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VladimirLem
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[*] posted on 21-12-2014 at 11:51


Quote: Originally posted by Turner  
60% yields


this is really strange...

exactly like the text from the link: 2g Erytrol -> 3.6g ETN, isnt really good

i dont get it...most infos say, 1g Erytrol to 2g< ETN (and thats with using nitrate salts/65%HNO3+H2SO4)
how can there be less yield, using higher quality chemicals?
Is it like making TNP, that using over 80%HNO3 will oxidize the material? *confused*



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DubaiAmateurRocketry
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[*] posted on 25-12-2014 at 15:27


What are a list of journals that publishes articles on EM frequently ?
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[*] posted on 4-1-2015 at 12:15
Hmtd as sensitizer in mixture with lead styphnate and potasium nitrate


I searching a sensitizer for a mixture of lead trinitrorezorcinate or lead picrate and potassium nitrate as replacement for tetrazene because I don`t have it and my searching favorites are : HMTD, cooper azide, silver acetylide.
This sensitive materials are very dangerous alone but if I used 5 % of composition work and delivered ignition when mixture is struck by a blow but what make me to post this topic is chemical stability of my mixture in time.
I prefer to use HMTD because is easy synthesized and work good but I don`t have information about selflife and chemical reactivity with lead styphnate and potassium nitrate plus the container surface will be painted cooper wall to prevent corrosive reaction with this
Please help me with some advices to find best replacement and don`t make a mixture who make boom without mechanical stimuli

[Edited on 4-1-2015 by otonel]
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[*] posted on 4-1-2015 at 12:45



Quote:

Please help me with some advices to find best replacement and don`t make a mixture who make boom without mechanical stimuli

I advise you to stop using organic peroxides immediately, then learn more about such compounds reactivity & chemistry before attempting to make or use other explosives.

NO! DON'T mix Lead or other metallic compounds with HMTD. Don't contain HMTD in Copper metal, even if you have "painted" it.

You have been a member since 2005, I see. Almost as long as I have- What are you trying to do???




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[*] posted on 4-1-2015 at 13:36


Bert , I`m not stupid to blow up my fingers but look at this Priming mixture patent
I don`t know if that mix what used , but if that was so dangerous why they patented , or it was a improvised solution for war ammo

[Edited on 4-1-2015 by otonel]
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[*] posted on 4-1-2015 at 14:08


There were a number of such patents and attempts to use HMTD for primary explosive in military and industrial applications. Reactivity to common metals mostly put an end to these experiments.

If any got past testing stages, I do not know of it. Rosco or other professionals may correct me on that.

Mere existence of the patent doesn't mean it was practically used, or a good idea for one to try for their self.

Are you trying to make a priming compound for small arms?




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Rosco Bodine
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[*] posted on 6-1-2015 at 21:05


Quote: Originally posted by otonel  
Bert , I`m not stupid to blow up my fingers but look at this Priming mixture patent
I don`t know if that mix what used , but if that was so dangerous why they patented , or it was a improvised solution for war ammo

[Edited on 4-1-2015 by otonel]


That was patented to scam money out of Remington

HMTD is not storage stable and nobody's patent makes it stable.
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[*] posted on 7-1-2015 at 12:04


Quote: Originally posted by Bert  


Are you trying to make a priming compound for small arms?

Yes I m trying )
Thanks for your answers , I tried to find an alternative solution for a sensitive compound but what I find as available for me is not good as chemical stability and have reactivity with metals, the mixture with hmtd works but my safety is more important them my research as hobbyist
I will return to traditional materials used as sensitive compound and right now I search some sources for aminoguanidine nitrate for synthesis tetracene or sodium hypophosphite.
For aminoguanidine synthesis I have urea , sulfuric acid and silica gel , and sodium hypophospite can be made from this stuff foliar fertilizer ?
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[*] posted on 11-1-2015 at 15:16
low yields with ETN


Quote: Originally posted by VladimirLem  
Quote: Originally posted by Turner  
60% yields


this is really strange...

exactly like the text from the link: 2g Erytrol -> 3.6g ETN, isnt really good

i dont get it...most infos say, 1g Erytrol to 2g< ETN (and thats with using nitrate salts/65%HNO3+H2SO4)
how can there be less yield, using higher quality chemicals?
Is it like making TNP, that using over 80%HNO3 will oxidize the material? *confused*


I also have tryed many ways of nitration of E and always the yeields are really poor. With 15gr of E i end with no more than 12gr of ETN.
I use a really boiled H2SO4 and really dry AN but the results are poor. Everything is really dry, well mixed and powdered.

[Edited on 11-1-2015 by underground]
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VladimirLem
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[*] posted on 12-1-2015 at 09:22


Quote: Originally posted by underground  
Quote: Originally posted by VladimirLem  
Quote: Originally posted by Turner  
60% yields


this is really strange...

exactly like the text from the link: 2g Erytrol -> 3.6g ETN, isnt really good

i dont get it...most infos say, 1g Erytrol to 2g< ETN (and thats with using nitrate salts/65%HNO3+H2SO4)
how can there be less yield, using higher quality chemicals?
Is it like making TNP, that using over 80%HNO3 will oxidize the material? *confused*


I also have tryed many ways of nitration of E and always the yeields are really poor. With 15gr of E i end with no more than 12gr of ETN.
I use a really boiled H2SO4 and really dry AN but the results are poor. Everything is really dry, well mixed and powdered.

[Edited on 11-1-2015 by underground]


i guess your H2SO4 has a bad a quality...


I "made" ETN, using 500ml HNO3(95%<;), 300ml H2SO4 and 100g Erytrit and i fucked it up
Result: 80g ETN:mad:
Check US Patent 1691954

I dissolved 100g E in 150ml H2SO4 (little bubbles visible). That mixture was like wood glue.
Then adding it to the HNO3...FUCK! the mixture was absolutly "insoluble"/hard to mix with the HNO3 that would have resulted in a EXREMELY low yield, so i just want to try the nitration with fine E powder and already mixed around 150ml of H2SO4 into my HNO3 but then i said, give it a try and added the E-H2SO4 mixture again and it become very good soluble into the H2SO4...

well....i added the mixture completely (around 10ml got lost) and have to say that nearly ZERO themerature have risen...i dunno if this is a good or bad (if i have to guess, bad LOL) sign but i was able to drow around 10ml of it at once into the HNO3+(only)150ml H2SO4

this was all done in around 15minutes lol...
so, then i thought that this was damn fast and i heated the whole acid mixture carefully in a waterbath up to 32C. the Acid now bacame clear as water. Only a few lumps of (i guess) undernitrated* ETN floating inside of the acids where visible and then cooling it down
*I added around 10g of fine powdered E to the acids after i added the around 90g E (from the E-H2SO4 mixture)

The whole nitration was around 20-30 minutes...i dont know if it was to short? I cant imagine, cause normaly i dont heat the acides (byside RDX) and the yield is VERY good (at least at mannitol, PE)...never did ETN syn before...

Can anyone say what went THAT wrong at my syn?

Vlad
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[*] posted on 15-1-2015 at 11:36


I am back )
My last priming compound has made from :
-25% lead trinitrorezorcinate
-17% red phosphorus from matches box
-5% tetril
-53% Pb(NO3)2
- some glass powder , and calcium carbonate as anti acid from red phosphorus
I test that mixture and work good and I want your opinion about chemical stability and what can be improved
My source of inspiration was this patent https://drive.google.com/viewerng/viewer?url=patentimages.st...
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[*] posted on 15-1-2015 at 12:05


Quote: Originally posted by otonel  
I want your opinion about chemical stability and what can be improved


It is usual to use some kind of binder and a liquid to make pellets for primer use. How are you handling that?

The red phosphorus will slowly oxidize away in air- Match book striker material is an unknown, but certainly contains ground glass, adhesives, probably shreds of paper fibers and whatever binders/inks/fillers the paper is made with.

Red phosphorus with COATINGS will oxidize less & last longer than the raw or salvaged product, most likely.

https://www.google.com/patents/US8540828

Here's a coating process:

https://docs.google.com/viewer?url=patentimages.storage.goog...

And here's a nice long home made primer thread on a reloading/shooting forum. You may recognize some names there.

http://castboolits.gunloads.com/showthread.php?182089-can-yo...










Rapopart’s Rules for critical commentary:

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2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.

Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).

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[*] posted on 15-1-2015 at 12:23


Thanks, very useful your answer Bert
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[*] posted on 24-1-2015 at 04:47


Does anyone know the VoD for sucrose octanitrate? I can't seem to find it, though it appears to have had some commercial use early last century, so I'd think it'd have been more studied.
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[*] posted on 24-1-2015 at 09:09


Quote: Originally posted by Trotsky  
Does anyone know the VoD for sucrose octanitrate? I can't seem to find it, though it appears to have had some commercial use early last century, so I'd think it'd have been more studied.

-If Sucrose is C12H22O11
-Then Sucrose octanitrate is C12H14N8O27
-Assuming density between 1.5 and 1.7 g/ccm (based on density of nitrostrach (1.6) and nitrocellulose (1.67)
-Based on enthalpy of formation evolution from 11%N to 13.3%N nitrocellulose: enthalpy of formation must be between 0 kJ/mol and -1450 kJ/mol.

Entering datas into Engager's SMF detonation calculator utility program:
*With Hf°= -0.1 kJ/mol
if d= 1.7 g/ccm
VOD = 8784 m/s
PCj = 344 kbar

if d= 1.6 g/ccm
VOD = 8382 m/s
PCj = 304 kbar

if d= 1.5 g/ccm
VOD = 7980 m/s
PCj = 267 kbar

*With Hf°= -1450 kJ/mol
if d= 1.7 g/ccm
VOD = 7919 m/s
PCj = 161 kbar

if d= 1.6 g/ccm
VOD = 7567 m/s
PCj = 142 kbar

if d= 1.5 g/ccm
VOD = 7216 m/s
PCj = 124 kbar

Nitro-sugar is considered too unstable for practical use and stabilization is much harder than Nitroglycerin.


[Edited on 24-1-2015 by PHILOU Zrealone]




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[*] posted on 24-1-2015 at 11:14


Quote: Originally posted by Trotsky  
Does anyone know the VoD for sucrose octanitrate? I can't seem to find it, though it appears to have had some commercial use early last century, so I'd think it'd have been more studied.


Trotsky,

According to [1], sucrose octanitrate is a solid with a melting point of 85.5°C. If heated slowly, sucrose octanitrate decomposes at about 135° and if heated rapidly deflagrates at about 170°C. The fused and solidified material has a specific gravity of 1.67 g/cm<sup>3</sup>.

The experimental heat of formation (HOF) taken form [2] is HOF= -1364 kJ/mol.

Sucrose octanitrate has a slightly negative oxygen balance (OB%= -9.1) so the BKW thermochemical code [3] with RDX set of parameter is suitable for the calculation of the detonation performance (DCJ & PCJ).

Based on the experimental density of 1.67 g/cm<sup>3</sup> and HOF of -1364 kJ/mol we have:

DCJ= 7821 m/s
PCJ= 264 kbar.

References:

[1] TENNEY L. DAVIS, The Chemistry of Powder and Explosives, p.p 242.

[2] P.J. Linstrom and W.G. Mallard, Eds., NIST Chemistry WebBook, NIST Standard Reference Database Number 69, National Institute of Standards and Technology, Gaithersburg MD, 20899, http://webbook.nist.gov.

[3] Mader, C. L. 2008. Numerical Modeling of Explosives and Propellants. 3rd ed. Boca Raton, FL: CRC Press.

Dany.
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[*] posted on 25-1-2015 at 01:22


You're not kidding about difficulty stabilizing it. I washed 3x with bicarbonate until it measured neutral with my ph paper. Let it sit in a glass jar for 3 hours while I napped. Came back afterwards and found that it'd completely decomposed to a black mass that reaked hard of nitrous oxides. Glad it wasn't worse.

I'm gonna give it another go, but I'll leave it sit in a saturated bicarbonate solution until I'm ready to use it.
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[*] posted on 1-2-2015 at 10:22


If I have a lot of lead acetate cam make lead nitrate using alkaline nitrate without using nitric acid?
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[*] posted on 1-2-2015 at 12:37


Quote: Originally posted by otonel  
If I have a lot of lead acetate cam make lead nitrate using alkaline nitrate without using nitric acid?


Its technically a question for the general chemistry forum, but you can use gibbs energy methods to determine this. I don't have the entropy of lead(II) acetate but here is what I have.

lead(II) nitrate H -451.7kJ/mol, S 217.9J/K mol, G -256.9 kJ/mol
lead(II) acetate H -960.9kJ/mol
sodium nitrate H -467.9kJ/mol, S 116.5J/K mol, G -367.0kJ/mol
sodium acetate H -708.8kJ/mol, S 123.0J/K mol, G -607.2kJ/mol

It looks unfavorable based on the enthalpies of formation at least at room temperature.
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[*] posted on 1-2-2015 at 14:51


If I had lots of lead acetate I would just use that as my soluble lead salt, in place of lead nitrate. At least for my purposes it normally wouldn't make much difference which salt was used.



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[*] posted on 2-2-2015 at 13:03



Quote:

If I had lots of lead acetate I would just use that as my soluble lead salt, in place of lead nitrate. At least for my purposes it normally wouldn't make much difference which salt was used.

I understand that , but for making lead hypophospite and double salt is necessary lead nitrate.
Lead acetate was made from old car battery by boiling lead dioxide with acetic acid, is not very pure but is workable ,and I have same lead sulfate with impurities
If I boil lead acetate with sodium or potassium nitrate what will result will be lead nitrate and sodium acetate but both are soluble .
From this concentrated solution lead nitrate can precipitate due to his low solubility?
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[*] posted on 2-2-2015 at 19:11


It is quite an unfavorable enthalpy hole to dig yourself out of, theoretically. If you have a pile of reactants, give it a try, this is science after all. If you can play with solubilities (find a solvent that only lead nitrate is insoluble) you may be able to help yourself since some unfavorable reactions become favorable due to precipitation effects.
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[*] posted on 2-2-2015 at 19:16


A while back I too took lead dioxide from an old car battery, but I didn't try and react the lead dioxide with acetic acid and I am not sure that it would even work. I made sure the lead dioxide was well rinsed of sulfuric acid then I put it in an old steel soup can with a loose fitting steel cover. I then put the steel can on/in a bed of hardwood coals in my wood stove and opened the draft to let more air/oxygen in and make the coals hotter. The soup can was held at bright red/orange (ca. 650-800C) for 10-15 minutes or so at which point the can was removed and cooled. The lead dioxide was nearly all converted to yellow lead monoxide. Yellow lead monoxide can be easily converted to lead acetate or nitrate with the corresponding acid.

I know you said that you don't have nitric acid, but you must be able to get or make at least low concentrated nitric acid. Even 10% nitric acid can be used, it just means removing more water to concentrate the lead nitrate solution later on. Add an excess of yellow lead monoxide to fairly warm or hot nitric acid and then filter out what does not dissolve before concentrating the lead nitrate solution. There are a few more details, but that should get you started.


[Edited on 4-2-2015 by Hennig Brand]




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[*] posted on 5-2-2015 at 13:21


Oh, here is a neat tip with regards to lead dioxide calcination in a steel soup can. Keeping the can at bright red/orange for 10-15 minutes will cause some rust to form on the inside of the can and flake off into the lead dioxide/oxide. When I first saw this I was not pleased, since the idea of picking little bits of rust out of lead monoxide sounded tedious and possibly unhealthy even. I remembered that iron oxide formed at high temperatures like this is normally magnetite, (Fe3O4), and judging by the very dark color of the rust it did appear to be mostly magnetite. Just as the name sounds, magnetite is magnetic. Gently stirring the yellow lead monoxide and Fe3O4 mixture with the magnet end of a small magnetic pickup tool quickly collected almost all of the rust contamination. I was once again happy. :D



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[*] posted on 6-2-2015 at 12:43


You have right Henning Brand, my synthesis was inspired by this article homemade lead acetate and I forgot step with lead oxide because I make this a couple of months ago.
I boil lead acetate with potassium nitrate and I have some white precipitate to dry, I don`t know right now what exactly is.

[Edited on 6-2-2015 by otonel]
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