Sciencemadness Discussion Board - Short question / quick answer - Thread

I have never work with picrate salts so beter someone who have work with them will answere you question. You can try to store few mg into a metal container to see if it will react over time.

Glutamate looks that it can be nitrated (OH and NH2 bonds) but HE containing metals usually has low performarmance. Better use your acids for ETN/PENT in my opinion.

Thank you!

Quote: Originally posted by Bert

Quote: Originally posted by joseph6355

Question number 2: Does Ammonium picrate react with metals the same way as picric acid does?

From UXO info:

Quote:

Thank you.
Mineral water usually do not contain any of these metals. The majority of mineral water's minerals are sodium, potassium, calcium, and so on...
Are metal picrates usually too sensitive to friction?

joseph6355 - 29-5-2018 at 20:54

For some reason I cannot edit my last post.

Would I be able to prevent picrate formation by adding sulfuric acid to the mineral water and converting the salts to their respective sulfates?
I remember reading something about this. The french used to add a little sulfuric acid to their water in order to melt the DNP/TNP mixture in that water bath.
Giving that I know the approximate amount of salts that are present in the water, I could add a slight excess of sulfuric acid to sulfonate them.

I suppose that the TNP would dissolve more in that sulfuric acid mixture.

underground - 12-6-2018 at 11:17

I did my 1st ever PETN synthesis with h2so4 (98%)/kno3. The procedure was like ETN synth but i increased the temp to 45 C. It was looking like a got some good ammount of petn cause the mixture became thick. After i finish the nitration, i poored the mixture into cold water with stirring, the water turned like milk and with filtration, it passed all through it. Any ideas or advise ?

MineMan - 13-6-2018 at 14:11

Underground your description is vague. Please tell us more about your filtering. What kind of filter did you use. Were there PETN particles finely suspended that caused this milk?

underground - 13-6-2018 at 14:45

Yea it looks like that. I tried again with a double filter and it works great. It was my 1st synth so i do not know that much about PETN. It is a bit strange, it looks like Lime when it is wet with water.

[Edited on 13-6-2018 by underground]

joseph6355 - 15-6-2018 at 18:46

I did my 1st ever PETN synthesis with h2so4 (98%)/kno3. The procedure was like ETN synth but i increased the temp to 45 C. It was looking like a got some good ammount of petn cause the mixture became thick. After i finish the nitration, i poored the mixture into cold water with stirring, the water turned like milk and with filtration, it passed all through it. Any ideas or advise ?

Wash it with a good amount of water.
Metal sulfates are usually very soluble in water. PETN on the other hand, isn't.
The milky stuff will dilute and the PETN will stay as a solid.
Just make sure to use a very fine filter paper to make sure that your solids stay on it.

Bert - 16-6-2018 at 07:23

If you're going to keep it for more than a few days, dissolve the PETN in a water miscible solvent such as acetone, neutralize carefully and recrystalize. Lots of discussion and information about this here, Rosco pposted a DuPont patent in the thread.

PETN is about as stable as this class of HE gets, but it's not going to be long term stable with ocluded acid- Which PETN will certainly have unless you have recrystalize it.

[Edited on 6-16-2018 by Bert]

improving straw caps

underground - 16-6-2018 at 11:01

I tried to detonate about 3.5g of pressed PETN that I made (really powerful, looks much more powerful than ETN with the same amount). I am using HMTD straws as a cap. I tried 2 charges and i think the second one did not detonate with full power, i noticed that some HMTD burned before detonation, so i guess the remaining HMTD was not enough to fully detonate the PETN. I am thinking now to improve a bit the straw by a) adding some amount of pressed ETN at the end of the HMTD straw, b) make a small cone (shaped charge) at the end of the HMTD straw with a pencil, or c) do both a) and b) (add ETN shaped charge at the end of the HMTD straw). Which one do you think is better ?

[Edited on 16-6-2018 by underground]

Rocinante - 16-6-2018 at 21:53

Using straws (or anything that bends easily) for blasting caps is a certain way to hospital and/or cemetery. Use plastic syringes or even better - plastic test tubes (like for urine samples) ... at the very least.

underground - 16-6-2018 at 22:05

I am always very careful and i almost never touch it except few seconds before initiation and that with great care. I always transfer it one by one inside big plastic bags away from my body and each one is less than a gram. I am planing to built an ebw tho with some ETN for initiation.

Rocinante - 17-6-2018 at 00:36

You can never be careful enough. Use better material. Primaries are OK, just as long as you use proper tubes ((i.e. not bendable and one end without any seals.. like test tubes or pre-made blasting ap cavities (which are sold))). A small bucket filled with gypsum powder works better. You can detonate 1 g of explosie in 2 kg of powder and you won't hear that much.

NeonPulse - 17-6-2018 at 23:14

Just be aware that Using a plastic straw can create a static electricity charge that could potentially be enough to activate HMTD. This would obviously be disastrous. I also recall it not being compatible with Aluminium either. A few people have had accidents with HMTD including one involving a plastic straw I recall reading on the old E&W forum some time ago but I don’t recall the specifics.

Bert - 17-6-2018 at 23:43

HMTD is flat out incompatible with common capsule metals.

If Du Pont their own bad selves couldn't cost effectively make it a safe to handle and effective commercial primary, why do YOU handle this organic peroxide? Because it is EASY TO MAKE??? Wiping your ass and picking your nose without fingers won't be easy and needing to do it that way would go on for a long, long time.

Rocinante - 18-6-2018 at 01:09

Any primary explosive is dangerous if handled improperly (direct contact with fingers..etc). Also, wet lead azide is incompatible with copper leads, too. But, of course, avoid HMTD/metal comb, TATP/metal works better (if you can't get anything else). The leads change in color due to re-sublimation and HCl evolution but in general the BC stays OK for several months (if stored at ~ 15°C).

Look here for basic ideas: https://www.instructables.com/id/How-to-Make-a-Blasting-Cap-...

And.. again.... bitte... forget about straws... already!

Laboratory of Liptakov - 18-6-2018 at 08:43

HAha.....First step: Wiping ass is of course more easily before preparation any primary.....:-) Second step: The wiping ass is very difficult, after fail at preparation of primary. With restrict count of fingers. But main idea, my opinion is, that if you use copper hexamine perchlorate(CHP), as primary, your fear will teh past and memories only......I remember my fear well. Many years ago I used 100x HMTD and azides and SADS. I was always afraid. What if by chance. But with CHP, fear is really past..... :cool:

....my opinion only.... :cool:

underground - 18-6-2018 at 11:21

I am going to make an EBW circuit soon. I do not have access to make any other primary that is why i am using HMTD so far.

[Edited on 18-6-2018 by underground]

roXefeller - 18-6-2018 at 14:53

Reading that instructable, it looks very familiar. I think someone on this board developed it. Anyway I like the suggesting to use an extraction string for removing caps from failed shots. Not so easy for stemmed holes or mud capped shots, so cap reliability is still a necessity for those shots.

+10 for Bert, easy is short sighted.

Edit: why is hmtd in straws so common as a starting point? Is that a Ragnar Benson or Anarchists Cookbook thing?

[Edited on 18-6-2018 by roXefeller]

nitro-genes - 20-6-2018 at 14:42

Does anyone know the critical diameter of hydrogen/oxygen mixtures? Seeing these HHO torches and welders on YT everywhere, I was wondering if this could be an easy way to prepare something similar to NONEL, which uses HMX/aluminium dust IIRC (https://en.wikipedia.org/wiki/Nonel). Would be extremely cheap and easy to make and maybe nice for demonstrations as per weight, only very small amounts of explosive material would be needed.

Laboratory of Liptakov - 21-6-2018 at 13:00

Interest idea. Because VoD seems a pretty good: https://deepblue.lib.umich.edu/bitstream/handle/2027.42/3730...

mackolol - 22-6-2018 at 03:36

I have a question, when I'm distilling liquid of smaller density (higher phase) and higher boiling point then its a steam distillation and it should go easier. But when I'm distilling liquid of higher density (lower phase) and lower boiling point, is it much harder to distill it off and does it require higher temp than normal?

joseph6355 - 29-6-2018 at 22:50

I was looking for an OTC source for P2O5 and I found a fertilizer that allegedly contains it in its mixture.
The manufacturing process makes me skeptical of recovering any of it though. But I thought that it would be worth talking about it at least.
It is obtained by the fusion (or casting?) procedure of phosphorus, calcium, magnesium, silicon and other micronutrients. The natural phosphate, enriched with magnesium silicate, is then cast inside an electric furnace at a temperature of 4530 ºF. The incandescent mass is then submited to a thermal shock with a water jet and then dried, ground and packed.

Guaranteed concentrations of at least:

Phosphorus (P2O5) - 16 %
Calcium (Ca) - 16 %
Magnesium (Mg) - 6,5 %
Sulfur (S) - 6 %
Boron (B) - 0,1 %
Copper (Cu) - 0,05 %
Maganese (Mn) - 0,3 %
Silicon (Si) - 9 %
Zinc (Zn) - 0,55 %

I can't think of any way of separating it out of the mixture of whatever this is. Ideas are welcomed.

JJay - 29-6-2018 at 23:13

That's just the analysis; it's not a good source of phosphorus pentoxide or elemental calcium. I don't think phosphorus pentoxide is available OTC. It is available to amateurs but can be a little hard to find at times.

joseph6355 - 30-6-2018 at 13:47

Quote: Originally posted by JJay

That's just the analysis; it's not a good source of phosphorus pentoxide or elemental calcium. I don't think phosphorus pentoxide is available OTC. It is available to amateurs but can be a little hard to find at times.

That sucks. :\
Where can I find elemental phosphorus OTC then? Even a child could make P2O5, you just have to burn it with enough oxygen in a dry environment.

underground - 13-8-2018 at 23:37

Which is the easiest way to make acetyline gas? I can not find anywhere calcium carbide and acetyline cylinders are huge and expensive. Is there any other way to make acetyline ?

Just type in google "synthesis of acetylene" found it on first found website

mackolol - 14-8-2018 at 00:36

F is a wide-necked 250 ml bolt-head flask, to which is fitted a double-surface reflux water-condenser C and the dropping funnel D. From the top of C, a delivery-tube leads down to the pneumatic trough T, where the gas can be collected in jars in the usual way. 100 ml of rectified ethanol and 25 g of powdered potassium hydroxide are placed in the flask F. The mixture is gently boiled under reflux until the potassium hydroxide is almost entirely dissolved. 15 ml (or 33 g) of 1,2-dibromoethane is place in the dropping funnel D, and added drop-wise into the boiling solution of potassium hydroxide in ethanol. A rapid reaction occurs, acetylene being generated and potassium bromide precipitated. Generated acetylene is passes through the apparatus until all the air is expelled. Then acetylene is collected under water or directly used for an experiment.

You can try this with 1,2 dichloroethane instead, which is cheaper and can be made by esterification of ethylene glycol with hydrochloric acid and see if it works.

A-glass-apparatus-for-the-preparation-of-acetylene-from-12-dibromoethane-and-potassium-hydroxide-369x379.png - 63kB

[Edited on 14-8-2018 by mackolol]

underground - 14-8-2018 at 02:43

My purpose is only for making silver acetylide. I guess air is not a broblem as it will not react with the silver nitrate solution. So i am thinking to pass directly the gas into the solution and skip the reflux condenser cause i dont have it

DrManhattan - 24-8-2018 at 06:57

Q. After running a solution of ETN/methanol through a filter during recrystallization i am left with an unknown white precipitate in the filter. Not much at all, but it certainly is not ETN as i have tried to burn it but it is completely inert. It does not even melt under a blowtorch. It has the consistency of a very fine powder and is not crystalline. Any ideas on what is it? I used the hno3/sulfuric acid route for the synthesis.

[Edited on 24-8-2018 by DrManhattan]

OneEyedPyro - 24-8-2018 at 14:23

Quote: Originally posted by DrManhattan

Q. After running a solution of ETN/methanol through a filter during recrystallization i am left with an unknown white precipitate in the filter. Not much at all, but it certainly is not ETN as i have tried to burn it but it is completely inert. It does not even melt under a blowtorch. It has the consistency of a very fine powder and is not crystalline. Any ideas on what is it? I used the hno3/sulfuric acid route for the synthesis.

[Edited on 24-8-2018 by DrManhattan]

No idea... Maybe it's some kind of impurity in your sulfuric acid?

I have seen weird things with AN/H2SO4 nitrations of impure erythritol (namely Truvia). I often had a bit of precipitate that was insoluble in water, alcohol or acetone. Maybe it's the same compound, I never bothered to do anything but dispose of it.

After going to pure erythritol and HNO3 rather than raw Truvia and nitrate salt I've never had this happen.

Magnesium nitrate as a dehydrating agent

underground - 17-9-2018 at 15:19

When magnesium nitrate forms it tends to absorb water forming a hexahydrade. What about using it in the rdx preparation ? In theory if you add mangesium metal into nitric acid it will concentrate it. Has anybody ever tried it ?

[Edited on 17-9-2018 by underground]

DrManhattan - 11-11-2018 at 05:45

Hi, just wondering if Mercury Fulminate is compatible with aluminium as i have heard most people say that brass should be used for a mercury fulminate cap.

walruslover69 - 11-11-2018 at 08:25

I would not recommend using anything aluminium with mercury or its salts.

greenlight - 11-11-2018 at 08:27

Mercury fulminate reacts rapidly with aluminium forming Al2O3 when in direct contact. The trace amounts of elemental mercury within the product would as well forming amalgam. Copper is another no no.

I have read that it reacts much slower with other metals like brass and bronze but faster if moisture is present. One metal that ot does not react with is nickel though.

You can either use a more compatible metal and apply a protective coating to the surface so it does not come in direct contact or use another primary.

Hope that helps.

DrManhattan - 12-11-2018 at 02:51

Exactly the answer i was looking for. Many thanks.

Herr Haber - 12-11-2018 at 04:17

Copper has been used for MF during WW1 and I've seen a good deal of copper in WW2 items aswell.
Are you certain about this ?

greenlight - 12-11-2018 at 08:38

I will check some literature when I get home but I am quite sure that the copper was coated in a protective lacquer. I will get back to you though

greenlight - 12-11-2018 at 10:50

From Primary explosives, pg 48;

"Moist MF reacts with copper giving copper fulminate which is less sensitive to impact but more sensitive to friction the MF itself. The presence of moisture is necessary for the formation of copper fulminate. Another side effect the reaction of copper is the precipitation of mercury which forms an amalgam that may weaken the copper cap which the MF is embedded in.
It is therefore necessary to prevent contact of MF with copper in its applications protective coating or nicking of the copper surface."

Seems like these reactions are very slow though but my money would be on the fact that these WWll copper detonators would have been protected in some way from direct contact with the mercury fulminate.

[Edited on 12-11-2018 by greenlight]

underground - 19-11-2018 at 12:19

An idea that i was thinking for a long time but i did never posted cause i thought that maybe it will be a dump idea but i decided to post it anyway :p

I was thinking if it is possible to increase the density of an energetic material by cooling it.

nitro-genes - 22-11-2018 at 16:49

Cooling the energetic material could indeed improve it's density, though how much would really depend on phase transition temperatures and on the chemical structure. Water for example forms an extensive hydrogen bond network on cooling, making ice actually less dense than water itself. For most compounds shrinkage on cooling is only a few percent, so the effect for most compounds would probably not be very significant. It is an interesting question though what would happen with the detonation velocity at very low temperatures, it is well known that some primaries only make DDT reliably at warmer temperatures and can fail when cold (DDNP for example). If anything, I would say preheating a explosive could potentially increase its detonation velocity (Not sure though).

Hmmm, has this ever been tested? Take the most dense and heat stable explosive, heat it to the brim of its existence, detonate and measure VoD compared to cold?

Dornier 335A - 25-11-2018 at 02:12

Cooling a HE would indeed increase its detonation velocity and detonation pressure. Those properties are much more strongly affected by density than energy of the material, where the thermal energy is included. Initiating detonation would probably be more difficult as you say nitro-genes, since the compound needs more of a kick to start a self sustaining detonation. I remember reading something about hot molten TNT being almost as sensitive as NG but it surely has lower VoD. I also think Urbanski listed the VoD of frozen NG to 8000 m/s, quite a bit higher than the normally reported 7700 m/s.

underground - 25-11-2018 at 07:12

Yea that is the point. For example maybe cooled PETN or ETN could achieve density and peformance like HMX or even higher.

Daffodile - 25-11-2018 at 18:05

Bought a bunch of "Calcium Ammonium Nitrate" cold packs today from the store. However these things are rarely what they said so I tested it with Copper and some Sulfuric Acid, expecting a precipitate of Calcium Sulfate and emission of brown gas. The gas was produced but no precipitate occurred. Is Calcium Sulfate soluble in highly acidic solutions or is my salt likely just Ammonium Nitrate? Its hydrated but not hygroscopic.

walruslover69 - 26-11-2018 at 12:01

try to get a precipitate with sodium sulfate, or sodium carbonate

FeedMe94 - 12-1-2019 at 17:35

Is Lead Styphnate the "best" primary explosive ?

Edit^
I'm sure its not. I'm just asking because it is used in almost all commercial explosives

[Edited on 13-1-2019 by feedme94]

snooby - 13-1-2019 at 09:38

No, its used as the first kickstart in a blastingcap, because ist very flame sensitive. The leadazide that follows is the real initiating compound. So beter for dextrinated leadazide, since it also quite sensitive towards other, safer priming compoundss. For example blackpowder.

Furthermore, there are better primarys (tetrazoles, which also have drawbacks btw). Go for BNCP is you want the holy grale in my opinion.

FeedMe94 - 14-1-2019 at 20:49

At the moment im on my way for SADS and TACP

otonel - 20-1-2019 at 06:15

I want to work with hydrazine hidrate and I want to ask about protective equipment required .I'll work out and wear gloves but I need to use the gas mask?

snooby - 23-1-2019 at 00:11

He. At the moment I am researching about Nickel -tris carbohydrazide perchlorate (NiCP). You may have heard from it.. So since I want to make the precursors myself, I want to synthesise NiCLO4 myself. Before I am buying a lot of expensive things I want to check if my thoughts are right....

Add basic nickel carbonate (cheap chemical) to a 10 - 70 % solution of HCLO4 until no more carbonate dissolves anymore - or - till the PH becomese neutral. Exces of carbonate will just not dissolve, because it is almost insoluble in water. So the solution of NiCLO4 can be filtered of. The solution is evaporated till crystalisation and the hygroscopic NiCLO4 is dried in a descecator (with sulphuric acid?).

underground - 23-1-2019 at 03:23

It looks correct to me. I am using CaCl as a descecator

FeedMe94 - 23-1-2019 at 07:26

Is 46-0-0 fertilizer , pure Urea ? That's what the guy from fertilizer shop told me

snooby - 23-1-2019 at 09:22

I have neutralised HCLO4 to a ph of 7 using sodiumcarbonate (the hydrate), to regular household soda. Now I eveporated the solution and crystals appear. Since i used a slight excess of carbonate, there is contamination of some sodiumcarbonate. I want to use this NaCLO4 to convert it to Ammoniumperchlorate. I was thinking of using ammoniumchloride, since the sodiumchloride that will be formed is much more soluble then the ammoniumperchlorate. I have also ammonium bicarbonate. Which route would be preferabme?

http://www.chlorates.exrockets.com/ammper1.html (found it)

[Edited on 23-1-2019 by snooby]

underground - 23-1-2019 at 18:01

Why you want to do it with the hard way ? Why you did not just neutralize your HCLO4 with ammonium bicarb to form directly ammoniumperchlorate ? You can also bubble ammonia gas into Hclo4.

[Edited on 24-1-2019 by underground]

Nitromethane Sensitizers

underground - 24-1-2019 at 06:50

Anyone have any information for any easy to make/find NM sensitizer ?

MineMan - 24-1-2019 at 09:37

Anyone have any information for any easy to make/find NM sensitizer ?

Underground. I thought microballoons and al work fine... I take it you want a chemical sensitizer though??

underground - 24-1-2019 at 11:03

Not only a chemical sensitizer would be better but also i do not have access to microballons.

[Edited on 24-1-2019 by underground]

Laboratory of Liptakov - 24-1-2019 at 11:22

https://www.amazon.com/Glass-Microspheres-1-Quart/dp/B00MNSE...

underground - 24-1-2019 at 17:51

https://www.amazon.com/Glass-Microspheres-1-Quart/dp/B00MNSE...

NaCLO4

snooby - 25-1-2019 at 00:00

Underground: yes a even better way to make AP is to neutralise HCLO4 with strong ammonia solution, this way you get pure AP.

HOWEVER: my plan was to make NaCLO4, not AP. At the last moment I received info that I could buy NaCLO4 :cool:

.

Back to the NaCLO4 synthesis, I still want to make a litle.bit of pure NaCLO4.
So now I have probably around 90% NaCLO4 with some NaCO3 (quite a lot:cool

. How can I purify this?? I was thinking to redisolve the NaCLO4/carbonate again, and then add diluted HCLO4 in it until no CO2 anymore is noticable. Then again evaporate the very diluted HCLO4 / NaCLO4 solution is evaporated on hotplate.

However: is this safe to do?? Can I just evaporate this without problems. I gues its just the azeotrope of HCLO4 will evaporate with the water, but I just want to be SURE. Furthermore, which temp does this be done..? I cant find evaporation point of diluted perch acid (only 70% is around 203C)...

So wich temp should i use to eveporate remaining acid (10percent hclo4), or just not do it?

Edit edit.. Should have figure this out earlier:

Solubility of Na2CO3 compared to NaCLO4

At 1 degrees C: 7 grams of Na2CO3 in 100 ML H2O
167 grams of NaCLO4 in 100 ML H2O
Done..

Sorry for lots of messages but I just like to figure this kind of stuff out myself, I have had only veryyy basic science on high-school

[Edited on 25-1-2019 by snooby]

Herr Haber - 25-1-2019 at 04:42

Anyone have any information for any easy to make/find NM sensitizer ?

An acid, a strong base. Urbanski has all the ideas.

Nitromethane gel on cap No.8 sensitive:

Laboratory of Liptakov - 25-1-2019 at 05:28

Nitromethane.....................................80%
commerce nitrocellulose (12,4N).......10%...(best is shotgun NC propellant)
Aluminium bright color type................5%....(or Mg, Magnalium, any Al)
Glass microballoons...........................2%....(best is 125g/liter type)
Variable contents for NC....................3%+............ :cool:

..................LL

[Edited on 25-1-2019 by Laboratory of Liptakov]

NaClO4

Laboratory of Liptakov - 25-1-2019 at 06:18

@snooby : You have HClO4?....Thus you can prepare anything. KClO4, NaClO4, NH4ClO4, LiClO4 and lot nexts. You leave the think on boiling dillute HClO4. All around 10 meters will incredible oxidized from steam. And if you will have NaClO4 is it also almost all, what you need..... :cool:

FeedMe94 - 25-1-2019 at 08:39

Will this ball mill do the job for Black Powder and aluminium ?
Im not sure cause of that shape of the drum

Screenshot_20190125-183433_eBay.jpg - 333kB

underground - 25-1-2019 at 08:45

Nitromethane.....................................80%
commerce nitrocellulose (12,4N).......10%...(best is shotgun NC propellant)
Aluminium bright color type................5%....(or Mg, Magnalium, any Al)
Glass microballoons...........................2%....(best is 125g/liter type)
Variable contents for NC....................3%+............ :cool:

..................LL

[Edited on 25-1-2019 by Laboratory of Liptakov]

Laboratory of Liptakov is it storage stable that mixture or you made it before use ?

Will this ball mill do the job for Black Powder and aluminium ?
Im not sure cause of that shape of the drum

It should work

Note that

Critical speed = 265.45 / sqrt (jar ID - media diameter) (diameters in inches)
Optimal speed is 65% of the critical speed.

[Edited on 25-1-2019 by underground]

nitro-genes - 25-1-2019 at 10:39

Planning to write sort of an more in depth essay about the copper/ascorbic reduction with some additional information about the literature concerning the selective mono reduction of some polynitroarenes. Does anyone know if mono reduction of 2,4,6-trinitroanisole has been attempted and the resulting isomer distrubution for the amine?

Laboratory of Liptakov - 25-1-2019 at 11:17

@underground ....Nitromethane gel is stable. Is nothing what should by reacting together there. Storage in close jar, of course. Against evaporation of NM......... :cool:

FeedMe94 - 26-1-2019 at 02:16

Will this ball mill do the job for Black Powder and aluminium ?
Im not sure cause of that shape of the drum[/rquote]

It should work

Note that

Critical speed = 265.45 / sqrt (jar ID - media diameter) (diameters in inches)
Optimal speed is 65% of the critical speed.

[Edited on 25-1-2019 by underground]

Any idea what media to use? Im trying to find Lead Antimony spheres but the only thing i can find is small metal balls used as ammunition. Also found Alumina ceramic balls. The company says no sparks can be produced

Edit*
My jar is 3 litres. I need 1.5 litres of milling media ?

[Edited on 26-1-2019 by FeedMe94]

underground - 26-1-2019 at 08:34

Yea you are going to need 1,5 litres of media.

By the way, why don't you try to make one on your own, it shouldn't be hard to make it and it would be much more better and cheaper. Thick pvc pipe will do the job as a jar.

@underground ....Nitromethane gel is stable. Is nothing what should by reacting together there. Storage in close jar, of course. Against evaporation of NM......... :cool:

Thanks

P.S. Laboratory of Liptakov i have seen you have made some plastics with scapa P.I.B and 5/40 motor oil with very good results. Have you ever try it with methyl ricinoleate instead of 5/40 motor oil ?

[Edited on 26-1-2019 by underground]

underground - 3-2-2019 at 01:57

Can organic perchlorates like HDP or Perchloric acid be made fromm POTASSIUM Perchlorate without distilation ?

loading and pressing powder in an irregular hole

C6(NO2)5CH2CH(CH3)N(NO2)2 - 5-2-2019 at 16:44

suppose you had an irregularly shaped cavity ~1cm wide by 10cm long that you wanted to put an explosive powder in, but the only hole to access it was 5-8mm wide. What would be the best way to pack the powder inside? I can't pour a powder in and fill the voids with a liquid-phase explosive, because of chemical compatibility issues with the walls of the container. So, what's the best way to press a powder to a high density when you only have a small hole to introduce it through?

underground - 6-2-2019 at 01:34

Melted ETN, then allow it to cool

[Edited on 6-2-2019 by underground]

mayko - 7-3-2019 at 19:06

(edit)
sorry I was looking for the general-purpose short questions thread

[Edited on 8-3-2019 by mayko]

underground - 18-3-2019 at 06:53

Is there any soluble hexamine salt ? (In order to use for metathesis reaction for HDN /HDP production )

I can not find any info from net

Daffodile - 18-3-2019 at 20:09

Anyone done the cyanamide-hydrazine aminoguanidine synthesis?

Just tried it but got no/ negligible yield.

I know my Calcium Cyanamide was decent quality, and my Hydrazine Sulfate was as well at some point (bottle is two years old, however the sample has become quite acidic).

Problems emerged when the pH would not increase substantially during the reaction, as it should with formation of free base Aminoguanidine.

I also accidentally let the thermometer come out of the solution, so the temperature increased to boiling for several minutes.

The Bicarbonate was added as a mostly-dissolved slurry. It all dissolved in the filtered reaction mixture and effervescence persisted for several minutes.

No precipitate formed.

I'm stuck. Any ideas where this could have gone wrong?

FeedMe94 - 26-3-2019 at 01:33

Can i recrystalize ETN with Isopropyl alcohol or acetone ? Should i also add bicarb or ammonia ?

Herr Haber - 26-3-2019 at 05:02

Can i recrystalize ETN with Isopropyl alcohol or acetone ? Should i also add bicarb or ammonia ?

Yes, yes and yes.
Acetone is not as bad as people say.
You can crash your ETN in water with a little bit bicarbonate.
You can also use bicarbonate if there's enough water + solvent before crashing.

FeedMe94 - 26-3-2019 at 08:22

I had some ETN made 6 months ago. I just recrystalized it using hot acetone and the crushed it into cold water with some drops of Ammonia Water. Got some ETN back but a lot of oily substance was at the bottom. I added more water and turned all into ETN. The ETN i got is like crumble , not like the one without recrystallization which was like flour

Herr Haber - 26-3-2019 at 11:17

More water next time

Redissolve the crumble!

FeedMe94 - 26-3-2019 at 12:53

Redissolve in acetone ? Can i recrystalize the old batch and a new one together ?

Herr Haber - 27-3-2019 at 04:43

Well I suppose you are not going to grind this crumbe into a mortar and pestle !

So yeah, redissolve with the new batch, it's the same molecule so it doesnt matter. The worst you can do is purify further.

Would I be correct to assume some of that crumble adhered to the walls of the recipient you crashed it in ?
If so, definitely not enough cold water. Use acetone to clean the container, pour it straight in cold water. Do not scrape it !
ETN isnt soluble in water so it'll always be better to use more water than less. Filtration will be slower but who cares ?

snooby - 28-3-2019 at 14:22

Someone got an english synthesis of copper Glycinate perchlorats?

FeedMe94 - 29-3-2019 at 03:59

Yesterday i made some PETN and recrystalized it. I also recrystalized some old PETN i had. The difference i found is the the old PETN is like free flowing and the new PETN acts like kinetic sand. Whats going on?

itsafineday - 29-3-2019 at 05:49

Can I make nh40h/methanol/dcm extraction solvent by mixing nh4oh with methanol / dcm azeotrope distilled from paint stripper? I guess I'm wondering how miscible nh4oh is with the azeotrope of methanol and dcm. I'd rather not wash out the methanol just to add it back.

Laboratory of Liptakov - 29-3-2019 at 12:08

@FeedMe94 error is in solvent, which content some the fat or else grease impurities.

FeedMe94 - 29-3-2019 at 13:38

@FeedMe94 error is in solvent, which content some the fat or else grease impurities.

I dont think so because the other PETN i recrystalized i used the same Acetone, its 99.6%.
Anyway i recrystalized it again as you told me and i will wait for to dry

Rosco Bodine - 30-3-2019 at 06:39

Quote: Originally posted by snooby

Someone got an english synthesis of copper Glycinate perchlorats?

snooby,

Haven't got one handy but can speculate a method that should probably work via metathesis reactions from NH4ClO4. React Ca(OH)2 with NH4ClO4 in aqueous medium to form solution of Ca(ClO4)2 and filter out excess unreacted Ca(OH)2. Heat to drive off excess byproduct NH3. Treat solution with CuSO4 to form Cu(ClO4)2 and filter out byproduct low solubility CaSO4.

Treat solution of Cu(ClO4)2 with glycine, heated together 2 hours and allow to stand for up to a week for crystals to form. (lit)
Evaporation with heating to the point of initial crystallization and then cooling should speed up the process.

Nickel and Cobalt analogues could have interest also. Betaine analogues also could have interest and may form similarly.

[Edited on 3/30/2019 by Rosco Bodine]

Laboratory of Liptakov - 30-3-2019 at 11:04

@Rosco Bodine
If it works, your post is one of the most valuable in the past few months. Your described method is cheap, simple, safe, and available components. She looks brilliant.....Cu(ClO4)2 is keys formula for a lot nexts attempts... :cool:

...LL

[Edited on 30-3-2019 by Laboratory of Liptakov]

MineMan - 1-4-2019 at 22:31

Tetrazole lvr on YouTube has had success with this. Says it works just as well as CHP. Only problem is I can’t find copper perchlorate

. Check out his videos.

Laboratory of Liptakov - 2-4-2019 at 01:25

Yes, success with copper-glycine-perchlorate is great. (CGP).
Advantage of CGP are neutrals crystal. But CGP has difficulty preparation. CHP s very easy preparation. But is partially unstable for free NH3/4 free bond. However CHP is basically stabille. His energetic properties are same after 1/2 year. In detonator, or in glass close jar. Confirmed..... :cool:

...LL

FeedMe94 - 3-4-2019 at 23:34

Im about to make some impact firecrackers with KCLO3 , Dark Al and Sulfur. My sulfur has impurities in it. What is the best way to purify it ?

fusso - 4-4-2019 at 04:48

Im about to make some impact firecrackers with KCLO3 , Dark Al and Sulfur. My sulfur has impurities in it. What is the best way to purify it ?

Recrys from CS2. If no CS2, then toluene is ok.

ETN using H2SO4/HNO3

twelti - 7-4-2019 at 09:33

Sorry if I'm floggin a dead horse, but..
I am attempting to follow H2SO4/HNO3 parameters suggested by Microtek, and generally agreed to give a good yield:

Quote:

"18 ml H2SO4 (96%), 12 ml HNO3 (62%) and 3 g erythritol, I got a yield of 6.3 g (85 %). The acids were mixed first, then cooled to ca. 0 C. The erythritol was ground to a very fine powder and gradually added by sprinkling into the stirred acids, keeping the temperature under 5 C. Stirring and cooling was maintained for 30 minutes after the end of addition, and the mix was then dumped into 500 ml of rapidly stirred ice water. Product was then filtered and washed again a few more times before being neutralized with NaHCO3 soln."

I doubled the amounts and used a little less E (wanting to keep it thin so I can use my stirrer). Only difference is that my acids did get up to maybe 20 C. during initial mixing, but cooled back down before adding E. Mixture remained easily stir-able using magnetic stirrer. Temp rise with incremental addition of E was very easily manageable. When I crashed it, I did see flakey precip in the ice cold water, though most of it collected at the top. Filtered and partially dried, I only got maybe 30% more than the E I put in. I tried a burn test (letting it melt first) of a few small flakes, seems to deflag, not detonate. I'm guessing it was a fail, but not sure why.

[Edited on 7-4-2019 by twelti]

Laboratory of Liptakov - 7-4-2019 at 10:25

My experiences is, that E must be absolut dry. Fine powder E heat on 100 C by 10 minute in thin layer on some pan. If is not perfect dry, yields are for example 2/3 against dry E. Only experiences. Reason can be else..... :cool:

...LL

twelti - 7-4-2019 at 10:55

My experiences is, that E must be absolut dry. Fine powder E heat on 100 C by 10 minute in thin layer on some pan. If is not perfect dry, yields are for example 2/3 against dry E. Only experiences. Reason can be else..... :cool:

...LL

Forgot to mention, I did grind the E for 1/2 hour in morter/pestle to very fine, and left overnight in a small baggie with dessicant. Maybe not long enough?

Now finished reX, using denatured alcohol. Most (3/4? ) did dissolve in the 50-55 degree EtOH. Filtered it before crashing into stirred cold water. That small amount of filtrate looked fairly crystalline. After crashing, and cooling for 45 min, final filter, got only 2.5 g (very slightly wet). This final product is white, clumpy, and almost "silvery" looking. Not silvery color but silver sheen, if that makes any sense. I have pics, not sure what the forum policy is...

Laboratory of Liptakov - 7-4-2019 at 11:28

Your entire procedure is OK. Consistency looks as mica is OK. Sometimes is impossible say, where is error. In procedure was the step of increase temperature on 25 C by 30 - 60 minute? Without mixing? It is final step, when is all E converted on tetranitrate. Without this step arises mixture of Dinitrate, trinitrate and tetranitrate of erythritol. Dinitrate and trinitrate are dissolve in water. Tetranitrate not.

twelti - 7-4-2019 at 12:26