Microtek
September 23rd, 2004, 04:56 AM
I would like to report some of the properties of the title compound, which I have just synthesized. Firstly, the method of preparation:
- 0.28 g 5-Aminotetrazole, which I had left from the nitrotetrazole synthesis of a few months ago, was added to 0.55 g 60% perchloric acid. It was stirred and heated slightly ( 30-40 C ) until all was dissolved.
- The solution was evaporated to dryness on a hotplate set to mild heating.
The mass of colourless crystals which appeared is very hygroscopic and very water soluble, but it is sufficiently sensitive that even a significant water content ( up to perhaps 30 % ) doesn't render it unresponsive to impact.
Flame sensitivity was tested as follows: A small amount ( ca 1 ug ) was placed on the tip of a spatula, and held over a candle flame. The sample quickly melted and fizzed from the moisture content that was boiling off. Then the remaining material burned with a quick flash, rather like smokeless whistle mix.
A sample was confined in Al foil and suspended over a candle flame. It deflagrated with about as much violence as blackpowder under similar circumstances.
Impact sensitivity was next: A sample was confined in Al foil ( I do this so I will be able to strike the sample multiple times without having the powder scatter all over the place ) and hit with a hammer on a steel anvil. It exploded with great violence, seeming about as sensitive and powerful as PETN in this test ( but note that RDX doesn't seem nearly as powerful as PETN when initiated in this manner, so it is a measure of its willingness to detonate from impact rather than its power ).
Friction sensitivity: Several small samples were ground with a ceramic pestle on the steel anvil. In one instance, there was a slight crackle, though not nearly enough to account for the entire sample decomposing. Other than this, no response was achieved.
Detonability: A brass tube having an ID of 2.0 mm and a wall thickness of 1 mm was prepared. It was filled to a depth of 14 mm with ATZ-perchlorate ( hand packed to a density of ca. 1.5 g/cc ), 3 mm PETN and primed with lead azide/styphnate 80/20.
On detonation, the witness plate showed a full detonation with almost no difference in dent size between PETN and ATZ-perchlorate.
Another test was done, with the title compound confined in a 2.5 mm drinking straw and initiated only with the azide/styphnate. This seemed to be a low-order detonation with very little deformation of the witness plate over the entire length of the charge. Obviously, I should have changed only one parameter, but I haven't got much to experiment with...
Conclusion: This seems to be a decent explosive although the precursors and the hygroscopicity makes it impractical as anything but a novelty for most of us. Having said that, it would probably be possible to remove the hygroscopicity by treating with a solution of blasting gelatin in acetone as was done in one of the patents on the ftp ( explosive composition from NG, NC and lead azide ) to remove the CO2 sensitivity of lead azide.
Another interesting point is that the noise from the detonation of ATZ-perchlorate seems to be quite low relative to its power ( I could be wrong; it is a little difficult to tell from such small charges ).
- 0.28 g 5-Aminotetrazole, which I had left from the nitrotetrazole synthesis of a few months ago, was added to 0.55 g 60% perchloric acid. It was stirred and heated slightly ( 30-40 C ) until all was dissolved.
- The solution was evaporated to dryness on a hotplate set to mild heating.
The mass of colourless crystals which appeared is very hygroscopic and very water soluble, but it is sufficiently sensitive that even a significant water content ( up to perhaps 30 % ) doesn't render it unresponsive to impact.
Flame sensitivity was tested as follows: A small amount ( ca 1 ug ) was placed on the tip of a spatula, and held over a candle flame. The sample quickly melted and fizzed from the moisture content that was boiling off. Then the remaining material burned with a quick flash, rather like smokeless whistle mix.
A sample was confined in Al foil and suspended over a candle flame. It deflagrated with about as much violence as blackpowder under similar circumstances.
Impact sensitivity was next: A sample was confined in Al foil ( I do this so I will be able to strike the sample multiple times without having the powder scatter all over the place ) and hit with a hammer on a steel anvil. It exploded with great violence, seeming about as sensitive and powerful as PETN in this test ( but note that RDX doesn't seem nearly as powerful as PETN when initiated in this manner, so it is a measure of its willingness to detonate from impact rather than its power ).
Friction sensitivity: Several small samples were ground with a ceramic pestle on the steel anvil. In one instance, there was a slight crackle, though not nearly enough to account for the entire sample decomposing. Other than this, no response was achieved.
Detonability: A brass tube having an ID of 2.0 mm and a wall thickness of 1 mm was prepared. It was filled to a depth of 14 mm with ATZ-perchlorate ( hand packed to a density of ca. 1.5 g/cc ), 3 mm PETN and primed with lead azide/styphnate 80/20.
On detonation, the witness plate showed a full detonation with almost no difference in dent size between PETN and ATZ-perchlorate.
Another test was done, with the title compound confined in a 2.5 mm drinking straw and initiated only with the azide/styphnate. This seemed to be a low-order detonation with very little deformation of the witness plate over the entire length of the charge. Obviously, I should have changed only one parameter, but I haven't got much to experiment with...
Conclusion: This seems to be a decent explosive although the precursors and the hygroscopicity makes it impractical as anything but a novelty for most of us. Having said that, it would probably be possible to remove the hygroscopicity by treating with a solution of blasting gelatin in acetone as was done in one of the patents on the ftp ( explosive composition from NG, NC and lead azide ) to remove the CO2 sensitivity of lead azide.
Another interesting point is that the noise from the detonation of ATZ-perchlorate seems to be quite low relative to its power ( I could be wrong; it is a little difficult to tell from such small charges ).