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nuclearattack
October 15th, 2004, 04:49 AM
I decided to open this thread because i noticed that a lot of members wrote some questions on these subjects in Nitroglycerin thread or in others thread.
There isn't a thread dedicated only to EGDN or blasting gelatine so it can be usefull to have a thread that concentrates all the questions about nitric esters and gelatine based compounds.
I love very much nitric esters and i think that blasting gelatine is one of the best HE because of its power and because it is relatively easy to prepare.
In the nitroglycerin thread i read that kinetic and others members are interested in the BG sensitivity when it is stored for a long time, well i haven't got a lot of experience in this trouble because i always prepare my BG some hours before detonation but i read on COPAE that adding AN and a fuel (Al powder should be the best fuel) will give a good sensitivity even after long storage. This is good because you can prepare a lot of Ng and convert it in BG that is safer.
However there is a question in my head that i want to discuss.
Everybody knows that NC is a bit hard to neutralize and you have to wash it a lot of times to have a stable product. Now suppose that a little acid NC is used to make BG...how this little NC acidity affects the BG stability?
Can BG become too sensible or instable?
This is important especially when large amounts of BG are used and with large amounts i mean also only 50 gr!

me234
October 15th, 2004, 11:55 AM
BG becomes less sensitive with storage because when it's made, lots of miniscule air bubbles get trapped inside it, these provide sites for hotspots to occur at I think. With storage these 'fade away' or something, leaving the BG less sensitive.

I think it has something to do with any energy in the explosive (heat and the like) being unable to diffuse away from the air bubble as quickly as in other places. This should be due to the lower heat capacity of air as opposed to the explosive. In the rest of the explosive the energy diffuses away uniformly from wherever point the energy is being supplied to, but against the side of an air bubble it can't as some of the places it would have diffused through are occupied by the air. The energy builds up, hot spot.

Just soes you know this is just my theory, I don't actually know what precisely happens.

Myrol
October 15th, 2004, 01:53 PM
Umm, well. I made some months ago a sample of Blasting Gelatin with ?ml NG 3,5g NC and 5g Al. The whole mix weighed 34g and filled up 3/4 of a small Filmcanister. I added a lot of NC compared to NG because my NC gelled the NG to bad that it worked with the aimed 2,5g. The Explosion made a very sharp shockwave and a Flame even inside a muddy Jet/Mushroom. I also want it very often to make some original Methylnitrate to compare the performance with pure NG. Methyl Alcohol is very rare here, yes I can Distill it out of Racing Fuel but thats sucking time, wich I dont have! Has somebody an Idea how to stretch EGDN with Aluminium without adding a solid powder like AN? I want to see the power of my EGDN with 25% Al but I think it sinks to fast down to mix it thourougly...Gelatinizing is probably the only way so I need NC!!

nuclearattack
October 18th, 2004, 08:23 AM
To ME234:
your theory is interesting, air bubbles create hot spots for sure but they also lower the BG density, it works like microballons in ANFO or other kind of insensitive explosives.
Al powder should do the job very well and it adds a lot of energy output but i think that adding too much Al will decrease the sensitivity, 20% of Al should be a good choice but i have to make some tests to say this for sure.
Actually i'm out of NC, i noticed that making NC is not so easy, sometimes i have a good NC that burns fiercely and gells very well, sometimes i have a pathetic NC with surely low Nitrogen content.
I'm bothered about wasting all this acid for NC so i'm looking for single base smokeless powder (pure NC), as i have smokeless powder i'll do some tests.
What if i use DBSP? It has a bit of NG in it so it is more powerfull but i think that it is unusefull because to make BG i'm already adding a lot of NG!

To Myrol:
I'm interested too in Methylnitrate but the problem in making BG with it is it's volatility. You should use a airtight container.
Another problem should be how to dry it from water without let it evaporate too much. You know that when you wash it after synthesis you have to let it on a dish to evaporate the water in it, but myrol (not you! i mean the explosive!) evaporate faster than water! I don't like to distill it. It could be dangerous and it's boring, and you will lose some in any case because of the apparatus losses.
What do you think?
Also EGDN evaporates faster than water, what is your experience with it?
About Methyl alchool i can buy it in racing shops but it contains 5% of castor oil, it is not so much oil so the nitration should work without distillation.
However i'm looking for another supply store that sells pure Methyl alchool.
Myrol should be the most powerfull nitric ester and also the most stable in a acid environment, it is also less shock sensitive than NG.
You have to do this synthesis to honor your nickname!
About me it's better that i don't honor my nickname!

Alek
October 18th, 2004, 02:40 PM
i think DEGN is great and you must try it.
it's better than EGDN because it's not airy and after nitration you haven't got head ache :)

Myrol
October 19th, 2004, 01:55 PM
Hi Nuclearattack! Do you really think that EGDN evaporates faster than Water? Well, my EGDN evaporates significant, I can smell the Alcoholic odor if I open the Bottle but faster than Water? Im confused, could be true.

In the sooner Future, I will buy me some Liters Methanole. Nitric Acid is no Problem, so Myrol seems to be a must for me :D :D I have made PETN around 85g. I have made EGDN know around 60ml. I have made NG more then 300ml but Myrol?? Not the slightest trace :o Damn, its also embarassing for me that I haven't never made Picric Acid. Thats a Just-for-Fun stuff. Typical Lab Job huh?

You can make Myrol in two ways: Via Distillation with Nitric Acid or via Nitration like the way with our all known Blasting Oil's :) I think I try the second method, safer and faster! Washing must be also done with very cold Water, otherwise you get terrifying headaches. Myrol evaporates extremly fast. Like Ether with the boiling poinbt of CH3OH. The plus is his good stability against Acids. I store my Explosives mostly over a long period, so I think I will wash him very good to prevent a bad surprise. To get the rid of the Water in it: Filtrate it over dry Sodium sulphate. Distillation is also a way. Pure Methyl nitrate boils very safe without any problems, I have a Vacuum pump so I can do it under minimized pressure perhaps at Roomtemperature :p Pretty funny that stuff, hahaa we'll see. I'll do my Honor :)

me234
October 25th, 2004, 02:01 AM
I was also thinking about how to dry methyl nitrate. I agree with myrol, Glaubers salt sounds promising for dehydration. The other salt I should like to try would be calcium chloride. It's used quite often to dry organic liquids. If I ever get up the nerve to make some methyl nitrate I'll test some of each to see if there're any reactions, but I doubt there would be.

nuclearattack
October 26th, 2004, 06:18 AM
I'm thinking about the sensivity of blasting gelatine after long storage. As just said, BG lose sensivity because it becomes stiffer with long storage and the air bubbles disappear. Is it possible to refresh BG after long storage to increase the sensivity?
My idea is to add acetone to BG until it becomes more soft and it loses NG.
When acetone evaporates there should remain a new fresh BG.
I don't know if it works, maybe it's a stupid idea, but i want to make a test as i get some smokeless powder to make BG.

About Myrol:
Myrol has an energy content higher than NG and this is also for EGDN but what is the more powerfull between EGDN and Myrol?

Ropik
October 26th, 2004, 01:27 PM
One of my blasting handbooks says that the BG has a metastable detonation without the bubbles, but stable det can be achieved by small (10 grams) PETN or RDX initiating charge or (this is the important thing) by kneading BG thoroughly, because this should (presumably) put new bubbles into it. Maybe its that simple - little acetone (preferably, but not entirely necessary) is added and the BG kneaded. End of story.

nuclearattack
October 30th, 2004, 03:34 PM
Today i tried for the first time to make EGDN. I never made it because i'm very satisfied with NG but now i want to see how works EGDN.
I started the reaction as for NG and i have to say that i was very satisfied for the short time it is required for EGDN to form. This is the main problem i think! I was nitrating the last 4 gr of EG (the entire quantity to nitrate was 27 gr) when suddenly it started to make "hssssss" and very thick red fumes started to form very quickly. Noooooo! A runway nitration i thought!
Damn i started to sweat cold! I immediately poured some cold water in the baker and the solution started to cool down. Wow! This is my first runway and i hope this is the last!
I wonder, i made NG lot of times and it is far more stable during the reaction!
I think it is because glycerin is more dense and requires more time to react so it is easier to control the temperature. Ethyl glycole is very liquid, less dense and this make it to react very quickly. The reaction was proceding perfectly and suddenly all went wrong!
EGDN is more shock stable than NG, and it is less sensitive in a acid environment than NG but i'm sure that NG's nitration is safer!
What is your experience with EGDN nitration?
It is only sufficient that i increase the time reaction letting it rest between the ethyl glycole addictions? This should let it cool down more during the reaction.
In NG procedure is used to extract the baker from the ice bath and let it rest until it reaches room temperature, then the solution is stirred for some minutes and poured in water. What if i do this for EGDN? Do you think that it will start to runway when i extract it from the ice bath?
I made a step back about EGDN until i see perfectly how to make a perfect nitration.

Myrol
October 30th, 2004, 06:01 PM
Well, Nuclearattack......Yes the Nitration of EG give you somewhat more heat as for the same amount Glycerine. This and the greater mobility result in a more violent Nitration as for NG. In my first attemtion to make EGDN I had no problems to control the heat. With a Bucket full of Ass-cold Water it shouldn't be a problem to do our Job. I dont remeber when I made my EGDN.....but its so stable that it shows absolutely no sign of decomposition even after this long period of Time. I think its older than two months.

The EGDN wich stands beside me was washed very very good. A 50ml sample only neutralized with distilled Water. Soon, I will make a lot more. The most trouble brought PETN to me. Tooked a lot effort with cooling and resulted again in a "nearly-runaway" :o :mad: Umm, pure Ethyl nitrate should be also a strong Explosive, huh? If try to Nitrate some Ethyl Alcohol with my freshly arrived Nitric Acid it could be worth to get some terrible headaches :D

grendel23
October 31st, 2004, 01:08 AM
nuclearattack,
You should never add water to strong acid, it is not safe. Instead, dump the beaker into the cold water bath you have ready in case of a runaway.

nuclearattack
October 31st, 2004, 04:09 AM
To grendel:
yes i know that is not a good thing to dump water in acid but during the runway i thought: there is a runway and the EGDN that is just formed is in a supersensitive state, if i move the beaker the vibrations can make it explode.
This is why i decided to don't move the beaker, plus there were so nox thick fumes that i wasn't able to take the beaker infact i poured the water in it from the distance.

me234
November 4th, 2004, 06:21 AM
OK Myrol, time to earn your namesake. You say that more heat is evolved per mass of ethylene glycol nitrated, than for propan triol, so I'm guessing the same applies for methanol. When you say this, are you just refering to the lower molar mass of EG, hence more moles reacting per mass than for glycerine, at approx. the same molar heat of reaction (guessing here), therefore more heat per mass for EG?

Sorry if it sounds jumbled, couldn't quite find the words I was looking for.

nuclearattack
November 9th, 2004, 08:25 AM
To Myrol and Me234:
I have extracted all of my EGDN from the water and i let it dry on a plate for 3 days. I noticed that i lost some of it but not too much.
How much EGDN do you lose during the drying phase?
How much do you wash your EGDN to neutralize it?
I'm asking this because i'm very satisfied about the high yelds of EGDN but i want to minimize losses during washing and drying.

nuclearattack
November 20th, 2004, 02:42 PM
I nitrated another batch of EGDN and i must say that it gave me very good yield, more than NG. With 66gr of ethylene glycole i had 89gr of dry EGDN.
Very good! I optimized the drying phase extracting some water with a syringe so it needed only one day to be dry, i can say that i didn't lost significant EGDN from evaporation.
About EGDN power i know that it is a little more powerfull than NG with the same taken weight, but NG is more dense. Maybe that NG is more powerfull than EGDN from the volume point of view. If i fill the same charge with NG it will weight more than with EGDN and it should be more powerfull than with EGDN.
Of course the difference should be very small and it should be very difficult to compare without a precise trauzl test.

nuclearattack
December 3rd, 2004, 05:57 PM
I bought 1 kg of smokeless powder, on the label is written: pure 98% nitrocellulose.
I always make my blasting gelatine with homemade nitrocellulose and i can say that it worked well but surely it is too expensive to make NC so i decided to try with smokeless powder.
This SP is dark gray grains and when i try to gelatinize it in acetone it becomes a stiff black mass not so soft and jelly like homemade NC.
I poured this mass in EGDN, it is about 4 gr of NC and 90 gr of EGDN, the SP coloured the mixture black but not all the SP gelatinized with EGDN.
I added more acetone and after 1 day the mixture seems to be more uniform and jelly type, now i'm waiting some days before let evaporate acetone because i'm going to test this BG next week.
I don't know why this SP is black, if it is pure it should be white or at least slightly yellow. Is there some other additive to the nitrocellulose?
The label says 98% pure nitrocellulose...what is the remaining 2%?
I know that heating the mixture will gelatinize it better but i fear some evaporation of EGDN and i don't feel very safe to eat EGDN. I think it's a psicologyc thing even if i know that isn't dangerous to heat EGDN.
Will DBSP gelatinize better?

Myrol
December 4th, 2004, 05:43 PM
Hi Nuclearattack! My next order should arrive next week, so I think I have then 7Liters of Nitric Acid handy! 6Lites 65% and one 53% for Nitric Salts! I have also ordered 5Liters Methyl Alcohol, 5Liters Nitromethane and some other useful stuff, espacilly 20kg pure Ammonium nitrate in Prill form! For sure I'll make some Methyl Nitrate, but perhaps I should prepare myself for some terrible headaches ;)

I know, EGDN is significant volatile, at roomtemperature is has even a heavy odor! Something like sweet Alcohol. I wash my EGDN very good. First I pour the whole Nitration mix into four times of water stirr good and suck or pour most of the upper layer away. I have a Canister for waste Acid, he's fille dwith thick plumes of NO2.....bad thing.....ok after this I pour new cold water over my EGDN and stir very very good till everthing acidic is extracted by the Water! Then I add slowly under stirring saturated Sodium carbonate solution, if you have sucked the waste acid good away you need not very much base! I add so much base till the fizzing stops entirely plus an extra sip (drop) of solution because if you let the the mixture sit a while, you will see a lot of gasbubbles everywhere due to slow full-neutralization. I let it stand mostly 4h, its then absolutely neutral and the EGDN is stable for Years now! I suck it up fill it in a Bottle and place the bottle in a small dessicator with Na2SO4, it absorbs all the Water without loosing to much EGDN! Ok better I stop now writing to long posts, I dont want NBK flaming in my Ass!

nbk2000
December 6th, 2004, 06:16 PM
You're improving Myrol! You actually used the RETURN key once! :)

:rolleyes:

nuclearattack
December 6th, 2004, 06:44 PM
I use the same procedure Myrol and i have good results, this makes the nitroesters synthesis a pleasure for me!
But now i have to resolve my question on nitrocellulose...what kind of nitrocellulose do you use? Is it homemade or commercial grade smokeless powder? Is it dark? Is it difficult to gelatinize with EGDN or NG?

Myrol
December 7th, 2004, 02:36 PM
Arrggh, damn sorry NBK2000 :rolleyes: . Yes I HAVE forgotten often the Return key whilst typing such a big post.......I promise next time its a lot better!! ;) ;)

To Nuclearattack: My NC gelatinized my NG not very good.....it was homemade one but with NM it worked very well! I haven't tried EGDN, but with NM it was REALLY fast!

Ha haaa, soon my Methyl Alcohol will arrive, than its time to make Myrol :D , I'm sure like hell it's being a tough stuff! Viscosity should be even lower then water, right?

Smokeless powder??? Umm, ok I'm 17 years old.....and in Germany its nearly impractical to get something not being an adult :( , but we all have our homemade way :D :D .....

nuclearattack
December 11th, 2004, 10:42 AM
Yes Myrol is less viscous then water and less dense then Ng. It is a bit more powerfull then NG if you take it by the weight but i think that if you take the same volume NG is better then myrol and EGDN because it's more dense.
What is the most powerfull (in the trauzl test and from the energy released by weight) nitric ester? PETN? Myrol? MHN? NG?

Boomer
December 13th, 2004, 04:42 AM
My books give 600/550/515/500 ml for EGDN/NG/PETN/MHN. Nothing on myrol.

I wonder how they do the sand tamping with the liquids? The above numbers are for sand. Water tamping gives higher values, I suspect the very high values (>600ml) you sometimes see for the oils are caused by the experimenter using water for simplicity.

I also read that the higher values for myrol + EGND compared to NG are caused by the lower density: the area they work on is higher, as they fill the hole in the lead block to a higher level.

Myrol
December 13th, 2004, 01:31 PM
Well, I have compared a lot of Books about Trautzl values from Nitric esters etc. and with sand-tamping the facts are as follows: EGDN 625ccm, pure Methyl Nitrate 615ccm, NG 550ccm, PETN 520ccm and MHN 510ccm.

The Scientist fill liquids in Glassampoules inclusive Detonator and fire them!

Original Myrol is a mix of 75% Methyl Nitrate and 25% Methyl Alcohol wich boils as an azetrope at around 66°C (I'm not very sure!). Watertamping gives especally with EGDN a very high value.....650cc thats a dent! Pure Methyl nitrate ist around 1% stronger than NG.

Its a VERY thin liquid and detonates very easy even in small diameters! I see, you all need results! Ok ok, after my first synthesis I'll post my results! Damn, I hope the headaches aren't that worse as I expect!

Somebody an Idea how strong Methyl Nitrate dissolves other things, perhaps Plastic Polymers, Water or other all daily things?

nuclearattack
December 14th, 2004, 11:04 AM
I'm agree with Boomer...EGDN and Myrol are less dense then NG so they need a big hole to have the same weight in the trauzl block, the working area is a little bigger and maybe gives a vantage to EGDN or Myrol. An interesting test should be using the same volume so NG should give better performance due to it's density. I'll keep in mind for the future, next months i'll do some tests but for the moment i want to investigate more on BG and gelled HEs.
Yesterday i made a test with 240gr of blasting gelatine, i made it with 6gr of smokeless powder, 90gr of EGDN, some acetone, about 100gr AN powder and some NM.
I used 5gr of AP in a small copper pipe as a detonator.
It completely failed! The detonator worked perfectly but the BG didn't detonate not even a gram! Around the site i found only some chunks of BG and some pieces of american tape i used to place the charge on a steel beam.
I cannot give an explanation to this! I know that sometimes BG is hard to detonate at high vod but this is disappointing! Not even a gram of BG is detonated, nothing!
Maybe the charge was too dense? Maybe i should increase the blasting cap power? Maybe i should increase the AN?
However the BG was very dense and thick maybe i added too much NC but if this is the reason what about cordite or balistite that have a very high NC content?
Any suggestion? Comments? Experiences?

Boomer
December 14th, 2004, 12:28 PM
I also had similar comps fail or go very low order. In my experience they are easier to initiate if they contain solid particles as sensitisers, if no bubbles are persent or microbaloon etc are used. AN is very insensitive, it might only work by its simply being there (to create hot spots between crystals or whatever). A crystalline HE that does not dissolve, like RDX/HMX works better of course.

I would also suggest a stronger detonator. Note I said stronger, not necessarily bigger. Till now, a 2.5g MHN compound cap worked all the time. The first 2g are pressed in a big vice to max density (1.72 = 8000+ m/s), 1/2 g is hand pressed on top, followed by either an EBW or simply 1/2g AP with nicrome or fuse.

Pressing the base charge *hard* is important. Assuming you reach half that density with hand tamping, you loose 88% performance! Yes really: twice the density gives approx. twice the VoD. Det pressure is proportional to VoD^2 x density, meaning EIGHT TIMES the pressure shock from the same cap!

BTW what you made is more like a 45% ammon-gelite (German for extra gelatine dynamite, extra meaning AN is added) than BG.

nuclearattack
December 14th, 2004, 06:34 PM
Next time i'll try with less NC to reduce the density and with a stronger detonator, for the moment i don't have MHN but i'm thinking to use a mixture of NC/AP in the middle of the cap and super pressed NC in the bottom, on the top of the cap only handpressed AP. It should be a good compound cap.
However the trauzl tests mentioned by Myrol demonstrates that vod is not a good measure of power...infact NG is a bit more powerfull then PETN even if PETN is faster. It is said that BG is one of the most powerfull HE but i would like to test the difference between differents kind of BG.
For example MHN/NG blasting gelatine should be a good alternative to NC/NG.
MHN is faster then NC so this BG should be more brisant, i don't know if MHN produces more gas or more pressure then NC but it is close to NG so i think that this kind of BG is superior to the traditional one. On COPAE MHN gives a little better performance on trauzl test then NG...i have the impression that is quite difficult to compare perfectly different kind of HEs.
The vantage of NC is that it is cheaper while MHN yelds are not very good, you can also buy commercial grade NC at a good price.
There is also one thing: on COPAE is written that RDX is closer to PETN (about performance), if NG is more powerfull then PETN this means that is also more powerfull then RDX! I always thought that RDX is more powerfull then NG and that only BG has the same power.

Boomer
December 15th, 2004, 10:59 AM
That depends on what the author calls power! The orders are as follows (books from the 80ies)

Heat of explosion: EGDN=6590, BG=6470, NG=6220, PETN=5920, MHN=5780, RDX=5540, HMX=5510 (?) kJ/kg

Specific energy: EGDN=1370, BG=1320, NG=1310, PETN=1300, MHN=1230, RDX=1150, HMX=1150 (?) kJ/kg

The (?) means how can the spec. energy of RDX/HMX be the same, if the heat of expl. is lower for HMX (which makes sense since the molecule is more stable)?

Brisance/det pressure order: HMX-RDX-PETN-MHN-BG-NG-EGDN decreasing from 1.98 to 1.49 MW/cm^2 or from ca. 300 to 180 kbar. All at max density - btw MHN is underestimated here, because Mega gives the value for hand-pressing (7000 m/s at 1.5) while at 1.73 it goes to 8250 m/s. That is why I recommend the vice!

Especially the pressure values vary much depending on what book you read / what formula you use. E.g. for HMX the simple "1/4 x VoD^2 x d" gives 395 kbar, while a much more complex formula (including co-volume, non-ideal gas etc) gives only 267 kbar. I will have to look that one up though.

Oh, and the MHN/NG gelatine is much more insensitive than the single compounds make you think. At least towards a cap. That is why I always add RDX (even HDN works for more internal surface). Currently I am testing nitro starch for MHN as it needs less distilled acid. All I can say for now is you need more of it compared to NC, and less compared to MHN/ETN/PETN etc. And it is sticky as hell. Det tests coming soon... :D

Microtek
December 15th, 2004, 01:04 PM
The discussion about power versus brisance is an old one, even here on this forum. There really isn't one good way for ranking explosives because explosives aren't used for just one thing. Even if you want the "most powerful" explosive around, you will have to define what sort of conditions will be prevalent.
For example, if the charge is placed inside something which is to be blown apart, Trauzl-tests are good as the situations are similar.
If a surface charge without tamping is going to be employed ( such as when blowing a hole in a wall for some special forces guys to jump through ), a plate dent test is more appropriate. Then there is target material to consider.

Myrol
December 19th, 2004, 02:27 PM
Brilliant! Today, I've made some pure Myrol because the stuff intrested me for a long time.

45ml 65% Nitric Acid and 90ml 96% Sulphuric Acid were mixed with 26ml Methyl Alcohol under good cooling. The Reaction was very vigorous, the first drops of Methyl Alcohol were so fast Nitrated that it fizzed a little one of three mainreasons why my Yield was lower than it should be!

After the complete Nitration I poured everything into 500ml Water and waited to let the Myrol settle out. I sucked it into another Beaker with fresh Waterneutralized it a little and sucked him in my storage botlle. Ok the purity is only average good, but I blow it for sure tomorrow up so I dont think its very important to produce an extremly clean product ;)

The things I learned with this synthesis were:
1. The produced heat is enormous! After adding 2ml Alcohol the Temperature increased from 12 to 16°C!
2. With totally closed apparates you must look for the Vapor pressure! My Thermometer was popped once out of the ground glass joint after I nitrated the Methyl Alcohol a little to fast.
3. Myrol isn't to less watersoluble, dont use to much washing water and never wash it warm. Myrol is very volatile, you lose some product if you wash it warm.
4. Try to work in cold places! If you live in Sweden for example you will loose only some percents of your total-yield. Today I worked a little sloppy, so I lost perhaps 5ml Myrol via vaporization, dissololution and remaining droplets in the apparatus. My Yield: 19,5ml.

nuclearattack
December 20th, 2004, 06:39 AM
Hi Myrol
good work! Your yeilds are not so bad considering that is the first time you are making myrol and you can improve the procedure for better yeilds.
Only one question:when you suck (with a syringe i suppose) the myrol from the washing solution and you put it in the storage bottle how do you dry it?
Even if you are using a syringe there should be some water in it, probably is quite impossible to let it evaporate because it evaporates faster then water i suppose.

The_Rsert
December 20th, 2004, 09:00 AM
Myrol.
The yield of your synthesis is really bad!
I've made myrol with an amazing yield by destilling of a neutralised an thinned emulsion of Myrol.
4g myrol will dissolve in about 100ml water at 20°C.
So use ice-water or destill the myrol (boils at 65°C) carefully.
Or you can extract the myrol with (for example) dichlormethane.
You will get a much better yield.

Myrol
December 20th, 2004, 09:22 AM
To Nuclearattack: You can dry the Myrol via Filtration over anhydrous Sodium sulphate or Calcium nitrate, works very good not only for Methyl Nitrate. If you add some Sulphate to EGDN or NG let it stand for some hours and filter the Salt away, you will get a very translucent clear Product!

My Myrol was yesterday a little milky not like NG, jsut a little!
Today he is totally clear! Even with my sick washing and the unaccurate separation I have now a translucent product. :) Myrol is Fun!

Is it possible to salt some diluted Methyl Nitrate out via adding enough table salt for example? I mean, there some solvents wich can. Hmm but a distillation does a lot more effort and isn't perhaps not worth the extra yield. We'll see.

The problem with headaches isn't very big, ok I worked at 5°C outdoor Temperature but if you aviod warm conditions you get absolutely no headaches ;) Thats a plus because I HATE Headaches.

nuclearattack
December 26th, 2004, 10:32 AM
Adding a solid\cristalline to BG will increase the sensivity even after long storage, now i'm thinking about adding a solid HE that not only help to transmit the detonator shockwave but also increase the sensivity chemically.
Maybe that this is a stupid idea but what about adding AP in BG?
The trick should be to add only the minimum quantity to rise the sensivity and not to make it dangerous. Too much AP will give a super sensitive BG and this is not what we want but a few grams could work well.
I'm planning some tests with different quantities.
What is your opinion?

The_Rsert
December 26th, 2004, 03:26 PM
No, don't do that!
I have heard that a drop of HMTD to isopropyl nitrate caused a huge
detonation.

You can test this in little scale, but be very careful!

nuclearattack
December 26th, 2004, 05:34 PM
Don't worry the tests will be surely on small scale but however AP is not as reactive as HMTD. AP is used in some HE compound like APputty or APAN with success and it doesn't react with metals. I made some tests storing for 4 months AP in contact with copper and iron...it didn't react.Otherwise HMTD is incompatible with metals and a lot of substances.

Myrol
December 27th, 2004, 04:32 PM
To Nuclearattack: Your Idea of adding a little AP to Blasting Gelatin should work!
I'm pretty sure because just around 5% AP makes the super insensitive Ammonium Nitrate detonatable with a Nr.6 Blasting Cap!

So let's play our mind's......Blasting Gelatin detonate with around 7700m/s if lots of microbubbles are occluded in the soft sticky Gel. The Velocity can fall to less than 2500m/s if there aren't present. Some AP COULD manage this lack of detonation-uniformity because it detonates very easily and should transmit the reaction via working as "microbubbles".

2% AP and not more could be worth a try, unfortunately it decreases the Oxygenbalance a little but you know what huge effect this can do! Blasting Gelatin is only that strong because NG and a SPECIAL nitrated sort of NC combine their surplus and lack of Oxygen to give an extra Expansion in the Leadblock expansion test.

If there is some AP present with -151,3g O2 per 100g you'll notice this for sure in the total-performance....but who care's? Screw the Stuff, we have our plans :D

Umm, Nuclearattack: If you have some Photos from your Blasting Gelatin especially if NG/NC, can you please send me them? I cant wait to see it.

It sounds very cool, an Explosive wich is so soft that you can push a detonator full into the plastique and BAAAAAM, blow it up! Yeah, I must do it too :D

With 7Liters 65% Nitric Acid can I make a LOT of NG, EGDN, NC AND PETN!!!

For the Mods: Congratulations to the new Design! I like it, looks like a High-Tech Forum! Ok, I wear glasses :cool: and my eyes are not the best, but even if I have to pinch my eyes together to come clear with the sharp contrast, it just looks cool!

nuclearattack
December 27th, 2004, 05:15 PM
Hola Myrol my friend!
I just bought a digital camera so i can send to you videos and photos, i'm planning a big scale BG test at the end of january, i'll send you the video by mail.
Just a bit of patient because i really cannot anticipate the test!
About the AP oxygen balance it can be resolved adding AN to the mixture.
10% APAN should work good because it has 0 oxygen balance, just a bit of it and you will have a sensitive and powerfull BG with very high vod.
About BG vod i read on COPAE that it can reach 8000 m\s, this is right because NG has 7700 m\s but adding NC will give a perfect oxygen balance that will rise the vod. Another very good stuff should be adding DPPP to BG, there is a thread on it and i'm trying to sinthetize it...with 9000 m\s it could make a super BG that kicks ass!! :eek: :D :cool:
About your nitric acid i can only envy you! :(
I searched a lot but H2NO3 is really too much expensive for me and i want 99% because i'm pretty interested in RDX or PETN. There is also the problem of PE...in my country seems to be impossible to find for a private.
Sigh sigh! :( :(
We have two things that we both want: i have a lot of smokeless powder and you have PE and H2NO3. Fucking distance!
Oh yeah! The new forum style is cool!

Myrol
December 28th, 2004, 12:47 PM
Nuclearattack, no Problem! Perhaps, if Italy isn't to far away I can do something for you that you can get your hands on some Nitric Acid and Pentaerythrite.

Well, I pay'd around 65€ for those 7Liters Nitric, and for my 1,5kg Pentaerythrite I had to pay a little under 30€......Just send me an E-Mail and we'll see what I can do ;) :D

Just the distance couldn't be a problem for such a gentle man, right? We manage it, I promise!

So back to BG: I see you have a lot of expierience with it, but I'm lacking some data. Do you have the Temperature of Explosion and the Density etc.?
That BG can detonate with 8000m/s seems to be really true, umm I heard it very often only Urbanski said it can reach 7,7km/s max. , thats why I thought it has this velocity!

This summer I have made a test with 34g Aluminized BG wich was very impressive!
The shockwave was HARD, really hard for just 34g HE. Just my NC was a little bad so the Gelatin was more a slurry as a gelatin. Thats an Idea! Why not stretching some Blasting Gelatin with PETN and Al??? PETN does not decrease the Energy, no no it increases even the density and Aluminium lengthen the pressure phase! Nuclearattack you are a Genius! :D Because I have 130g PETN in my cupboard ready for use and a new batch NC is planned for tomorrow!

Well, I think I just need some new NG even if I like EGDN more!

nuclearattack
December 29th, 2004, 10:58 AM
Hi Myrol
one of this days i'll mail you so we can discuss about our things. :D
About some data on BG in this moment i have in my hands only COPAE and i took from it this data:
density 1.63
lead expansion test (with 7% NC) 600cc
heat of explosion (from boomer post) 6470 kj/kg
specific energy (from boomer post) 1320 kj/kg
explosion temperature 3540 °C
specific volume liters 710

I'm planning to print others manuals like Fordham and Fedhoroff so in the future i will be able to give better details.
I have a bit of confusion about the specific energy and the specific volume liters...
about the spec energy i wonder that 1kg of BG has only 1320kj! This means that chocolate has more specific energy because 1kg of chocolate has more than 5000kcal! Of course chocolate doesn't release all of its energy in a fraction of second!
About the specific volume i don't know the initial volume of the BG sample, it ends the expansion with 710liters of gas but what is the initial volume?
I'm a bit confused, maybe that i seem stupid and ignorant...i have to study more on others HE encyclopedia!

Hey Myrol your BGAL test is good but what is the ratio you used? How much Al and NC?

trinitride3
December 29th, 2004, 11:37 AM
Hey Myrol, can you tell me the type of aluminum powder you used in you BG, (mesh size, coated or un-coated, bright or dark, etc.). Im going to order some AL powder today and figured Id ask what type worked best in your tests. Did the aluminized NG seem much more sensitive in your tests?

Myrol
December 29th, 2004, 12:54 PM
Oh dear.....well I think I used 2g NC 4g Al and 28g NG, yes thats it!
My NC wasn't very good, thats why my gel was a little thin perhaps like Honey!

I poured it into a Filmcanister and inserted a HMTD-Detonator, 1,5g total to be on the safer side! In the next time I will use more of this composition: 70% PETN 15% EGDN and 15% Al. I tried it once with only one single gram but it was even then very loud and powerful, surfacedetonation on ordinary soil made a Man's Fist sized crater 5cm deep because I confined the charge with an old trainer :D .

Unfortunately, the trainer got absolutely no damage, perhaps the rubberbottom was to strong :confused: ? The aluminized mix with 15% EGDN has also the advantage of beeing like BG a little plastic! You can press it into every container very easily and you have then quite high densities wich results in good shattering effects against rock, steel, wood and concrete.

P.s. 29th of December, the shops started selling fireworks and it's always disgusting like every year: you hear each minute a tiny bang from a firecracker or a rocketshell.....what the hell are such tiny firecrackers useful for? They must have REAL Blastpower to be worth the price! 15g perfect Blasting Gelatin....that would be a deal, huh :D :D ;) ?

Chris The Great
December 31st, 2004, 12:55 AM
I know what you mean, here they only sell fireworks around halloween, and there are always little snaps off in the distance. Then, on halloween, kids wander around tossing hammered screechers, which cost $1 each, and are about as loud as a gram of packed AP.

As I'm going to be making some of this stuff when I buy some nitric (2.5L 70%), I'll have to set off a few grams on halloween in the open to make them all feel inferior. :D

Although, sometimes they make pipebombs and get in the newspaper. It was, according to the police, a bunch of hammered screechers and bottlerockets in a pipe, and had the power of "a small stick of dynamite." It left a fist sized hole in the windsheild and some shrapnel damage. Right.....

Nevermore
January 2nd, 2005, 06:36 AM
I bought 1 kg of smokeless powder, on the label is written: pure 98% nitrocellulose.
I always make my blasting gelatine with homemade nitrocellulose and i can say that it worked well but surely it is too expensive to make NC so i decided to try with smokeless powder.
This SP is dark gray grains and when i try to gelatinize it in acetone it becomes a stiff black mass not so soft and jelly like homemade NC.


The SP is dark gray because a lot of other components are added to improve the use in firearms:
Flegmatizants are added in order to slow down the burning ratio and decrease sensitivity,
stabilizant and preservatives also added
color is added
gelificant, plastificant agents are also in..
then, most of SP have the grains covered in graphite to decrease absorbtion of humidity.

The Sp i use is green, i cared to get one very fast burning one in order to lower the quantity or flegmatizants, and i was pleased to know it was just 10% Ng so was not covered with graphite.
However, i must say that my experiments with Ng-jel were not so succesful, adding too much Sp makes the gel very hard, and the border between too liquid and too hard is very thin, is very easy to end up with a rather hard mass..
beside that, while storing it is completely safe and effective (i stored a gel made of 70% Ng 20% MHN and 10% Sp) storing it for more than one month brings to an excessive decrease in sensitivity..
After one good year of storage i was able to reach only metastable detonations even if i used a MHN booster (0.8g), the mass became pretty hard and not kneadable at all, plastic appearance, more or less like soft rubber...
My plain Ng is MUCH more sensitive to initiate, 100mg of double salts + 200-400mg of MHN are plenty to initiate any kind of charge..


:D

nuclearattack
January 3rd, 2005, 05:25 AM
Yes Nevermore! It's graphite! Now that you remind me i recognize it!
Infact when i gelatinize it there are lot of micro particles suspended in the jelly mass...damn i have to buy DBSP...this is not a problem!
However i have the same observations of yours...a bit of NC can make a very big difference and a too plastic BG is very hard to detonate.
Have you ever tried adding Al powder? I'm looking for cheap Al powder but it seems hard to find.
What do you think about my idea of adding a bit of AP to sensitize BG?
Note that i said "a bit"! ;)

Nevermore
January 3rd, 2005, 10:43 AM
absolutely.
my hard NG jelly is hard like stone to detonate, plus that has aged a little made that very insensitive even to a good booster charge..
Al powder, i have searched for it, i was not able to find, could be useful for thermite too, but well, is almost impossible to find.
about AP:
is damn sensitive, unstable, not powerful, not storable, corrodes metals, if ages became dangerous, why the hell you want to waste the good properties of bg by mixing with that shit..
you won't get an higher VOD for sure, plus, you will shit ur pants every time you have to knead it..better to mix some sorbitol or mannitol nitrate.
i told you some time ago, but i will repeat here, trash that damn AP there are much better primaries around, i love double salts, and if you mix them with MHN during preparation you will get a primary+booster that is able to initiate almost everything in the 100-600mg range.

nuclearattack
January 4th, 2005, 06:37 AM
No Nevermore AP is not all that shit as everyone think, i know that isn't the best primary (probably the worst) it is weak and not as stable as others primaries but it can be used safely. I made lot of tests to verify AP sensitivity and stability and i can say for sure that it isn't so unstable. To set off my AP i need a good hammer blow, it doesn't detonate if temperature rise a bit and it doesn't react with metals.
I made a test about it's reactivity with metals and i saw that it's perfectly stable in contact with metals, i posted a test on the thread "Danger AP" read it. It didn't react in contact with copper after 4 months.
Anyway you don't understood my target about mixing AP with BG.
Since BG is very insensitive i want to sensitize it with a bit of AP or maybe DPPP, if i add MHN as you suggested i will have a thick jelly insensitive like classic BG.
About compound caps i use a mix of SP and AP, it works well but i want to substitute AP with DPPP.

trinitride3
January 4th, 2005, 11:55 AM
Do you think its possible that the problems your having with insensitive BG is related to the quality or percentage of NC your using to gelatinize it? I have set off numerous charges of BG in recent tests ranging from 50 - 300 grams in weight, 40 - 105mm in diameter. I use a 6% NC content (Bullseye DB) and find my BG quite easy to kick off using 6mm aluminum bodied AP caps (.5 g). I press the caps (remotely) with a vice to the neighborhood of about 2500 psi. I don't believe I've had any low order or partial detonations to date. One more thing I wanted to mention is how important I find it to use an accurate scale when figuring the percentage of NC to add, especially when your working with smaller sized charges. If your using an average cheapo digital scale its quite easy to have your NC content off by 3% or 4%, and that will surely wreak havoc on your BG's sensitivity to detonation.

Myrol
January 4th, 2005, 01:03 PM
Aluminium Powder is a very very good Idea because it increases the Explosion energy a LOT! Damnit, you all need Al-powder....and I have over 2,5kg good 50micron fine one at Home!!! Since the arrival of this shitload Al I mix nearly EVERYTHING with Al to increase the power :) It worked with APAN to APANAl (->SIGNIFICANT more "pressure") with ANNM to ANNMAl and especially with PETN/EGDN-Plastique to a 70% PETN,15% EGDN,15% Al mix. Its a little plastic, easily compressable and VERY brisant explosive.

So if you all need a more sensitive Gelatin, try Aluminiumpowder. Could do wonders :D Paint grade Aluminium is just a little unpleasant. A little whiff of Air and you're standing in a big cloud of Al-Flakes! With my grey heavy uncoated powder its absolutely no problem.

I have just one question left because since my last Myrol-attempt I was a little disappointed with the Yield but this time I think I will use another method of preparation.

Myrol can be also prepared via Distillation of Methyl Alcohol, Nitric acid 60-70% and a little Urea. It's a noble reaction, you need no Sulfuric Acid for a Nitric Ester!
I'm just a little confused how much Nitric Acid I should use. An Excess of it seems to be totally necessary.

I calculate 15% Acid-excess in, so you end up with roughly 300ml 65% Nitric Acid for 150ml Methyl Alcohol. But how much Urea??? The Urea should get instantly neutralized trough some Nitric Acid and you're loosing then some of it. I'll try the Distillation on Thursday if nothing comes between it.

Methyl Nitrate is quite intresting for me for three reasons: It's a very thin and fluent liquid, you get no problems to wash you glassware like with the sticky NG. Methyl Nitrate can be dissolved away or it evaporates fast if you use hot water!
2. Methyl Nitrate seems to be chemically as stable as PETN. I stored a very rough washed sample over 2 weeks with absolutely no visible sign of decomposition. It just smelled typical like Myrol (Alcoholic sweet oder, a little like Chloroform)
3. Its very strong, even a little stronger than EGDN (as Meyer& Köhler sais!) and mechanically more stable than almost all other high-nitrated Blasting Oils like NG, EGDN, PGDN, BTTN, NIBGTN and so on.
Ok I found another reason Nr.4: You can Initiate Myrol very easy! 0,4g HMTD are enough for a High-Order Detonation. The critical diameter is between 2 and 3mm.

Against misunderstood's: Original German Myrol is an azetrope boiling mix of 75% Methyl Nitrate and 25% Methyl Alcohol. I just say Myrol for the PURE stuff Methyl Nitrate because it saves me some seconds writing and saves Forum space :D (even if just some tiny bytes!).

Myrol
January 5th, 2005, 01:48 PM
to trinitride3: I've made a picture from my Aluminiumpowder for you.
It should stick on this post :) You can see also some other chemicals from me in this picture.

All my stuf is ordinary in the cellar, just the metalpowders, wich are easily corrodable and my Pentaerythrite do I store in my Room. These two white packs are full with Pentaerythrite around 1,5kg and the two grey packs are Aluminium dust The bigger bottle contains around 1,5kg and the ziplockbag is filled with 1kg Al 50micron. At the Edge can you see a bag with PETN. 95g but not total visible.

Today I have made a sample-Nitration of Ethylene Glycol to see how much EG will be Nitrated and how good the Yields are under real conditions.

I started with 50ml 65% Nitric acid, 90m 96% Sulfuric Acid and 22g (20ml) Ethylene Glycol. The Nitration was after 30min. complete and I poured everything into 500ml Icecold Water.

The whole solution warmed up to 23°C and the smell of EGDN was "pleasant present". I removed carefully almost all of the waste Acid and added some extra 250ml fresh water to remove more H3O+. I poured the water again carefully away and added some new 300ml fresh water to wash the EGDN completely.

I cleaned all my glassware, grabbed the beaker and neutralized it very carefully in my "Lab". I added warm saturated Sodium carbonate solution till no CO2 evolved out of the solution. I swirled sometimes to be sure it IS neutral and added occasionally some ml solution until I was unable to see a "disturbance" in the sol. whilst I held the beaker against a lamp. (Damnit long sentences huh :rolleyes: ). I sucked all the EGDN in a tared (not TARed, tared from a scale!) bottle and got finally 40g EGDN. It's a Yield of 73,3% calculated from the Nitric Acid and you get around 182g EGDN from 100g EG with this method!

trinitride3
January 10th, 2005, 07:20 PM
Hey Myrol, This weekend I had a chance to experiment with some aluminum enriched BG. WOW, what a difference a small amount of aluminum makes in the power of the BG. I only had time to experiment with one charge but I will have more time next weekend to try different ratios of aluminum. The BG-AL charge I detonated was about 150 g. I first gelatinized my EGDN with 5% NC then added 15% aluminum powder slowly stirring it in with a popsicle stick. I put the mixture in a cardboard tube and went to my test site. I found a nice oak tree stump that was about meter tall and almost a meter wide, slightly rotten in the center. I inserted a .5g AP cap into the BG-AL and placed the charge in the middle of the stump. The explosion devastated the stump leaving nothing but a nice crater in the ground! It was just about dusk and I observed a nice flash. The explosion was way more powerful than ordinary BG. I will be using aluminum powder in my BG for now on, cant wait till next weekend! :)

nuclearattack
January 13th, 2005, 04:30 PM
To trinidide:
yeah! This thermobaric mixture is very powerfull but i think you hadn't developed the max power of it because of the small detonator. Try with more AP mixed with a more powerfull HE like MHN or simply smokeless powder. This will assure the max vod and output power. I used successfully a compound detonator made with AP and smokeless powder, the bottom of the cap is only filled with SP, the middle part is a mix of the two powders (AP and SP) and the top of the cap is only AP.
This simply compound cap is easy and fast to make and i had good results with it.
Anyway if you have MHN or PETN it's a very good choice!
I'm going to substitute AP/SP mixture with DPPP if it works well as it seems to be...we'll see. ;)

trinitride3
January 14th, 2005, 12:32 AM
To nuclearattack:
Thanks for the advice. I just ordered some mannitol and erythritol the other day for use in detonators I plan to make in the future. In the mean time I would really like to try the compound detonator you recommended, I thought about using SP in the past but never had a chance to experiment with it. Could you tell me the amount of SP and AP you used in each part of your compound detonator and also how hard I should press the SP at the bottom of the det?

nuclearattack
January 16th, 2005, 10:57 AM
To trinidide:
i always make the cap as long as the charge to ensure a high rate of detonation, my detonators are also large at least 10 mm. I divide (virtually) the detonator in three equals parts, the first part (bottom) filled with hand pressed SP, the middle part with a mix of SP\AP hand pressed and the third part with only AP also hand pressed. The quantity of SP and AP is so variable from how long is the cap, generally i use 3gr of SP and 2gr of AP but it vary a lot if the charge is long or big.
I have very good results with this compound det, at least it is fast and cheap also for ANFO charges that requires strong detonators.
:)

nuclearattack
February 22nd, 2005, 02:36 PM
Is there someone that knows the exact vod for EGDN?
I searched on the web and also in COPAE but i found nothing...it should be close to NG but i'm curious about the exact value.

tomu
February 22nd, 2005, 04:17 PM
7300 m/s at a density of 1,48 g/cm3 according to Koehler Meyer, Explosivstoffe, 9th Edition 1998.

My guess is you could get different velocities with each different test method/setup. So this might not be exactly exact. For all practical purposes a few meters give or take will not matter anyway.

Chris The Great
March 13th, 2005, 01:17 PM
Yay, my first nitration :)

I gathered the materials, all of which were fairly easy for me to obtain, methanol (99.9%), H2SO4 (boiled battery acid) and NH4NO3 (instant cold pack).

100mL of H2SO4 was cooled in an ice bath, while I measured out 65 grams of NH4NO3. This was mixed into the H2SO4 with lots of stirring, and let sit for 10 minutes until the mixture had achieved an even consistancy and had time to cool down.
29mL of methanol was slowly added with a syringe over a peroid of 30 minutes with constant rapid stirring. Occasionally I stopped and checked on the temperature.
Before addition 3.0*C
2.5mL 8.0*C
10 min (10mL) 11.5*C
15 min (15mL) 11.5*C
20 min (20mL) 10.0*C
27 min (29mL) 12.0*C
After this there was a ~1cm thick oily layer floating on the surface, that vibrated rapdily for several seconds when the jar was lightly tapped, indicating a very low viscosity.

http://img81.exs.cx/my.php?loc=img81&image=after0pm.jpg

I did a little dance at this point, as it meant I was probably successful.

I extracted the top layer of methyl nitrate with a syringe, squirting it into ice water to rinse it. I then removed the ice cubes and sucked it out again with a syringe and squirted into sodium bicarbonate solution, and then from there I transferred it to a small jar. About 20mL was obatined.

Another layer was forming on top, so I extracted it and got another 4 to 5mL.

http://img81.exs.cx/my.php?loc=img81&image=product0ou.jpg

The warning is for my dad, who has the other half of the workshop, and often moves things because he likes them to be clean. I would rather him not be moving my myrol around.

More myrol was floating to the top of the mix, so I capped it with a blue PVC pipe endcap and left it for the night.
I went back about 16 hours later, to find the inside of the blue plastic had turned a nice purple colour, the acid mix had cleared up and there was more myrol floating on top. Another 3 to 4mL was obtained.

Total yield is about 28mL (34 grams), or alot less than theorectical.
However, there are some little beads of water (maybe 0.25mL total) of water floating on top, and it isn't clear, it is slightly murky. I think I need to get rid of it quickly before it gets rid of itself.
It smells very nice however, much like chloroform. I haven't got a headache from inhaling it deeply however, though apparently some people don't get them.

Chris The Great
March 13th, 2005, 01:17 PM
Yay, my first nitration :)

I gathered the materials, all of which were fairly easy for me to obtain, methanol (99.9%), H2SO4 (boiled battery acid) and NH4NO3 (instant cold pack).

100mL of H2SO4 was cooled in an ice bath, while I measured out 65 grams of NH4NO3. This was mixed into the H2SO4 with lots of stirring, and let sit for 10 minutes until the mixture had achieved an even consistancy and had time to cool down.
29mL of methanol was slowly added with a syringe over a peroid of 30 minutes with constant rapid stirring. Occasionally I stopped and checked on the temperature.
Before addition 3.0*C
2.5mL 8.0*C
10 min (10mL) 11.5*C
15 min (15mL) 11.5*C
20 min (20mL) 10.0*C
27 min (29mL) 12.0*C
After this there was a ~1cm thick oily layer floating on the surface, that vibrated rapdily for several seconds when the jar was lightly tapped, indicating a very low viscosity.

http://img81.exs.cx/my.php?loc=img81&image=after0pm.jpg

I did a little dance at this point, as it meant I was probably successful.

I extracted the top layer of methyl nitrate with a syringe, squirting it into ice water to rinse it. I then removed the ice cubes and sucked it out again with a syringe and squirted into sodium bicarbonate solution, and then from there I transferred it to a small jar. About 20mL was obatined.

Another layer was forming on top, so I extracted it and got another 4 to 5mL.

http://img81.exs.cx/my.php?loc=img81&image=product0ou.jpg

The warning is for my dad, who has the other half of the workshop, and often moves things because he likes them to be clean. I would rather him not be moving my myrol around.

More myrol was floating to the top of the mix, so I capped it with a blue PVC pipe endcap and left it for the night.
I went back about 16 hours later, to find the inside of the blue plastic had turned a nice purple colour, the acid mix had cleared up and there was more myrol floating on top. Another 3 to 4mL was obtained.

Total yield is about 28mL (34 grams), or alot less than theorectical.
However, there are some little beads of water (maybe 0.25mL total) of water floating on top, and it isn't clear, it is slightly murky. I think I need to get rid of it quickly before it gets rid of itself.
It smells very nice however, much like chloroform. I haven't got a headache from inhaling it deeply however, though apparently some people don't get them.

Chris The Great
March 13th, 2005, 01:17 PM
Yay, my first nitration :)

I gathered the materials, all of which were fairly easy for me to obtain, methanol (99.9%), H2SO4 (boiled battery acid) and NH4NO3 (instant cold pack).

100mL of H2SO4 was cooled in an ice bath, while I measured out 65 grams of NH4NO3. This was mixed into the H2SO4 with lots of stirring, and let sit for 10 minutes until the mixture had achieved an even consistancy and had time to cool down.
29mL of methanol was slowly added with a syringe over a peroid of 30 minutes with constant rapid stirring. Occasionally I stopped and checked on the temperature.
Before addition 3.0*C
2.5mL 8.0*C
10 min (10mL) 11.5*C
15 min (15mL) 11.5*C
20 min (20mL) 10.0*C
27 min (29mL) 12.0*C
After this there was a ~1cm thick oily layer floating on the surface, that vibrated rapdily for several seconds when the jar was lightly tapped, indicating a very low viscosity.

http://img81.exs.cx/my.php?loc=img81&image=after0pm.jpg

I did a little dance at this point, as it meant I was probably successful.

I extracted the top layer of methyl nitrate with a syringe, squirting it into ice water to rinse it. I then removed the ice cubes and sucked it out again with a syringe and squirted into sodium bicarbonate solution, and then from there I transferred it to a small jar. About 20mL was obatined.

Another layer was forming on top, so I extracted it and got another 4 to 5mL.

http://img81.exs.cx/my.php?loc=img81&image=product0ou.jpg

The warning is for my dad, who has the other half of the workshop, and often moves things because he likes them to be clean. I would rather him not be moving my myrol around.

More myrol was floating to the top of the mix, so I capped it with a blue PVC pipe endcap and left it for the night.
I went back about 16 hours later, to find the inside of the blue plastic had turned a nice purple colour, the acid mix had cleared up and there was more myrol floating on top. Another 3 to 4mL was obtained.

Total yield is about 28mL (34 grams), or alot less than theorectical.
However, there are some little beads of water (maybe 0.25mL total) of water floating on top, and it isn't clear, it is slightly murky. I think I need to get rid of it quickly before it gets rid of itself.
It smells very nice however, much like chloroform. I haven't got a headache from inhaling it deeply however, though apparently some people don't get them.

The_Duke
March 13th, 2005, 06:39 PM
there are some little beads of water (maybe 0.25mL total) of water floating on top, and it isn't clear, it is slightly murky. I think I need to get rid of it quickly before it gets rid of itself.

The Methyl Nitrate is “murky” or turbid due to the fact that there is water still in it. The beads of water floating on top are actually (for lack of a better word) “secreting” from within the Methyl Nitrate. Just let it sit in a desiccator for awhile. ;)

The_Duke
March 13th, 2005, 06:39 PM
there are some little beads of water (maybe 0.25mL total) of water floating on top, and it isn't clear, it is slightly murky. I think I need to get rid of it quickly before it gets rid of itself.

The Methyl Nitrate is “murky” or turbid due to the fact that there is water still in it. The beads of water floating on top are actually (for lack of a better word) “secreting” from within the Methyl Nitrate. Just let it sit in a desiccator for awhile. ;)

The_Duke
March 13th, 2005, 06:39 PM
there are some little beads of water (maybe 0.25mL total) of water floating on top, and it isn't clear, it is slightly murky. I think I need to get rid of it quickly before it gets rid of itself.

The Methyl Nitrate is “murky” or turbid due to the fact that there is water still in it. The beads of water floating on top are actually (for lack of a better word) “secreting” from within the Methyl Nitrate. Just let it sit in a desiccator for awhile. ;)

me234
March 14th, 2005, 12:47 AM
Chris, try some sodium sulphate (anhydrous of course). It works really well for drying organic liquids out. I love it. Check your local pharmacy for Glauber's Salt if you have any difficulty finding it.

me234
March 14th, 2005, 12:47 AM
Chris, try some sodium sulphate (anhydrous of course). It works really well for drying organic liquids out. I love it. Check your local pharmacy for Glauber's Salt if you have any difficulty finding it.

me234
March 14th, 2005, 12:47 AM
Chris, try some sodium sulphate (anhydrous of course). It works really well for drying organic liquids out. I love it. Check your local pharmacy for Glauber's Salt if you have any difficulty finding it.

Chris The Great
August 6th, 2005, 01:53 AM
I've long since lost my myrol to evaporation (doh!) and a couple tests. I dried my myrol by adding a chunk of magnesium sulfate. The myrol turned yellow after a while but it was still stable to survive being hit with a hammer on an anvil. I did this because it wasn't drying fast enough just by sitting in a dessicator.

The several test included detonating 1 to 2mL of methyl nitrate with about a gram of pressed AP, using small metal casings that where originally batteries. 1mL of methyl nitarte left a half foot crater in my yard, and lobbed a chunk of dirt about 50 feet away, and to quite some hieght. I was amazed, just the detonater under identical conditions merely made a small hole, about an inch across. They where about a half foot below the surface, and the ground was quite hard and I made sure to not break it up much when I buried the charges (last time I dug a hole and then packed the dirt back over a 'device', and the first time I set off an explosive, it blew the dirt out but didn't do much else)

However I do admit it was quite a lucky detonation- it was perfectly set up to transfer maximum energy to cratering. There was very little noise or ground shock. The other times I've put it to deep and got a very deep *thump* and not much flying debris.

I recently aquired a substantial quantity of ammonium nitrate, and so I will be making more methyl nitrate, hopefully quite soon.

Barnacles
August 7th, 2005, 03:30 AM
I was wondering when you hit it with a hammer on the anvil. Did you soak the myrol into cotton, otherwise you are not getting the real sensitivity of it and might end up being more liberal in it's handling then you should.

Vinci
August 10th, 2005, 10:26 AM
Two failed detonation with blasting gel ... :(
I made 2x 110g charges today. One was NG/NC and the other one EGDN/NC, both initiated with 1g HMTD. Now why the hell didn´t they detonate ?

I almost set a corn field on fire, because the charge was spreaded all over the dry ground.

tomu
August 10th, 2005, 04:06 PM
If the blasting gelatine was freshly prepared 1 g HMTD should be more than adequate to detonate it.

Are you sure you used NG or EGDN respectively or did you just have assumed for some reason that it were NG or EGDN?

Have you done some tests with the NG or the EGDN?

Where did you place the detonator, was it fully embedded in the charge?

In what type if any container was the explosive in?

Vinci
August 10th, 2005, 04:17 PM
The blasting gel was more a chewing gum than a gel. 92/8 doesnt seem to be a good ratio with my NC.

Of course the detonator was fully embedded in the charge.
And I used a glasbottle, so I´m pretty suprised by the failed detonation too.

I wonder if it makes any difference if good or bad nitrated NC is used. My last batches wasn´t that good.

Barnacles
August 11th, 2005, 06:15 AM
Sounds like maybe the HMTD deflagerated. I remember seeing a video somewhere where HMTD was in a pill bottle and deflagerated into a big ball of fire. Was the HMTD pressed and confined? Try more maybe. Also what type of container did you use for detonator? for main charge?

tomu
August 11th, 2005, 06:32 AM
The blasting gel was more a chewing gum than a gel. 92/8 doesnt seem to be a good ratio with my NC.

Of course the detonator was fully embedded in the charge.
And I used a glasbottle, so I´m pretty suprised by the failed detonation too.

I wonder if it makes any difference if good or bad nitrated NC is used. My last batches wasn´t that good.

The consistency seems alright to me. BG is always more rubber like a substance.

I don't know what do you mean with good or bad NC. There are simply differnet grades of NC which differ in Nitrogen content. In case of making blasting gelatine "bad" NC meaning NC with a lower N-content (collodion) is the right stuff to use, it gelatinizes NG much better as does NC with a high N-content.

I have absolutely no idea what went wrong if as you said the BG was freshly prepared, if the cap was fully embedded in the main charge and if the cap didn't fail to detonate. As I said in my previous post 1g of HMTD is more than enough to get fresh BG going. Really old (at least several month old) straight BG (only NG/NC) will require a booster charge to detonate it.

Vinci
August 11th, 2005, 10:32 AM
With bad nitrated I mean it didn´t deflagrate like good batches do. And I´m not an idiot, the HMTD detonated very well, otherwise the glass bottle wouldnt have blown into pieces...
The detonator was made from a straw.

The blasting gel itself was maybe a week old.
I´ll try it again when I´m back from holidays.

Chris The Great
August 13th, 2005, 04:05 AM
I was wondering when you hit it with a hammer on the anvil. Did you soak the myrol into cotton, otherwise you are not getting the real sensitivity of it and might end up being more liberal in it's handling then you should.

I hit a few drops without it being soaked into anything, and then soaked it into a paper towel piece, which just splattered when I hit it. I was quite surprised, but then again it needs a 40cm drop with 2kg, and my hammer is maybe 0.5kg....

Apparently friction sensitivity is quite high however, so I was quite careful with it as I don't know exactly how sensitive.

me234
October 3rd, 2005, 01:39 AM
Vinci, how big were the pieces of glass after the failed det.?
Can you give us more specifics regarding your arrangement? Containers, pressing methods, ignition system (i.e. fuse, electrical) etc.

When you say it nearly set a field on fire, do you mean it was spread all over and could have caught alight, or do you mean it was actually on fire?

I'm going to hazard a guess that if the glass pieces where kinda big, not small (a few mm each) then a partially failed HMTD charge would be consistent with these results.
You say that the field nearly caught fire, I assume you say this because the BG was burning. A deflagrated HTMD charge would have sufficient force to break apart a bottle, especially one packed with a somewhat incompressible, viscous fluid, and from my own 'experiences' of burning open HMTD, the flame lasts a suprisingly long time. Taken together, one might conclude that your detonator failed.
If you're thinking that a deflagrated charge wouldn't blow a bottle to pieces, I suggest you put a firecracker into a similar bottle, and observe the results after it goes off.

We aren't calling you an idiot, we're just trying to get some perspective and throw some ideas out there and see if anything makes sense or is inspired.

P.S. Are you the same Vinci from APC? If so, that's for all the pyroscene.de books you put up, I got a lot of shit from there before it stopped working and I really appreciate the work.

nuclearattack
October 3rd, 2005, 12:01 PM
The blasting gel was more a chewing gum than a gel. 92/8 doesnt seem to be a good ratio with my NC.

Of course the detonator was fully embedded in the charge.
And I used a glasbottle, so I´m pretty suprised by the failed detonation too.

I wonder if it makes any difference if good or bad nitrated NC is used. My last batches wasn´t that good.


92/8 is too hight! i use 97/2 or 96/4 but the edge beetween a sensitive BG and a rubber insensitive gel is very thin...it depends a lot from your NC.
a suggestion: use always a compound cap or a booster charge...it makes difference!

Vinci
October 3rd, 2005, 12:41 PM
I totally agree. 92/8 is not a good mixture for homemade blasting gel. The second mixture you mentioned (96/4) gives way better results. I´ve done a detonation with 180g of EGDN/NC blasting gel wich was 95/5, detonated fine from 0.8g HMTD.

Its more a gel, not a solid like 92/8.

92/8 may work if the cap gets allready placed in the charge when their is still acetone in the mixture, otherwise its hard to get the cap fully surrounded by the BG wich can result in a failed detonation.

nuclearattack
October 4th, 2005, 06:12 AM
i usually add nitrometane instead of acetone...and some alluminium to increase sensitive and power.
don't add too Al or the BG become too insensitive...only 10% is sufficent.

mike16
April 25th, 2007, 05:40 PM
Sorry for bringing up an old thread, but I did not want to start a new thread for this.

Methyl Nitrate is a very interesting explosive for me since I have found out that it is capable of dissolving guncotton.

Because of this I have decided to use it to make blasting gelatin to help the NG dissolve the guncotton instead of using acetone and having to wait for it to evaporate, also I have thought of mixing it with straight NG, 40% Methyl Nitrate with 60% NG to get a near perfect oxygen balance which could make a powerfull liquid explosive.

Anyway a few days ago I made some Methyl Nitrate and here are the
pictures:

Starting materials: left: 40ml Methanol middle: 80ml 70% HNO3 right: 80ml 98% H2SO4:http://i155.photobucket.com/albums/s300/kpppppk/Picture003.jpg

Mixed acid: notice the fumes:http://i155.photobucket.com/albums/s300/kpppppk/Picture005.jpg

Adding methanol:http://i155.photobucket.com/albums/s300/kpppppk/Picture021-2.jpg

The mixed acid gets cloudy and the Methyl Nitrate forms its layer on top:http://i155.photobucket.com/albums/s300/kpppppk/Picture024-1.jpg

After all the methanol has been added, a thick clear layer of Methyl Nitrate sits on top:http://i155.photobucket.com/albums/s300/kpppppk/Picture032-1.jpg

http://i155.photobucket.com/albums/s300/kpppppk/Picture026-1.jpg

http://i155.photobucket.com/albums/s300/kpppppk/Picture028.jpg

After the layer has formed, the clear layer of Methyl Nitrate is sucked off with a pipette and transfered into a few ml of fresh water for washing:http://i155.photobucket.com/albums/s300/kpppppk/Picture036-1.jpg

During the reaction the tempreture never rose above 25 degrees.

Final yield was 35ml, there was a few more ml's floating on the acid, but it dissolved in the 500ml of water that I poured the acid mix in.

It is very important not to wash it with too much water as it is very water soluble, just 5ml or so is enough so you can add bicarb.

Here is a video of 2 drops of Methyl Nitrate deflagrating:http://s155.photobucket.com/albums/s300/kpppppk/?action=view&current=MethylNitrate1.flv

This is the fiirst time I have detonated this stuff and I find it to be very brisant, it sounds a bit like NG, but makes more of a loud crack than a boom.

Here is a video of the 35ml detonated in a small 50ml whisky bottle, the diameter of the bottle was 30mm to ensure a full VOD of 8000m/s, it was set off with 1 gram of pressed AP:http://s155.photobucket.com/albums/s300/kpppppk/?action=view&current=IMG_0001.flv

MartinT
September 12th, 2007, 07:52 AM
To dry my EGDN I used some MgO that reacts with water and also neutralizes the remaining acids...I think that's the best way to dry a liquid nitric ester, since the drying process takes only a few minutes, and you can obtain a very transparent product.

lucas
September 22nd, 2007, 05:36 AM
My preferred technique is to add glycerine to chilled nitric acid and slowly add sulphuric acid last. This is of course only a preference which works. Adding glycerine as the third reagent is fine as are other methods.
I usually take well over an hour to complete the addition of sulphuric acid.
I chill the acids in a freezer before use.
I like to keep the reaction below 15 degrees C after additions during the early stages, and below 20 degrees C later once the reaction should be more steady.
I use magnetic stirring with an ice bath.
I use per 10ml glycerine(12.6g) 30ml 70% nitric acid(containing abut 30g HNO3) and 45ml 98% sulphuric.
Or if I have 95-99% nitric I use 20ml nitric(30g HNO3). and 30ml Sulphuric
Either way this represents about 15% excess nitric acid and 1.5 volumes of sulphuric acid per volume of nitric acid
I have used a separatory funnel, but I sometimes use a 20ml needleless syringe and a fine glass pasteur pipette for separations.


I find that temperature increases are most significant during the early additions of sulphuric acid, particularly when using 70% nitric rather than 90+% nitric. My belief is that the addition of sulphuric is more exothermic when free water is present. Once the water has been bound up by the sulphuric acid the temperature rises settle and additions can be larger. I am very slow during all additions

With this method, addition of 10-20% of the total sulphuric acid shows no visible signs or reaction. Later addition of sulphuric will cause cloudiness to form. This is a suspension of nitroglycerine forming. After this stage, the additions of sulphuric are larger. I like to leave the reaction mixture stirring after final addition for about half an hour while still being chilled by crushed ice. After stopping stirring two distinct layers form, however I do not separate at this stage. I drown the mixture in plenty of cold water and a litte crushed ice.

Washing is per standard methods, with lots of water washings and then sodium carbonate solution. and then water again. I find even after many washings, if the NG is allowed to stand in water, the water will become acid to limus or indicator strips.

About 24-48 hours over silica gel in a dessicator turns wet cloudy NG clear and dry.

I have found that even after many any washings with water and carbonate. The dessicated material can turn litmus redish. I have then returned to washing stages.


With regard to smokeless powder use. (I have slow burning coarse rifle powders)
-It will not dissolve in NG on it's own. No surprise.
-It will make a gelled mass if acetone is poured over it.
-If added to swirling acetone it will not clump up as much.
-The granules take a long time for the acetone to reach the centre. The outside of the granules become visibly translucent but the centre of the granule stays dry for a long time.

When using 2.5g smokeless powder in 20ml acetone and 5ml ether I found that:
Placing the container of 80/20 acetone/ether mixture and smokeless powder in a tumbler(ball mill) such that it was being inverted end to end speed up dissolution. The mixture was a viscous liquid and the evaporation of the solvent took days to make progress. Use of less solvent and finer powder like a shotgun powder would be adventagous.

The smokeless powder in question is not labelled as single or double base which is unfortunate. It is green and gives a lovely colour to the gel made but this is of no practical consequence.

I believe that stablisers used in smokeless powder are likely to stablise any blasting gelatine made from it in starage and possibly in use too. The former point is an advantage, the latter a moot point. Only on one occasion has such blasting gelatine been used (5% SP content) . It was succesfully initated by a number 8 detonator, which is no surprise and woked as a booster for cast, high TNT content, torpex type explosive. It has not been tested with improvised detonators.


"Reloader" brand powders seem to have ingredients on the side and may be distinguished as DPSP or SBSP. Reloader 15 does anyway, it is double based and I think the stabliser was listed too.

Billy Bones
April 11th, 2008, 03:06 PM
"My I love it when people say this....they are back the next day, ready to argue till the end of time about some retarded point. Calm the hell down and remove yourself from this thread should you feel the need to. Its like you're having your period or something. Fight and flame elsewhere, we can get along fine without you."

No Problem! How can I erase my previous posts?

Deceitful_Frank
April 11th, 2008, 03:33 PM
I don't think that our ears can really distinguish between the sound of an explosion that takes 1/200,000 of a second to occur and one that takes 1/750,000 of a second! (assuming that the explosive gel was 1cm thick in all directions around the cap)

In my experience LVD does not SOUND much different to HVD and even with minimal confinement that charge should have gone high order or not at all... my guess is the latter. The damage to the ground was simply caused by the HMTD in the cap. Looks to me about what you would expect from this excellent and powerful peroxide and your gel simply acted as a hydraulic medium to transfer the energy efficiently to the asphalt.

Did you use no acetone or NM this time to help that NC to dissolve?

EDIT:

Ok I have read through your post a second time and noted the TWO cm deep hole in the ground... 1 gram of HMTD would not have the power to acheive this. Maybe 5mm to one cm but not two. I think that what you have here is simply the result of a small ill-confined charge.

The critical diameter of this blasting gelatine has resulted in a layer maybe 5mm thick around the whole charge that failed to go high order if at all and because it was a small charge, this layer accounts for a large portion of the whole.

If you imagine a cube of sides 3cm, even a layer 5mm thick around the whole would account for a whopping 19/27 of the entire mass! the oppposite is true for instance if you were to detonate a large UNCONFINED sphere of plastic explosive. Those few mm around the outside that go low order or just end up as a thin film on their surroundings account for a tiny proportion of the whole, massive charge.

Billy Bones
April 11th, 2008, 05:03 PM
Are you serious??? The target was hard as rock asphalt concrete, 1 gr. HMTD can’t even make a scratch on the surface.

“Looks to me about what you would expect from this excellent and powerful peroxide and you gel simply acted as a hydraulic medium to transfer the energy efficiently to the asphalt.”

This is some joke or what…

Deceitful_Frank
April 11th, 2008, 05:37 PM
Discussing high explosives is no time for joking. Misinformation and complacency kills.

Asphalt and concrete are completely different. Asphalt has a base of bitumen derived from heavy fractions of crude oil, is elastic but not particularly tough where as concrete is composed of hydrated portland cement, sand and aggregate... which is it?

I have personally seen 0.7g of handpressed HMTD in a bic pen lid remove a 3cm X 2cm area of ASPHALT (the shit the make cycle paths out of) to a depth of 5mm.

Billy Bones
April 11th, 2008, 06:00 PM
http://en.wikipedia.org/wiki/Asphalt

http://en.wikipedia.org/wiki/Asphalt_concrete

I think the pictures and my post was quite clear. The target was ordinary asphalt concrete. What don’t you understand?

“Discussing high explosives is no time for joking. Misinformation and COMPLACENCY kills.”

Ok, NOW I get the picture!