Sciencemadness Discussion Board
Not logged in [Login ]
Go To Bottom

Printable Version  
 Pages:  1  2
Author: Subject: HMTD Decomposition Rate and Recrystallization
Bot0nist
International Hazard
*****




Posts: 1559
Registered: 15-2-2011
Location: Right behind you.
Member Is Offline

Mood: Streching my cotyledons.

[*] posted on 26-2-2012 at 19:30


Quote: Originally posted by NitricSynth  
Me and dawson are chemical engineers. :D

[Edited on 27-2-2012 by NitricSynth]


No, you are irresponsible teeny bombers who practice a total disregard for established procedures and have little knowledge of chemistry and a lack of desire to gain it. This can and will lead to disasters. I do hope that in practice you have less of a cavalier attitude about the experiments you conduct than you do in your posts. I know you are aware that these things your playing with have a great capacity for causing lots of misery and remorse. Not trying to flame you NitricSynth. Just expressing a concern.

In my opinion you, Dawson, and Holmes are all the same.

Could you prepare and post a well thought out experimental model comparing your "warm synth" HTMD to some made according to Davis? Maybe establish a control and use a series of tests like weight drop on anvil, heating from below, flame contact, etc. Strive to keep all the variables the same except for the ones your testing. If you provided this it would help us see some validity in your claims. Also, I wonder how much the "warm HTMD's" VOD is affected along with its supposed reduced sensitivity.




U.T.F.S.E. and learn the joys of autodidacticism!


Don't judge each day only by the harvest you reap, but also by the seeds you sow.
View user's profile View All Posts By User
Bot0nist
International Hazard
*****




Posts: 1559
Registered: 15-2-2011
Location: Right behind you.
Member Is Offline

Mood: Streching my cotyledons.

[*] posted on 26-2-2012 at 20:48


Quote: Originally posted by SB15  


Edit: Also, it should be known that NitricSynth is not dawson01912/holmes1880. They have similar writing styles and share a strong disdain for theoretical chemistry, but they are not the same person.

[Edited on 2-27-2012 by SB15]


And the same spelling quirks, again. They both misspell Rosco the same. The writing style is identical. Why do you declare they are different. Different IPs only says proxy to me.

Whether they are one or three, they/he should move beyond peroxides, as it seems he is. Also, the obsession with NPED? interesting concept, but primaries are so reliable. As Rosco says, look at bullets. Each one has a primary in it, and there are a lot of bullets on earth. IMO, an explosive train initiated by a contemporary, commercially/militarily tested primary is the most reliable way to work with high explosives.


Quote: Originally posted by NitricSynth  
LoL... Roscoe... Have you ever even synthesized or worked with secondary explosives? The way you talk about them tells me you have zero field, military, or industrial experience in working with them.

Go out in the field and tell me how comfortable you are inserting a AgC2.AgNO3 cap into a block of PETN/ETN plastique and do the same with a non primary device and tell me your comfort levels.

I have not discovered a design of NPED that uses NG that works within 6mm tubing. I have some ideas but nothing tested yet. Perhaps a mixture of needle ETN, NG, and a touch of DBSP will yield a non flowing shock sensitive composition that can be initiated via Flash.

Even 1.5 Micron Aluminum 70/30 Flash cannot initiate MHN recrystallized any way you can think of at any density tested in 6mm Tubing. ETN... Don't bother! It's only 1/4th more sensitive than PETN.

[Edited on 27-2-2012 by NitricSynth]


Quote: Originally posted by holmes1880  
I call some BS into question on that document. Those are some very old recordings........most data is missing.

Plus, we don't even know if it is recrystallized or not, I remember never getting DDT from ETN once recrystallized, but if you just get a bit lazy and not bother recrystallizing, ETN can be set off in a confinement with black powder. And it was consistent, to about 85%. NG is far more sensitive than ETN when it comes to impact, that's not to be disputed.

Roscoe, what is so dangerous about mixing ETN......just don't go crazy with it(like using drill mixer for 1 hour) and check the temperature to stay below 30C and nothing will ever happen. Mixing is good for preventing hot spots.......the temperature can be 25C on the thermometer, but on a surface you have a bugger that is 40C+ and then it starts....:(


[Edited on 14-12-2010 by holmes1880]


Quote: Originally posted by dawson01912  
However, you are forgetting that explosives are not meant to be studied in the lab! They are to be used in doing work, whether it is digging a canal, demolitions, or killing innocent Iraqis:(. When you are doing something, you have to keep an objective in mind of why you are doing something. I have an objective, I want to have fun and do it with 100% feeling that I am safe and if anyone is around, that they are safe too. I also want to give kids out there a device that they can safely use without having to make AP or HMTD.

I have set out to create an ultimate NPED device that a 15 year old Phone could have made safely and still had fun... Kids are desperately jumping to AP and HMTD because they want the thrill and are young enough to ignore dangers of those chemical, while not having the resources and knowledge to make a more complex, stable primaries.


I am at the last testing stage of this device. For 18 months I've came up with bunch of flawed methods and now I got it. As long it passes the effective initiation of kinepack mixtures, I'm giving out for the kids to use. Kids who are already making AP/HMTD/MEKP will have a safe option. And kids who are too young definitely won't be able to make it.......it's not like flash powder "bang". And the ill-intentioned won't be able to employ it because it can't be set off remotely/fuse in any way shape or form nor can it pass metal detection in any public place.


I have looked for an effective method for someone to make explosives truly safe and accessible and was disappointed. What exactly can you contribute by calculating energy release of some formula? Squat, that's what.

Me, I'll actually save people's lives because I did not do chemistry with blinders on and looked for a problem solution.


[Edited on 27-2-2012 by Bot0nist]




U.T.F.S.E. and learn the joys of autodidacticism!


Don't judge each day only by the harvest you reap, but also by the seeds you sow.
View user's profile View All Posts By User
Pulverulescent
International Hazard
*****




Posts: 793
Registered: 31-1-2008
Member Is Offline

Mood: Torn between two monikers ─ "hissingnoise" and the present incarnation!

[*] posted on 27-2-2012 at 02:16


Quote:
Everyone here is a bunch of nerds.

You flatter us . . . (:))

P




"I know not with what weapons World War III will be fought, but World War IV will be fought with sticks and stones"

A Einstein
View user's profile View All Posts By User
Rosco Bodine
Banned





Posts: 6370
Registered: 29-9-2004
Member Is Offline

Mood: analytical

[*] posted on 27-2-2012 at 03:06


Nerds rule.
View user's profile View All Posts By User
Etanol
Hazard to Self
**




Posts: 73
Registered: 27-2-2012
Member Is Offline

Mood: No Mood

[*] posted on 27-2-2012 at 04:17
recrystallization HMTD


HMTD can be recrystallized from DMSO.
20C 0.5g HMTD/100g DMSO
90C 1g HMTD/100g DMSO
The solution was then diluted with water or ethanol

HMTD is a very fine powder.
Absolutely no odor.
View user's profile View All Posts By User
Pulverulescent
International Hazard
*****




Posts: 793
Registered: 31-1-2008
Member Is Offline

Mood: Torn between two monikers ─ "hissingnoise" and the present incarnation!

[*] posted on 27-2-2012 at 05:50


If there's a fishy odour it hasn't been fully washed . . .
Recrystallising isn't necessary!

P




"I know not with what weapons World War III will be fought, but World War IV will be fought with sticks and stones"

A Einstein
View user's profile View All Posts By User
NitricSynth
holmes1880





Posts: 22
Registered: 24-2-2012
Member Is Offline

Mood: No Mood

[*] posted on 27-2-2012 at 13:35


I was just trying to get finer powder and stability.

Has anyone ever fully tested to see if HMTD reacts with aluminum and how fast? I spilled like 2mg on some zinc anodized blasting cap crimpers and left it on there for a while accidentally... Stripped the 0.18mm zinc coating off within hours making little dots.

I'm going to mix a half a gram 75/25 with aluminum, dark and atomized superfine and test it every couple weeks and see if it's properties and appearance change.
View user's profile View All Posts By User
Pulverulescent
International Hazard
*****




Posts: 793
Registered: 31-1-2008
Member Is Offline

Mood: Torn between two monikers ─ "hissingnoise" and the present incarnation!

[*] posted on 27-2-2012 at 13:50


HMTD is a peroxide!
Al is quickly passivated by contact.

P




"I know not with what weapons World War III will be fought, but World War IV will be fought with sticks and stones"

A Einstein
View user's profile View All Posts By User
Rosco Bodine
Banned





Posts: 6370
Registered: 29-9-2004
Member Is Offline

Mood: analytical

[*] posted on 27-2-2012 at 13:55


Check these links which arise from a search parameter Callery
Also get and look at the patents listed in the link

http://www.sciencemadness.org/talk/search.php?token=&src...

There is some useful reading in the archived E&W forum also

With regards to reactive targets. The liquid energetic AP/MEKP which appears reasonably stable was tested by Axt as a sensitizing liquid added to NH4NO3 and the composition was reactive to bullet impact and video was posted.

Reactive target compositions are commercially sold legally as a binary dry mix combined for activation just prior to use.

Either one of those mixtures are likely more stable than any mixture including HMTD. There is an inherent chemical instability and chemical reactivity about HMTD, which is rate affected and aggravated by ordinarily warm, meaning normal room temperature alone, and aggravated further by impurities. That decomposition may progress quietly or
suddenly and violently without complete predictability as to which.

[Edited on 27-2-2012 by Rosco Bodine]
View user's profile View All Posts By User
NitricSynth
holmes1880





Posts: 22
Registered: 24-2-2012
Member Is Offline

Mood: No Mood

[*] posted on 27-2-2012 at 17:24


Quote: Originally posted by Pulverulescent  
HMTD is a peroxide!
Al is quickly passivated by contact.

P


You mean it's even more passivated than air can do? And what of the breakdown products as the oxygen attacks the Al? Hmmm...

[Edited on 28-2-2012 by NitricSynth]
View user's profile View All Posts By User
Rosco Bodine
Banned





Posts: 6370
Registered: 29-9-2004
Member Is Offline

Mood: analytical

[*] posted on 28-2-2012 at 02:40


Trimethylamine is a principal decomposition product of HMTD and it is basic, corrosive, hygroscopic and stinks like fish. Attached is an article which is pertinent.

Attachment: Oxley_ThermochimActa_2002.pdf (155kB)
This file has been downloaded 539 times

View user's profile View All Posts By User
Pulverulescent
International Hazard
*****




Posts: 793
Registered: 31-1-2008
Member Is Offline

Mood: Torn between two monikers ─ "hissingnoise" and the present incarnation!

[*] posted on 28-2-2012 at 03:34


Thanks for that Rosco, a quick glance suggests that Jimmie Oxley (an attractive female, BTW) finds TATP more stable, less sensitive and more brisant than HMTD!
Interesting . . .

P




"I know not with what weapons World War III will be fought, but World War IV will be fought with sticks and stones"

A Einstein
View user's profile View All Posts By User
NitricSynth
holmes1880





Posts: 22
Registered: 24-2-2012
Member Is Offline

Mood: No Mood

[*] posted on 28-2-2012 at 23:29


I have been testing these two and am starting to think TATP is best. However... It has to be physically stabilized.

For physical stabilization I think a more flexible plastic is best to prevent physical stress. TATP is mixed 50/50 with 80/20 NG/DBSP with just enough acetone as solvent. Not too much or the TATP won't stay properly suspended. It is then sucked into a syringe and dropped by the droplet into plastic straw molds. The straws are pre-cut down their length with a razor knife so they will come apart. These 75-100mg amounts of composition are removed from their plastic molds safely once dry with two sets of needle nose pliers and then loaded. To initiate the composition Flash is used.

The reason for using 50% NG/DBSP with TATP is that there will be little to no crystal to crystal friction. This should sufficiently prevent the TATP from subliming away too...

When it comes to TATP this is the best technique I can think of. :/

It may actually be better just to use 93/7 NG/NC mixed with TATP 50:50 in 100mg amounts on a small piece of Al foil. The TATP should be held properly in suspension. The composition is then picked up with needle nose pliers with it's 2x2cm piece of Al foil and crumpled and pressed into the detonator. Following that is pressed in a 1mm Al plug which is pressed to compact the composition and Al foil to density behind a blast shield. Initiation is via flash. Anyone want to try this one? I'm going to laugh if flash powder can't initiate this stuff through a 1mm Aluminum plug...

Question, does TATP stored underneath ethanol change it's crystal structure?


Going to test compacted HMTD storage in contact with Al foil. I am kinda skeptical it's going to oxidize it any more... An alternative is just to place the HMTD inside a piece of Al tape before loading. The adhesive coating provides a good enough barrier provided it doesn't react with the crap...

This is just curiosity testing as I only use thermal shock/runup NPEDs to initiate anything more than a few grams.

[Edited on 29-2-2012 by NitricSynth]
View user's profile View All Posts By User
Adas
International Hazard
*****




Posts: 711
Registered: 21-9-2011
Location: Slovakia
Member Is Offline

Mood: Sensitive to shock and friction

[*] posted on 29-2-2012 at 08:34


Quote: Originally posted by NitricSynth  
Question, does TATP stored underneath ethanol change it's crystal structure?
[Edited on 29-2-2012 by NitricSynth]


I think TATP is soluble in ethanol and when it recrystallizes it makes bigger crystals, naturally.

The best method to store TATP is to store it as saturated solution in toluene - This won't explode using #8 blasting cap.
Source: One paper I have read in the past. You can find it on Google.




Rest In Pieces!
View user's profile Visit user's homepage View All Posts By User
ScienceSquirrel
International Hazard
Thread Pruned
29-2-2012 at 12:54
ScienceSquirrel
International Hazard
*****




Posts: 1863
Registered: 18-6-2008
Location: Brittany
Member Is Offline

Mood: Dogs are pets but cats are little furry humans with four feet and self determination! :(

[*] posted on 29-2-2012 at 12:59


We are a science society.
Let us keep the discussion civilised.
View user's profile View All Posts By User
ScienceSquirrel
International Hazard
Thread Pruned
29-2-2012 at 13:14
Rosco Bodine
Banned





Posts: 6370
Registered: 29-9-2004
Member Is Offline

Mood: analytical

[*] posted on 29-2-2012 at 14:00


Quote: Originally posted by EatsKewls  

I do have a question for Rosco about those extremely stable primaries that surpass the shock and impact stability of PETN. They surely cannot transition into detonation without a significant column length and very heavy confinement?
For some of them that is the case yes. Ideally what
is desirable for the properties of a primary depends on the application and the intended "trigger" stimulus. What works best for fuse ignition but is not responsive to other trigger stimuli would have safety advantages if the application is a fuse cap. It is generally a compromise of properties which is involved in commercial designs.
Quote:

I would assume the ignition is quite easy and that would really be the only advantage of these compounds over a secondary like PETN. It would be a disadvantage at the same time since it would present the static danger.

Any firing train has elements which have specific function enabling sequencing of the tandem elements in a reaction progressing and accellerating to the high order output. There is a lower limiting critical diameter and a "critical mass" at that diameter. The critical diameter practical for one ignition scheme is not necessarily the same critical diameter for another ignition scheme. The trend is towards larger diameters and larger devices when the "soft start" and DDT scenarios are implemented, and depending on the materials chosen, the device can become impractically large. You have made it very clear that you think an NPED design is superior because what you value as the criteria for what is superior is safety to the exclusion of all other considerations. By that logic a baseball bat is a "superior" weapon to a glock because a baseball bat is less susceptible to accidental discharge.
View user's profile View All Posts By User
EatsKewls
holmes1880 (banned)
***




Posts: 126
Registered: 29-2-2012
Member Is Offline

Mood: No Mood

[*] posted on 29-2-2012 at 15:06


Quote: Originally posted by Rosco Bodine  

Any firing train has elements which have specific function enabling sequencing of the tandem elements in a reaction progressing and accellerating to the high order output. There is a lower limiting critical diameter and a \"critical mass\" at that diameter. The critical diameter practical for one ignition scheme is not necessarily the same critical diameter for another ignition scheme. The trend is towards larger diameters and larger devices when the \"soft start\" and DDT scenarios are implemented, and depending on the materials chosen, the device can become impractically large. You have made it very clear that you think an NPED design is superior because what you value as the criteria for what is superior is safety to the exclusion of all other considerations. By that logic a baseball bat is a \"superior\" weapon to a glock because a baseball bat is less susceptible to accidental discharge.


Yes, very true about ignition methods. Now, which considerations are we talking about here? I have met most size and delay requirements. Two successful designs I\'ve tested in excess of 50 times, have an electrical delay of maybe 500ms, tops. Yeah, it\'s a bit more than 20-30ms delay of a traditional detonator, but there are plenty of applications of a cap with such a small delay. So regarding safety, I made very few sacrifices. It used to be requirement of steel embodiment, but I\'ve circumnavigated that little problem just recently.

I am not convinced of the analogy of primers in bullets and those in blasting caps. I think the quantity makes the comparison obsolete.
View user's profile View All Posts By User
Rosco Bodine
Banned





Posts: 6370
Registered: 29-9-2004
Member Is Offline

Mood: analytical

[*] posted on 29-2-2012 at 16:08


Artillery rounds or even some .50 cal or 20mm projectiles do contain primary explosives in the projectile itself, not just in the primer. The setback shock from firing is enormous but the projectiles do not "just go off" in the gun barrel from
the shock of firing. That should tell you something. It is a very application specific firing train which is useful and reliable depending on the configuration. All those G's don't set off a "sensitive primary" until the precise stimuli intended to cause the initiation occurs. You seem to have an idea that the reality that exists and has existed for more than a hundred years is subject to your interpretation. Generalities which you are making don't really show a depth of understanding. Mishandling of gasoline can result in accidents, but that doesn't mean that diesel is in all ways superior. With regards to NPED's it seems like you are obsessing about a non-issue, but you believe it's an issue. What you think doesn't necessarily square with what is. So you are not understanding the materials which you are then mischaracterizing based upon what you think because your thinking is based upon some over generalizing about some highly specific scenarios. Firing trains are engineered like key in lock to fit the application. There are different ways these devices can be made. NPED is not necessarily "the best" configuration except that for you,... you "think" it is "the best". You think it is the best so what do you think is more likely, that for more than a hundred years ordnance designers are all dullards and if only you had been there to tell them how to do their jobs properly then the whole world of industrial use of explosives would be different and safer now? Simple economics may be governing what choice is "the best" for a rock quarrying application, while a different configuration may be "the best" for underwater demolition. If what you are really getting at is what is the best way of making IEDS, do not expect that I will be going there with this discussion.
View user's profile View All Posts By User
EatsKewls
holmes1880 (banned)
***




Posts: 126
Registered: 29-2-2012
Member Is Offline

Mood: No Mood

[*] posted on 29-2-2012 at 17:02


To be fair, anything you make at home is pretty much an IED. I do think there are economical insentives to eliminate primaries out of the caps. I am not familiar with the industry, but I'd imagine facilities working with primary explosives pay higher premiums on insurance and have additional regulations that add to fixed costs.

Whatever my reality is, it is a fact that primary explosives are generally less stable than secondary explosives and allow less room for error. And considering that eliminating primary explosives without sacrificing performance and related characteristics is very much possible and not very difficult to accomplish, there is no reason to not use them in the field. I mean, Nonel NPEDs have taken quite the market share, dispite some of their drawbacks. Europeans like them some non primary caps, and there was even something as ridiculous as RED detonator. Atrocious design, but there was apparently enough to demand to warrant its production.

As far as making IEDs, which everyone has, there is very little debate that cutting out primary explosives would make for a much safer amateur experimentation. I am not intending to share 'how to's" with anyone here, as there is in fact no real danger with using primary explosives. Here is an inert design for your viewing pleasure:
http://oi40.tinypic.com/16h6mj8.jpg . I've had a pic of electrical one, but can't seem to find it.


[Edited on 1-3-2012 by EatsKewls]
View user's profile View All Posts By User
Rosco Bodine
Banned





Posts: 6370
Registered: 29-9-2004
Member Is Offline

Mood: analytical

[*] posted on 29-2-2012 at 17:48


For most primary explosives your generalization would hold true. But you make it sound like an unavoidable rule which has no exceptions while it has several. Something like cyanoguanidine or perhaps betaine stabilized nitromannite
could probably be initiated with any of several basic lead picrate or basic lead picrate complex salts. I haven't tried this with experiments to confirm but it should work. I suppose there are different levels of sophistication for what is "improvised" depending on the tooling and skill of persons doing the improvising. Many of us have experience loading and reloading ammunition and the result of what may be improvised may be not very far removed and may even be superior quality and output to a commercially manufactured similar item. A bit of knoweldge and skill and tooling is required and it is not childs play at all, but is not terribly difficult either.

One thing that you need to confirm about any DDT configuration is that you are in fact getting a high order detonation and not a low order detonation. Witness plate evidence of brisance and field tests successfully initiating a relatively insensitive secondary like urea nitrate would be confirming high order output.
View user's profile View All Posts By User
EatsKewls
holmes1880 (banned)
***




Posts: 126
Registered: 29-2-2012
Member Is Offline

Mood: No Mood

[*] posted on 29-2-2012 at 19:12


Quote: Originally posted by Rosco Bodine  

One thing that you need to confirm about any DDT configuration is that you are in fact getting a high order detonation and not a low order detonation. Witness plate evidence of brisance and field tests successfully initiating a relatively insensitive secondary like urea nitrate would be confirming high order output.


Of course, I don't make that amateur mistake of testing BCs alone. Small 10-20g 'confirmation charge' taped to the base of the cap is used. Most, if not all, tests are performed underwater, because if there is a flaw in a design it is most likely to fail when submerged. Hence, the improvised Bickford-style fuse.

One could go to the lengths of making caps on par with commercial with with those reloading tools available, but the costs would run up. I may invest one time into jacket swaging setup to create close end tubing, but as of now, cheaper improvised means have been sufficient.



P.S. Interesting that you site lead picrate as the preferable primary. SB and I have debated whether this fellow who had accident with nitrotetrazole, don't know if you heard full story on it, was simply reckless or just very unlucky. SB keeps mentioning that he was a just very unlucky and that there were trace amounts of contaminants during synthesis, which caused spontaneous detonation. I don't know the details of the synthesis he was working off, but I would still argue he was just reckless. Could there be such a scenario where just trace amounts of contaminants during that synthesis cause such an accident, or was that kid just reckless? Or perhaps both.


[Edited on 1-3-2012 by EatsKewls]
View user's profile View All Posts By User
Rosco Bodine
Banned





Posts: 6370
Registered: 29-9-2004
Member Is Offline

Mood: analytical

[*] posted on 1-3-2012 at 01:54


You are incorrectly reading beyond what I actually said. I did not cite lead picrate as being the preferable primary. Neither did I specify that it would have to be a loose charge or in tandem with a segment of mixture with the nitromannite as an intermediate increment capable of making the runup to high order detonation of the nitromannite base increment. And I didn't cite lead picrate but basic lead picrate or basic lead picrate complexes, meaning the basic salt as opposed to the neutral salt. The clathrate complexes which have included azide would do well in such a configuration. A low compression damp loaded dextrin or similar bindered pellet of a coprecipitated or even mixed lead azide and lead styphnate composite should work fine and require no loose igniter charge. This kind of configuration could even be in a plastic housing like a disposable syringe body or plastic test tube or an empty marker pen. Any even minimal housing should work fine. I am not advocating that anyone should do this, but simply saying that it is technically possible to do.
View user's profile View All Posts By User
quicksilver
International Hazard
*****




Posts: 1820
Registered: 7-9-2005
Location: Inches from the keyboard....
Member Is Offline

Mood: ~-=SWINGS=-~

[*] posted on 1-3-2012 at 15:31


To underline what Roscoe had said lead styphnate is a high flame sensitive material and has been used in strata or as a mix to sensitize to flame spit or hot wire initiation. Tetrazene had also been experimented with as a high flame sensitive material but tetrazene had other qualities that made it less desirable in that capacity.
I have looked at the lead clathrate (patent examples) and the "Roscoe clathrate" latices with some fairly decent microscopes and the "Roscoe" design has a more clearly defined crystal make-up.
Of the "azide sensitivity" to initiation to PETN there is quite a bit of material and very small weights (compressed) will initiate. Of the clathrates a bit heavier composition (approx 0.125gr) has a empirical ability to initiate. However considering the uniquely low weight of lead/silver azide, this means very little overall. I have little data as to a clathrate's ststaic sensitivity and would treat it as the same range as an azide. Unfortunately it does not respond as well to "dextrination" as do the common azides. The crystals are well defined and this MAY be one reason why the clathrates have not be a common commercial primary material.

I QUOTE Roscoe here from a prior post:

"My theory is that the way in which the host complex is made and the conditions under which the azide is subsequently added to the host complex has a bearing upon increasing the upper limit of how many moles of entrapped lead azide it may contain, and the saturation limit can vary also according to the particular host compound, 16 moles of included lead azide may be possible from indications in some of my experiments with host compounds mentioned but not specifically detailed in the patent US3431156 as experimental examples. This is what I meant by saying that "A similar process can be used to provide enrichment to the properties of the compound in example 4 of US3293091."

To my thinking the patent US3431156 is a "goldmine" of data as a technical disclosure itself, as well as suggesting further general experiments or refinements related to the example compounds it discloses. It really surprises me there are no subsequent patents having been published since 1969 regarding further work on the same general type of compounds. Perhaps Remington Arms and DuPont have done further experiments but kept the research confidential for business reasons. There was an earlier mention of the formation of complexes of this sort in a 1922 patent GB180605, by the German chemist Dr. Walter Friedrich, (see line 98 page two), however there were no detailed examples. It seems likely that some of the early references to "mixed salts" may have in fact been clathrates, but many years would pass before the details would be described extensively for the first time as an advanced art in US3431156.

Described below are the synthesis details for my experiment with a slightly enhanced variation of the general type of compound described in US3431156, example 5. It is interesting when when a synthesis produces quantitative yields, for several reasons. It is a rare result, and many times the stability of a product from a quantitative yield synthesis is excellent. The resulting product has formed from a synergy of reactions which went to completion without side reactions and byproducts, and efficiently formed the target compound as the single "most probable" result, excluding other possible products. The intended product of a high yield synthesis will often prove to be very stable and high purity compound. The inherent quality control involved is desirable for materials to be used as explosives. A synthesis of 4 (basic lead picrate, lead nitrate, lead azide) 12 (lead azide) molecular weight 9603.08

NOTE: In my opinion the proportional formula designation for clathrates is somewhat arbitrary, but the ratios are correct. For example the theoretical minimum molecular weight might be only one fourth of 9603.08, or the actual molecular weight could be any one of several multiples of that number. Its a damn mystery, so I shall leave the true structural determination to others who have the instruments required and the interest to pursue such questions. Crystallographers are sure to enjoy pondering the actual structure of this energetic "Buckyball" sort of molecular matrix".

Below is a rather old commentary, copy of the Kenny patent, & assorted comparisons with the aspects of use of BASIC Lead Picrate
Please Note - - IF you SEARCH, you can find some wonderful material on the Forum.....


Attachment: azo-clathrates.pdf (1.7MB)
This file has been downloaded 568 times

[Edited on 1-3-2012 by quicksilver]




View user's profile View All Posts By User
 Pages:  1  2

  Go To Top