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Author: Subject: Pseudo-Pentolite via ETN and TNT?
Hennig Brand
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[*] posted on 8-12-2014 at 04:50


Oh at least one more; someone with a great deal of experience and skill in the art of frugality could likely squeeze in several more shots. :D;)



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[*] posted on 8-12-2014 at 07:09
Tetrolite Friction Sensitivity Testing


A crude friction test was performed on ETN, melt/cast ETN, co-precipitated Tetrolite and melt/cast Tetrolite. A set of bathroom scales was used to measure downward force applied. A marble pestle, from a pestle and mortar set was used. A piece of carbon steel with surface rust was used, which was extremely abrasive. Downward force was kept between 40-45lbs as the pestle was drug over the sample (ca. <5mg sample weight). The pestle was rubbed across each sample six times or until ignition. The only sample that was initiated by this treatment was the melt/cast ETN, which produced a loud snap.

1. Powder ETN....................................No ignition
2. Melt/cast ETN..................................Ignition
3. Co-precipitated Tetrolite (granular)....No Ignition
4. Melt/cast Tetrolite............................No Ignition


Equipment.jpg - 256kB Measuring Downward Force.jpg - 253kB

Note:
I suppose the rust could be seen as a contaminant and could have altered the sensitivity of the sample it mixed with. It was of course a crude test and if anything the rust would have likely increased sensitivity not decreased it.


[Edited on 8-12-2014 by Hennig Brand]




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[*] posted on 8-12-2014 at 09:58




[Edited on 8-12-2014 by Laboratory of Liptakov]
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[*] posted on 8-12-2014 at 10:12
Holes


This is a pretty good method. Test friction. And the results are good. Sensitivity is low.
I also have results ........:cool: Also, saving material....LL

det.jpg - 456kB
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[*] posted on 8-12-2014 at 10:33


Nice collection! I would have quite a pile too, at this point, if I went around and gathered everything up.
I was thinking of performing an impact sensitivity test on molten Tetrolite. I could easily heat a small anvil up with a propane torch to above the melting point of Tetrolite. I have a small 11lb anvil that would likely work well.


TNT Acidity

It was brought into question a while ago whether or not the acidity of TNT would be a stability problem for mixtures of it and ETN. I still don't have a definitive answer, but I understand better now what I am dealing with. ETN is much less storage stable than PETN and this instability gets worse in the presence of acidity. Gladly, it turns out that TNT has extremely low acidity. Also, TNT and ETN are non hygroscopic and have very low solubility in water. The attached jpg image below was made from the first few paragraphs of page 300 from Urbanski Volume 1.


TNT has extremely low acidity.jpg - 245kB


[Edited on 8-12-2014 by Hennig Brand]




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[*] posted on 10-12-2014 at 05:57


Acidity of TNT only express in strong alcaline media (NaOH for example)...the resulting compound is coloured red and this is a proof of an aci-nitronic/nitronate form. The resulting form is also more sensitive to shock (impact sensitivity).

The rest of the aromatic ring has been left aside because it doesn't enter the reaction
CH3-C=C-NO2 <==--> CH2=C-C=N(O)-OH
CH2=C-C=N(O)-OH =NaOH=> CH2=C-C=N(O)-ONa + H2O

So there is no acidity concern to fear about TNT in admixture with ETN...as long as both ingredients are wel acid-free washed
and recristallized.

[Edited on 10-12-2014 by PHILOU Zrealone]




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[*] posted on 10-12-2014 at 13:25


Thanks for the great description.
There really are a lot of things that can be done with TNT that can't be done with picric acid. For instance, because it has virtually no acidic properties, a relatively low melting point and great compatibility with most other explosives, among other desirable qualities, TNT can form many useful mixtures with other explosives. Picric acid has its place too though; it is much easier to make and many other useful explosives can be made from it. Picric acid seems a bit easier to use as a base charge as well. Both of these cousins have a lot going for them.


[Edited on 11-12-2014 by Hennig Brand]




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[*] posted on 19-12-2014 at 12:47
Cast 50/50 Tetrolite Base Charge Explosive Testing in 7.6mm id Aluminum Casing


I found some more witness plates, so this is the last time I will show this over exploited old one.

A while ago now I tested some cast 50/50 Tetrolite. A stainless steel pot with ca. 60-70C water was used to melt the 50/50 tetrolite. The aluminum cap casing was taped to the side of the pot so that it would also be above the melt point, which prevented premature solidification and also provided a larger thermal mass allowing for slower cooling of the casting. The tetrolite was melted in a small polypropylene plastic container partially submerged in the hot water.

Three cast 50/50 tetrolite explosive tests have been performed all with similar results. The first test involved 1g cast tetrolite with 0.2g of lead azide pressed on top. The second test involved 1g of cast tetrolite and 0.3g of LA pressed on top. The third test involved 0.75g of cast tetrolite, 0.25g of granular tetrolite pressed on top and 0.3g of LA pressed on top of that. A little basic lead picric was used as flash igniter in all tests. None of the tests showed the plate penetration that the pressed granular material displayed. The cast material did however make by far the biggest dents in the witness plate that I have seen so far. I assume at this point that cast 50/50 tetrolite has a lower detonation velocity at the 7.6mm charge diameter than does pressed tetrolite. I will need to test the cast tetrolite at a larger diameter to see if that shows an improvement (I suspect it will).

Attached are a few pictures from one of the tests. The hole/dent and scab on the right, in the witness plate top and bottom views, are from this test. Last time using this witness plate I promise. :)

Melt-Cast Tetrolite.jpg - 162kB Cap in place.jpg - 212kB Witness Plate Top View.jpg - 241kB Witness Plate Bottom View.jpg - 221kB Witness Plate Side View.jpg - 195kB


[Edited on 20-12-2014 by Hennig Brand]




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[*] posted on 20-12-2014 at 07:00
Tetrolite Impact Testing


I built an impact testing machine in the last few days. I spent a bit of time in the past watching a large electromagnet being used to move scrap metal around at a scrap yard and noticed that when the electromagnet was de-energized the steel fell basically instantaneously and straight down. I though it would make a great quick release mechanism for a fall hammer. The fall hammer quick release could be controlled from as far away as desired by running a thin copper pair with a switch at the end. An electromagnet was made from an old 16V, 1A, "wall wart" type DC power supply transformer. The core was cut off at one end with a hack saw and the 16V secondary winding was removed. The top of the hammer head was too small and rounded so a steel plate was welded onto one end for the magnet to attached to. It was found that 5V DC, across the 120V primary winding, was more than enough to hold up the 2.85kg hammer, but 9V DC was used instead which could hold the weight of at least several times the weight of the hammer. A wooden slide was made, for height adjustment, which could be fixed in place by tightening a wing nut. A plumb line was made from a bit of nylon cord and a steel nut was used as the plumb bob which allowed me to determine exactly where the fall hammer would land and position the anvil and punch assembly accordingly. Simply because of availability, 13/16 inch soft steel round stock was used to make the anvil and punch (roller bearing would have been preferable and possibly in smaller diameter). A wooden holder was made for the anvil and punch with two large vent holes for explosive gases and flash to escape from. The bottom end of the 13/16 inch anvil sits on the large blacksmith's anvil below.

This test was a quick and dirty test in a number of ways. It was in large part an excuse to test the apparatus. The ETN used for the ETN test was of unknown purity and not freshly made; it was removed from a section of detcord which was made over 3 years ago and was a very fine powder. From earlier testing of the machine, I knew about were the starting height should be for this sample of ETN. The sensitivity of the ETN tested seemed uncharacteristically low. The test will be repeated when a freshly made, recrystallized, sample of ETN is available. Also, as has been discussed before, wrapping the sample in aluminum foil does effect the results, at least to a small extent, as it is soft and will absorb some of the force of the blow. The height was increased by 2 inches after each no go test.


Results (2.85kg Fall Hammer and 13/16 Inch Punch and Anvil):

ETN Powder
22 inches - no go
24 inches - loud bang

Tetrolite 50/50 Co-precipitated/Granular
24 inches - no go
26 inches - loud bang

Tetrolite 50/50 Cast
26 inches - no bang but smell
28 inches - no bang but smell
30 inches - small snap, a lot of smoke and smell



Here are a few pictures of the apparatus:

Homemade Electromagnet.jpg - 249kB
Hammer Magnet and Height Adjustment.jpg - 180kB Anvil, Punch and Hammer.jpg - 275kB Sample On Anvil.jpg - 150kB Hammer Lined Up With Punch.jpg - 287kB Hammer Lined Up With Punch (2).jpg - 302kB Set-up for Test.jpg - 307kB


[Edited on 20-12-2014 by Hennig Brand]




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[*] posted on 20-12-2014 at 07:46


I continue to be impressed with your testing program.

I spoke about drop tests some time back with a manufacturer of industrial testing & quality control equipment. They did indeed use an electromagnetic drop mechanism. The rig also automatically reset, logged heights of tests, all the tech did was set a new anvil plate & sample in place-

It was HIDEOUSLY expensive, came with a nice software suite though.




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[*] posted on 20-12-2014 at 08:53


Thanks, good to know I was on the right track with the electromagnet as well. Much better electromagnets can be made or bought. I watched a professor pick up a ca. 120lb girl off the floor, who was holding a handle or sitting in a harness attached to a steel plate, using a small round electromagnet (ca. 2-3 inches in diameter) powered by one, 1.5V, D sized battery in a first year electrical engineering class. The magnet he used was rated for up to 500lbs, IIRC, and was obtained mail order from a scientific supply company. I think they went for about $100 the last time I checked. The professor told me the same D battery had been used for about 5 years to do the class demonstrations. Those designs are much more highly optimized than the one I made from an old transformer, but the one I made does the trick (at least for this application). Making a highly optimized and powerful electromagnet has been on my to do list for a while.


[Edited on 20-12-2014 by Hennig Brand]




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[*] posted on 20-12-2014 at 14:33
hammer


I have this idea. Why use a plumb line? Motion in the picture. Replaceable paper tube. Small window for precise adjustment and control before the test. The paper tube is a plug-in. Not too much force. Not too freely. In short, just right. I suggest pipe inner diameter of about 15 mm. If it blows, the paper will be destroyed. But if not, it can be used again. On the right in the picture is a simple version without solenoid. Plastic pipe with a diameter of about 50 mm or 2 inches....:cool:....LL

kast.jpg - 89kB
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[*] posted on 20-12-2014 at 15:24


The plumb line is only used to position the anvil under the hammer then it is put up out of the way during the test. So in your design the anvil, punch and hammer all fall onto the main anvil below? All of the commercial designs that I have seen have a track or guide of some sort on either side of the hammer, which has advantages. For starters, it guides the hammer to the target and the hammer doesn't need to be picked up off the ground either. The free fall design has some advantages too, however, it is simpler and cheaper to build, one can be sure that there is no resistance to motion other than wind resistance during the fall as well. I think your plastic tube idea could probably work, not sure about the release mechanism though. I wanted a true falling hammer and I wanted it simple and I suspected that if I got into shoots and tracks and things that I could easily get into problems with friction unless I went complicated or expensive (tracks). The solution to not having to aim the hammer every time is to build a better stand for the apparatus. The stand could have been made with two vertical members, like in Markx's design and most commercial models, which were carefully made as close to perfectly vertical as possible and well fixed in that position. With this setup, no matter what height the hammer was put at it would always hit more or less the same place every time (gravity is a wonderful thing; very reliable). Even one vertical member could be used but it would need to be made to more exacting standards than I made mine. This is only a prototype model. :D


Laser Plumb Line

Ok, I just thought of a nice solution to the hassle of the plumb line. The plumb line I am using now must have its length adjusted nearly every time the hammer height is adjusted and being so long it can be a bit unwieldy to work with and a bit of a bother to make steady. I have been thinking of how to use a laser level or laser pointer in some way that would be more convenient but still be as reliable. I kept discarding ideas because most of them seemed less reliable and less accurate compared to a plumb line. A laser plumb line though incorporates the good points of both the laser and the plumb line and loses most of the negative attributes of the regular plumb line. It can be made much shorter and never needs to be adjusted for height, since the laser beam can travel the distance and mark the landing spot. Since the plumb line is shorter, it is easier to steady and also easier to put up out of the way during tests. I found the attached picture of one online.


Laser Plumb Bob.jpg - 5kB


[Edited on 21-12-2014 by Hennig Brand]




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[*] posted on 21-12-2014 at 15:34
nice work


OK results are important and these are at the top. Tetrolite granules cast and are less sensitive than ETN. That's the main thing. All three samples have low sensitivity. That's good, nice work ....:cool:...LL
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[*] posted on 21-12-2014 at 18:33


Thanks, I expect that the sample of ETN powder I tested was less pure and more insensitive than it should be however. You are right though, tetrolite both granular co-precipitated and cast is definitely at least a little less sensitive to impact than ETN which is an important thing to know.



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[*] posted on 21-12-2014 at 23:33


Excellent work, Hennig!
The ETN sensitivity really seems very low, a characteristic result for a fresh recristallised and purified sample would lie on the order of 30-40cm drop height which translates into about 10-15 inch. At least it does so on my particular drop test machine. Then again the results of drop test may vary quite significantly between different machines depending on construction, materials, placement and substrates. Hence it is hard to compare the values from different testers, but comparing the relative differences of samples tested on one and the same apparatus should give a better perspective.
Perhaps you could also incorporate a mechanical failsafe for the electromagnet in case the power circuit should fail or become damaged for some reason. Electromagnets are strong, but the only thing keeping the hammer from falling is the electrical current...one bad solder joint or damaged switch and a premature drop is the result. There is no real danger of a serious injury if the sample weigths are kept normal, but the effect of thescare that the noise from a 3kg hammer hitting an anvil accompanied by the possible detonation of the sample can give you is quite enough for me to incorporate some preemptive measures into the system.
Also building a basket around the anvil to catch the falling hammer after if has hit the target is really convenient....and prevents the thing from landing on your toes after every test :D

Perhaps something like the one I did here:

http://www.sciencemadness.org/talk/viewthread.php?tid=32296&...





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[*] posted on 22-12-2014 at 05:10


Thank you. Yeah, that ETN is very likely much too insensitive. The ETN used to make the tetrolite was from a much more recently made batch. I built the apparatus in a bit of a hurry as well, so I should go back and carefully check that the anvil and punch surfaces are really flat and smooth and actually flush with each other. The aluminum foil probably shouldn't be used either, but I would need to test to see how much of a difference going without it would make. A basket to catch the fall hammer would be convenient for sure. I have a procedure which I think is fairly safe though. The sample is placed on the anvil and lined up under the hammer release. The hammer is put in place last and then a bit of downward force is placed on the hammer by hand to be sure that it is really secure. The position of the anvil is verified with the plumb line before the line is moved out of the way for the test. Currently about 15 feet of speaker wire (copper pair) is used which allows me to be well away from the apparatus, and behind cover if desired, when the current flow is removed from the magnet.


Battery Backup Failsafe

Some of the old backup lighting systems, security system and things had a very simple battery backup system, so I was told by a technician years ago, that used a single diode. I have used the following concept several times in the past. If the AC power, or power supply, fails for whatever reason current will immediately start flowing through the diode from the battery when the voltage on the cathode side of the diode drops below that of the battery by about 0.6V (for a silicon diode). This is a very simple circuit compared to many modern battery backup systems, without some of the advantages, but it is very reliable, simple and cheap. I made a little sketch with paint to illustrate the concept. Of course a mechanical failsafe could also be used, with or without the battery backup.


Simple Battery Backup For Electromagnet.jpg - 48kB


[Edited on 22-12-2014 by Hennig Brand]




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[*] posted on 23-12-2014 at 15:50


It just occurred to me that what I need are adjustable feet for the fall hammer apparatus. The vertical member could maybe have been positioned closer to perpendicular the base, during assembly, but the truth is almost no floor or ground is perfectly level anyway. A way to quickly make adjustments to make the apparatus level would be a good addition. This would reduce the need to make adjustments of anvil position below the fall hammer whenever the height was adjusted.


[Edited on 24-12-2014 by Hennig Brand]




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[*] posted on 30-12-2014 at 19:22


Here is an alternative to an electromagnet for the drop hammer device. It is a permanent magnet inside a light casing for picking up iron, steel and other magnetic objects. A spring is inside which holds the magnet against the thin non-magnetic bottom plate. When the handle, which is attached to the magnet by a rod, is pulled the magnet comes away from the plate which releases any objects magnetically coupled. If a suitable commercial model could not be found, to hold up the fall hammer used, one of these could be built or the magnet in a commercial model could be replaced with a more power magnet. Before I built the electromagnet I was playing around with a car speaker magnet. These speaker magnets are often extremely strong and have no problem holding up a hammer head of several kilograms. Some sort of lever or pulley arangment, above the permanent magnet assembly, could be used to change the direction of force and possibly provide mechanical advantage allowing the hammer to be released from a safe distance by pulling a thin cord.

53.360.jpeg - 32kB


[Edited on 31-12-2014 by Hennig Brand]




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[*] posted on 2-1-2015 at 12:37


Quote: Originally posted by Hennig Brand  


Results (2.85kg Fall Hammer and 13/16 Inch Punch and Anvil):

ETN Powder
22 inches - no go
24 inches - loud bang

Tetrolite 50/50 Co-precipitated/Granular
24 inches - no go
26 inches - loud bang

Tetrolite 50/50 Cast
26 inches - no bang but smell
28 inches - no bang but smell
30 inches - small snap, a lot of smoke and smell


A freshly made and recrystallized from methanol sample of ETN was just tested three times and the average fall height which resulted in initiation was 15 inches using exactly the same testing method and apparatus as was used for the earlier testing. The temperature in the building where the testing was done, this time and last, was below zero Celsius which could have at least partially resulted in lower values for sensitivity. Since the tetrolite was made with ETN that was only a month or two old and was recrystallized and well stored, it is safe to say with a high degree of certainty that tetrolite, either co-precipitated or cast, is significantly less sensitive to impact than straight crystalline ETN.




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[*] posted on 2-1-2015 at 14:07
etn


This is an interesting change, but it's still pretty good sensitivity. Clean fresh ETN, hammer almost 3 kg, height 38 cm, it is still good ...:cool:...LL
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[*] posted on 7-1-2015 at 13:12


I got an idea about another melt-castable based on TNT. It could maybe be called "hexolite", but not from mannitol hexanitrate. The much more potent and denser oxidizer hexanitroethane should give a slightly better bang. 63.4% HNE and 36.6% TNT is oxygen balanced and should be possible to cast safely, at least with some care. A similar but non-cast mixture with HNE and tetryl was tested in an old thread found here

The downside would be that the mixture can prove to be quite sensitive. Pure HNE is like PETN, but a mixture with a fuel will likely be more sensitive; that's at least the case with TNM-based mixtures.
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[*] posted on 8-1-2015 at 02:42


Perhaps coprecipitation from a common solvent or solvent system could also yield interesting results with some combination of energetics....and likely be a safer practice compared to melt casting. I do not particularily like the idea of melting together highly potent substances...



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[*] posted on 8-1-2015 at 10:23


Hard to ignore the great ease with which very well incorporated mixtures can be cast at high density and with great uniformity however. The advantages for shaped charge applications, for instance, are tremendous. Pentolite is a very common melt/cast mixture that is used both militarily and commercially and all reports I have seen would indicate that it is fairly safe to work with. Tetrolite (ETN-TNT) can be melted below 50C using hot water much below the boiling point. As long as open flames, or other intense localized heat sources, aren't used the melt/cast process should be fairly safe in my opinion. I have several samples of tetrolite which have been sitting around for a month or so, both co-precipitated and melt/cast, and so far there appears to be no signs of decomposition. The melt/cast samples have been re-melted and cast several times too. I do proceed with caution though when working with such things.



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