terrestrial fanatics or extra-dimensional fanatics not covered by the preceding limits
would of course be pure speculation
Science and philosophy and science and religion are inextricably linked in the purpose of seeking greater knowledge and if that fact doesn't reside
comfortably
with some individuals belief preferences, then they lack maturity. There is simply no honest intellectual basis
for bias and ridicule there concerning "superstition" than
there is for racial or gender bias. Men from earth in a spacecraft orbiting the moon were overwhelmed by the experience of what they were seeing and
it was near Christmas as I recall many years ago when they got on their radio and began transmitting back to earth what they felt
compelled to be reading ......from Genesis. My family was
directly involved in that Apollo mission so I have a special
insight concerning the linkage between science and religion.
[Edited on 23-6-2009 by Rosco Bodine]
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Hennig Brand
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What I meant in my first sensence of my last post was that I did not understand all the implications of using nitrates, advantages or disadvantages. I
am aware that you have used solid nitrates to great effect, and was not questioning this whatsoever. It does say in some of the more reputable books
that the use of nitrates and weak HNO3 was more of an expedient method for certain goverments at certain times, at least from phenol when producing
Picric Acid. I just added that for edification and by no means was trying to discredit the nitrate methods. I did say in my last post and will repeat
that you have been very successful in your use of nitrates to produce Picric Acid. I will say that those methods are less straight forward (in my
opinion), as far as being a more difficult nitration proceedure and more difficult to purify. I would say that it is a great advantage to not need to
acquire HNO3 which could easily more than make up for any added difficulty in using the nitrate. You personaly probably have the proceedure down to
such an exact science that the difficulties are probably precieved as much less, as well you have NaNO3 which is far superior to both KNO3 or NH4NO3
in function in a ASA nitration(I think?)
In a lot of ways what I wrote was an appeal for more exact information from others. For instance I wouldn' t mind hearing a bit about the greater
nitrating effect of some nitrates, if you wouldn 't mind ellaborating a bit.
After looking it up it appears that the word expedient doesn' t necessarily mean inferior at all .(maybe in a military context it would be different).
It mostly means to me to carry something out in the most advantagious way, by way of short time and good results and is an adaptation usually of the
usual techniques.
I don' t think you would tell me to convert my HNO3 into a nitrate prior to nitration, would you? I know this is probably a rediculous thing to say
but I thought it might make a point.
I would judge that any technique using ASA to produce Picric Acid could be aptly called expedient. I do feel that these procedures can be very useful
and get good results, and am not trying to take anything away(it is just not seen as the usual methods by our "main chemical institutions", or most
desirable if one had every chemical and convenience at their fingertips at industry prices). Maybe for the hobbiest ASA routes are the norm, and
others the expedient?
[Edited on 23-6-2009 by Hennig Brand]
[Edited on 23-6-2009 by Hennig Brand]
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Rosco Bodine
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Some of your questions would be answered already in the earlier posts in this same thread and in other threads, I can't really go back and review it
all right now to more specifically answer your posts. Do your homework and most of what you are looking for is already there. Ordenblitz did a good
photo documentary and there is another thread where
some temps and times were very specificially noted. That
specificity is accurate and important for reproducing the results. Get sloppy and results could vary, unpredictably.
[Edited on 23-6-2009 by Rosco Bodine]
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Hennig Brand
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You are correct that I like many others should do more reading and understanding, rather than talking. There is however a recognized process in
learning by which every time a topic is revisited it tends to be done in a little greater depth, and new ideas come fourth as a result of building on
the old. I apologize for boring you.
I do agree with your opinions about athiests and agnostics, although have never realy verbalized it quite as well as I feel you have. It does seem
realy dishonest to take a rigid fanatical view about religion and science most of the time. I have seen in many who profess to feel this way, what I
believe to be a desire to be pugilistic, and threatening to others about something that is personal and emotional for many. This seemingly irrational
anger/aggression towards the possibilty of something not understood and possibly greater than what we are could be just the way their fear is being
manifestated. Human emotions come out in a lot of strange ways, and I would say it is at least important to try and be honest with ourselves about
what we are realy feeling(I have gone through some of these same processes myself at different times). The thought of uncertainty just plain makes
some people really nervous to the point of acting irrationally. I am not saying that there isn' t some athiests that are being fairly truthful about
their feelings. The truth is that most people(especially with out science training or backround use much emotion in decision making(I believe), and
the more emotional charged the issue the less rational processes are used effectively, in some extreme cases little rational thought is used at all.
There was some really good stuff in a Time magazine a couple years ago about the brain and how it works in different situations.
[Edited on 23-6-2009 by Hennig Brand]
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Rosco Bodine
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I applaud your perspicacity for recognizing that there are those among us who would push other peoples buttons
for sheer amusment, as if they were the walking incarnation of the left hand of an accordion player,
and the world was their polka
And your posts did not bore me, I just don't have time
right now to research the old posts or I would be more helpful.
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quicksilver
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@ Hennig Brand
I have a source for you....
ADVANCED PRACTICAL ORGANIC CHEMISTRY, J. Leonard, Lygo, & Proctor (especially CH 16 "What To Do When Things Don't Work) - saved my efforts many a
time...
It's inexpensive & many folks here have read it. I still have mine & that was a 1st edition. I go back to it every so often as it answer
things like this so concretely & gives examples of how to set up an example for the use within a common lab. It's a paperback (cardboard back)
& inexpensive. You'd love it; as it doesn't start off with useless material.
MANY people begin to turn to undergrad-university textbooks in this hobby as the answers for the "little things" are readily available. What's more it
teaches you how to find the answers! Your horizons will expand as the thirst of idiosyncratic info is always there and patents may lead you astray due
to the "trade secrets" phenomenon! My other suggestion when searching these things out is to look toward chemistry practiced in the turn of the
19-20th century because that is what we often practice in hobby chemistry (unless we have a grad background).
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grndpndr
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Ive been a fan of the late19th early 20th century literature
not as cutting edge perhaps which is an adavntage for me
frankly.Id love to be capable of mastering or even an understanding of cutting edge technology but late 19th/earlt 20th is difficult enough.Might I be
able to find the book you referenced online for the downloading?Hope springs eternal.Failing that a source of the book+ approx cost?
Kill 2 birds with one stone (dual thread) a recent experiment by someone im communicating with desires to use TNP in a composite cap, possible
booster.he related 1gr AP failed to detonate 1gr TNP using al tubing with epoxyed endcaps.Both were pressed to 1.2 gr cc3.That should be optimum for
AP but lightly pressed for picric acid thus making TNP easier to detonate though with less VOD than optimum of 1.6-1.7 gr cc3? personally Ive never
had faith in AP seeing and hearing of to many failure as well as instances where quite large quantities of AP were used in fac t Inordinate amounts to
achieve detonation both in caps and as booster charges.Never having been a fan of AP its my suspect as the TNP appears to be good TNP by all the
recognized tests.Hammer /anvil det.Melting to decomposition and deflagration with a small pop with black soot byproduct.a result of testing a known
good synthesis of TNP. Failures with AP never with unrefined/ OT washed mer ful of 1 gr
pressed to the equivalent of abit more than 3gr cc3 4250+MPS.Merc ful. being quite difficult to press to full density even using a med size vise and
dowel arrangement/plexiglass shield and protective gear including EARPLUGS. Suggestions,comments?
[Edited on 23-6-2009 by grndpndr]
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497
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My suggestion would be HMTD. It seems to be far superior to AP in almost all aspects, especially initiating ability (not just in my experience, many
others have said the same). Of course it is still very dangerous stuff, but no more so than AP or MF. I would imaging less the 0.5g would do the trick
for TNP. I have found HMTD is best initiated by a small amount of pyrotechnic material coating a nichrome wire, rather than direct nichrome. Sometimes
with a power source that is too weak or nichrome that is too thick, it can fail to DDT. Never had it fail by initiating with a "Solar Flare" igniter
(used to start model rocket engines.) I'm sure a visco fuse would do just as well, but I don't trust them for large scale stuff.
[Edited on 24-6-2009 by 497]
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JohnWW
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Quote: Originally posted by quicksilver  |
ADVANCED PRACTICAL ORGANIC CHEMISTRY, J. Leonard, Lygo, & Proctor (especially CH 16 "What To Do When Things Don't Work) - saved my efforts many a
time...
It's inexpensive & many folks here have read it. I still have mine & that was a 1st edition. I go back to it every so often as it answer
things like this so concretely & gives examples of how to set up an example for the use within a common lab. It's a paperback (cardboard back)
& inexpensive. You'd love it; as it doesn't start off with useless material. |
http://rs554cg.rapidshare.com/files/150690239/0748740716.djv... 2.0 Mb - Advanced Practical Organic Chemistry - J Leonard et al (CRC-2nd Ed) -
also http://ifile.it/hyrvb3f/0748740716.rar
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grndpndr
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Appreciate both replys gents.497 HMTD was suggested as he has all the precursors for both the fulminate and the HMTD
which I wasnt aware of.The more i looked at HMTD the more I was impressed ,particularly the lack of that nasty ass Mercury.
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The_Davster
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| Quote: Originally posted by 497 | My suggestion would be HMTD. It seems to be far superior to AP in almost all aspects, especially initiating ability (not just in my experience, many
others have said the same). Of course it is still very dangerous stuff, but no more so than AP or MF. I would imaging less the 0.5g would do the trick
for TNP. I have found HMTD is best initiated by a small amount of pyrotechnic material coating a nichrome wire, rather than direct nichrome. Sometimes
with a power source that is too weak or nichrome that is too thick, it can fail to DDT. Never had it fail by initiating with a "Solar Flare" igniter
(used to start model rocket engines.) I'm sure a visco fuse would do just as well, but I don't trust them for large scale stuff.
[Edited on 24-6-2009 by 497] |
HMTD is comparable to lead azide in terms of initiation ability, which is a better initiator than Hg fulminate.
Federoff states that 0.06g of HMTD will initiate picric acid.
That said, it still has the metal reactivity issues, and the instability/decomposition during storage.
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Rosco Bodine
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Federoff would have to be citing data for a reenforced cap and it will require a whole lot more to do the job.
Lead Azide or the azo-clathrate will work better. Picric Acid is relatively insensitive and not easily initiated, as is true for many nitrated
aromatic compounds, being only slightly more sensitive than TNT to initiation. Styphnic acid is a bit easier to initiate and almost as powerful as
TNP, probably on par with TNT, but more easily nitrated, synthesized. Initiation of these relatively insensitive materials is a task for an
"unequivocal primary" especially in an unreenforced cap, and HMTD isn't one of those.
On a humorous note, cleverness can lead to a smile
of self-satisfaction which is similar to a cat that ate the canary scenario, however one should be watchful ....
as that may not be the end of the matter
http://www.youtube.com/watch?v=DkLwFfAwbts&feature=relat... Bill The Cat
[Edited on 24-6-2009 by Rosco Bodine]
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Hennig Brand
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Even a relatively thin steel tube has much greater strength than just about any common aluminum one, doesn' t it? Just how reinforced do you mean? Or
is this way just not very practical? There really is just no comparison between aluminum and steel, as with the primaries I haven' t had a chance to
play with the better ones yet. Time to dig up some azide! That stuff on clathrates looks nice, powerful and staight forward.
Thanks for the links and info in the last half dozen posts or so, it is very helpful to me.
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hissingnoise
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Common metals other than aluminium shouldn't be used with HMTD as they react with and sensitise this primary. . .
A reenforced detonator contains a small inner cap which contains the primary.
When the base-charge is loaded the reenforcing cap is inserted on top of the base-charge and pressed firmly to fix it in place.
Davis describes reenforced caps in the section on detonators in COPAE!
They're not reinforced as such.
In general, reenforced detonators are more effective than non-reenforced detonators. . .
[Edited on 24-6-2009 by hissingnoise]
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The_Davster
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Oddly enough, 0.05g reinforced cap, 0.06 unreinforced. For a non-unequivocal primary this seems wrong. (Page H84 )
Also interesting is the sand crush data, 42.5g for HMTD vs 16.5 for Hg fulminate 
Perhaps it is an under-appreciated primary?
Still go with one of the unequivocal ones, and to add to rosco's suggestions: silver nitrotetrazolate.
[Edited on 25-6-09 by The_Davster]
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Rosco Bodine
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Federoff is basically a collective encyclopedia of assorted
data and some of it is just plain wrong data from the source. HMTD is not going to self accelerate quick enough to make the DDT in those quantities,
much less
to function as an initiator, and yeah similar misreporting
exists for remarkable initiating ability of other compounds which simply don't have nearly the sass as is reported,
DDNP is another. I look at some of those figures and wonder if they are by a decimal place overoptimistic. There would have to be some really
unusual "trade secret" sort of configuration being used to somehow get some materials to do the tricks reported, because those reported results sure
aren't confirmed by my own observations, and I always trust my own data, at least those times when I double check just to make sure. And I have
double checked HMTD. It will do the job as a quick improvised and near term usage material, but it is not useful except for the short term because it
has a definite stability problem with deterioration that is a clock that starts running when it is made and is definitely temperature dependant
stability favored by cold and
instability effected by even ordinary, mild, not even warm temperatures.
An interesting improvised cap which might be a worthy experiment is a betaine permanganate base charge having a lead nitranilate initiator, or a
mixture
of the two materials as an initiator for picric acid.
If workable, this would probably be a step above HMTD in terms of sophistication, yet less technically difficult than azide or tetrazole initiators.
[Edited on 25-6-2009 by Rosco Bodine]
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The_Davster
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Curiously these extravagant claims are not referenced nicely like the other HMTD properties indicated. I would like to try to find the original
'exaggerators'. I bet it is a patent.
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497
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| Quote: | but it is not useful except for the short term because it has a definite stability problem with deterioration that is a clock that starts running when
it is made and is definitely temperature dependant stability favored by cold and
instability effected by even ordinary, mild, not even warm temperatures. |
Many people have said this, but I have yet to see anyone mention any actual first hand experience with this problem.. Also is there even any real
tested data/information on the mechanism of decomposition, the products, the effects of conditions, or anything related to the decomposition of HMTD
in storage? Virtually everything I've seen regarding HMTD instability seems to be speculation or referencing to something that is speculation..
The reason I'm a little doubtful, is I have seen with my own eyes a sample of HMTD that has been kept by a friend for over a year now at room
temperature in a barely sealed plastic container. After a over a year it has undergone no noticeable change in appearance, smell, quantity,
sensitivity or power.. So maybe the instability issue is a little overblown?
I do agree that something like azoclathrates would be preferable, but for simple experimentation (no need for storage, small scale) I think HMTD is
perfectly usable.
[Edited on 25-6-2009 by 497]
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hissingnoise
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I too found that HMTD could be stored safely without special precautions. . .
The product of my first synthesis was incompletely washed and smelled of methylamine.
After several months sitting in an open container it developed a slight cream colour but its explosive properties were unaffected.
A thoroughly washed sample was kept for around two years in a garden shed which heated considerably in summer and although I checked regularly for
signs of decomposition no changes were found.
I eventually gave up checking and all but forgot its existence for about a year after which time I took it out to demonstrate its deflagration to some
friends. . .
They were suitably impressed!
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Rosco Bodine
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HMTD instability is something that I have observed consistently is a predictable problem which is also reported in the literature. It is not
speculation and
the deterioration by weight loss confirmed due to chemical decomposition has been charted and published.
IIRC there is something charted regarding the decomposition rate in COPAE. That decomposition is the rule and if there is a stable sample of HMTD
then it is the anomaly.
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quicksilver
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HMTD was found to be too UV, temperature, friction, & compression sensitive to be of practical use in industry. USBoM did quite a few tests w/
HMTD compressed at various levels & unfortunately it "didn't stay put" in that it would loose it's compaction over time easier than many other
materials of the day. UV sensitivity was a comparative unknown to many & HMTD's UV issues were fairly great. As mercury was starting to get
expensive and in warmer climates the fuse caps were not lasting 6 months in magazines that could easily rise to 60C (or warmer) for periods of the
day. Even with Bake-a-lite capsules the USBoM felt it was just not the best choice.
Hydrazine was easily enough synthesized & the concept of a primary that could have an almost limitless shelf life was highly desirable. Prior to
this Pb Picrate with a compressed TNP base was experimented with and found to be useful to the #6 level. This let many off the hook as a #6 was all
that was appropriate with many materials used at the time. This was also why many in Europe believed TNP to be the most versatile energetic material
to mass produce.
One of the last books I posted in the "Worst Books" thread had this material directly from the USBoM, the tests, results, etc. Hydrazine became of age
much later than one would have expected but many people felt that the industrial investment in mercury fulminate to too costly to switch to an
unproven material (politics of DuPont).
Thus HMTD's instability was not speculation. Tests really were done quite extensively at the time. This was due to it's ability to be a great
initiator. But the factors (as above) put it out of the running unless sciences know today would have been employed (vacuum sealing, non-metallic
capsules of high strength, etc.).
[Edited on 25-6-2009 by quicksilver]
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Rosco Bodine
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There is a quite lengthy thread at E&W where I posted a bunch of historical patent references
http://www.roguesci.org/theforum/showthread.php?t=367&hi...
I never explored solvent recrystallization for purification to see what may be helpful there but that is a possibility
for experiment, as well as possible double salt formations which are sometimes a means of stabilizing an otherwise unstable material.
I try very hard not to do bad science nor report bad data,
and when I speculate or propose unknowns I generally try to identify that sort of qualified information for what it is as intuitive or hypothetical.
The instability of HMTD is a fact for every sample I ever made and there have been quite a few.
The thread which Axt started about 2,3,5,6-Tetraazidobenzoquinone which evolved into chloranil and nitranilic acid related discussion could lead to
some interesting experiments. I keep having to go back and take another look there so maybe I have an idea brewing subconsciously
The lead azo-clathrates definitely still bear further investigation and in my opinion are actually the most intriguing thing to arise, of lesser
technical challenge than the energetic tetrazoles which are of course top of the heap. I pretty much said this same thing many years ago and so far
anyway, it still holds true in my estimation.
The hydrazine nitranilate or some of the possible nitranilate complexes in possible mixture with lead nitranilate or other materials also has an
interesting potential for experiments.
[Edited on 25-6-2009 by Rosco Bodine]
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