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Author: Subject: Perchlorate compositions
Marsh
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Perchlorate compositions

Greetings everyone...

I would like to discuss perchlorate mixtures with those who have experimented with them.

I recently tried detonating two perchlorate mixtures...both turned out to be failures using about 1.2g PETN. I believe I may have obtained partial detonation with one cheddite.

The goal I am after, is mainly an ammonium, or possibly potassium perchlorate mixture with a high (>5000m/s) Vod whilst having a decent sensitivity to smaller det charges - if this is obtainable, not a must. I have heard it discussed that there are very powerful (>6000m/s Vod) NHCLO4 mixtures which exist but I cannot find specifics on some of these as to the various formulas brisance. Thus I haven't really settled on one to experiment with due to lack of knowledge about sensitivity, vod's, etc.

A gel/slightly aqueaus solution is ok in this scenario as well.

I first tried a variation of the good old KCLO3 + petrolium jelly mixture with perchlorate instead. I used KCLO4 at a ratio of 90/10 with the petrolium jelly. This is where I believe I may have achieved partial detonation. I still am unsure truthfully though.

I know the more sensitive and common KCLO3 mixtures only used about 5-8% petrolium for fuel, and more than that would substantially lower sensitivity.

Being that the perchlorate contributes more oxygen, and being that the comp it is already oxygen rich, I increased petrolium to the 10% in hopes this would satisfy for fuel. It may have decreased sensitivity too much for detonation.

Has anyone experimented with a KCLO4 mixture instead or the more common chlorate mixtures with petrolium fuel? What about NHCLO4/petrolium jelly? Is there disadvantages to the perchlorates in the reaction? I assumed Vod may be higher in the perchlorate reaction, but sensitivity may be the bigger factor which is reduced.

The second mix I tried was ammonium perchlorate with about 5% vaseline binder, and 10% Al powder added. I assumed the fuel/oxidizer in this reaction would be much more favored under conditions (also being more dense), but I did not achieve detonation. Does this sound like a detonatable comp if possibly used with more PETN, or did I miss by a longshot?

I have also heard about NHCLO4 with hexamine mixed dry as a powerful composition. Could this be improved by a ethyl glycol solution into which the ammonium perchlorate/hexamine is desolved and bound with guar gum to form a gel HE? Or would it make more sense to leave the hexamine out of this reaction?

Another thing I would like to mention, I realize that nitromethane would appear to be a good fuel for an APNM mixture, but I have heard rumors of very low sensitivity in this mix, due to the NHCLO4 being less hygroscopic, and thus less fuel is absorbed by it. So I am avoiding NM in this instance.

Any info on these perchlorate compositions as well as other possible high Vod formula would be greatly appreciated.

Cheers.
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Mood: @%&$ing hardcore baby  Quote: Originally posted by Marsh Greetings everyone... Another thing I would like to mention, I realize that nitromethane would appear to be a good fuel for an APNM mixture, but I have heard rumors of very low sensitivity in this mix, due to the NHCLO4 being less hygroscopic, and thus less fuel is absorbed by it. So I am avoiding NM in this instance. Hygroscopicness has to do with a compound sucking up water from its surroundings... I don't believe hygroscopicness would have anything to do with AP asorbing nitromethane. Marsh Hazard to Self Posts: 79 Registered: 28-7-2006 Member Is Offline Mood: No Mood True, I'm sorry... But, I do believe the NM mixtures which have been experiemented with take very large booster charges to achieve complete detonation, due to the non-complete incorporation of the fuel into the binder (I compaired this to being non-hygroscopic). I believe the APNM mixtures have lower Vod's as well. [Edited on 29-7-2006 by Marsh] DeAdFX National Hazard Posts: 339 Registered: 1-7-2005 Location: Brothel Member Is Offline Mood: @%&$ing hardcore baby

 Quote: Originally posted by Marsh True, I'm sorry... But, I do believe the NM mixtures which have been experiemented with take very large booster charges to achieve complete detonation, due to the non-complete incorporation of the fuel into the binder (I compaired this to being hygroscopic). I believe the APNM mixtures have lower Vod's as well.

How long did you let the Nitromethane soak into the Ammonium Perchlorate? Prehaps you need to let the fuel soak in for longer.
Marsh
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Quote:
 Quote: Originally posted by Marsh True, I'm sorry... But, I do believe the NM mixtures which have been experiemented with take very large booster charges to achieve complete detonation, due to the non-complete incorporation of the fuel into the binder (I compaired this to being hygroscopic). I believe the APNM mixtures have lower Vod's as well.

How long did you let the Nitromethane soak into the Ammonium Perchlorate? Prehaps you need to let the fuel soak in for longer.

I have not tried the NM mixture myself. I have followed a few on their experiments and it seemed to be a less desireable mixture from what it appeared, as I said with incomplete detonations. I know a smaller amount (1/2kilo) was detonated with over 20g RDX.

Are there any predicted Vod's on APNM?

Do you have any comments on the formulas which I tried specifically which failed?

I'm mainly discussing KCLO4 and NHCLO4 because I have them both in hand and would like to see what I can come up with from them.

Edit: I have found available NM (I originally thought it was very expensive; but still moderately)...

What about AP/NM/AL 50/25/25? This seems like a more sensitive mixture but again I do not know if Vod's would be favorable against other compositions.

Would there be another method to sensitize this formula a bit more?

It seems that something which dissolves the AP would produce the favorable high-Vod's. Again, like diethylene glycol/AP with possibly some Al added.

[Edited on 29-7-2006 by Marsh]
Rosco Bodine
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What should be worth experimentation is the matter of whether and ammonium perchlorate reaction with
formaldehyde and urea would occur similarly as the
reaction of ammonium nitrate in this regard , the product being principally the methylamine salt , along with lesser amounts of the di and tri methylamine salts as minor further reaction products . If the parallel reaction occurs
as I suspect it does , for the formation of methylamine
perchlorate , then a powerful mixture would be the result , having a power and velocity as good as TNT or better , and higher sensitivity to detonation .

There are patents for the Ammonium nitrate reaction with formaldehyde , and the molar equivalent of ammonium perchlorate could simply be substituted as a starting point
for experimenting .

The two " formite " ( formaldehyde / AN reaction mixture ) patents that I know about are

EP0037862

GB1548827

Patent related to such mixtures value in cast melts

US1968158

[Edited on 29-7-2006 by Rosco Bodine]
Marsh
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Rosco, this is quite interesting...

I believe an experiment may be in store.

I'm going to see what I can come up with and I will reply back.

Thanks.
Rosco Bodine
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Glycine perchlorate is another possibility that has occured to me . Depending on the solubility , and I suspect this would work ....you could make a strong solution of glycine nitrate which is highly soluble and mix this with a saturated hot solution of ammonium perchlorate , and
hopefully ( possibly ) a precipitate of glycine perchlorate would result by double decomposition .
Of course if the glycine perchlorate is like urea perchlorate
which is extremely soluble this may not happen .

An alternate approach which may be better is to make a paste of glycine with a little water , add with stirring sufficient d1.4 nitric acid to neutralize the slurry and while still hot add solid ammonium perchlorate to the still hot paste , keeping it hot if necessary while continuing to stir the mixture until reaction is complete . This should force the reaction if the solubility of the glycine perchlorate is
high enough to cause problems with the first method .

The reaction should hopefully proceed by one of these methods , and the glycine perchlorate should be a
powerful explosive somewhere between picric acid and tetryl , probably more sensitive , and the hygroscopic
properties are unknown . I couldn't find any references to
glycine perchlorate , but the nitrate has been reported here in this group .

A similar reaction might proceed for hexamine dinitrate
and ammonium perchlorate , although the temperature
and time of reaction would be of consequence due to
the thermal instability of hexamine salts .

Double salts or sensitive mixtures could result from any of these reactions even if a precipitate does not occur ,
so drying to a residue and testing the residue mixture
should be part of the plan even if no obvious precipitate
appears .

Also a paste of urea nitrate and ammonium perchlorate
would likely result in a powerful mixture but this one is known to be hygroscopic . However it would form a powerful
slurry or perhaps a binary component of a melt having other
ingredients . It would be hard to get it dry and keep it dry
but of course it would be detonable that way too and it would be more powerful than the mixtures using only nitrates .

And then there is the possibility of Betaine Perchlorate
from the nitrate of Betaine .... lots of possibilities .

[Edited on 29-7-2006 by Rosco Bodine]
National Hazard

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Mood: @%&$ing hardcore baby  Quote: Originally posted by Rosco Bodine Shortened.... [Edited on 29-7-2006 by Rosco Bodine] I have some Trioxane which is the trimer of formaldhyde. The creation of formit requires a 37% solution of formaldhyde and ammonium nitrate. I wonder if the usage of water could be avoided and instead molten Trioxane could be subsituted in? Trioxane is the only OTC source of formaldhyde I have. @ the glycine idea. If all else fails you could find a eutetic mixture of Ammonium Nitrate/Perchlorate and glycine that melts at a lower temperature than 65C unless Ammonium Perchlorate eutectic mixtures are unaffected by the decompisition point of 65C. @ marsh.... I hear that Amines and Ammonium compounds sensitize explosive mixtures of nitromethane. I can't personaly comment on this because I haven't made Nitromethane explosives before... Ammonium Perchlorate has the lowest solubility of any Ammonium compounds in water that I am aware of. Your better off with Nitromethane, the suggested perchlorate compounds by Rosco, or possible Ammonium perchlorate eutectics. If you had Ammonium Nitrate or Sodium Perchlorate slurry based explosives would probably be a better choice. [Edited on 29-7-2006 by DeAdFX] Rosco Bodine Banned Posts: 6370 Registered: 29-9-2004 Member Is Offline Mood: analytical  Quote: Originally posted by DeAdFX I have some Trioxane which is the trimer of formaldhyde. The creation of formit requires a 37% solution of formaldhyde and ammonium nitrate. I wonder if the usage of water could be avoided and instead molten Trioxane could be subsituted in? Trioxane is the only OTC source of formaldhyde I have. It would be my guess that trioxane would possibly work even better than formalin or para in the methylamine salt formation reaction with ammonium salts , but I think some water will be required and the mixture will need to be stirred and may need to catalyzed at the start with a bit of hydrochloric or sulfuric , possibly phosphoric or acid . Enough formic acid should be produced as the reaction proceeds to maintain the depolymerization of the trioxane . It would be prudent to test this with a small batch at first , since this depolymerization and methylation reaction has potential for becoming autocatalytic and self-accelerating rapidly depending on the exotherm possibly resulting in a sudden boiling and even explosive decomposition if too little water is present to control the temperature by boiling away . This potential needs to be surveyed before scaleup to any large batch . Possibly urea may have to be omitted for this reaction to go properly using formaldehyde in the form of trioxane .....or maybe not , I am not sure . But the basic reaction should proceed . It might work as a melt phase reaction , but it could detonate .....this might be a good test for a small quantity in an expendable beaker on an expendable hotplate , melted together and observed remotely from behind some protective blast shield . Marsh Hazard to Self Posts: 79 Registered: 28-7-2006 Member Is Offline Mood: No Mood  Quote: I hear that Amines and Ammonium compounds sensitize explosive mixtures of nitromethane. I can't personaly comment on this because I haven't made Nitromethane explosives before... Ammonium Perchlorate has the lowest solubility of any Ammonium compounds in water that I am aware of. Your better off with Nitromethane, the suggested perchlorate compounds by Rosco, or possible Ammonium perchlorate eutectics. If you had Ammonium Nitrate or Sodium Perchlorate slurry based explosives would probably be a better choice. I have heard of them sensitizing ANNM, but used in low quantities I believe; thus being of limited use here it would seem. I would like to try an experiment with urea nitrate reacted with ammonium perchlorate. I am not familiar with these eutectics which you speak of either. And when you say AN/SP slurrys, are you referring to a slurry containing both of these in a water mix? DeAdFX National Hazard Posts: 339 Registered: 1-7-2005 Location: Brothel Member Is Offline Mood: @%&$ing hardcore baby

 Quote: Originally posted by Rosco Bodine SNIP

I have some time to do some experimenting. I will try melting Ammonium Nitrate 70%(.7) and Trioxane 30%(.3g) in a test tube. Nitrates seem to be very forgiving oxidizers. If I feel comfortable with AN/Trioxane then I will try AP/Trioxane. The test tube will be in a 400mL beaker containing water(I think 50-150mL sounds good enough). I will provide pictures too...
Marsh
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 Quote: Originally posted by DeAdFX I have some time to do some experimenting. I will try melting Ammonium Nitrate 70%(.7) and Trioxane 30%(.3g) in a test tube. Nitrates seem to be very forgiving oxidizers. If I feel comfortable with AN/Trioxane then I will try AP/Trioxane. The test tube will be in a 400mL beaker containing water(I think 50-150mL sounds good enough). I will provide pictures too...

Did you ever get to try this idea?

Anyways, on another note, can anyone comment on the possibility to detonate NH4ClO4 bound with HTPB or PBAN without booster?

I realize this is rocket propellant, but I was thinking with the right amount of binder it may be possible. Or is this simply much too insensitive a mixture? Personally I don't think it is possible, but if anyone else thinks otherwise I will try it.

I have both and I could test this tomorrow if there is possibility.

[Edited on 6-8-2006 by Marsh]
APCP
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 Quote: Originally posted by Marsh Did you ever get to try this idea? Anyways, on another note, can anyone comment on the possibility to detonate NH4ClO4 bound with HTPB or PBAN without booster? I realize this is rocket propellant, but I was thinking with the right amount of binder it may be possible. Or is this simply much too insensitive a mixture? Personally I don't think it is possible, but if anyone else thinks otherwise I will try it. I have both and I could test this tomorrow if there is possibility. [Edited on 6-8-2006 by Marsh]

Hmm, it *may* be possible to detonate if only a minute amout of binder is used. This would be similar to ANFO compositions, except, ofcourse, AP being used.

In actual APCP propellants used in HPR, the propellant can't be detonated (atleast in how I believe a detonation occurs.) Possibly a minute amout does detonate, but the majority does not. I have tested this using the grain from an Aerotech G80. It should have AP, HTPB, CuO, and possibly an anti-oxidizing adjent. To attemp to detonate, I used a cap containing half a gram of acetone peroxide, the 1 gram of ETN pressed to .8 g/in^3. The cap fired, and ripped the propellant into "chunks."

I will attempt this again at the next rocket launch (late August) to try to back up this data.

I'm not sure if anyone here knows, but the BATFE is trying to greatly restrict APCP motors by defining them as an explosive. The rocketry organizations are fighting this ruling and are, so far, winning. The final ruling by the courts has been pushed back to mid October.

Under the spreading chestnut tree, I sold you and you sold me. There lies they and here lies we, under the spreading chestnut tree.
Marsh
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 Quote: Originally posted by APCPHmm, it *may* be possible to detonate if only a minute amout of binder is used. This would be similar to ANFO compositions, except, ofcourse, AP being used. In actual APCP propellants used in HPR, the propellant can't be detonated (atleast in how I believe a detonation occurs.) Possibly a minute amout does detonate, but the majority does not. I have tested this using the grain from an Aerotech G80. It should have AP, HTPB, CuO, and possibly an anti-oxidizing adjent. To attemp to detonate, I used a cap containing half a gram of acetone peroxide, the 1 gram of ETN pressed to .8 g/in^3. The cap fired, and ripped the propellant into "chunks." I will attempt this again at the next rocket launch (late August) to try to back up this data. I'm not sure if anyone here knows, but the BATFE is trying to greatly restrict APCP motors by defining them as an explosive. The rocketry organizations are fighting this ruling and are, so far, winning. The final ruling by the courts has been pushed back to mid October.

I have CuO, and 200 mic NH4ClO4. I will mix up some batches (with detonator holes cast) to be attempted tomorrow.

I am into HPR myself; I never have understood the "banning" of AP as I personally have never once seen it used as explosive. Well whatever the gov't *tries* to do, I can assure they will never impede on my ability to continue experimental AP motors (the bastards can try, I'm stocked for life ). I have donated to this legal fund, and from what I have heard the BATF has so far poorly backed their side of the arguement in the courtroom. I'm really not too concerned as I don't think we'll lose.

Anyways to the point...I don't think there is anyway you could have det'd that G80 grain...being that it is probably >18% binder.

I don't have any PETN ready at the moment, but I will try 2.5g acetone peroxide on the following plastic mixture:

3% HTPB
1% CuO
7% Al
89% NH4ClO4

Then, same proportions of solids with 5% and 10% binder amounts in exchange for perchlorate (which will almost surely be too insensitive at this point).

I will post results as they cure, hopefully by tomorrow night.

[Edited on 8-8-2006 by Marsh]
Marsh
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Ok, grains have been cast but they cannot fire tonight unfortunately.

It was very hard to be precise at these amounts with curative on my scale, and is still quite soft; I may have used slightly too little isocyanate (but that's ok).

On the topic of perchlorates, I'm thinking about sensitizing NH4ClO4 with MEKP for a gel explosive. I do not know if the MEKP will absorb properly, though. I guess I will find out once I try it.

I don't know the exact molar weights for MEKP, but judging by an AN/MEKP ratio of 9:1 I found, I would believe something on the order of 6-8% by weight MEKP should be appropriate to do the trick, bound by xanthum gum.
APCP
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Yes, that should be fine.

When you do fire the charges, please video tape them, and record as much data as you can. More than just the members here will be curious on the results.

As for MEKP with NH4ClO4, it will work, I'm doubtful if it will form a gell. It will most likely have the texture of MEKPAN, but should give better results.

Under the spreading chestnut tree, I sold you and you sold me. There lies they and here lies we, under the spreading chestnut tree.
Marsh
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Reverting to my last post, I have been thinking...if MEKP/NH4ClO4 isn't quite sensitive enough for non-boosted detonation, there also exists the possibility of a three way MEKP/TCAP/NH4ClO4 mixture. This would allow higher solids content through addition of the TCAP and thus increased density of coarse, while allowing an obtainable desired density available by the MEKP/TCAP ratio, while also remaining less sensitive than a dry NH4ClO4/TCAP mixture alone.

Does this sound too good to be true, crazy, or probable to anyone?
Marsh
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NH4ClO4/TCAP/MEKP Success...

Well, the above mentioned combination sure as heck worked alright.

I started by the dual synthesis of TCAP in MEKP, with there being more MEKP product (should have been approximately 2:3 TCAP:MEKP). Of coarse you could simply add the TCAP to the MEKP, but I did it this way to kill two birds with one stone.

My MEKP this morning was very clear with just a slight white haze, and all MEK had evaporated out after getting it to about 95% last night.

I used a NH4ClO4:TCAP/MEKP ratio of 80:20, which I now believe could have been possibly 85:15 for more brisance. I arrived at this assuming a -150% oxygen balance from MEKP, so a correction may be in store if I'm off.

Cap used was about 2.5g TCAP (det in the photo is partially stuffed with kleanex, not full), and full-detonation occurred, with a very nice boom (but heck what doesn't have a nice boom...).

The total charge weight was 250g. As you can see I placed it into a cup, and set this inside the corner of a very heavy steel mining bucket. The steel in the very corner was a combination of layers up to 1" total thickness which it bent out. I really need to aquire some flat steel plate from somewhere, to test this against ANFO etc without confining the charge in the bucket. It would seem this stuff would nearly have to be much more powerful than ANFO, with the available fuel/oxygen content. I guess the main competitor would be ANNMSA or ANNM/Xylol. By the way, I only gave this about 10 minutes to sit after mixing as more rain was coming.

I will make more MEKP tonight, and test some other batches over the next few days, I'll try the other bucket corner next with 85:15.

Marsh
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85:15

Alright, for some reason I thought that the little dent the charge made earlier was high and mighty...

I decided I had to go back out tonight once the rain let up and test another charge, this time using a more correct 84:16 ratio for higher brisance.

This was a night and day difference. The charge completely mangled the steel surrounding it. The 1/4" thick base it sat on was easily penetrated and is gone.

I hate to make assumptions so quickly, but this stuff seems pretty darned powerful...possibly more than ANNMSA (the support bars this bent were 3/4" steel). I really need to do a plate test between them at this point.

The charge was slightly larger this time, at 285g (I decided to throw in the remaining bit left), but as you can see, the extra 35g was little in the whole perspective here.

It was again mixed and packed into a plastic cup, detonated with 2.5g TCAP.

[Edited on 11-8-2006 by Marsh]
Marsh
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Thought this powerful composition would have generated more interest, but I guess not...

I have thought about using Al in this composition to further increase power, but if I recall the MEKP may react with the Al in a negative way to do so.

At this point it is realized that the TCAP can be left out of the mixture, assuming sensitivity is still going to be moderate. It would help brisance just a bit to use the TCAP, and it remains in the liquid MEKP, but I do not know if it is worth the added trouble for anyone. I realize these primaries typically strike fear in large quantity, but with the MEKP in the mixture I feel this is a generally safe explosive when precaution is taken during the mixing/handling of it.

I will be testing some more of this tomorrow, hopefully I can locate a large plate to dent test this time.

I assume Vod's may be too low, but I would also like to try this in a few shaped charges to see if it is capable of anything good.

[Edited on 12-8-2006 by Marsh]
Eclectic
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Here is a link to a short discussion about a LiClO4/epoxy homogenous propellant formulation:
http://www.geocities.com/CapeCanaveral/Campus/5361/chlorate/...

There was a concern expressed that it might be detonatable. Anyone want to test it?
Marsh
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 Quote: Originally posted by Marsh I assume Vod's may be too low, but I would also like to try this in a few shaped charges to see if it is capable of anything good.

I managed to try this composition in a shaped charge tonight.

This charge had almost no confinement (plastic cup), and used a very mediocre means of a liner cone...a plastic rocket nose.

I can not get ahold of any copper cones, so I figured all I could do would be to try a design which more than likely wouldn't produce results, but just might.

Well needless to say, the results look promising. I used 200g total ammonium perchlorate/MEKP, at 85:15. It achieved almost 7mm of crater depth, at around 27mm max diameter. The plastic cone used was about this diameter, and about 35mm tall. Standoff was 30mm. There wasn't much overhead above the cone tip, so the wave may not have leveled.

Regardless, from a charge which in my opinion would have done nothing with an AN mixture, this achieved penetration. I believe with the use of a copper liner, this should easily be a composition suitable for shaped charges.

Since I cannot produce any copper cones myself, would someone out there be willing to test this composition who does have them? I have reason to believe vod's may be quite high, and I have interests in finding out if this is indeed true.

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I think partly the reason that people do not comment is because not many have access to ammonium perchlorate. If you did the same thing with NH4NO3, it might be of more direct use to people. However I think this's been discussed a lot elsewhere.
But don't fret, we all read it with interest!

BTW, for 200 g, do you really think this is impressive? It is quite a large amount.... and SC's have been made with smaller amounts. Did you try the same wiht proper HEs?

PS I also don't think you'll get much appreciation for mixing x with AP - I think it has been established that this is a risky thing to do.
I do like the MEKP idea though!
PS2 I can't imagine that a 5 % difference in AP supposedly makes such a big difference! ARe you sure there weren't other factors involved? This would be most surprising.

[Edited on 13-8-2006 by chemoleo]

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Rosco Bodine
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Clearly you got some jet formation to erode that crater
in the steel .

You are on the right track to use the coprecipitated
50/50 AP/MEKP as it is more dense and intense than
either peroxide alone . Some suggested mixture ranges
for this with NH4NO3 should be adaptable in the same way for NH4ClO4 oxidizer which you are using . Even though the mixture is sensitive enough to be set off
by an AP cap , it may not be producing its maximum velocity with that lazy sort of initiating impulse . To
really see what may be the maximum velocity you
should use a stronger detonator with a conventional
HE base charge like PETN or picric acid . It is also unknown what could be the practical minimum diameter
and charge mass for the composition to be useful as a shaped charge . For example at 50mm the composition may show no clue what it may be capable at 88mm ....it just depends on what the tests show about this sort of parameter .

I definitely would not mix anything else with such a mixture of organic peroxides and oxidizer , and avoid
contact with plastics other than polyethylene , maybe PET , or polypropylene or flourocarbons ....no vinyl , styrene , ect . and no metals either due to the reactivity of the MEKP .
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