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MadCompSci
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[*] posted on 1-9-2015 at 20:16
Where does the Oxygen come from?


This web site provides the equation for the reaction of KNO3 with Sorbitol as:
5O2 + 4KNO3 + 2C6H4O6 -> 12CO2 + 4H2O + 2N2 + 2K2CO3

http://aeroconsystems.com/tips/PotassiumNitrate_Sorbitol_mot...

In a rocket engine where does the extra 5O2 come from? It looks like the KNO3 oxidizer cannot provide enough oxygen for a stoichiometric reaction. It is a closed system so no O2 from the air ...

Is this why this fuel performs better with an excess of oxidizer?

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[*] posted on 1-9-2015 at 22:03


Quote: Originally posted by MadCompSci  
It is a closed system so no O2 from the air

Technically it is an open cycle. By F=ma it must be. If it's a closed system then it's a bomb not a rocket.

Quote: Originally posted by MadCompSci  
In a rocket engine where does the extra 5O2 come from ?

The paper does not inform one of the source , what makes you think other readers have better psychic ability.

http://www.sciencemadness.org/talk/viewthread.php?tid=20438#...
CO burns outside of the motor , for this reason will not contribute thrust. If the exhaust is clear in daylight or shows little visible flame , then it is stoichiometric. A long Yellow flame indicates incomplete combustion. There is a possibility of harnessing fuel rich exhaust for propulsion through air by using an augmentor. http://www.aardvark.co.nz/pjet/augmentors.shtml




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[*] posted on 1-9-2015 at 23:32


I think you should take this paper with a grain of salt. It is produced by students and if you look at page 11 on the diagram of the test setup with safety distance, you can see the test being initiated by three characters who seem to include Jack Sparrow and Han Solo....
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[*] posted on 1-9-2015 at 23:36


If oxygen from any other source participates in the reaction, they should include it. Otherwise it is simply wrong.

Quote:
5O2 + 4KNO3 + 2C6H4O6 -> 12CO2 + 4H2O + 2N2 + 2K2CO3


I count left side 5*2 + 4*3 + 2*6 = 34
right side: 12*2+4+2*3 = 34

Please explain how you arrived at an extra 5 O<sub>2</sub>




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[*] posted on 2-9-2015 at 00:41


I suspect it's a mistake. As it is the equation makes little sense.



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[*] posted on 2-9-2015 at 05:06


The two C of K2CO3 are also created "ex nihil".



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[*] posted on 2-9-2015 at 05:17


The correct equation is:

26 KNO3 + 5 C6H14O6 -> 17 CO2 + 13 N2 + 35 H2O + 13 K2CO3

By the way, sorbitol has 14 hydrogen atoms, not 4.

[Edited on 2-9-2015 by Cheddite Cheese]




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[*] posted on 9-9-2015 at 15:36




In explanation of the circumstances leading to this question:


Quote:

I am a bit embarrassed to admit being careless. But the information could cause someone else to take greater care, and so I will post a (probably better edited!) version of this to the thread in explanation. Regards, Bert
Quote:
Quote:
There was perhaps 20ml of NG total in the mixture. Incorrect variety of ammonium nitrate prills (a jar of prills looks like any other jar of prills at 02:00!) was used for a H2SO4/nitrate synthesis of a small amount of NG. There was a significant amount of anti caking additive in the AN- Which settled as a fine solid along with the liquid NG on first washing of the NG. After neutralizing this "slush" and decanting 90% + of the first wash water, the remaining wet NG/water/solid contaminant was taken up in acetone and filtered to remove solids, filter cake rinsed with several portions of acetone afterwards. The photo is of a beaker containing the combined filtrate and acetone washes of unknown solids. This separated on standing... Pipettes were used to take a sample of each layer. Only the bottom layer contained appreciable quantities of NG, along with acetone and unknown acetone soluble solid(s). On gentle heating, the plate like crystals floating on the bottom layer dissolved- Top layer was nearly pure acetone/acetone soluble crap, middle 2 layers were mostly water/water soluble crap. This material was taken out and destroyed by burning shortly after last picture was taken. I did not like the color either! Regards, Bert
Thank you Bert for the explanation. Glad you disposed of it. Just a tiny question, why in PM? Might be informative to others... May I put your answer in the tread or must this remain secret :-? ?




If one had found a flask of a mixture of nitroglycerin, water and acetone- And the mixture had separated into 2 layers...

What might one reasonably assume to be the NG/acetone layer- Top or bottom?

I would ASSUME the BOTTOM layer would be acetone/NG, and the TOP to be either acetone/H2O or mostly plain H2O.

Edit:

It's gone totally Pousse-café!

FOUR layers. And a layer of plate like crystals floating on the bottom most layer...

Also the layers are STRATIFIED IN TEMPERATURE.

Sitting in a 40C water bath:

Top layer: 14C (all the acetone evaporating from top surface, no doubt- and a nice condensation ring is on the outside of beaker at this level)

Middle 2 layers: 30-32C (photo does not show, but a definite boundary layer is there)

Bottom layer: 35C.

image.jpg - 1.5MB image.jpg - 1.7MB

[Edited on 10-9-2015 by Bert]

[Edited on 13-9-2015 by Bert]




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shocked.gif posted on 9-9-2015 at 21:28


Where could you possibly have just found that laying around?
I'd assume the nitroglycerin, being densest would end up on the bottom, but I think we left the realm of things I know anything about once the layers started seperating like that. ಠ_ಠ

How long has it been mixed like that, and under what conditions?
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[*] posted on 10-9-2015 at 05:26


@Bert,
I don't like the colour of your NG/Aceton/Water mix...there might be decomposition at work and aceton/HNO3 is not very stable...easily going runnaway.

From the picture you have like 120 ml dense liquid (almost pure NG?) in a glass container...not really safe.

The crystals may be some ketal...from reaction between free alcohol groups (NG hydrolysis) and aceton.
(CH3)2C=O + HOCH2-CHOH-CH2ONO2 -HNO3-> cyclic propanone ketal of propanetriol mononitrate ester + H2O
(CH3)2C=O + 2 HOCH2-CHONO2-CH2ONO2 -HNO3-> (CH3)2C(-OCH2-CHONO2-CH2ONO2)2 + H2O
or some condensation/polymerisation products of aceton or of oxynitration of it (nitroaceton or methyl glyoxal monoxime)...

[Edited on 10-9-2015 by PHILOU Zrealone]




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[*] posted on 11-9-2015 at 22:22


I recently attempted to fractionally distill H2O2 out of an off the shelf 3% solution, by making a supersaturated salt solution, and pouring off the liquid that did not freeze. However, when I was done, much to my dismay, there was essentially white sludge with some liquid mixed in with the remaining now melted liquid. I attempted to determine the concentration of the H2O2 (if there is any) by carefully dripping it onto a piece of paper. Nothing occurred.

Am I missing something here?
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[*] posted on 12-9-2015 at 02:54


Quote: Originally posted by James Ikanov  
I recently attempted to fractionally distill H2O2 out of an off the shelf 3% solution, by making a supersaturated salt solution, and pouring off the liquid that did not freeze. However, when I was done, much to my dismay, there was essentially white sludge with some liquid mixed in with the remaining now melted liquid. I attempted to determine the concentration of the H2O2 (if there is any) by carefully dripping it onto a piece of paper. Nothing occurred.

Am I missing something here?

Fractionally crystalization not distillation.

What would you see happening by putting H2O2 onto paper?
Unless colourized paper, it will only be whiter than white...

Did you test the poured unfrozen liquid?

Maybe do a tiny test with a drop of each on a KMnO4 grain...should produce immediate O2 release.




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[*] posted on 12-9-2015 at 18:27


D'oh. Fractional crystallization and fractional distillation aren't the same thing? oops.

I didn't test the unfrozen liquid, as that wouldn't have made sense.... it was very much about 90% liquid with only a tiny amount (maybe 25-100ml total) frozen at the bottom.

My "test" though informal, was to see if it was high test enough to ignite paper. I doubt it would be even if I was successful, but I was more interested in the white sludge that also appears to be mixed in. It's probably salt, but I don't see how that could've happened, is what I mean. I feel as though I've made a mistake somewhere along this line of questioning, but can't determine where.
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[*] posted on 14-9-2015 at 04:45


TKX-50

dichloroglyoxime is the starting material for TKX-50.

i found a good prepartion method for it!?

http://russianpatents.com/patent/231/2313517.html


Althought the title of this patent is "Method for preparing dichloroglyoxime"
they are also talking about dichlorohexane.

So I want to ask: If you follow this synthesis, do you get
dichloroglyoxime or dichlorohexane?

thanks
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[*] posted on 14-9-2015 at 06:36


Quote: Originally posted by Mr.Greeenix  
TKX-50

dichloroglyoxime is the starting material for TKX-50.

i found a good prepartion method for it!?

http://russianpatents.com/patent/231/2313517.html


Althought the title of this patent is "Method for preparing dichloroglyoxime"
they are also talking about dichlorohexane.

So I want to ask: If you follow this synthesis, do you get
dichloroglyoxime or dichlorohexane?

thanks

Must be a translation typo from russian to English...chemically it is not possible to find dichlorohexane from such starting material as carboxyfuroxan (furoxanoic acid) or as dichlorogly(oxaldi)oxime...

Maybe they mean dichlorofuroxan or dichloroglyoxime




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[*] posted on 14-9-2015 at 11:51


I think it is actually dichloroglyoxime.
because in the same patent they say it is dichloroglyoxime.

This way to dichloroglyoxime is for an hobby chemist! :)


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[*] posted on 17-9-2015 at 09:23


If you read about DCG from Axt, he mentioned this process, but also mentioned that nothing crystallized for him. Another patent US5476967 discusses DCG, but further that glyoxime preferentially chlorinates to monochloroglyoxime, which decomposes soon thereafter unless it is further chlorinated to DCG. But when chlorine is lacking the process mostly moves to MCG and then decomposition. The crux of the patent is that glyoxime needs to be added to the chlorine (or simultaneously to) such that chlorine can't react with glyoxime but must react with MCG until the DCG is formed and further glyoxime is then added. I would consider trying the CaCl2/H2O2 reaction, but attempt to dose the glyoxime into the HCl liquor instead of the other way.

Attachment: US5476967.pdf (706kB)
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[*] posted on 19-9-2015 at 00:31
Higher density dopes for active base dynamites?


The origin of this question is some comments in Naoum on use of high density oxidizers for dopes in low NG wartime mining explosives (dynamite dope formulations): For example, the higher VOD resulting from density change when substituting KClO4 for NH3NO3 offsetting the lowered VOD otherwise caused by a very low NG content.

Off the top of your head-

What are the highest density choices available among inorganic perchlorates, nitrates or chlorates, qualifying as being of a reasonably non hygroscopic nature... That is, compounds that one could leave a sample of sitting exposed to air for several days at STP and around 90% relative humidity, and not have it convert itself into a puddle!

Extra points for compounds that are reasonably stable in storage from -40 to at least 80C., and don't present a horrible handling problem due to toxicity, corrosive/reactive towards common engineering materials, etc.

Industrial choices of oxidizers in military and civil pyrotechnics typically being driven by OTHER considerations than density (such as economics), what if we think outside the box...

Google has not been my friend (so far) on this question.

(Edit)
My first thought was Barium nitrate and perchlorate at densities around 3.29 & 3.2, respectively. But a bit toxic-

[Edited on 19-9-2015 by Bert]




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[*] posted on 19-9-2015 at 16:35
TATP detonator? WHy?


I have seen many youtube videos with people using this stuff as a detonator. Watchng those scares me. Some of the videos even say the stuff was pressed:o:o

If the stuff is so unstable why are people using it? It seems to be a death wish.
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[*] posted on 19-9-2015 at 19:29


^It is. There is also a video on youtube of a kid blowing his hand off. Its just easy to make and thus people go for it. I tried MEKP for a bit, but between finding it unwieldy and unstable, as well as being advised against it by people on this forum, I stopped messing around with it. Even in the 1-3 ml batches I made, it was just to dangerous.
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[*] posted on 20-9-2015 at 03:19


Quote: Originally posted by Bert  
The origin of this question is some comments in Naoum on use of high density oxidizers for dopes in low NG wartime mining explosives (dynamite dope formulations): For example, the higher VOD resulting from density change when substituting KClO4 for NH3NO3 offsetting the lowered VOD otherwise caused by a very low NG content.

Off the top of your head-

What are the highest density choices available among inorganic perchlorates, nitrates or chlorates, qualifying as being of a reasonably non hygroscopic nature... That is, compounds that one could leave a sample of sitting exposed to air for several days at STP and around 90% relative humidity, and not have it convert itself into a puddle!

Extra points for compounds that are reasonably stable in storage from -40 to at least 80C., and don't present a horrible handling problem due to toxicity, corrosive/reactive towards common engineering materials, etc.

Industrial choices of oxidizers in military and civil pyrotechnics typically being driven by OTHER considerations than density (such as economics), what if we think outside the box...

Google has not been my friend (so far) on this question.

(Edit)
My first thought was Barium nitrate and perchlorate at densities around 3.29 & 3.2, respectively. But a bit toxic-

[Edited on 19-9-2015 by Bert]


I like this question !

if we ignore the costs to be factor in judgement , Potassium/Ammonium Perchlorate/Chlorate would be better than AN since they are not hygroscopic, more powerful oxidizer , higher density.

the problem of chlorate and perchlorate is its sensitive/hazards when it is in contact to any organic material. This would be risk.
At certain temperature chlorine gas start to come out and this is not good as well !

the best in my idea is NG/NC mixture and there are lots of patents on how to achieve the higher VOD of it.

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[*] posted on 20-9-2015 at 03:35


People arguing about how sensitive TATP is and how they did things to it without detonation while others said that would detonate it makes me think only one thing : they are not talking about the same thing.I'm talking about DADP formation,improper acid neutralization...etc.You're just trying your luck with those things so you should stay away from trying to play with them.
It's like trying to use a chlorate/perchlorate mixutre as perchlorate to make fireworks.
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[*] posted on 20-9-2015 at 10:45


Quote:

TATP detonator? WHy?


Same as HMTD:

-precursors are relatively easy to get

-takes fire easily, unlike lead azide and several other primaries

-has more power than most other common primaries and is cheap. 1g of this stuff is very much cheaper than 1g of mercury fulminate or lead azide and more important, it is more likely to do the job alone, without any additional booster.

That's what makes it popular with many hobbyists.
It's a more dangerous shortcut to successful blasts.
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[*] posted on 20-9-2015 at 15:41


Agreed there. The precursors are easy to get and very little skill or knowledge is needed to make acetone peroxide the synthesis is widely published and common on many how to sites and the yields are good so why not? Also the younger more inexperienced really have no idea on just how bad an accident with this stuff could be. younger people do take more risks. See that video of the Indian kid pressing 1g of peroxide in foil with his bare hands? If he really knew what he was doing he would not be doing that.



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[*] posted on 20-9-2015 at 16:17


Bert,

Using Caesium instead of Barium would get you twice the number of heavy atoms per useful oxidiser anion. I would expect the perchlorate to be non hygroscopic but that's just off the top of my head. I'm not sure density is an end in itself though, you could mix an explosive with lead powder to increase the density, but it's pretty much dead weight as is the Barium or Caesium ion. Whenever I've gone on thought experiments like this I end up drifting to embedding channels of a fast explosive. Not so much over driving the det wave as just communicating it to the extremities of the slow explosive faster.
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