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ecos - 5-12-2015 at 03:58

AN+Al would be better than flash powder to break rocks.
Most of flash powders are sensitive. detonator won't be needed.

greenlight - 5-12-2015 at 04:25

You're right, an ammonium nitrate-based explosive would be better to break up rocks.
If you only had flash powder and no access to high explosives, it would work, but would be inefficient as you would have to use a lot more and stem the boreholes etc.
But yeah, high explosives would be much better to use by a mile.

PHILOU Zrealone - 5-12-2015 at 10:31

One mole of H-C#C-H takes roughly 22.41 L and weights +/- 26g.
CaC2 + H2O --> CaO + H-C#C-H
CaC2 + 2 H2O --> Ca(OH)2 + H-C#C-H

Your silver acetylide nitrate double salt requires much less than 10g you need much less than 1 mole of CaC2/2,6...

----------------------------------------------------
Flash powder depending on its composition produces some gases; but if no gas is formed, then the gas trapped between the particles may expand violently owing to the heat of reaction...
Pirat bangers containing flash powder are void for 4/5; only 1/5 is the flash; the rest is air entrapped in a solid container.

----------------------------------------------------
2 KNO3 + 4 Al + S → K2S + N2 + 2 Al2O3
doesn't take in account the formation of SO2 gas!

Bert - 5-12-2015 at 11:47

The flash powder mixtures with Sulfur or black Antimony sulfide do have both temporary and permanent gasses from their reactions. They are also more sensitive to work with- When young and foolish, some of us split up quite large, tough stumps with 50:25:25 Potassium chlorate:Antimony sulfide:American dark Aluminum powder. Wouldn't make that mix again...

Ammonium perchlorate:Magnesium flash has virtually all gasseous output, some temporary, some permanent. If you must try this, coat the Mg powder with dichromate using a Potassium dichromate solution and dry before mixing- And don't try to store it very long even then. See Shimizu FAST for details.

A (possibly safer) way to get some more gas output is to mix 50:50 flash powder:double based fast burning pistol or shotgun powder. Using equal weights of the standard 70:30 perchlorate:Al flash and a fast, high NG content pistol powder such as Alliant "Bullseye" produces quite a lot of gas & heat, hopefully without the added sensitivity of Sulfur or sulfides. I have NOT done formal drop hammer and friction testing on this mix, so please don't make any assumptions as to it being particularly safe to handle-

ganger631 - 5-12-2015 at 18:45

Question regarding Silver acetylide, what is the difference between Silver acetylide double salt and just pure silver acetylide? As far as i know, it just require extra nitric acid for its production and has higher vod. Are there any differences in terms of, stability, power and such.

KesterDraconis - 5-12-2015 at 21:23

Quote: Originally posted by Bert  
Google IS your friend...

Calcium carbide reaction with water:

CaC2 + 2 H2O → C2H2 + Ca(OH)2

So a 1:1 ratio of carbide to gas. But your starting material may not be very pure. Carbide lamp fuel pellets, "Big Bang" cannon ammo, etc. certainly are not.

Assume only 80% purity for such technical grade material, if freshly opened- Then do the stoichiometry. Need help with stoichiometry? We can move this to beginnings.


Well, I thank you for the help, and I'm sorry if my question was vague, but that isn't actually what I meant.

You see, you have to bubble the acetylene through the solution of silver nitrate and nitric acid. I don't quite know how much of the acetylene in these bubbles fully reacts before the bubbles escape form the solution. I don't think it all reacts does it? If that is the case, (and maybe I'm just really really showing my ignorance here), then don't I need a good excess of gas, and thus more calcium carbide than stoichiometric quantity?

None of the synths I have found specified an amount, mostly mentioning the amount of time they bubbled acetylene, such as "till it looked like there was no more precipitate forming" and "for about eight to ten minutes" and such. Such statements are rather unhelpful and seem to be unsound approximations.



[Edited on 6-12-2015 by KesterDraconis]

Hydrazine Hydrate Ethanol azeotrope

Keith Fletcher - 6-12-2015 at 08:59

Dose Hydrazine Hydrate form an azeotrope with Anhydrous Ethanol and if so what is the boiling point?

deltaH - 6-12-2015 at 12:20

While the dinitramide anion and its salts are well known, does anyone know of organic derivatives bearing that functional unit, i.e.

dinitramide derivatives.jpg - 4kB

Can primary amines be doubly nitrated under special conditions?

[Edited on 6-12-2015 by deltaH]

deltaH - 6-12-2015 at 22:36

Nevermind, I found my answer to my own question in the first-page preview of "An Overview on the Synthetic Routes and Properties of Ammonium Dinitramide (ADN) and other Dinitramide Salts" (requested).

Capture.JPG - 26kB

PHILOU Zrealone - 10-12-2015 at 10:24

Quote: Originally posted by ganger631  
Question regarding Silver acetylide, what is the difference between Silver acetylide double salt and just pure silver acetylide? As far as i know, it just require extra nitric acid for its production and has higher vod. Are there any differences in terms of, stability, power and such.

Silver acetylide Ag-C#C-Ag is formed from silver formate or acetate solution while bubbling acetylen through it.
As you can see it doesn't contain an oxydizer and so:
Ag-C#C-Ag --> 2 Ag + 2C
Only if air is present to some extend the following reaction occurs:
2C + 2 O2 --> 2 CO2

The double salt is Ag-C#C-Ag. x AgNO3. y HNO3 and it doesn't require nitric acid, only silver nitrate...
AgNO3 + H-C#C-H --> Ag-C#C-Ag. x AgNO3. y HNO3
As you can see there is nitrate oxydiser trapped inside the matrix. As such it produces of course more power and a higher VOD without need of external oxygen.

The basic salt (Ag-C#C-Ag) is said to be more sensitive vs the neutral (Ag-C#C-Ag.x AgNO3) and acidic (Ag-C#C-Ag. x AgNO3. y HNO3) ones.

For stability, as long as they are done correctly (demi water, demi water washed paper filter, no sunlight or strong light, clean chemically pure solvents, dried in the shadow at a moderate heat) and treated wel, they can store for years.

PHILOU Zrealone - 10-12-2015 at 10:37

Quote: Originally posted by KesterDraconis  
Quote: Originally posted by Bert  
Google IS your friend...

Calcium carbide reaction with water:

CaC2 + 2 H2O → C2H2 + Ca(OH)2

So a 1:1 ratio of carbide to gas. But your starting material may not be very pure. Carbide lamp fuel pellets, "Big Bang" cannon ammo, etc. certainly are not.

Assume only 80% purity for such technical grade material, if freshly opened- Then do the stoichiometry. Need help with stoichiometry? We can move this to beginnings.


Well, I thank you for the help, and I'm sorry if my question was vague, but that isn't actually what I meant.

You see, you have to bubble the acetylene through the solution of silver nitrate and nitric acid. I don't quite know how much of the acetylene in these bubbles fully reacts before the bubbles escape form the solution. I don't think it all reacts does it? If that is the case, (and maybe I'm just really really showing my ignorance here), then don't I need a good excess of gas, and thus more calcium carbide than stoichiometric quantity?

None of the synths I have found specified an amount, mostly mentioning the amount of time they bubbled acetylene, such as "till it looked like there was no more precipitate forming" and "for about eight to ten minutes" and such. Such statements are rather unhelpful and seem to be unsound approximations.



[Edited on 6-12-2015 by KesterDraconis]

Usually the expensive material is the AgNO3 and not the acetylen from CaC2...thus as such one usually exhaust the AgNO3 solution with an excess of acetylen by several filtrations, bubbling and demi water washings.

The white trouble is a clear evidence that some AgNO3 is stil present when bubbling acetylen through the solution...so filtration and washing then rebubbling, refiltration and rewashing is the best way to improve yield.

This explains why it seems so unclear...also if you have an excess of AgNO3 vs the acetylen, you may get the not suitable complex Ag-C#C-Ag. 6 AgNO3 (not detonable) so better use an excess of acetylen.

Finally the best design to use acetylen at best is long vertical reactor with a slow flow of acetylen from the bottom (long plastic tube to the bottom of a big vial for example); that way the gas has the time to dissolve a bit into the solution and to react with the AgNO3 all its way up to the surface.
Acetylen is moderately soluble into water and the solubility is reduced by solutants (dissolved salts, acids and bases) (see solubility of gases in water) and by heat.
--> Cold solution, avoid too much HNO3 (or avoid it at all), maybe add a little aceton (will boost up acetylen solubility).

[Edited on 10-12-2015 by PHILOU Zrealone]

PHILOU Zrealone - 10-12-2015 at 11:48

Quote: Originally posted by deltaH  
Nevermind, I found my answer to my own question in the first-page preview of "An Overview on the Synthetic Routes and Properties of Ammonium Dinitramide (ADN) and other Dinitramide Salts" (requested).

Organic dinitramides R-N(NO2)2 are relatively unstable.
You can check some related documents and infos in the chloronitramide (R-NCl-NO2) or ethylene dinitramide treads by Axt on this forum.

Beware that for EDNA (ethylene dinitramide) and MEDINA (methylene dinitramide) "dinitramide" refers to two nitramide groups -NH-NO2 and not to dinitramide -N(NO2)2...thus not to confuse with possible
-methylene bis-dinitramide (CH2(-N(NO2)2)2 = CH2N6O8)
-ethylene bis-dinitramide ((O2N)2N-CH2-CH2-N(NO2)2 = C2H4N6O8)

[Edited on 11-12-2015 by PHILOU Zrealone]

KesterDraconis - 10-12-2015 at 12:24

Quote: Originally posted by PHILOU Zrealone  

Usually the expensive material is the AgNO3 and not the acetylen from CaC2...thus as such one usually exhaust the AgNO3 solution with an excess of acetylen by several filtrations, bubbling and demi water washings.

The white trouble is a clear evidence that some AgNO3 is stil present when bubbling acetylen through the solution...so filtration and washing then rebubbling, refiltration and rewashing is the best way to improve yield.

This explains why it seems so unclear...also if you have an excess of AgNO3 vs the acetylen, you may get the not suitable complex Ag-C#C-Ag. 6 AgNO3 (not detonable) so better use an excess of acetylen.

Finally the best design to use acetylen at best is long vertical reactor with a slow flow of acetylen from the bottom (long plastic tube to the bottom of a big vial for example); that way the gas has the time to dissolve a bit into the solution and to react with the AgNO3 all its way up to the surface.
Acetylen is moderately soluble into water and the solubility is reduced by solutants (dissolved salts, acids and bases) (see solubility of gases in water) and by heat.
--> Cold solution, avoid too much HNO3 (or avoid it at all), maybe add a little aceton (will boost up acetylen solubility).

[Edited on 10-12-2015 by PHILOU Zrealone]


Thanks, I suppose there really is no definite way to find smallest amount of acetylene necessary. Its ok for me though, I solved that problem yesterday by finding a cheaper source of carbide, so I don't have to worry about saving it/running out nearly as much.

PHILOU Zrealone - 11-12-2015 at 10:52

Quote: Originally posted by KesterDraconis  
Quote: Originally posted by PHILOU Zrealone  

Usually the expensive material is the AgNO3 and not the acetylen from CaC2...thus as such one usually exhaust the AgNO3 solution with an excess of acetylen by several filtrations, bubbling and demi water washings.

The white trouble is a clear evidence that some AgNO3 is stil present when bubbling acetylen through the solution...so filtration and washing then rebubbling, refiltration and rewashing is the best way to improve yield.

This explains why it seems so unclear...also if you have an excess of AgNO3 vs the acetylen, you may get the not suitable complex Ag-C#C-Ag. 6 AgNO3 (not detonable) so better use an excess of acetylen.

Finally the best design to use acetylen at best is long vertical reactor with a slow flow of acetylen from the bottom (long plastic tube to the bottom of a big vial for example); that way the gas has the time to dissolve a bit into the solution and to react with the AgNO3 all its way up to the surface.
Acetylen is moderately soluble into water and the solubility is reduced by solutants (dissolved salts, acids and bases) (see solubility of gases in water) and by heat.
--> Cold solution, avoid too much HNO3 (or avoid it at all), maybe add a little aceton (will boost up acetylen solubility).

[Edited on 10-12-2015 by PHILOU Zrealone]


Thanks, I suppose there really is no definite way to find smallest amount of acetylene necessary. Its ok for me though, I solved that problem yesterday by finding a cheaper source of carbide, so I don't have to worry about saving it/running out nearly as much.

There is, you simply need a closed reactor and a pressure gauge (manometer) or water displacement system and a recirculating device for the undissolved/unreacted acetylen...while it reacts the initial volume will be reduced and the gaseous volume above the liquid will shrink...then by trial error, you may find the minimal amount...

KesterDraconis - 12-12-2015 at 10:08

Quote: Originally posted by PHILOU Zrealone  

There is, you simply need a closed reactor and a pressure gauge (manometer) or water displacement system and a recirculating device for the undissolved/unreacted acetylen...while it reacts the initial volume will be reduced and the gaseous volume above the liquid will shrink...then by trial error, you may find the minimal amount...


Hmm, you know that sounds like it would be quite a bit of work or money to either construct or buy such a device. At the same time it sounds like quite a bit of fun, and I think the information perhaps would be useful to people doing this synth in the future. I will consider it.

Mr.Greeenix - 16-12-2015 at 10:00

Sorry for interrupting this discussion :)

Does someone have a paper about a one pot synthesis of carbohydrazide (diaminourea)

I already have a paper but with a two pot synthesis of carbohydrazide.
The problem is that it is designed for industrial use and not very commercial for me. :(

PHILOU Zrealone - 16-12-2015 at 12:14

Quote: Originally posted by Mr.Greeenix  
Sorry for interrupting this discussion :)

Does someone have a paper about a one pot synthesis of carbohydrazide (diaminourea)

I already have a paper but with a two pot synthesis of carbohydrazide.
The problem is that it is designed for industrial use and not very commercial for me. :(

No paper but in principle reacting urea with concentrated hydrazine will evolve gaseous NH3 and leave you with aminourea and diaminourea (DAU)...

You may also work with common chemistry...
Phosgene + hydrazine -->DAU
Dimethyl carbonate + hydrazine --> DAU
...

[Edited on 16-12-2015 by PHILOU Zrealone]

ecos - 28-12-2015 at 16:59

I found a product in a store with 40% Ethylene glycol.
I am not sure about the rest 60% of the product. I am not sure if it is water or antirust material.
is it possible to get concentrated Ethylene glycol from this product. I was thinking about distillation but glycol has boiling point of 190 degrees and if I have water in the solution this won't work as I think.

any suggestion ?

Hennig Brand - 29-12-2015 at 00:32

From what I have seen the anti corrosion additive is normally in very small quantity. It depends on what the climate is like where you are how much, and if, antifreeze needs to be used at all; in Las Vegas I read that anti corrosion chemicals are added to plain deionized water and that can be used as coolant, where I am it gets pretty cold so 50% ethylene glycol is normally used (considerably less concentration could normally be used, but 50% gives a good margin of safety for really low temperatures and possible reduction in ethylene glycol concentration over time, etc). I can get 50% concentration which is made to be poured right into the rad without dilution and basically 100% concentration which is meant to be diluted with distilled or deionized water.

It has been a few years since I have distilled any but from what I remember it is extremely easy to distill with very high purity, concentration and recovery with even a very simple pot still and condenser (one stage). The still needs to be able to handle 200C or more and ethylene glycol dissolves most normal rubbers and plastics from what I have seen (ruined a few items playing with it originally), but something all metal can be easily improvised. I have only ever distilled the undiluted antifreeze, but the 50% or 40% variety could be distilled too if none of the 100% stuff could be found. When distilling 1L or so of the "100%" variety I remember a couple millilitres or so of nearly pure water coming over at around 100C and then literally only a couple drops coming over as the temperature rose from 100C to about 190C. At around 190-200C or so a steady stream of practically pure ethylene glycol came over. I remember getting significantly better yields of EGDN using the distilled ethylene glycol than NG when using glycerine from the drug store using the same acids.


[Edited on 29-12-2015 by Hennig Brand]

diddi - 29-12-2015 at 01:30

you can by almost pure ethylene glycol if you get concentrated coolant.

ecos - 29-12-2015 at 03:54

@Hennig,
If 60% is distilled water , I think water will evaporate at 100C before Glycol. do I need to add H2SO4 to avoid water evaporation ?
I also can heat till 100 C till water get out then start to distill and collect the concentrated Glycol.

If 60% is antirust, what should I do now ? :)

Hennig Brand - 29-12-2015 at 09:21

The coolant I had was a florescent green type color IIRC. I distilled to remove the tiny amount of water it contained but mostly to separate it from the dye and other higher boiling point materials. The distillate which came over at around 190-200C was crystal clear and basically anhydrous.

Ok, found some equilibrium data, there will be some losses especially when starting with coolant with a high concentration of water.

The equilibrium data came by way of the Wiki ethylene glycol data page. The data actually came from the following chemical engineering research database however.

http://www.cheric.org/research/kdb/hcvle/showvle.php?vleid=1...

I added a couple of columns and made the table into a pdf. Hope I didn't mess up the calculations, I feel rusty.


Attachment: Ethylene Glycol-Water Equilibrium Data.pdf (296kB)
This file has been downloaded 415 times



Here is an ethylene glycol data page as well.

Attachment: Ethylene Glycol Data Page.pdf (1.9MB)
This file has been downloaded 423 times


[Edited on 29-12-2015 by Hennig Brand]

Zephyr - 29-12-2015 at 09:36

I preformed a similar distillation of the glycol from the dark green dye and was very pleased with the very small amount of water that had to be disrcarded. ~35ml
I just began collecting around 180C.
The type I used was given to my by elementcollector and came from a black jug. It was meant to be used as a an antifreeze for RVs IIRC.



Zephyr - 29-12-2015 at 21:56

I have been told not to install an electrical outlet inside of my fume hood, I assume because of the risk of explosion. Is it really that unsafe? I hoped that by placing it near the sash I could minimise this chance greatly, it certainly seems safer than stringing cords around he outside...
Any input would be greatly appreciated.

Bert - 30-12-2015 at 00:14

It depends on what you are doing in your fume hood, but NOT having any non explosion proof electricals inside your hood gives you greater flexibility in what you CAN do safely.

Electric sparks and flammable/explosive vapors and dusts are a bad mix, M'kay? I have heard first hand horror stories from people about using diethyl ether and throwing a standard wall light switch, just before they lost their lab. How they saw that little flame exit the switch plate, right before the open solvent filled container exploded.

Alternatively, you can obtain explosion proof electrical boxes, use heavy walled conduit and explosive atmosphere rated wiring devices and feeds. We have done this in one shipping warehouse/magazine that needs to be used any time of day, the equipment is VERY expensive.

We also have a small prefab building just for handling explosives in preparation and re-packing. There are no electrical circuits inside it- Exterior LED lights shining in through windows near the roof allow use after dark. All conduits, electrical boxes and switches are OUTSIDE the building. Cheapest reasonably safe solution.

picric acid

idrbur - 31-12-2015 at 05:29

Somedays before i tried to make PA with aspirin but i obtained only few crystals .so i tried again but this time i doesn't get precipitate so i cold the solution to -3 degree but it doesn't worked .so again performed the process with new batches 2-3 times but i doesn't get ppt. Any time .

Can anybody tell me how can i precipitate picric acid from the solution.

PHILOU Zrealone - 1-1-2016 at 09:39

Quote: Originally posted by idrbur  
Somedays before i tried to make PA with aspirin but i obtained only few crystals .so i tried again but this time i doesn't get precipitate so i cold the solution to -3 degree but it doesn't worked .so again performed the process with new batches 2-3 times but i doesn't get ppt. Any time .

Can anybody tell me how can i precipitate picric acid from the solution.

Maybe you could use an organic solvant to extract picric acid from the mix...BTW What is in it?

Assuming you have only HNO3/H2SO4 and picric acid, you may allow the all batch to react with excess NH3 (NH4OH); then heat and evaporate (if needed) then cool down to 0°C.
I have found some datas on solubilities of NH4 picrate, NH4NO3, NH4HSO4 and (NH4)2SO4 from various sources and by crossing the datas, I got a diagram. Datas for NH4HSO4 in red have been extrapolated from phase diagram of NH4HSO4.
If you use excess NH3; there will only be (NH4)2SO4 in solution...
Solubility NH4 picrate vs NO3 vs HSO4 vs SO4 in H2O f(T).jpg - 95kB
From that you see that NH4 picrate is the least soluble and at 0°C in excess NH4(+) media from more soluble NH4NO3 and (NH4)2SO4, it should be virtually unsoluble (very close to 0,0 gr/ 100 gr water...)

So after filtration allow to react with 30% HCl and soluble NH4Cl will form while unsoluble picric acid will remain.

[Edited on 1-1-2016 by PHILOU Zrealone]

ecos - 3-1-2016 at 14:29


nitration process is one of the steps of synthesizing high explosive. I am thinking what EM that has no nitration at all. I figure out peroxide , permanganate ,chlorate and perchlorate families are the only ones.

peroxide family is very sensitive and has RE factor = 0.8 and VoD = 5300 m/s
permanganate /chlorate/perchlorate is less sensitive than peroxide but less powerful , VoD ~ 2500 m/s and max RE ~ 0.25

do we have other EM that has no nitration step and still not sensitive and has acceptable power?

greenlight - 30-1-2016 at 19:29

Other energetic materials that are not made by nitration would include:

* Azide explosives
* Picrate explosives
* Heavy metal acetylides

NeonPulse - 30-1-2016 at 21:42

I guess technically picrates do involve nitration to make picric acid as the starting material but Mercury and silver fulminate, silver oxalate,R-salt and Tetrazoles don't. RDX technically is not made via nitration either. PLX is another example along with FAE type mixtures. So I guess there's a few.

Liptex

Laboratory of Liptakov - 31-1-2016 at 00:44

Quote: Originally posted by ecos  

nitration process is one of the steps of synthesizing high explosive. I am thinking what EM that has no nitration at all. I figure out peroxide , permanganate ,chlorate and perchlorate families are the only ones.

peroxide family is very sensitive and has RE factor = 0.8 and VoD = 5300 m/s
permanganate /chlorate/perchlorate is less sensitive than peroxide but less powerful , VoD ~ 2500 m/s and max RE ~ 0.25

do we have other EM that has no nitration step and still not sensitive and has acceptable power?


Well, it is maybe question on me. This plastic explosive exist and it is Liptex. His power is see here:
https://www.youtube.com/watch?v=gyx2f9b2HFg
VoD is about 6000 m/s at density 1,5 g/cm3. This is density in video. At density 1,85 g/ cm3 is VoD 7000 m/s. Produce:

Liptex schema.jpg - 146kB
Process without nitration, acids. Time stability in closed container (15C) without limits. Free on air by 15 Celsia about 30 days, without explosive changes. This EM Slowly spend molecule NH3, evaporate. Minimum kick from 300mg LA. Or his equivalent. Standard kick No.8. From density 1,8+ is possible used as EM for EFP, SC etc. Oxygen balance has near nil. "C" in scheme is Celsia temperature during process.
Dr. Liptakov

greenlight - 31-1-2016 at 18:58

Nice LL, is that your own invention?

Does anyone know the difference between lead azide that has been coated with dextrin and lead azide that has been coated with PVA during synthesis?
Would one be safer or are they essentially the same in sensitivity?

Litpex

Laboratory of Liptakov - 1-2-2016 at 03:22

Quote: Originally posted by greenlight  
Nice LL, is that your own invention?

Well, it is not from any patents. Inventor is only Dr. Liptakov, special madness on field of energetic materials research.
(unfortunately, about Lead azide I know nothing)
Doc. :-)

PHILOU Zrealone - 1-2-2016 at 06:04

Quote: Originally posted by ecos  

nitration process is one of the steps of synthesizing high explosive. I am thinking what EM that has no nitration at all. I figure out peroxide , permanganate ,chlorate and perchlorate families are the only ones.

peroxide family is very sensitive and has RE factor = 0.8 and VoD = 5300 m/s
permanganate /chlorate/perchlorate is less sensitive than peroxide but less powerful , VoD ~ 2500 m/s and max RE ~ 0.25

do we have other EM that has no nitration step and still not sensitive and has acceptable power?

There are a lot of other explosive materials than nitration involved ones. See explosophoric groups or hazardous chemicals and lab chemical hazard reactions compendium to get a good general picture.

The assumption that permanganate, chlorate, perchlorate are less powerful than peroxides is wrong, you are probably refering to the ammonium salts...
Except maybe for permanganate, hydrazinium, guanidinium, methylaminium, hydroxylamonium, ethandiaminium, ... nearly all amines salts of oxoanions are much more powerful than peroxydes (VOD >6500 m/s).
Some may even be close or better than RDX or HMX.

Nitroaromatics may be accessed without HNO3 but from nitrite.
ex: Cl-CH(-CH=O)2 + AgNO2 -aceton-> O2N-CH(-CH=O)2 + AgCl
O2N-CH(-CH=O)2 (nitromalonaldehyd) -trimerisation/decarboxylation-> 1,3,5-Trinitrobenzen

Aromatic iodoxy compounds are explosive. Ar-IO2
Aromatic diazonium salts are explosive. Ar-N=N(+) especially with oxoanions (nitrate, perchlorate, ...)
Aromatic perchloryl compounds are explosive. Ar-ClO3
Liquid oxygen explosives.
N2O4 explosives (panclastites).
Bromate amine salts.
Iodate and periodate amine salts.
...
Very long list of reactions and examples.



[Edited on 1-2-2016 by PHILOU Zrealone]

Hennig Brand - 1-2-2016 at 09:14

Greenlight,

From, "Proceedings of the Symposium on Lead and Copper Azides", GW Taylor, 1966:

"It is possible to suppress spontaneous explosion by the addition of small amounts of various additives such as dextrin, polyvinyl alcohol and other hydrophilic colloids.

It is suggested that spontaneous explosion may be associated with nucleating conditions and not with super-sensitivity due to the presence of internal strain and sudden release of stresses in large crystals."

Dextrin is almost always listed first from what I have seen, but it appears that they both do more or less the same thing. Not completely sure though.


The following was taken from, "Technology of the Inorganic Azides, Energetic Materials Vol. 2":

"
A breakthrough came with the development about 1930 of dextrinated lead azide, which was considerably safer to handle than the unmodified material but still powerful enough to function satisfactorily in contemporary detonators and related devices. Dextrinated lead azide was the first initiating explosive to be manufactured* under carefully controlled conditions so as to produce an explosive with a more desirable range of properties. Subsequent developments followed the same principles and employed crystal-modification agents, or "phlegmatizers" (e.g., dextrin, polyvinyl alcohol, etc.), to produce a balance between reliable initiation, output energy, and safety in handling. Products were successfully developed to be free flowing for ease of introduction into small diameter detonators and to have a high bulk density to provide the maximum energy in pressed compacts. The trend in detonator and explosive-train design, which has continued into the 1970s, has been to smaller components, requiring decreased amounts and diameters of more efficient explosives. This trend itself has tended to emphasize the technological importance first of lead and then silver azide and to assure the continued modification of their properties by process development and control. In the United Kingdom the prewar development of Service lead azide represented a trade-off of some handling convenience and safety for increased output. During World War II, polyvinyl alcohol (PVA) lead azide was developed in the United States and resembled Service lead azide in appearance, output, and other properties. Then at the end of World War II, work began on lead azide modified by precipitation in the presence of sodium carboxymethylcellulose (CMC) [1]. Originally, CMC-type lead azide was developed to have the self-binding properties of dextrinated lead azide, so that it could be pressed into sleeves, yet have the initiation and output properties of the Service material. Later development in the United Kingdom led to a variety of new explosive products given "RD" serial numbers and in particular to RD1333 and RD1343 CMC-type azides. American versions of RD1333 were produced in both government plants and private industry and were ultimately produced in large batches as Special Purpose lead azide. CMC-type lead azide had supplanted to a high degree but not completely replaced Service lead azide, PVA lead azide, or dextrinated lead azide for military use in the United States, the United Kingdom, and most countries of the North Atlantic Treaty and South East Asia Treaty Organizations. Dextrinated lead azide remains the principal product for civilian use, for mining and demolition applications in general, and some military items. Other azides have been considered for use as detonants, but besides lead azide only silver azide possesses a combination of properties which has found favor in industry. However, in spite of its long-recognized virtues [2], no process was developed that would make silver azide in a form suitable for pouring and pressing into detonators. During the early 1950s, Taylor [3] and Williams and Peyton [4] developed processes for making granular silver azide. Taylor's process [3] was adopted for use in British ordnance factories, but it yielded only small (1.5 kg) batches in the standard British production vessels, and four hours were required to complete a batch. "

Given the preference given by the military to PVA lead azide, maybe it is superior in some ways to dextrinated lead azide.


Here are a couple references for you (I have just skimmed them a bit so far):


Attachment: Proceedings of the Symposium on Lead and Copper Azides - GW Taylor 1966.pdf (5.2MB)
This file has been downloaded 1139 times


Attachment: Technology of the Inorganic Azides - Energetic Materials Vol 2.pdf (8.4MB)
This file has been downloaded 1910 times


[Edited on 1-2-2016 by Hennig Brand]

greenlight - 1-2-2016 at 18:42

Thankyou for that information Hennig, as I am trying to decide whether to use dextrinated or PVA lead azide for the initiating charge in my detonators and it is a great help.

In the second file (Technology of the Inorganic Azides) it says this about PVA lead azide:

"In the United States it is manufactured solely by the Olin Matheson Corporation using patented pro- cedures [9] which give little insight into the actual manufacturing techniques used or the problems encountered. PVA lead azide is 96% pure and may contain some polyvinyl alcohol combined with lead, but not in the same manner as the lead dextrinate in dextrinated lead azide, for the product consists of transparent, well-defined crystals. It has an initiating efficiency equal to Service lead azide and, according to data published in the patent, about the same handling and sensitivity properties."

It seems that there is more information available about the properties of the dextrinated lead azide than the PVA variant.

It also states that the dextrinated lead azide has a purity of 92%, maybe it takes up extra phlegmatizer during synthesis.

ecos - 4-2-2016 at 06:14

Quote: Originally posted by PHILOU Zrealone  

There are a lot of other explosive materials than nitration involved ones. See explosophoric groups or hazardous chemicals and lab chemical hazard reactions compendium to get a good general picture.

The assumption that permanganate, chlorate, perchlorate are less powerful than peroxides is wrong, you are probably refering to the ammonium salts...
Except maybe for permanganate, hydrazinium, guanidinium, methylaminium, hydroxylamonium, ethandiaminium, ... nearly all amines salts of oxoanions are much more powerful than peroxydes (VOD >6500 m/s).
Some may even be close or better than RDX or HMX.

Nitroaromatics may be accessed without HNO3 but from nitrite.
ex: Cl-CH(-CH=O)2 + AgNO2 -aceton-> O2N-CH(-CH=O)2 + AgCl
O2N-CH(-CH=O)2 (nitromalonaldehyd) -trimerisation/decarboxylation-> 1,3,5-Trinitrobenzen

Aromatic iodoxy compounds are explosive. Ar-IO2
Aromatic diazonium salts are explosive. Ar-N=N(+) especially with oxoanions (nitrate, perchlorate, ...)
Aromatic perchloryl compounds are explosive. Ar-ClO3
Liquid oxygen explosives.
N2O4 explosives (panclastites).
Bromate amine salts.
Iodate and periodate amine salts.
...
Very long list of reactions and examples.

[Edited on 1-2-2016 by PHILOU Zrealone]


Liquid oxygen explosives. --> those are peroxides which are very sensitive !

I think azides are used as primary explosives because they are quite sensitive.

N2O4 ---> I couldn't find much info about explosives having this compound

I will explore the rest.

[Edited on 4-2-2016 by ecos]

PHILOU Zrealone - 4-2-2016 at 12:35

Quote: Originally posted by ecos  
Quote: Originally posted by PHILOU Zrealone  

There are a lot of other explosive materials than nitration involved ones. See explosophoric groups or hazardous chemicals and lab chemical hazard reactions compendium to get a good general picture.

The assumption that permanganate, chlorate, perchlorate are less powerful than peroxides is wrong, you are probably refering to the ammonium salts...
Except maybe for permanganate, hydrazinium, guanidinium, methylaminium, hydroxylamonium, ethandiaminium, ... nearly all amines salts of oxoanions are much more powerful than peroxydes (VOD >6500 m/s).
Some may even be close or better than RDX or HMX.

Nitroaromatics may be accessed without HNO3 but from nitrite.
ex: Cl-CH(-CH=O)2 + AgNO2 -aceton-> O2N-CH(-CH=O)2 + AgCl
O2N-CH(-CH=O)2 (nitromalonaldehyd) -trimerisation/decarboxylation-> 1,3,5-Trinitrobenzen

Aromatic iodoxy compounds are explosive. Ar-IO2
Aromatic diazonium salts are explosive. Ar-N=N(+) especially with oxoanions (nitrate, perchlorate, ...)
Aromatic perchloryl compounds are explosive. Ar-ClO3
Liquid oxygen explosives.
N2O4 explosives (panclastites).
Bromate amine salts.
Iodate and periodate amine salts.
...
Very long list of reactions and examples.

[Edited on 1-2-2016 by PHILOU Zrealone]


Liquid oxygen explosives. --> those are peroxides which are very sensitive !

I think azides are used as primary explosives because they are quite sensitive.

N2O4 ---> I couldn't find much info about explosives having this compound

I will explore the rest.

[Edited on 4-2-2016 by ecos]

Liquid oxygen explosives are not peroxydes...peroxydes means that the molecule contains the linkage R-O-O-R' where R, R' may be H, Alkyl, Aryl, or Acyl like:
CH3-O-O-CH3 (methyl ether peroxyde)
CH3-O-O-H (peroxymethanol)
H-O-O-H (water peroxyde)
C6H5-CO-O-O-H (perbenzoic acid)
CH3-CO-O-O-CO-CH3 (peracetic anhydride)

LOX is simply a mix of liquefied O2 and a porous fuel; It simply burns fiercely when set in flame in the open, maybe it may D2D when confined, and it detonates from detonator.

Some organic azides are not as sensitive as the mineral ones...
CH3-N3
N3-CH2-CH2-N3
N3-C6H2(NO2)3

Microtek - 5-2-2016 at 06:57

Many of the compounds in the recent family of energetic salts do not involve nitration at all (eg. aminotetrazole nitrate), and some employ borderline techniques such as dehydrating a nitrate to form a nitro compound (eg. aminonitroguanidine and its nitrate salt). Many of these are at the absolute cutting edge, performance-wise.

ecos - 6-2-2016 at 15:32

Quote: Originally posted by Microtek  
Many of the compounds in the recent family of energetic salts do not involve nitration at all (eg. aminotetrazole nitrate), and some employ borderline techniques such as dehydrating a nitrate to form a nitro compound (eg. aminonitroguanidine and its nitrate salt). Many of these are at the absolute cutting edge, performance-wise.


a compound that has a nitrate in its name would have a nitric salt or nitric acid treatment !!!
It is very hard now to me to access AN or diluted nitric acid thats why I want to avoid any nitration process

Laboratory of Liptakov - 7-2-2016 at 00:19

Ecos, If you haven't ammonium nitrate and nothing nitric acid, will be construction any EM pretty difficult. Maybe will be better put question, what you have. After will be answer easy. Doc.

greenlight - 7-2-2016 at 10:07

He is right, not having the ability to nitrate compounds take a massive chunk out of the energetics you will be able to use.
Can you get potassium nitrate as fertilizer where you are and sulfuric acid. If so you can distill your own nitric acid.

byko3y - 7-2-2016 at 10:38

As you might know, orgsyn.org publishes procedures tha usually provide some range of yields or maybe it's two numbers (one is ht eyield of original researcher, one is the yield of checkers). I was not able to find any explanation of the reason two numbers are usually provided for yields. Does anyone know?

Microtek - 8-2-2016 at 02:30

Quote: Originally posted by ecos  
Quote: Originally posted by Microtek  
Many of the compounds in the recent family of energetic salts do not involve nitration at all (eg. aminotetrazole nitrate), and some employ borderline techniques such as dehydrating a nitrate to form a nitro compound (eg. aminonitroguanidine and its nitrate salt). Many of these are at the absolute cutting edge, performance-wise.


a compound that has a nitrate in its name would have a nitric salt or nitric acid treatment !!!
It is very hard now to me to access AN or diluted nitric acid thats why I want to avoid any nitration process


Nitration is not the same as incorporating a nitrate anion, eg. by metathesis. If you can't buy simple precursors such as nitric acid or nitrate salts, then preparing these should be your focus. Everything is made from chemicals, it's "just" a matter of refining it into the chemicals you need.

ecos - 9-2-2016 at 08:59

Thanks a lot for your replies.

I have access to them but with small quantity. I have tons of questions when i buy AN grade fertilizer or diluted nitric acid (65%).
I just want to get rid of this headache.
I am thinking now to synthesis nitric acid , I am just reading now about how to do so through oxidation of ammonia gas.
I will write posts about this soon.

Hennig Brand - 9-2-2016 at 14:02

I always wanted to try bacterial fermentation like was done with the old nitre beds, but using more modern feed, equipment and techniques. For starters instead of manure and urine I would use fertilizer grade urea, and I would use a substrate able to soak up solution and still allow good aeration (peat moss?). Forced air from a blower would be used to provide proper air flow through the ferment. The temperature of the bed would be maintained at an optimum level with an electrical heater (heat the inlet air?). Even moisture level could be controlled; a moisture sensor could be used to monitor moisture level and the associated controller could spray the substrate/ferment as needed. IIRC, I have read that nitrates can be produced by fermentation in a fraction of the time as was achieved with the old fashioned nitre beds using modern techniques such as these. I have at least one or two journal articles discussing this, but they are on a different computer in another city.

Microtek - 9-2-2016 at 22:44

Yes, you could see such a deficiency in reactants as a golden opportunity to develop not only your chemical skills, but also your skills in chemical engineering (whether you went with bacterial nitrogen fixation or a more classical high voltage method or catalytic oxidation of ammonia). There are lots of interesting options.

OB%

greenlight - 10-2-2016 at 08:48

Just a quick question regarding oxygen balance.
My last batch of PE was made just using PETN as the energetic. I know that a perfect oxygen balance improves the explosives detonation properties. PETN is slightly underoxidized (-10%) and ETN is overoxidized slightly @ 5.2-5.3%.
Would a plastic explosive from a ratio of PETN to ETN that has been calculated to 0% be more powerful than the straight PETN plastic explosive or would the binder and plasticizer throw out the balance during detonation.

[Edited on 10-2-2016 by greenlight]

Hennig Brand - 10-2-2016 at 09:50

Plastic explosives are normally used in applications where maximum brisance and the ability to "disrupt" the target are of main importance. So extremely high brisance explosives, high energy density, with components mixed at the molecular level are typically what is desired. I don't think the oxygen balance of something not mixed at the molecular level is normally of great importance here, especially an inert plasticizer, binder mixture.

I thought this was kind of interesting.

Retrieved the following from the archive "Yarchive":

"
From: glhurst@onr.com (Gerald L. Hurst)
Newsgroups: alt.engr.explosives
Subject: Re: What is C4 made of?
Date: 11 Mar 1997 22:22:04 GMT

In article
, Daniel
John Krut says:

>I am a chemistry student at the U of C and am wondering how C4 is produced

C-4 is a simple mechanical mixture of powdered RDX (cyclonite) and
a plasticizing mixture in the ratio 91:9. The specific plasticizer
mix is comprised of:

Polyisobutylene 2.1
Motor oil 1.6
Di(2-ethylhexyl) sebacate 5.3

There is no particular magic in the specific plasticizer mix other
than that it has good stability and low-temperature plasticity. It
may be viewed as an inert diluent as far as explosive properties go.

Jerry (Ico)
"

OB

Laboratory of Liptakov - 10-2-2016 at 13:04

Counting oxygen balance for molecular explosive give nonsense. Thus, brisance ETN, PETN, RDX (and his mix) give highest brisance with minimum plasticizer (and other compounds, color etc). For this compounds OB does not count. Example: RDX plast with 9% PLF super brisance
PETN with 9% PLF good brisance.
ETN with 9% PLF less brisance.
Overall "power" is giving of content main of explosive (or most powerfull + main) of explosive in %. Different condition is for AN Fx. Here is OB from zero to - 10 very important. However, still applies rule, than overall "power" give main explosive compound. For example, A N + urea will be weakly, than AN + Hexamine. Problematic about it is of course more complex issues. This explanation is simplified for easy understanding. ETN + PETN on zero OB + PLF 9% will be weakly than PETN + PLF 9 %.
Doc.

[Edited on 10-2-2016 by Laboratory of Liptakov]

underground - 10-2-2016 at 17:47

What is PLF ?

Laboratory of Liptakov - 10-2-2016 at 23:49

Plasticizer, plastificator, PLF, my personal acronym, sorry....:cool:

PHILOU Zrealone - 11-2-2016 at 06:54

Quote: Originally posted by greenlight  
Just a quick question regarding oxygen balance.
My last batch of PE was made just using PETN as the energetic. I know that a perfect oxygen balance improves the explosives detonation properties. PETN is slightly underoxidized (-10%) and ETN is overoxidized slightly @ 5.2-5.3%.
Would a plastic explosive from a ratio of PETN to ETN that has been calculated to 0% be more powerful than the straight PETN plastic explosive or would the binder and plasticizer throw out the balance during detonation.

[Edited on 10-2-2016 by greenlight]

Because PETN and ETN have very close density (most active parameter in CHON EM brisance):
1°)then the use of ETN will be better for plastic explosive vs PETN since its unused oxygen will burn the plasticizer/binder fuel somehow providing a better/higher energy output...this will compensate the dilluting effect of the binder!
2°)Using an OB balanced mix of PETN/ETN will also be beneficial over PETN, but must be less interesting than pure ETN plastic.
3°)Using an active binder and PETN will outperform PETN plastic because the energy output will be higher. ETN plastic would be even better!
4°)Using an OB improved active binder (like NC) will be even better (ideally the denser active binder the best).
5°)Using both OB improved active binder and OB mix will be the summum. Ideally 0% OB binder and EM mix.

[Edited on 11-2-2016 by PHILOU Zrealone]

greenlight - 13-2-2016 at 03:22

Thanks for the replies everyone, it seems that most plastic explosives like C4 and semtex will end up having a negative oxygen balance in the end.
Would an ETN PE versus a PETN PE come a draw in the end because the PETN plastic would have a slightly higher detonation velocity to counteract the negative OB% or is ETN still superior?

Hennig Brand - 13-2-2016 at 13:32

From Meyer:

"
Brisance

Brisanz

The performance of an explosive cannot be expressed by means of a single characteristic parameter. Brisance is the destructive fragmentation effect of a charge on its immediate vicinity. The relevant parameters are the detonation rate and the loading density (compactness) of the explosive, as well as the gas yield and the heat of explosion. The higher the loading density of the explosive (molding or pressing density), the higher its volume specific performance; also, the faster the reaction rate, the stronger the impact effect of the detonation. Moreover, an increase in density is accompanied by an increase in the detonation rate of the explosive, while the shock wave pressure in the detonation front (Detonation) varies with the square of the detonation rate. Thus it is very important to have the loading density as high as possible.

This is particulary true for Shaped Charges.

Kast introduced the concept of “brisance value”, which is the product of loading density, specific energy and detonation rate.

Brisance tests are upsetting tests according to Kast and Heß; the compression of a copper cylinder is determined by actuating a piston instrument; alternatively, a free-standing lead cylinder is compressed by the application of a definite cylindrical load of the explosive being tested: Upsetting Tests.
"

ETN:

Specific Energy = 1091 kJ/kg
Detonation Velocity = 8000 m/s
Density = 1.6 g/cc (obtainable loading density?)


PETN:

Specific Energy = 1205 kJ/kg
Detonation Velocity = 8400 m/s
Density = 1.7 g/cc (obtainable loading density?)

Brisance Value = Loading Density * Specific Energy * Detonation Rate

Brisance ValueETN = 1600 kg/m^3 * 1091 kJ/kg * 8000 m/s
Brisance ValueETN = ca. 14 billion

Brisance ValuePETN = 1700 kg/m^3 * 1205 kJ/kg * 8400 m/s
Brisance ValuePETN = ca. 17 billion

Relative Brisance Value PETN / ETN = 17 / 14 = ca. 1.21

I may have underrated ETN in terms of density, but PETN still comes out significantly ahead in terms of brisance even with more optimistic numbers for ETN.

Note: Aluminum is added to PBXs and putties(plastic explosives) sometimes, but not in shaped charge applications, from what I understand, or other applications where brisance is much more important than energy output and a long drawn out impulse. Most applications that use these types of explosives require a high brisance shattering action. Simply because of the distance between atoms, the relatively poor mixing and the energy requirements of the reactions (probably other reasons) the secondary oxidation reactions are much slower and add to blast effect, but are not very helpful to brisance as I understand it. Particles of high explosive are embedded in a binder/plastic matrix (not well mixed at all in comparison to a molecule of high explosive!).


[Edited on 14-2-2016 by Hennig Brand]

PHILOU Zrealone - 14-2-2016 at 04:48

Quote: Originally posted by Hennig Brand  
From Meyer:

"
Brisance

Brisanz

The performance of an explosive cannot be expressed by means of a single characteristic parameter. Brisance is the destructive fragmentation effect of a charge on its immediate vicinity. The relevant parameters are the detonation rate and the loading density (compactness) of the explosive, as well as the gas yield and the heat of explosion. The higher the loading density of the explosive (molding or pressing density), the higher its volume specific performance; also, the faster the reaction rate, the stronger the impact effect of the detonation. Moreover, an increase in density is accompanied by an increase in the detonation rate of the explosive, while the shock wave pressure in the detonation front (Detonation) varies with the square of the detonation rate. Thus it is very important to have the loading density as high as possible.

This is particulary true for Shaped Charges.

Kast introduced the concept of “brisance value”, which is the product of loading density, specific energy and detonation rate.

Brisance tests are upsetting tests according to Kast and Heß; the compression of a copper cylinder is determined by actuating a piston instrument; alternatively, a free-standing lead cylinder is compressed by the application of a definite cylindrical load of the explosive being tested: Upsetting Tests.
"

ETN:

Specific Energy = 1091 kJ/kg
Detonation Velocity = 8000 m/s
Density = 1.6 g/cc (obtainable loading density?)


PETN:

Specific Energy = 1205 kJ/kg
Detonation Velocity = 8400 m/s
Density = 1.7 g/cc (obtainable loading density?)

Brisance Value = Loading Density * Specific Energy * Detonation Rate

Brisance ValueETN = 1600 kg/m^3 * 1091 kJ/kg * 8000 m/s
Brisance ValueETN = ca. 14 billion

Brisance ValuePETN = 1700 kg/m^3 * 1205 kJ/kg * 8400 m/s
Brisance ValuePETN = ca. 17 billion

Relative Brisance Value PETN / ETN = 17 / 14 = ca. 1.21

I may have underrated ETN in terms of density, but PETN still comes out significantly ahead in terms of brisance even with more optimistic numbers for ETN.

Note: Aluminum is added to PBXs and putties(plastic explosives) sometimes, but not in shaped charge applications, from what I understand, or other applications where brisance is much more important than energy output and a long drawn out impulse. Most applications that use these types of explosives require a high brisance shattering action. Simply because of the distance between atoms, the relatively poor mixing and the energy requirements of the reactions (probably other reasons) the secondary oxidation reactions are much slower and add to blast effect, but are not very helpful to brisance as I understand it. Particles of high explosive are embedded in a binder/plastic matrix (not well mixed at all in comparison to a molecule of high explosive!).


[Edited on 14-2-2016 by Hennig Brand]

I have made a comparison of various (poly)nitrate esters(*) from Josef Köhler and Rudolf Meyer (JK&RM) and other datas sources by plotting VOD vs density; the resulting diagram is kind of bi-linear (one slope for the liquid nitrate esters, and another one for the solid nitrate esters) but there is a problem with ETN; first I thought it to be due to the fact it might be into the median zone yielding properties between liquid NG and solid MHN but it is not that, the value of 1.6gr/cm³ is obviously wrong...ETN has a density much closer to 1.72 gr/cm³.
If you take a deep look into the book "Explosives" by JK&RM; there are a lot of typos and discrepencies :(.

If you correct that value of 1.6 into 1.72 then everything comes to normal in the graphic truly linear dependance.

I will try to find that graph back and post it here.
I will also try to make the detonic calculations for various ETN/PETN mixes and ETN/Binder vs PETN/Binder following JK&RM thermodynamic calculation instructions.(and post those here).

(*)
Liquids:
Methyl nitrate
Ethyl nitrate
EGDN
NG
Butyl glycol dinitrate
Butyl glycol trinitrate
NIBTN (nitroisobutyl trinitrate)

Solids:
Polyvinyl nitrate
Nitrocellulose
ETN
MHN (Mannitol hexanitrate)
PETN
TMDNETN (TetraMethylol-DinitroEthane-Tetranitrate)

nitro-genes - 14-2-2016 at 05:35

My guess would be that the positive oxygenbalance of ETN aids only very little to an increase in VoD, (and thus brisance) compared to PETN. The density of the charge as a whole is affected more by the density of the HE used. Also, the binder and etn are physically seperated, meaning only a small percentage of the binder will react in the reactionzone itself and actually aid to the increase in VoD. , 99% of the inerts that actually do combust, will combust from detonation products and or oxygen from the air long after the detonation wave has passed, increasing total energy output, but decreasing brisance.

PHILOU Zrealone - 14-2-2016 at 11:00

If this was true, then brisance of TeNM would'nt be so dramatically increased by organic aromatic fuels...wich only decrease the overal density...

Hennig Brand - 14-2-2016 at 14:24

OK, I would say you are correct and the crystal density of ETN is probably closer to 1.72 g/cc (I have references that state this as well). However, even if ETN and PETN are given equal densities and detonation velocities the higher specific energy value for PETN will give PETN a higher brisance value by about 10%.

TeNM, I have not worked with. I believe this is the chemical formula, C(NO2)4 (Tetranitromethane). TeNM isn't even an explosive in its pure form, it is an oxidizer. It makes sense that adding a liquid fuel to a liquid oxidizer, in the correct proportions, could make an explosive mixture. If they are miscible, which I imagine they are, the molecules of oxidizer and fuel would be about as well mixed as they could possibly be, unless they were part of the same molecule I suppose. Going from a non explosive oxidizer with a high density to an explosive with a lower density would increase the brisance. Even going from an oxidizer fuel mixture with a very high positive oxygen balance to a more balanced mixture would result in a much faster reaction--->(closer proximity of oxidizer molecules and fuel molecules, more even distribution of fuel and oxidizer and a higher energy density), ( more energy, more gas output)---> more specific energy.......even with a drop in density in this case. This is a special case, not very much related to plastic explosives (I think).


[Edited on 14-2-2016 by Hennig Brand]

nitro-genes - 14-2-2016 at 14:38

As two liquids it would be a different story indeed. What is interesting also is that different crystaI lattice structures for the same HE can affect sensitivities. IIRC correctly, this is f.e. true for beta hmx. I've always assumed this was due to the orientation and distance of the functional groups relative to each other, or due to physical properties from alterations in how the stimulus is transfered.

PHILOU Zrealone - 15-2-2016 at 04:40

Quote: Originally posted by Hennig Brand  
OK, I would say you are correct and the crystal density of ETN is probably closer to 1.72 g/cc (I have references that state this as well). However, even if ETN and PETN are given equal densities and detonation velocities the higher specific energy value for PETN will give PETN a higher brisance value by about 10%.

TeNM, I have not worked with. I believe this is the chemical formula, C(NO2)4 (Tetranitromethane). TeNM isn't even an explosive in its pure form, it is an oxidizer. It makes sense that adding a liquid fuel to a liquid oxidizer, in the correct proportions, could make an explosive mixture. If they are miscible, which I imagine they are, the molecules of oxidizer and fuel would be about as well mixed as they could possibly be, unless they were part of the same molecule I suppose. Going from a non explosive oxidizer with a high density to an explosive with a lower density would increase the brisance. Even going from an oxidizer fuel mixture with a very high positive oxygen balance to a more balanced mixture would result in a much faster reaction--->(closer proximity of oxidizer molecules and fuel molecules, more even distribution of fuel and oxidizer and a higher energy density), ( more energy, more gas output)---> more specific energy.......even with a drop in density in this case. This is a special case, not very much related to plastic explosives (I think).


[Edited on 14-2-2016 by Hennig Brand]

I'm not comparing pure ETN vs pure PETN...but an optimized OB mix of the two with binder or a mix of each with a binder/plasticizer...
You should read the chapter about "Thermodynamic calculation of Decomposition Reactions" in Explosives by J.Köhler and R.Meyer (about 25 pages included thermodynamic tables); they give step by step example, then you see that the central carbon atom into the PETN may be burnt during detonation proces by the extra oxygen from ETN ...thus the energy output from the OB ETN/PETN mix will be increased by kg of explosive.
I will do the calculation and graph to make it clearer to you.

The mix binder and EM if kneeded enough becomes like a solid solution of EM into the binder...there is close/intimate contact between molecules.
The use of binary liquid (oxydiser/fuel) that are soluble into each other makes the mix 100% homogenous, but with solids and binder (viscous solids) it is about the same even if not 100% homogenous on a molecular level.

*NH4NO3 prills and liquid/solid DNT wax/oil do detonate at higher speed and with more brisance than each compound appart.

*NH4ClO4/Triamino-Trinitrobenzene (binary solid mix) detonate at a much higher speed than each ingredient appart (+/- 9500 m/s) and the brisance is increased aswel.

*Tetranitromethane is an explosive on its own! (see Explosives book by J.K and R.M)
Specific energy: 687 kJ/kg
Energy of formation: +263.7 kJ/kg
Heat of explosion: 2259 kJ/kg
Volume of detonation gases: 685 l/kg
density: 1.677 g/ccm
VOD: 6360 m/s at 1.637 g/ccm
When mixed with DNT oil, the mix goes into the VOD regio 9000-9500m/s with extreme brisance.

*Hexanitroethane is also an explosive on its own! (see Explosives book by J.K and R.M)
Specific energy: 854 kJ/kg
Energy of formation: +473.2 kJ/kg
Heat of explosion: 3102 kJ/kg
Volume of detonation gases: 672 l/kg
density: 1.85 g/ccm
VOD: 4950 m/s at 0.91 g/ccm
VOD extrapolated at max density: 6800 m/s
When the solid is mixed with DNT oil, the mix should reach the 10000 m/s milestone with extreme brisance.

This shows that over-oxygenated EM and under-oxygenated EM suffer from the same problem...dead weight of unreacted detonation products (oxygen in the first case and carbon/fuel in the second one)...once this is circumvented by a binary (or more) system more oxygen balanced (that doesn't reduce too much the overal density); then the full volumic/weight power is reached.

Hennig Brand - 15-2-2016 at 05:57

I think we both have made some good points. I don't think everything either of us has said is completely correct, or at least not all of the time.

I'll have a look at that chapter, since a review couldn't hurt, but I think I still remember the fundamentals. I am not trying to pretend that the extra oxygen doesn't provide for more energy through combustion type reactions, I so far am unconvinced though that it does much to improve the brisance of the very brisant, ideal , molecular explosives. It is about the intensity of the impact (brisance), not total energy output. As far as plastic explosives having very well mixed HE component(s) and binder this is normally not the case at all, at least not relative to a molecule of ideal HE. The classic comparison is black powder and something like nitroglycerin or TNT. Even when extremely great lengths are taken to mill black powder (KNO3, S, Charcoal mixture) it is still an extremely coarse crude mixture in comparison to a molecule of nitroglycerin or TNT for example, with correspondingly inferior HE qualities. Another example is flash powder, even with extremely finely milled oxidizer and fuel components, still nothing in comparison to one of the better molecular explosives even though the energy output is huge. In comparison to a molecule, the particles of HE in the binder matrix of a plastic explosive are normally huge, from what I understand, and the binder layers have large average thickness as well and only contact the HE at the boundary layer surrounding the particles of HE. It is the proximity/closeness of fuel atoms and oxygen atoms to one another and nitrogen atoms to other nitrogen atoms, etc, and in good proportions, that makes an extremely fast reaction rate, high velocity, high brisance, HE. Many of the more crude things done to unideal explosives, such as AN, to improve performance, would often do very little or even often take away from an ideal, molecular, explosive if highest brisance is what is desired. When NG is added to AN, are we improving the AN or making worse the NG? An even better example might be mixtures of AN and the oxygen deficient TNT (I think I would use pure TNT in shaped charges). Depends on perspective maybe. I know there are many examples where there is a synergistic effect, greater sensitivity, more energy output, more gas output, etc, kind of enhancements especially with AN mixtures and some others, but these are normally unideal explosives and it is normally the more ideal, molecular, type explosives that are used in plastic explosives.

Hard to improve on (near) perfection!

I know that the HE component of a lot of mixtures often has the most control over the overall reaction rate (detonation velocity), often mostly due to its being the largest proportion, but the speed and brisance are still normally lower than for the pure molecular HE (I think).

Depending on how they were mixed a PETN and ETN mixture might get decent enhancement from the extra oxidation reactions, I don't know to what extent or under what circumstances exactly.


[Edited on 15-2-2016 by Hennig Brand]

KMnO4

Laboratory of Liptakov - 18-2-2016 at 09:04

Next short question: Has somebody experience with KMnO4 as explosive? As main oxidizer? I think not deflagration mixture. Nothing glycerine or sulphuric acid + permanganate. My reason is relatively (some week) stabile and non-hygroscopic mixture with VoD 2000m/s and more. I looking for on google, world patents, in S-mad in similarly thread. No place nothing (interesting) .Thanks, LL.....:cool:

Sulaiman - 18-2-2016 at 10:54

From experiments during my youth,
oxidiser + fuel mixtures behaviour is dependant upon the intimacy of mixing,
results that I remember;

KMnO4 + Mg coarse particles = POOF !
KMnO4 + Mg fine particles = BANG !
NaClO3 fine grains each coated with yellow P = CRACK !
The last one had such brisance that I think it was a detonation rather than deflagration.
sorry, no hard data.

wg48 - 18-2-2016 at 14:27

Quote: Originally posted by Sulaiman  
From experiments during my youth,
oxidiser + fuel mixtures behaviour is dependant upon the intimacy of mixing,
results that I remember;

KMnO4 + Mg coarse particles = POOF !
KMnO4 + Mg fine particles = BANG !
NaClO3 fine grains each coated with yellow P = CRACK !
The last one had such brisance that I think it was a detonation rather than deflagration.
sorry, no hard data.


I remember the last one from my youth too.

Put a coin on a sheet of aluminium.
Place a pile of NaClO3 or the K salt to cover the coin.
Drop P4 desolved in CS2 on to the pile to saturate it.
Wait for the SC2 to evaporate (not too long)
Tap with a long very long stick .... bang
Examine impression of coin on the aluminium.
Certainly a rapid conflagration if not a detonation

I saw it demonstrated on the TV (UK) around 1967. Back then you could order a kilo of white phosphorus from B&H Chemicals and pick it up a few days later no problem.

I do not suggest anyone try it LOL


TheIdeanator - 18-2-2016 at 20:18

How sensitive are the polyol nitrates, metal acetylides, and mixes like flash powder? Would I be able to transport them in a car to a site about 10 hours away or might I be better off preparing them on-site? I also plan on experimenting with shaped charges.

I've never made any EMs before and I want to do some amateur mining this summer.

Bert - 18-2-2016 at 22:17

Quote: Originally posted by TheIdeanator  
How sensitive are the polyol nitrates, metal acetylides, and mixes like flash powder? Would I be able to transport them in a car to a site about 10 hours away or might I be better off preparing them on-site? I also plan on experimenting with shaped charges.

I've never made any EMs before and I want to do some amateur mining this summer.


Start reading. All the information you requested is here.

In consideration of the other motorists and out of respect for any public safety personnel tasked with prying your sorry ass out of your wrecked and possibly burning vehicle, please do not transport primary and/or secondary explosives in said un-placarded, non commercially inspected vehicle being operated by a non hazmat licensed and non CDL driver.

Yes, you PROBABLY could get away with it. But no sensible person who knows enough to understand the exposure to those around you will sympathize with you doing such a thing. Risk your own life if you must, please leave random others OUT of the situation.

TheIdeanator - 19-2-2016 at 14:27

Quote: Originally posted by Bert  
In consideration of the other motorists and out of respect for any public safety personnel tasked with prying your sorry ass out of your wrecked and possibly burning vehicle


That is something I had not taken into consideration, thank you. My risk tolerance is pretty high but I definitely don't want anyone else getting hurt if and when I make a mistake.

After reading through "Statistical study of rock drilling by hypervelocity jets from explosive shaped charges" by John William Brown(a good resource if you want to blow holes in rock), it seems that shaped charges won't work as effectively as I'd like them to. The resulting holes are too small, only about 0.2 times the charge diameter. Since I wanted to limit my shots to a maximum of an inch wide with a minimum of explosive and have holes bigger than 3/16" it kills that idea and pretty much eliminates my incentive for HEs. Back to blackpowder and hard work.

This is my research phase for this project. Since I don't have the right power tools and want to avoid spending much on this I'm considering creative options.

nitro-genes - 19-2-2016 at 16:58

Quote Philou:

" *NH4NO3 prills and liquid/solid DNT wax/oil do detonate at higher speed and with more brisance than each compound appart.

*NH4ClO4/Triamino-Trinitrobenzene (binary solid mix) detonate at a much higher speed than each ingredient appart (+/- 9500 m/s) and the brisance is increased aswel."


Curious though at what percentage of DNT the highest VoD will be achieved for AN/DNT though. My guess would be that at close to 3-4%, actually close to ANFO (inert fuel). Although the fact that DNT itself is explosive (contributing to the detonation wave itself) may also contribute, as well as that for AN mixtures detonable density increases with sensitizing fuels, and thus VoD. The easy at which both fuel and oxidizer seperately decompose (activation energy) and total energry release also matter probably.

The VoD figure for AP/TATB is really incredibly high, amazing it can detonate at max density apparently, is there sensitation due to some amineperchlorates formed?. If a mixture of TNT and AP would be reasonably stable and show similar sensitivity/VoD at max density, why do these kind of composition seem to find little use?

Dornier 335A - 20-2-2016 at 05:38

The optimal ratio between DNT and AN in terms of VoD and detonation pressure will surely be a function of the particle sizes. With large AN crystals in a DNT matrix, the highest VoD is likely to be achieved with very little AN. This is because rather than being an explosive (AN) mixed with an inert fuel (DNT), it should be viewed as an explosive (DNT) mixed with an inert oxidizer - there is simply not enough time for the more slowly detonating AN crystals to oxidize unburned carbon from the DNT before the shock wave has long since passed. With very finely powdered components, or porous AN prills soaked with DNT, or fine AN powder mixed with or even partially dissolved in molten DNT (is that possible?), it's another story. The mixture should behave much more like an ideal explosive, i.e. the reaction has reached equilibrium at the CJ point. Such a mixture would indeed have its highest VoD when it is close to oxygen balanced.

The AP/TATB mixture's performance seems overestimated to me. It could be a theoretical value for a completely homogeneous mix at maximum density. Two non-ideal explosives mixed on a macroscopic level should not reach such velocities, and certainly not at the max density. HNE/Tetryl (again two solids, but both being ideal explosives) has been confirmed to be exceptionally brisant by a Sciencemadness member though. Its theoretical detonation performance is similar to that of HMX, but with much higher energy output.

PHILOU Zrealone - 20-2-2016 at 06:03

Quote: Originally posted by nitro-genes  
Quote Philou:

" *NH4NO3 prills and liquid/solid DNT wax/oil do detonate at higher speed and with more brisance than each compound appart.

*NH4ClO4/Triamino-Trinitrobenzene (binary solid mix) detonate at a much higher speed than each ingredient appart (+/- 9500 m/s) and the brisance is increased aswel."


Curious though at what percentage of DNT the highest VoD will be achieved for AN/DNT though. My guess would be that at close to 3-4%, actually close to ANFO (inert fuel). Although the fact that DNT itself is explosive (contributing to the detonation wave itself) may also contribute, as well as that for AN mixtures detonable density increases with sensitizing fuels, and thus VoD. The easy at which both fuel and oxidizer seperately decompose (activation energy) and total energry release also matter probably.

The VoD figure for AP/TATB is really incredibly high, amazing it can detonate at max density apparently, is there sensitation due to some amineperchlorates formed?. If a mixture of TNT and AP would be reasonably stable and show similar sensitivity/VoD at max density, why do these kind of composition seem to find little use?

AN and AP are very good oxydisers in such mixes...indeed at max density by opposition with conventional ANFO (VODmax between 3.5 and 4.5 km/s) where air needs to be incorporated into the mix in a way to sensitize (during detonation compression wave, the air voids induces adiabatic compression bubbles --> hot spots) but this reduces density and thus VOD.

Here we are talking about a ANFO with an active fuel like AN-NM that can detonate at max density.
But AN-NitroMethane (VOD between 4-6 km/s depending on NM%) suffer from the weak density of nitromethane (1.14 g/cm³), its lack of fuel to burn (fast turns into overoxygenated mix).
In the case of DNT oils that display a density of +/- 1.54 g/cm³ you already gain a lot on density vs NM, the VOD is of course less than TNT (= 6.9 km/s) because less dense and worst OB (--> in the range of 6,2 km/s (but close to NM)).
In the case of DNT thus the fuel is burned by the excess OB of the AN contributing to the energy output...theorically the 0% OB mix seems to be wanted but this needs to be verified by calculations.

This kind of mixes were used for cost reasons because DNT is cheaper to obtain than TNT and AN is a lot cheaper.

In the case of TNT/AN mixes "Amatols" they display lower brisance (80%) and VOD than plain TNT but much more total energy output for underground/mining and underwater applications...

TNT/AP mixes will be expensiver and probably more sensitive (to impact, heat, bullet) ...two factors very important for military use.

About such mixes...the idea to incorporate hydrazinium or hydroxylaminium nitrate,perchlorate or nitroformiate will kick the VOD and brisance up, since:
*N2H5NO3 has a VOD of 8.9 km/s
*N2H5ClO4 has a VOD of >7.5 km/s
*N2H5C(NO2)3 has a VOD of ??? probably over 7.5 km/s
*HONH3NO3 has a VOD of 8.0 km/s
*HONH3ClO4 has a VOD of ??? probably over 7.0 km/s
*HONH3C(NO2)3 has a VOD of ??? probably over 7.0 km/s
And this is way over those of NH4NO3 and NH4ClO4...

[Edited on 20-2-2016 by PHILOU Zrealone]

Sulaiman - 20-2-2016 at 06:32

Quote: Originally posted by wg48  
Quote: Originally posted by Sulaiman  
From experiments during my youth,
oxidiser + fuel mixtures behaviour is dependant upon the intimacy of mixing,
results that I remember;

KMnO4 + Mg coarse particles = POOF !
KMnO4 + Mg fine particles = BANG !
NaClO3 fine grains each coated with yellow P = CRACK !
The last one had such brisance that I think it was a detonation rather than deflagration.
sorry, no hard data.


I remember the last one from my youth too.

Put a coin on a sheet of aluminium.
Place a pile of NaClO3 or the K salt to cover the coin.
Drop P4 desolved in CS2 on to the pile to saturate it.
Wait for the SC2 to evaporate (not too long)
Tap with a long very long stick .... bang
Examine impression of coin on the aluminium.
Certainly a rapid conflagration if not a detonation

I saw it demonstrated on the TV (UK) around 1967. Back then you could order a kilo of white phosphorus from B&H Chemicals and pick it up a few days later no problem.

I do not suggest anyone try it LOL



When I did the P + NaClO3 (together with a friend at my parents house, my father's garage was also my 'Lab')
one heaped teaspoon of NaClO3 on a metal milk bottle top (UK 'sterilized' milk bottle, c2cm dia.?)
on a 1" thick concrete slab, completely unconfined.
The book said that it would explode once the CS2 evaporated,
we waited, and waited, .... nothing.
must be yet another failure, back into the garage for more experiments.
15 or 30 minutes later a very loud CRACK ! like nearby lightning,
we dashed outside to find the concrete slab cracked and not much else visible.
We never tried that one again !
I don't know where deflagration ends and detonation begins, other than what I've read,
but it seemed similar to silver acetalide (Disilver ethyndiide)
Maybe P + NaClO3 with CS2 is equivalent to damp black powder / too much F in ANFO etc.?

EDIT: just removed an erroneous remark, hopefully before anyone read it!

[Edited on 20-2-2016 by Sulaiman]

Deathunter88 - 20-2-2016 at 10:35

How can a chemical be above 100% pure? I have quite a few reagent bottles that state a purity upper value greater than 100%.

For example, my bottle of copper nitrate states a purity of 99-102% and my bottle of manganese dioxide states a purity of 98-101%.

PHILOU Zrealone - 21-2-2016 at 08:05

Quote: Originally posted by Deathunter88  
How can a chemical be above 100% pure? I have quite a few reagent bottles that state a purity upper value greater than 100%.

For example, my bottle of copper nitrate states a purity of 99-102% and my bottle of manganese dioxide states a purity of 98-101%.

Maybe the container is made somehow of the material thus giving you more for your money :P:D...
No! Just kidding!
Of course purity is at max 100% at least in our old physical world ;).

Sulaiman - 21-2-2016 at 15:39

Today I had my first go at nitrating cotton wool,
c5g cotton wool given a 2 hour soak in 20 ml 69% HNO3 with 50 ml 96% H2SO4 (drain cleaner),
rinsed in water, NaHCO3, water, NaHCO3, water, water, water,
now open air drying overnight.


1) Is there a simple titration (or other method) that I can do to estimate the level of nitration ?

2) also, would I be correct in thinking that if I ignite a sample and there is no carbon residue then it is probably fully nitrated ?

3) last but not least, I read a few a articles and watched several youtube videos before I started,
Is it COMPLETELY SAFE to squeeze out liquids from the nitrocellulose in my hand between rinses, like in so many videos ?
(being unsure I did not, in fact I was a little scared during the whole procedure)


MineMan - 21-2-2016 at 19:16

I can only speak to number 3. If it is wet you should have no worries... even if it is dry... it should not be a big concern.

NeonPulse - 21-2-2016 at 22:40

It is safe to squeeze wet. But you will need to do more than that to ensure it is completely acid free. If it is not the product can be dangerous and will deteriorate fairly rapidly. Boiling in a carbonate solution for a while will ensure it is acid free. And as for 2 you can be fairly sure you have a good level of nitration if no carbon is left. To what nitrogen percentage exactly is difficult to tell without the right equipment. But it should be in the region of 12-13%Nitrogen for a nice fast clean burn with no residue and a nice whoomp sound.

[Edited on 22-2-2016 by NeonPulse]

Sulaiman - 22-2-2016 at 00:16

OK thanks,
Since I did not boil in NaHCO3 I guess it may deteriorate,
I'll 'test' it all tonight when I get home from work. ::D

NC grain

Laboratory of Liptakov - 22-2-2016 at 06:26

And what use for neutralisation NC same process, as for ETN or PETN. Dry NC Dissolved in acetone, for example on 10% solution. And added NaHCO3 to neutral reaction on paper strip. Now written procedure for mechanical cracking nitrocellulose on grain 1x1mm. Or grain 2x2mm. Or grain 0,5 mm. You need some salt. Usually is possible used NaCl, or NH4NO3, because are cheap. On 10g NC-solution 10%, ( thus 1g NC dry) , is used 20g salt. Thus 5% mix NC in salt. Next step is drying and evaporate acetone, during process crushed. Almost dry mix is easy possible crushed through sieve 2x2, 1x1, 0,5 according fraction of using. We get defined dry grain of NC. Next step is total drying salt-NC. If is salt dry, all is pour to water. For example 100g salt to 1 liter of water. Boiled 1 minute. Or get water on 70 Celsia. Every salt remains in water. Separate grain of NC. Easy through fine sieve, for example 0,1. This process repeat again. Evaporate pure water, grain dry on hot plate by 70 Celsia. Stirring during evaporate. Important: total dry grain are very electro flying. This is my methode how to get nitrocellulose grain from nitrocellulose laquer, NC-glue or any liquid which contents NC. And you can filling to shotgun. Sieve determines the average grain size. ...:cool:...LL

James Ikanov - 22-2-2016 at 08:17

I believe that post was describing how to make grains of nitrocellulose, but honestly, it all went a bit over my head....


Well, anyway, aside from evaporation or the use of a saturated sodium chloride solution, how would one go about drying a sample of nitroglycerin?

Obviously, heating it seems like a rather poor course of action, but might mixing it with a quantity of something that evaporates rather quickly, such as 99% isopropyl, or Acetone or such, wait till it stratifies, and then separating it?

As an aside, I've read that one should expect about 2.5 units of nitroglycerin for each unit of glycerin that is used. Is this a theoretical yield, or a projected yield? I attempted such a nitration about thrice, and the third time yielded roughly 30% of what I was expecting at best.... the other two times, well, they had to be drowned, but they were quite adequate learning experiences for my purposes.

Finally, is there a combination of solvents that will dissolve nitrocellulose that does not require ether?

greenlight - 22-2-2016 at 09:34

I dry mine in a desiccator overnight but if you don't have one I'm sure sitting the beaker of NG in a sealed jar on a layer of moisture absorber (Damprid) would do just as well. Goes in cloudy and comes out crystal clear like the original glycerine.
Nitroglycerin dissolves in acetone which would be more handy for making dynamites once it is dried.

The yield for NG depends on the concentration of the acids (how much water is in the reaction) and the nitration time I would assume, you would probably be able to get 250% yields if the Nitric was above 90%. I usually get about 1.5 to 2 times original volume using 70% Nitric acid depending on how long it gets left before crashing into cold water.

Also, I am not aware of any mixtures of solvents that do not involve ether for dissolving NC.

[Edited on 22-2-2016 by greenlight]

NG Theoretical Yield

Hennig Brand - 23-2-2016 at 06:03

Glycerol
C3H8O3
MW - 92.09382 g/mol
Density - 1.26 g/cc

Nitroglycerin
C3H5N3O9
MW - 227.09 g/mol
Density - 1.6 g/cc

Basis 1g Glycerol
Assume anhydrous glycerol

Theoretical Yield (100% conversion, no losses):

Mass
1g glycerol / 92.09382g/mol * 227.09g/mol = ca. 2.47g NG

Volume
(2.47g / 1.6g/cc) / (1g / 1.26g/cc) = ca. 1.95cc NG from 1cc glycerol

Microtek - 23-2-2016 at 23:18

Why would you want a more complex method for drying NG, when a simpler one would work at least as good? You could do it a number of ways, such as dissolving it in alcohol, adding anhydrous sodium sulfate or other drying agent, filtering and evaporating the alcohol. But there would be no point, since you could just use one of the ways you mentioned yourself. Personally, I use both: First saturated NaCl, then letting it stand in the open after separation; this also serves to separate a small amount of occluded NaCl from the NG. NG isn't hygroscopic so you really don't need a desiccator.

Acetone works very well for dissolving NC, and so does nitromethane.

gsd - 24-2-2016 at 00:58

Quote: Originally posted by Deathunter88  
How can a chemical be above 100% pure? I have quite a few reagent bottles that state a purity upper value greater than 100%.

For example, my bottle of copper nitrate states a purity of 99-102% and my bottle of manganese dioxide states a purity of 98-101%.


Copper Nitrate is Cu(NO3)2.3H2O, MW = 241.6, Cu content = 26.3%
If during drying even if a very small part of "3H2O" gets evaporated leaving behind a small fraction of anhydrous or partially hydrated Cu(NO3)2, then the overall Cu content will go above 26.3 %.
Since 26.3 % Cu corresponds to 100 % Cu(NO3)2.3H2O, the purity of "overdried" crystals will be above 100%

Similarly in case of MnO2, which is either synthetically made or is a natural ore, contains some presene of "lower oxides of Manganese" such as MnO, Mn2O3 or Mn3O4. If they are estimated as MnO2, then you will get purity which exceeds 100%.

gsd

nitrocellulose in blasting cap ???

Antoine - 24-2-2016 at 14:09

HI! on youtube, i've seen some people using nitrocellulose in their blasting caps. For example, in one of these videos, the men put 200mg of lead azide and 1500mg of nitrocellulose. the lead azide is compressed but do you think it's sufficient to acieve the detonation of nitrocellulose?
sorry for my bad english :(

James Ikanov - 24-2-2016 at 15:22

I'd say it's likely enough, but depends on the grain size of the NC among other things... also depends greatly on the quality of the NC as well. Quality of the Azide would also be a big factor in whether it detonated. If either was poor quality I doubt the NC would really detonate, and if the grain size was wrong I also think that would cause a failure. It would be at best unreliable, based on your description....

I also can't imagine any real benefit over using it compared to a more reliable secondary explosive like loosely packed ETN, PETN, or Tetryl.... and if you can make NC, you can probably just as easily make ETN instead, which is more powerful anyway.

Your English is actually fairly good, by the way. Nothing to worry about. :)

Antoine - 24-2-2016 at 15:36

Ok thank you for the replie! yes i think it's better to use etn or another secondary. I just need to find erythritol :)
and thanks for my english ;)

Herr Haber - 24-2-2016 at 15:49

1500mg of NC in a blasting cap?
I'm also interested in the grain size and / or the size of the blasting cap.
That seems like a big volume of NC to stuff into a tiny blasting cap.
I totally agree with James Ikanov: if you can make NC, you'll be better of making ETN instead.
a) It's less costly in acid
b) I'll be a lot more efficient.

Though in my personal experiences (I should really make a post about it) "loosely" packed ETN doesnt give great results. Melting some, then adding some ETN powder on top (and finally you azide with a thin al foil separation) gives great results.

Abbott242 - 25-2-2016 at 11:31

Hey, does anybody have any tips on locations to do tests? I was planning to detonate a few grams of ETN, but am unsure of exactly how loud it will be, and how far I will need to be from other people to avoid attention.

PHILOU Zrealone - 25-2-2016 at 13:50

Quote: Originally posted by Abbott242  
Hey, does anybody have any tips on locations to do tests? I was planning to detonate a few grams of ETN, but am unsure of exactly how loud it will be, and how far I will need to be from other people to avoid attention.

Burried charge will do much less noise than open one...
Maybe if you have a large enough sand bucket...you could do it indoor for a few grams.

Abbott242 - 25-2-2016 at 14:07

Okay, thanks- I'll consider a buried charge instead.

James Ikanov - 27-2-2016 at 10:33

Hmm.

A quick browsing of wiki suggested that nitrous oxide could be reacted with oxygen to yield nitric oxides.

Given that nitrous oxide is virtually unregulated, and widely available, and oxygen easily created from electrolysis of water, I'm very curious to find out if it's plausible one could do this at any scale that would produce usable amounts of nitric oxides.

Synthesis of dulcitoloctonitrate

octonitrocubane - 17-3-2016 at 07:34

Just before I try, would nitrating dulcitol in the same way as sorbitol of xylitol be able to form the octonitrate? I know that if it did, it would be potent...

PHILOU Zrealone - 17-3-2016 at 08:26

Not 8 nitrates but 6.
Dulcitol is a hexan-hexol just like sorbitol or mannitol...nitrodulcitol (dulcitol hexanitrate) power and sensitivity will be very close to those of SHN and MHN...

chemrox - 17-3-2016 at 18:22

I posted in the wrong place-sorry. Why does NaBH4 react with MeOH? Does it?

Metacelsus - 17-3-2016 at 18:26

It does react (forming hydrogen gas and borate esters/salts) but the reaction is slow at room temperature. This side reaction (among other reasons) means borohydride needs to be used in excess when methanol is used as the solvent.

Mr.Greeenix - 19-3-2016 at 07:20

I have a rather stupid question in storage! ;)

'cause I need help with some comprehensibility problems I have, about the potassium dinitramide synthesis!!

The nitration part isn't clear for me. So how much of the potassium salt of the sulfamic acid do you actually use? 17g? or 17 on the beginning and the end so 34 or what???


Here are two ?opposing? quotes ?

Quote:

17g potassium sulfamate was added in small portions (0.5- 1 g ) to a mixture of 16mL 98% concentrated sulfuric acid and 45 mL fuming nitric acid, with continual stirring of the mixture. The mixture was kept between (minus) -35 and -45 degC, using an ice bath consisting of dry ice and methylene chloride. (The reaction temperature need only be below -25 degC, if care is taken to avoid overheating) The viscocity increased as the reaction proceeded, and potassium bisulfate precipitated. Dinitramidic acid is not stable under acidic conditions so the pH must subsequently be raised to avoid decomposition.


Quote:

45 ml fuming nitric acid and 16 ml sulphuric acid (95%) were mixed in a narrow, high bowl of a diameter of about 5 cm. The nitration mixture was cooled to about -30°C with a mixture of dry ice and dichloroethane. The reaction vessel (bowl) was fitted with a propeller agitator. The potassium salt of the sulfamic acid was now added in small portions of 0.5-1 g during very powerful agitation. The viscosity increased significantly as the reaction proceeded when KHSO4 precipitated. The amount of dinitramidic acid formed was checked by taking off 1 ml of the solution, diluting it to 1000 ml and examining it by means of a UV spectrometer. The acid has a maximum absorbance of 285 nm. Since the acid is not stable in acid environment, the acid content of the reaction mixture begins to decrease after a certain reaction time. By UV spectroscopy, a suitable point of time for interrupting the reaction so as to obtain an optimum yield of the acid can be determined. In this manner, 17 g of the potassium salt were added, and the reaction was interrupted after about 20 min. The reaction mixture was poured into a bath containing 150 g of crushed ice and 150 ml of water, and the neutralisation was immediately initiated.

PHILOU Zrealone - 19-3-2016 at 10:21

Quote: Originally posted by Mr.Greeenix  
I have a rather stupid question in storage! ;)

'cause I need help with some comprehensibility problems I have, about the potassium dinitramide synthesis!!

The nitration part isn't clear for me. So how much of the potassium salt of the sulfamic acid do you actually use? 17g? or 17 on the beginning and the end so 34 or what???


Here are two ?opposing? quotes ?

Quote:

17g potassium sulfamate was added in small portions (0.5- 1 g ) to a mixture of 16mL 98% concentrated sulfuric acid and 45 mL fuming nitric acid, with continual stirring of the mixture. The mixture was kept between (minus) -35 and -45 degC, using an ice bath consisting of dry ice and methylene chloride. (The reaction temperature need only be below -25 degC, if care is taken to avoid overheating) The viscocity increased as the reaction proceeded, and potassium bisulfate precipitated. Dinitramidic acid is not stable under acidic conditions so the pH must subsequently be raised to avoid decomposition.


Quote:

45 ml fuming nitric acid and 16 ml sulphuric acid (95%) were mixed in a narrow, high bowl of a diameter of about 5 cm. The nitration mixture was cooled to about -30°C with a mixture of dry ice and dichloroethane. The reaction vessel (bowl) was fitted with a propeller agitator. The potassium salt of the sulfamic acid was now added in small portions of 0.5-1 g during very powerful agitation. The viscosity increased significantly as the reaction proceeded when KHSO4 precipitated. The amount of dinitramidic acid formed was checked by taking off 1 ml of the solution, diluting it to 1000 ml and examining it by means of a UV spectrometer. The acid has a maximum absorbance of 285 nm. Since the acid is not stable in acid environment, the acid content of the reaction mixture begins to decrease after a certain reaction time. By UV spectroscopy, a suitable point of time for interrupting the reaction so as to obtain an optimum yield of the acid can be determined. In this manner, 17 g of the potassium salt were added, and the reaction was interrupted after about 20 min. The reaction mixture was poured into a bath containing 150 g of crushed ice and 150 ml of water, and the neutralisation was immediately initiated.

To me both quotes seems quite identical process except the % of H2SO4, the sligth T° difference and dichloroethane instead of dichloromethane...

So 17g is the way to go not 17g+17g= 34g!

Making Nitrocellulose. How much cotton?

Camroc37 - 19-3-2016 at 12:41

Ratio of Cellulose to HNO3 to H2SO4 while making Nitrocellulose?
ex. (3.1g Cellulose for every 10ml of 50/50 HNO3/H2SO4 acid mix.
more specifically I am using KNO3 as an acid bath, mixing 80g KNO3 for every 65ml H2SO4. Sorry if this is a bit long/confusing, but I haven't found an answer yet. Thanks.

Hennig Brand - 19-3-2016 at 23:00

I made a spreadsheet in Excel a while back which is attached in the "Bullet Propellants" thread that should make life easier for you. It helps one determine quantities and strengths of acids needed for a particular percentage nitrogen NC. Often times acids of lower concentration can be used, for a particular %N, by adjusting the quantities used, but sometimes not. Keep in mind, the spreadsheet does not account for acid, cellulose or NC losses due to oxidation, acid losses due to evaporation, acid dilution due to absorption of water, etc, etc. Proper technique is still required!

http://www.sciencemadness.org/talk/viewthread.php?tid=22649&...

Attachment: Cellulose Nitration Diagram & Spreadsheet.xlsx (129kB)
This file has been downloaded 81 times

Attachment: Cellulose Nitration Diagram & Spreadsheet (compatibility mode).xls (143kB)
This file has been downloaded 85 times


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