Sciencemadness Discussion Board - Short question / quick answer - Thread

Does hydroxylammonium salt of azide, dinitrourea, dinitroguanidine exist? I havent found much information on them.

See http://link.springer.com/article/10.1023%2FA%3A1022503310689...

It seems that dinitrourea reacts with hydroxylamine to form hydroxynitrourea, and with hydrazine to nitrosemicarbazide.

underground - 6-3-2014 at 05:04

It seems that dinitrourea reacts with hydroxylamine to form hydroxynitrourea, and with hydrazine to nitrosemicarbazide.

How hydroxylamine solution can be prepared ?

Dissolving PIB

underground - 7-3-2014 at 03:54

With a little search i have found that the bicycle tire inner tube is made out of PIB, so. i just took a small piece of that material, and dip it into some gasoline, but it looks like it can not be dissolved by gasoline, so i was wondering what else solvent can i use to dissolve that ?

[Edited on 7-3-2014 by underground]

confused - 7-3-2014 at 04:10

Have you tried using hexane or pentane?

[Edited on 7-3-2014 by confused]

VladimirLem - 7-3-2014 at 08:46

With a little search i have found that the bicycle tire inner tube is made out of PIB, so. i just took a small piece of that material, and dip it into some gasoline, but it looks like it can not be dissolved by gasoline, so i was wondering what else solvent can i use to dissolve that ?

[Edited on 7-3-2014 by underground]

PIB is soluble in gasoline (benzine) but if it is some layer of a pipe, it will need days to dissolve...if you had a block of PIB, just make it tol small pieces with a scissor

DubaiAmateurRocketry - 7-3-2014 at 09:41

Does hydroxylammonium salt of azide, dinitrourea, dinitroguanidine exist? I havent found much information on them.

See http://link.springer.com/article/10.1023%2FA%3A1022503310689...

It seems that dinitrourea reacts with hydroxylamine to form hydroxynitrourea, and with hydrazine to nitrosemicarbazide.

Ive just saw that before i saw your post, thx anyways.

Do you know any other routes to nitrosemicarbazide?

and for underground, have you tried acetone ?

underground - 7-3-2014 at 10:20

and for underground, have you tried acetone ?

PIB can not be dissolved by acetone

PIB is soluble in gasoline (benzine) but if it is some layer of a pipe, it will need days to dissolve...if you had a block of PIB, just make it tol small pieces with a scissor

I used gasoline (i guess it is different than benzine) from petrol stations, is this going to work or not ? Does it need pure benzine ?

[Edited on 7-3-2014 by underground]

VladimirLem - 7-3-2014 at 12:42

I used gasoline (i guess it is different than benzine) from petrol stations, is this going to work or not ? Does it need pure benzine ?

[Edited on 7-3-2014 by underground]

jesus...i allways hated the way american people call this stuff...

just benzine/petrol for cars...

The_Davster - 7-3-2014 at 12:47

It seems that dinitrourea reacts with hydroxylamine to form hydroxynitrourea, and with hydrazine to nitrosemicarbazide.

How hydroxylamine solution can be prepared ?

Methanol. NH2OH.HCl. NaOH. Stirr till NaOH has dissolved and filter precipitated sodium chloride. Gives a methanolic hydroxylamine solution.

underground - 8-3-2014 at 08:55

Quote: Originally posted by The_Davster

It seems that dinitrourea reacts with hydroxylamine to form hydroxynitrourea, and with hydrazine to nitrosemicarbazide.

How hydroxylamine solution can be prepared ?

Methanol. NH2OH.HCl. NaOH. Stirr till NaOH has dissolved and filter precipitated sodium chloride. Gives a methanolic hydroxylamine solution.

From were i can obtain NH2OH ?

Also for those who are interensted in BIP, read this topic
http://parazite.nn.fi/roguesci/index.php/t-1739.html

Zyklon-A - 8-3-2014 at 08:59

I'm interested in dissolving PIB too.

underground - 8-3-2014 at 11:28

jesus...i allways hated the way american people call this stuff...

just benzine/petrol for cars...

So i correctly use that thing, correct ? It looks like for some reason benzine/petrol (

) can not dissolve bicycle tire inner tube

roXefeller - 8-3-2014 at 12:14

It seems that despite the confusion over petrol/gasoline/benzin pib should be soluble in either. But it could be difficult given the molecular weight. You may need small pieces and refluxed until it softens or dissolves. That would also be a good time to add the plasticizer. I found quicksilver's suggestion of bird repellent polybutene a good alternative.

The_Davster - 9-3-2014 at 01:28

Quote: Originally posted by The_Davster

It seems that dinitrourea reacts with hydroxylamine to form hydroxynitrourea, and with hydrazine to nitrosemicarbazide.

How hydroxylamine solution can be prepared ?

Methanol. NH2OH.HCl. NaOH. Stirr till NaOH has dissolved and filter precipitated sodium chloride. Gives a methanolic hydroxylamine solution.

From were i can obtain NH2OH ?

Also for those who are interensted in BIP, read this topic
http://parazite.nn.fi/roguesci/index.php/t-1739.html

That was NH2OH.HCl, hydroxylamine hydrochloride. no OTC source that I know, but it can be made, see old posts by I think Axt.

DubaiAmateurRocketry - 9-3-2014 at 08:11

does II salts of diamino/triamino guanidine exist? The interesting derivatives would be diamino/triamino dinitrate, which is mentioned in this patent.

http://www.google.com/patents/EP1121336A2?cl=en

These 2 compounds will have high gas production/ nitrogen content/ density/ and low sensitivity/cost/ and carbon content.

No other papers/patent or any report or research has mention these 2 compounds, or at least on google.

[Edited on 9-3-2014 by DubaiAmateurRocketry]

underground - 9-3-2014 at 14:52

Quote: Originally posted by The_Davster

That was NH2OH.HCl, hydroxylamine hydrochloride. no OTC source that I know, but it can be made, see old posts by I think Axt.

I can not find anything about NH20H solutions

I found only some informations about how to form hydroxylamine hydrochloride from NM acetic acid and HCL. But i do not know if a solution of NH2OH.HCL can react with other nitrogroups like dinitrobiuret to for dihydroxylammonium dinitrobiuret, or dinitroguanidine to form hydroxylammonium dinitroguanidine e.t.c.

DubaiAmateurRocketry - 14-3-2014 at 12:10

Is there any energetic compound on hydroxygaunidine and its derivatives?

It can be protonated to produce salts like http://www.sigmaaldrich.com/catalog/product/sigma/h7654?lang...

I also think its derivatives would be very interesting/ energetic.

Dany - 15-3-2014 at 04:33

Is there any energetic compound on hydroxygaunidine and its derivatives?

It can be protonated to produce salts like http://www.sigmaaldrich.com/catalog/product/sigma/h7654?lang...

I also think its derivatives would be very interesting/ energetic.

Compared to guanidine, hydroxyguanidine represent a better oxidized moiety. Energetic material (salt or molecular compound) may have interesting energetic properties (performance) however when you realize that 50 mg of hydroxyguanidine sulfate salt cost 220 euro or 306 USD, any interesting applications for these compounds is lost until a new synthetic method is found to produce hydroxyguanidine derivatives in low cost.

Dany.

[Edited on 15-3-2014 by Dany]

Trinitrophenol - 15-3-2014 at 06:37

Xylene also works. Some types of chewing gum contain PIB as a base. So if you want to isolate pure PIB dissolve as much impure PIB such as bike tire or chewing gum in xylene as possible. Then there will be a clear layer ontop of the xylene witch conatains the PIB. Then go ahead and extract this layer with a syringe or pipete. Then combine the PIB/xylene With acetone at a 50/50 ratio. This will then precipitate your pure PIB.
Then just Fish this up with a little match stick or something similar and dry it.

Btw if the rubber dosent dissolve in xylene its not PIB ;

Why you want to isolate PIB btw?

DubaiAmateurRocketry - 15-3-2014 at 11:32

Quote: Originally posted by Dany

Alright true, but, Sigma extremely over price everything.

http://www.sigmaaldrich.com/catalog/product/aldrich/s849022?...

this compound can be synthesized from 2 extremely industrialized cheap compound - Nitropropane and formaldehyde, however they sell 50mg for nearly 100 dollars!

Do you have any information about my question 2 posts above?

Thanks

Dany - 16-3-2014 at 03:12

Maybe Sigma-Aldrich are overpriced but you must take onto account the purity of the compound. It is true that a compound may be possess a facile synthesis but this is not all the story. Purifying the resulting products can be very challenging and tedious, so the compound may be very expensive. Other chemical company can sell chemicals with competitive price. I prefer TCI chemical when compared to Sigma-Aldrich.

For the second question, my quick search didn't result in any high energy materials based on hydroxyguanidine.

Dany.

DubaiAmateurRocketry - 16-3-2014 at 04:37

Quote: Originally posted by Dany

Maybe Sigma-Aldrich are overpriced but you must take onto account the purity of the compound. It is true that a compound may be possess a facile synthesis but this is not all the story. Purifying the resulting products can be very challenging and tedious, so the compound may be very expensive. Other chemical company can sell chemicals with competitive price. I prefer TCI chemical when compared to Sigma-Aldrich.

For the second question, my quick search didn't result in any high energy materials based on hydroxyguanidine.

Dany.

Yes, ive also found TCI cheaper in many products.

I meant 2 post up as in this post, the diamino/triamino guanidine dinitrate salt.

does II salts of diamino/triamino guanidine exist? The interesting derivatives would be diamino/triamino guanidine dinitrate, which is mentioned in this patent.

http://www.google.com/patents/EP1121336A2?cl=en

These 2 compounds will have high gas production/ nitrogen content/ density/ and low sensitivity/cost/ and carbon content.

No other papers/patent or any report or research has mention these 2 compounds, or at least on google.

[Edited on 9-3-2014 by DubaiAmateurRocketry]

^ When I said on google I meant my searches, you might find something else.

Also, the last time I purchase chemicals, I used an intermediate company, they search the market to find the cheapest pricing for the products I wanted out of countless chemical companies, and then they order them for me and send it to me, its much cheaper in the end if you only buy from 1 company because some company are better than others in producing one product. You just have to pay them little bit service fee.

[Edited on 16-3-2014 by DubaiAmateurRocketry]

PHILOU Zrealone - 16-3-2014 at 06:12

Funny

About two monthes ago I had the same ideas.

The compounds should be cheap but as not requested much their price is very high.

Like amino, diamino and triaminoguanidine or amino and diamino urea... it is only a mater to allow the free base to react with urea or guanidine...more volatile NH3 is freed from the reaction media (NH3 is more volatile than N2H4 or NH2OH).

As potent materials with increased density, stored energy and OB; there are also:
-hydroxyurea (HONH-C(=O)-NH2)
and
-dihydroxyurea (HONH-C(=O)-NHOH)

-hydroxyguanidine (NH2-C(=NH)-NHOH)
-dihydroxyguanidine (HONH-C(=NH)-NHOH)
and
-trihydroxyguanidine (HONH-C(=NOH)-NHOH)

Note that the basicity of such hydroxylamino derivatives will be less than urea and so very strong acids will be needed to make salts with them (nitrate, perchlorate, nitroformiates, tetranitroethandiates, dinitramides,...). There is a chance it doesn't work for the trihydroxyguanidine or dihydroxyurea.

They will eventually be acidic and form primary salts.

They might cyclise into 1,2,4,5-tetrazine derivatives especially the molecules bearing both amino/imino and hydroxylamino/hydroxylimino groups.

[Edited on 17-3-2014 by PHILOU Zrealone]

DubaiAmateurRocketry - 17-3-2014 at 08:36

So dinitrate salts are possible?

Yes, however can we still protonate compounds like trihydroxyguanidine? will it be unstable?

Also, does hydroxyhydrazine exist ? or aminohydroxylamine.

Don't want to continue sidetracking of "Tetranitomethane/toluene explosive mixture myth" thread, BUT:

Bert - 17-3-2014 at 08:54

Crazy thought- Anyone tried mixing a small % of microballoons into Hg(ONC)₂ and pressing the mixture at a similar pressure as is known to "dead press" the straight material?

n-nitrodiethylamine

roXefeller - 17-3-2014 at 09:31

I'm looking at my chem shelf at a couple bottles of diethylamine HCl and I'm thinking, can this be taken to a nitramine, or maybe just a nitrate salt? It is already strongly alkaline and the warning against mixing with oxidizers is there. Low temps are a must. It has a rather low density so I'm not sure there is any value to it, unless it can form with a lead nitrate salt.

underground - 19-3-2014 at 07:23

I have found that there are some plastics that they can really dissolved in gasoline, so i was wondering if it is PIB, is there any other type plastic that gasoline can dissolve ?

VladimirLem - 19-3-2014 at 09:34

I have found that there are some plastics that they can really dissolved in gasoline, so i was wondering if it is PIB, is there any other type plastic that gasoline can dissolve ?

polystyene do...so maybe other hydrocarbons do too? dunno

if its not PIB, i think you could use this stuff for some kind of phlegmatising (if you want to^^)...

underground - 19-3-2014 at 09:56

polystyene do...so maybe other hydrocarbons do too? dunno

if its not PIB, i think you could use this stuff for some kind of phlegmatising (if you want to^^)...

What do you mean by that ? My english are a little bit poor

[Edited on 19-3-2014 by underground]

PHILOU Zrealone - 19-3-2014 at 13:15

So dinitrate salts are possible?

Yes, however can we still protonate compounds like trihydroxyguanidine? will it be unstable?

Also, does hydroxyhydrazine exist ? or aminohydroxylamine.

The number of protonations that are possible into a single molecule with near or viccinal molecular protonated groups depends strongly:
-on the basicity of the various groups (each time a protonation occurs the next protonation is harder).
-on the acid it is exposed to. If the acid that is submitted has a lower acidity than the protonated base (conjugated acid) then the acid base reaction will not be efficient.
HA + B <-=> a(-) + bH(+)

HA is a strong acid low pKa
B is a strong base high pKa (= low pKb)
a(-) is a very weak conjugated base of the strong acid HA (near neutral like Cl(-) in water)
bH(+) is the weak conjugated acid of the strong base B

As explained for (poly)hydroxyguanidine the presence of the hydroxy will reduce the basicity of each nitrogen so the first protonation will be less easy...and the other after even harder...

underground - 22-3-2014 at 03:10

Can i prepare HDN with the same way as Urea nitrate ? With HCL, Hexamine and NH4NO3 ?

edit: Also once i made some UN out of urea, HCL and AN, but when i was trying to neutralized it with sodium carbonate, it just disappeared, i guess it just hydrolyzed or react with sodium carbonate , so how can i neutralized it ?

[Edited on 22-3-2014 by underground]

DubaiAmateurRocketry - 22-3-2014 at 04:08

So dinitrate salts are possible?

Yes, however can we still protonate compounds like trihydroxyguanidine? will it be unstable?

Also, does hydroxyhydrazine exist ? or aminohydroxylamine.

What about aminohydroxylamine ? HONHNH2

http://www.sciencedirect.com/science/article/pii/S0040609002...

Apparently, it is sold by some chem suppliers, and ive never seen its use any where...

http://mastersearch.chemexper.com/cheminfo/servlet/org.dbcre...

PHILOU Zrealone - 22-3-2014 at 05:57

Quote: Originally posted by roXefeller

I'm looking at my chem shelf at a couple bottles of diethylamine HCl and I'm thinking, can this be taken to a nitramine, or maybe just a nitrate salt? It is already strongly alkaline and the warning against mixing with oxidizers is there. Low temps are a must. It has a rather low density so I'm not sure there is any value to it, unless it can form with a lead nitrate salt.

Diethylamine is volatile (eb 55°C) and a strong base full smelling.

It can be made into (CH3-CH2)2N-NO2 but it will be less powerfull than dimethylnitramine. It can be nitrosated easily ((Eth)2N-N=O) and reduced into diethylhydrazine ((Eth)2N-NH2) also a valuable compound.

You might get more pleasure form the nitrate salt or even the perchlorate salt. The best would be the nitroformiate salt of it for OB reasons.

One may consider the making of colorfull complexes with transition metals like Cu(ClO4)2(tetracoordinates) and Ni(ClO4)3 or Ni(C(NO2)3)3 (hexacoordinates).

PHILOU Zrealone - 22-3-2014 at 06:14

polystyene do...so maybe other hydrocarbons do too? dunno

if its not PIB, i think you could use this stuff for some kind of phlegmatising (if you want to^^)...

What do you mean by that ? My english are a little bit poor

[Edited on 19-3-2014 by underground]

He means that if PIB doesn't dissolve into benzine; then maybe something else could be dissolved into benzine like polystyrene and then PS could be used as phlegmatiser...but PS is hard brittle and not elastic/rubber like.

Polystyrene is a polymer and has dus a long molecular lenght but surprisingly it dissolves readily into CH2Cl2, into aceton, into benzene, toluene, and hydrocarbons like benzine.
Styrofoam/Expanded Polystyrene/Frigolithe is chewed by aceton drops just like if it was alien-blood .... very good to scare childrens

or to make a little show.

PHILOU Zrealone - 22-3-2014 at 06:18

Can i prepare HDN with the same way as Urea nitrate ? With HCL, Hexamine and NH4NO3 ?

edit: Also once i made some UN out of urea, HCL and AN, but when i was trying to neutralized it with sodium carbonate, it just disappeared, i guess it just hydrolyzed or react with sodium carbonate , so how can i neutralized it ?

[Edited on 22-3-2014 by underground]

No It won't work as good because in UN the relative unsolibility of UN is taken as an advantage to facilitate separation vs Urea hydrochloride.

HDN is not particularly unsoluble nor is Hexamine dihydrochloride; so the best is stil to use HNO3 and hexamine. Then to evaporate in dry air or to add some ethanol and ether to force cristallisation of the salt.
Avoid heating of HDN it may lead to an explosion if dry heated.

PHILOU Zrealone - 22-3-2014 at 06:37

So dinitrate salts are possible?

Yes, however can we still protonate compounds like trihydroxyguanidine? will it be unstable?

Also, does hydroxyhydrazine exist ? or aminohydroxylamine.

HO-NH-NH2 is an hydrated form of nitrene ...
HO-NH-NH2 --> H2O + H-N=N-H

If it exist at all, I suspect it is very unstable.

Don't trust those kind of links ... the following http://www.chemicalregister.com/Companies/AName/Page293/aidH.htm even does mention of tetrachlorohydrazine, tetrahydroxyhydrazine, nitrohydrazine and nitrosohydrazine ... just as if it could be bought...maybe they postulate it may exist one day and so they anticipate CAS numbers.

To give you an example:
Hydrazine and nitrite ester provides a way to azide compounds (typical butyl nitrite is used or other not too volatile related ester)-This is a known reaction:
H2N-NH2 + O=N-O-R --> H2N-NH-N=O + R-OH (alcohol)
It goes via an intermediary nitrosohydrazine (that is listed in the list of compounds here-up) what rearranges spontaneously into hydrazoic acid via internal dehydration...
H2N-NH-N=O <==> H2N-N=N-OH --> HN3 + H2O
Azothydric acid is usually caught by a base like NaOH to finally get NaN3.

I don't think a chemical company will sell hydrazoic acid 70% in water (what is equivalent to HN3.H2O or to H2N-NH-N=O).

[Edited on 22-3-2014 by PHILOU Zrealone]

underground - 22-3-2014 at 07:34

PHILOU Zrealone, what about this process that i found:

An alternative to using nitric acid in this synthesis is to use a nitrate salt and hydrochloric acid. The yields may be a bit less, but the result is the same. Instead of preparing a hexamine solution, prepare a nitrating solution by dissolving 28 g (0.35 mol) of ammonium nitrate in 80 mL (0.8 mol) of 31.45% hydrochloric acid in a 250-mL beaker. Cool this solution in a salt-ice bath to 0 degrees. Again, it is not necessary to use the specified concentration of hydrochloric acid as long as the proper molar amount is added. Dissolve 14 g (0.1 mol) of methenamine in a minimum amount of water (about 21 mL). Quickly add this solution to the nitrating mix with rapid stirring; a precipitate should soon form. Filter and wash the crystals as above. One could substitute sodium nitrate or potassium nitrate of the same molar mass in place of ammonium nitrate.

[Edited on 22-3-2014 by underground]

DubaiAmateurRocketry - 22-3-2014 at 07:44

So dinitrate salts are possible?

Yes, however can we still protonate compounds like trihydroxyguanidine? will it be unstable?

Also, does hydroxyhydrazine exist ? or aminohydroxylamine.

HO-NH-NH2 is an hydrated form of nitrene ...
HO-NH-NH2 --> H2O + H-N=N-H

If it exist at all, I suspect it is very unstable.
Don't trust those links the following http://www.chemicalregister.com/Companies/AName/Page293/aidH.htm even does mention of tetrachlorohydrazine, tetrahydroxyhydrazine, nitrohydrazine and nitrosohydrazine just as if it could be bought...maybe they postulate it may exist one day and so they anticipate CAS numbers.

Oh right,

I also wanted to ask you about nitrene aka diazene. H-N=N-H

It can be protonated for H-N=NH2+ and I think the nitrate salt may be interesting! Do you have any papers/ reference about diazenium cation?

robart - 22-3-2014 at 11:28

Hi guys.
As you can see I'm the new guy to the forum.
My name is robart and I live in Canada.
My question is what is the best (safest) way to get sodium azide out of some airbags I have? The airbags are out of a 2003 Chevy tracker.
Thanks in advance for your replies.
Robart

Bert - 22-3-2014 at 17:02

This would be a good place to learn about making Sodium azide from common over the counter products, rather than asking for information not really having much to do with learning chemistry.

Airbags are built with the intent NOT to ever come apart. Also most do not contain azide any more, the stuff is similar to cyanide in toxicity and was a liability for auto shops to have around.

I personally know an individual who tried to harvest Sodium azide from several 1990's era inflators back about 12 years ago. He succeeded once and failed twice. On the failed attempts, the inflators went off in his face. He lost hair, got 2nd degree burns and some eye damage the second time- The gas generated is very hot, those airbags are lined with fabric woven from stainless steel wire to stand up to the heat. People who have had their bare faces bounced off a working airbag usually are mildly burned from that contact.

DubaiAmateurRocketry - 29-3-2014 at 14:20

Does tetrahydrazine nitroxylate or tetrahydroxylammonium nitroxylate exist? It would make some good NHO salts.

The nitroxylate anion, although with a 4- charge, should be considered/ used more. Its synthesis is not very hard.

Tetrahydroxylammonium nitroxylate seems promising with a perfect OB. [(NH3OH)4]4+ [(O2N-NO2)]4- or empirically N6H16O8. This compound have an perfect OB at an insane hydrogen % of 7%. If this salt have a density of just 1.0g/cm3, it's hydrogen % will be same as liquid hydrogen.

Dany - 30-3-2014 at 01:47

To my knowledge these compounds don't exist. However, the idea of introducing the nitroxylate group seems terrible. For example, sodium nitroxylate Na₂NO₂ is described as a bright yellow substance. Extremely sensitive to O₂ , NO, CO₂.
sensitive to H₂O; hydrolyzes to N₂O, H₂N₂O₂ and NO. Stable up to 100°C. Decomposes at 130°C, emitting sparks and evolving N₂, see [1] page 515. Na₂NO₂ is produced by the reaction of metallic sodium Na and sodium nitrite NaNO₂.

this shows that the nitroxylate anion is at the edge of stability. The combination of the nitroxylate anion with other energetic moiety is very likely to produce very sensitive and dangerous HEDM.

Reference:

G. BRAUER, Handbook of preparative inorganic chemistry, Vol.1 , 2nd edition.

Dany.

DubaiAmateurRocketry - 30-3-2014 at 01:58

Thanks, I did not find its sensitivity until the referrence.

What about the Hyponitrite 2- anion? Again dihydroxylammonium hyponitrite seems interesting with perfect OB (NH3OH)2(N2O2). The hyponitrite anion seems more stable than the nitroxylate.

Also what do you think about nitrosyl hyponitrite anion? the hydroxylammonium salt will be a isomer of ADN - N4H4O4, however this compound might be denser due to the hydrogen bonds, and maybe more sensitive.

http://pubs.acs.org/doi/abs/10.1021/jp204967h?journalCode=jp...

[Edited on 30-3-2014 by DubaiAmateurRocketry]

Dany - 30-3-2014 at 02:21

Yes, sodium hyponitrite (Na₂N₂O₂) is more stable than sodium nitroxylate. the former is produced from the reaction of sodium nitrate NaNO₃, H₂O and metallic sodium or by the reaction of sodium Na with gaseous NO (see also reference [1] mentioned in the last reply). Dihydroxylammonium hyponitrite don't seem to exist. However, hydroxylammonium hyponitrite may exist. This compound has been mentioned in this reference.

Dany.

[Edited on 30-3-2014 by Dany]

Potassium Dichromate/Aluminum Flash Powder

Zyklon-A - 30-3-2014 at 09:42

Is the equation for said flash powder: 4 Al + K₂Cr₂O₇ → K₂O + 2 Al₂O₃ + 2 Cr? Or does the Cr not get reduced all the way to elemental state?
Of course either reaction is possible, but with is more energetic?
I tried the first reaction but saw a green residue on the test site. Which implies at least some Chromium(III) oxide.

Bert - 30-3-2014 at 10:06

Here is the decomposition formula:

4 K₂Cr₂O₇ --> 4 K₂CrO₄ + 2 Cr₂O₃ + 3 O₂

A good source for such information is:

Takeo Shimizu

Fireworks: The Art, Science & Technique

Please remember that hexavalent chrome is some seriously BAD stuff-

If you want flash, avoid the chromates. If you want to coat Magnesium to prevent degradation in a pyrotechnic mixture, chromates are useful...

Quote:

Time to post this - yet again.....

The Wrong Chemical -- In The Wrong Place!!
Donald J Haarmann is The WiZ
Originally published in The American Fireworks News

Potassium dichromate K2Cr2O7 (potassium bichromate, red potassium
chromate). Familiar to most pyros because of its bright orange-red color. Has
many uses:

"Dichromate" magnesium against chemical attack.

Added to compositions containing highly reactive zinc, e.g.,

Weingarts Electric Spreader Star

Potassium dichromate 15 parts
Zinc dust 72
Potassium chlorate 15
Granulate charcoal 12
Dextrin 2

Increase burning rate reaction of: Perchlorates:Re: Dichromate....safety concerns over-rated??

From: "donald haarmann" <donald-haarmann@xxxxxxxxxxxxxxxx>
Date: Tue, 06 Feb 2007 22:26:15 GMT
"mikes2653" <mikes2653@xxxxxxxxxx>|

[snip]

| Still, it is remarkable how much exposure to many toxic substances is
| necessary before even minor symptoms are noted. The healthy human body
| is much more robust than many people believe. Excessive worry about
| environmental toxicity seems to me a species of hypochondria.

Dave Blesers Red Strobe

Ammonium percolate 50%
Potassium dichromate +5
Magnesium 25
Strontium sulphate 25

Shimizus' Burst Charge #44

Potassium dichromate 5%
Potassium perchlorate 70
Hemp coal 30
Rice starch 2+

Takeo Shimizu reports the burning rate of a 75/25 K perchlorate/hemp coal
increased by 55% when 4-5% potassium dichromate was added.

In Orange (toxic) smoke (Ellern #133)

Potassium dichromate 35%
Magnesium 15
Lead dioxide 50

It is not, however, used as an oxidizing agent despite an attracting 38% oxygen
content. he decomposition reaction as given by Takeo Shimizu shows why-

4 K2Cr2O7 --> 4 K2CrO4 + 2 Cr2O3 + 3 O2

A little quick math reveals that - 1176 grams of potassium dichromate yield a
miserly 48 grams of oxygen! (4% of starting weight!) Thus potassium dichromate
is a very weak pyrotechnic) oxidizer. Shimizu also notes; It is difficult to ignite or
to explode a mixture of potassium dichromate and red phosphors or sulphur even
by impact between iron surfaces.

Sadly the pleasing orange color hides a less then pleasant personality. While
classified by he NFPA a Zero for Fire hazard and Reactivity (Will not burn. -
Normally stable. Not reactive with water). It rates a Three for Health (Can cause
serious injury despite medical treatment.) Quote the Merk Index: Human Toxicity:
Internal a corrosive poison. Industrial contact may result in ulceration of hands,
destruction of mucous membranes and perforation of nasal septum. Not a
ingredient a pyro would handled in a careless manner! Non pyros are another
matter.

Civilian uses are as many as they are pedestrian: Tanning, dyeing, painting,
decorating porcelain, photolithograpy, staining wood, bleaching palm oil, wax,
and sponges, in dry cells as a depolarizer.

Then there is South Africa -- Where a third to two-thirds of blacks have been
estimate to receive frequent purgative enemas consisting of plant extracts though
truncated cow horn and hollow reeds administered by traditional healers. These
methods with increasing urbanization are being replaced by domestic and
industrial chemicals given with rubber tubing and syringe. Indeed among the
black population in Cape Town, tribal healers have been using potassium
dichromate in purgative enemas! A bad case of the wrong chemical in the wrong
place!! Even infants may receive 50 enemas a year.(The herbal version, not the
hexavalent chromium-tissue binding, don't try this at home kids, colon/kidney
destroying, dichromate version.)

All this probable proves something. I'll leave it to the reader to supply their own
comments.

Dunnn LP, et al. Colonic complications after toxic tribal enemas. British Journal
of Surgery, 1991; 78: 545-48. Abstracted in The Lancet July 20, 1991

--
donald j haarmann
------------------------------------
What passes for woman's intuition is
often nothing more than man's transparency.
George Jean Nathan

[Edited on 30-3-2014 by Bert]

DubaiAmateurRocketry - 31-3-2014 at 14:15

Does detonation wave travel faster/slower in different materials ?

Bert - 31-3-2014 at 14:47

Why do you think so much time is spent working towards higher VOD materials and highest density of plasticized, cast or pressed charges?

Have you encountered the concept of explosive lenses and wave shaping, particularly in regard to implosion type fission weapons?

Explosive wave shaping technology DEPENDS on this-

[Edited on 31-3-2014 by Bert]

DubaiAmateurRocketry - 31-3-2014 at 15:19

I have not studied about weapons or shapes/types of charges or the physics of detonation etc. My friend asked me if sound travel faster in solids, eg metal, than air, does detonation wave? I think not, but I could be wrong, so im here looking for an answer.

roXefeller - 31-3-2014 at 15:35

Sonic speed is a function of incompressibility. Sound travels better underwater than air because air compresses. Likewise solids, which have similar compressibilities.

Zyklon-A - 31-3-2014 at 16:03

Ok, thanks Bert.

Storage of Formaldehyde

BobD1001 - 31-3-2014 at 19:03

I purchased a quantity of Formaldehyde from Elemental about 6 months ago. I received it in an opaque HDPE container, and it has since been stored along other similar liquids within a storage cabinet in my semi-temp controlled garage. The minimum temperature this cabinet will see in the winter is approximately 55* F. Upon taking inventory today, I noticed a thick layer of white residue on the bottom of the bottle. At first I thought the bottle was losing its integrity and becoming porous, but I quickly realized that it was in fact a white solid at the bottom of the container. A quick search reveals that this is most likely Paraformaldehyde forming due to the colder temperatures. My question is, upon warmer temperatures will this redissolve to reform the formaldehyde solution, or will it require more elevated temperatures. Here is a link to a picture of the bottle and its bottom layer. Link

Dany - 1-4-2014 at 06:49

Does detonation wave travel faster/slower in different materials ?

First the question is not clear at all. If your question is about detonation wave in inert materials, well in this case we don't call the wave a detonation wave but a shock wave. A detonation wave is a shock wave supported by chemical energy like the one encountered in a detonating chemical explosive (the explosive can be solid, liquid or a gas). A detonation wave is a shock wave followed by a short, attached reaction zone (according to the Zeldovich-von Neumann-Doring theory known as ZND theory). The reaction zone terminate at the CJ plane or sonic locus where D_cj= c+u_p ( c= sound speed in the gas at the CJ state and u_p is the particle velocity). behind the CJ plane the gaseous detonation products begin their expansion along the isentrope (the exapnsion creats a rarefaction wave or Taylor wave). A shock wave in an inert materials decay with time because it is not supported by a chemical enegy. A shock wave is always faster than the sound speed in the media where it propagate. sound speed in solids is grater than liquid and finally gases. For example the sound speed in metallic beryllium is approx. 13 km/s, so a shock wave travelling in beryllium should be grater than 13 km/s if one want to call it shock wave. Any shock wave in any inert media will decay with time/distance as it travel inside the material and finally the shock wave will decay to become a sound wave.

Dany.

[Edited on 1-4-2014 by Dany]

TheAlchemistPirate - 1-4-2014 at 13:10

Hello I am making HNO3 by distilling H2SO4 and KNO3(no vacuum) and I have no idea what the best temperature for making it would be. I am going to insulate the apparatus with aluminum foil so I can do it at a lower temperature( to prevent decomposition). Also, Im not sure how to store it. I have several new amber glass bottles from homesciencetools.com and a garage to store them in that doesn't usually get any hotter than 70 degrees F. Im pretty sure this nitric acid will be above 90% concentration.

DubaiAmateurRocketry - 1-4-2014 at 13:55

To store your acid, you can read replies on this thread. All you need is a new fridge for your acids.

http://www.sciencemadness.org/talk/viewthread.php?tid=29837

There are also tips for distillation of nitric acid on the forum.

DubaiAmateurRocketry - 4-4-2014 at 15:49

Can this be nitrated?
http://en.wikipedia.org/wiki/Dihydroxyacetone

And, can someone help me find synthesis of dinitroethane? or trinitroglycerin? Just interested to see the impact sensitivity and other properties of these liquid EM since the ONO2 group give much more impact sensitivity than NO2 group. I have searched on spinger and WOL, but not much related contents are shown. Thanks.

copperastic - 4-4-2014 at 15:58

Hi, I was trying to make an iron II sulfate crystal and when i dissolved the iron II sulfate in water the turned yellow. Is it supposed to become yellow?
Thanks

Zyklon-A - 4-4-2014 at 16:10

This thread is specifically for EM. And the answer is yes BTW.

[Edited on 5-4-2014 by Zyklonb]

copperastic - 4-4-2014 at 17:00

Oh ok zyklonb. Sorry i thought this was the all round one.

Mr.Tzzzz - 4-4-2014 at 18:02

What would it happen if someone surrounds a sphere of metal with plastic (or any other) explosive and detonates it? For example would the metal be compressed to a new crystalline state with a higher density?

Bert - 4-4-2014 at 19:17

Well, if the explosives were properly shaped and carefully detonated in a fashion that produced a converging spherical shock wave- it MIGHT just work- But this is just blue sky theory, right?

[Edited on 5-4-2014 by Bert]

TheAlchemistPirate - 4-4-2014 at 19:46

Isn't this an atomic bomb?! Or am I just an idiot?

Bert - 4-4-2014 at 19:53

Well, click on the link & see!

Dany - 4-4-2014 at 22:18

Quote: Originally posted by Mr.Tzzzz

What would it happen if someone surrounds a sphere of metal with plastic (or any other) explosive and detonates it? For example would the metal be compressed to a new crystalline state with a higher density?

Since an implosion is a convergent shock/detonation wave, high pressure (in the order of megabars) can be encountered. Yes, a convergent shock wave will compress materials to a higher density. The reason to do an implosion in an atomic bomb is to compress the plutonium pit to a higher density (or smaller volume) so as to reach the supercritical mass necessary for the beginning of the explosive chain reaction (after neutron initiation, of course). You don't need an implosion to obtain a phase transition or higher density in metals. For example, consider a steel cylinder loaded with high explosive. When the explosive is detonated the cylinder wall will be accelerated. Experimentally, it has been found [1] that the initial wall velocity is smaller than theoretical one. under shock loading, the steel will undergo a phase transition from the α phase to the ε phase. The process of phase transition absorb energy and thus decrease the cylinder wall velocity by a factor of 1.9

Reference:

[1]Joseph E. BACKOFEN and Chris A. WEICKERT, OBTAINING THE GURNEY ENERGY CONSTANT FOR A TWO-STEP PROPULSION MODEL, Shock Compression of Condensed Matter - 2001: 12th APS Topical Conference. AIP Conference Proceedings, Volume 620, pp. 958-961 (2002).

Dany.

DubaiAmateurRocketry - 5-4-2014 at 01:42

Dany, up to megabars ?! Can we synthesize diamonds from explosives since the pressure needed is only kilobars? If as you said, implosion pressure of megabars, it could probably make diamond if you put carbon in the middle?
__________________________________________________________________________________________________

Can this be nitrated?
http://en.wikipedia.org/wiki/Dihydroxyacetone

And, can someone help me find synthesis of dinitroethane? or trinitroglycerin? Just interested to see the impact sensitivity and other properties of these liquid EM since the ONO2 group give much more impact sensitivity than NO2 group. I have searched on spinger and WOL, but not much related contents are shown. Thanks.

Dany - 5-4-2014 at 02:03

Dany, up to megabars ?! Can we synthesize diamonds from explosives since the pressure needed is only kilobars? If as you said, implosion pressure of megabars, it could probably make diamond if you put carbon in the middle?
__________________________________________________________________________________________________

Can this be nitrated?
http://en.wikipedia.org/wiki/Dihydroxyacetone

And, can someone help me find synthesis of dinitroethane? or trinitroglycerin? Just interested to see the impact sensitivity and other properties of these liquid EM since the ONO2 group give much more impact sensitivity than NO2 group. I have searched on spinger and WOL, but not much related contents are shown. Thanks.

You don't need a special explosive geometry to produce diamond. When an oxygen deficient explosive detonate part of the carbon generated as a detonation product is converted to nanodiamond. This was a major question in the detonation science. Charles MADER in his book Numerical modeling of explosive and propellant, answered this question. The phase of the carbon formed (graphite or diamond) depend on the initial density of the explosive. For example TNT give graphite in the detonation products up to d= 1.55 g/cm³. Above this density the carbon formed is diamond. The carbon phase change from graphite to diamond is clearly visible on the detonation velocity vs density plot. @ 1.55 g/cm³, a change in the slop of D(ρ ) is visible. the increase of detonation velocity with density above 1.55 g/cm³ is slower (but always linear) than the increase of D_cj under 1.55 g/cm³. See the book of Charles MADER for more information. A complete book is devoted to the production of nanodiamond via explosive charge detonation, see:

Detonation Nanodiamonds: Science and Applications

Dany.

DubaiAmateurRocketry - 5-4-2014 at 02:15

Oh thanks, but not as what I was expecting. Is it possible to make a piece of diamond by putting a piece of graphite in the middle of a spherical charge?

Bert - 5-4-2014 at 04:51

Oh thanks, but not as what I was expecting. Is it possible to make a piece of diamond by putting a piece of graphite in the middle of a spherical charge?

The first publication of this idea I've seen is over a century old. There's even a chapter about someone TRYING in Hudson Maxim'a "Dynamite Stories"

Although the pressure conditions are rather more than sufficient, collecting the diamond dust after is a bit of a challenge- And if you can work out how to apply that amount of force without "distributing" your product as VERY fine dust around the neighborhood... DeBeers will put a contract on your life.

[Edited on 5-4-2014 by Bert]

DubaiAmateurRocketry - 5-4-2014 at 06:35

''Stories'' Is it real? Any ways,

Does any one know what are the ABL,TC impact sensitivity measurements? It is stated in the only table of this patent,
https://docs.google.com/viewer?url=patentimages.storage.goog...

DubaiAmateurRocketry - 7-4-2014 at 03:17

10900 m/s? Is this even real? Tetranitroaminoethane's tetrasodium salt have a calculated detonation velocity of 10.9km/s at its crystal density! and it is reported to have a VoD of 9570 at only 1.84g/cm3 I am trying to find for information if this is true. The tetraammonium, hydrazine, hydroxylammonium salt of this also seems interesting.

I frist saw this russian paper.
Download link(press the pdf) = http://yadda.icm.edu.pl/yadda/element/bwmeta1.element.baztec...

I then searched for the english name and this paper poped up. This is a review, the tetrasodium salt of tetranitroaminoethane is on the last page.

Attachment: A brief review of publications of Russian scientists on energetic materials.rar (1.5MB)
This file has been downloaded 725 times

Dornier 335A - 7-4-2014 at 04:54

Regarding the production of diamonds: Mythbusters did it!
Graphite powder was pressed in a steel pipe which was welded shut in both ends. It was then placed in the middle of a large ANFO charge. But the result was just a tiny quantity of diamond powder. Here is a quick video of the process: https://www.youtube.com/watch?v=0mWQUvxcANE

DubaiAmateurRocketry - 7-4-2014 at 05:20

ANFO is weak. it generates around only 35 kbar(Diamond need at least 45 kbar) while TNT can create over 200 kilobars, RDX near 400, and HMX, Cl-20 almost 10 times the pressure needed to create diamonds. So maybe they should try TNT with that

underground - 7-4-2014 at 07:16

Quote: Originally posted by Dornier 335A

Regarding the production of diamonds: Mythbusters did it!
Graphite powder was pressed in a steel pipe which was welded shut in both ends. It was then placed in the middle of a large ANFO charge. But the result was just a tiny quantity of diamond powder. Here is a quick video of the process: https://www.youtube.com/watch?v=0mWQUvxcANE

I do not think so that if they were successfully made diamonds, they would say that.

Dornier 335A - 7-4-2014 at 07:24

So you suggest they are lying? The idea is a century old as Bert said. Certainly not a secret.

underground - 7-4-2014 at 08:20

Quote: Originally posted by Dornier 335A

So you suggest they are lying? The idea is a century old as Bert said. Certainly not a secret.

Not lying, but i believe that it can be done, but surely it is going to need a lot of practice

Bert - 7-4-2014 at 08:36

Regarding "Myth Busters": This is entertainment, not scientific research.

It CAN be fun to watch sometimes, but the more you know, the more you see them mess up.

They allways jump from testing hypothesis to "LET'S BLOW SOMETHING UP!" to a hasty, dumbed down conclusion, instead of collecting a meaningful amount of data and analyzing it properly!

[Edited on 7-4-2014 by Bert]

underground - 7-4-2014 at 09:14

Quote: Originally posted by Bert

Regarding "Myth Busters": This is entertainment, not scientific research.

It CAN be fun to watch sometimes, but the more you know, the more you see them mess up.

They allways jump from testing hypothesis to "LET'S BLOW SOMETHING UP!" to a hasty, dumbed down conclusion, instead of collecting a meaningful amount of data and analyzing it properly!

[Edited on 7-4-2014 by Bert]

Yea that is true, they just do whatever they must to do to have as much viewing as possible, that is all, they do not care about nothing more.

[Edited on 7-4-2014 by underground]

Dany - 7-4-2014 at 09:52

The experiment is serious. For those who don't know the man with "Mythbusters" team, his name is Dr. Van ROMERO:

He is a known detonation physicist, he done a lot of research on detonation of high explosives. He was the vice president of new mexico Institute of Mining and Technology.

Dany.

underground - 7-4-2014 at 10:30

So why do they use ANFO and not somethink like TNT?

Dany - 7-4-2014 at 12:08

For all the hasty members (moderator included) who directly replied to Dornier post by saying that the experiment is not serious and not scientific...Well, ladies i'm affraid to tell you that the experiment is very scientific and serious...As i posted above, Dr. Van ROMERO who conducted the experiment is a known detonation physicist and he know exactly what is he doing. First, lets go back to the video posted by Dornier . One might ask, why they used a coaxial metal tube for conducting the experiment? as one can see at the beginning of the video, Dr. Van ROMERO is holding a coaxial metal tube, then they put the carbon in the inner tube. The reason is described in two US patent .

US3823044 A: Increasing the detonation pressure of ammonium nitrate/fuel oil compositions

&

US3667911 A: Method of treating solids with high dynamic pressure

Quoted from US3823044 A:

"In the shock synthesis of diamond from non-diamond carbon by the proces described in US. Pat. 3,667,911, issued June 6, 1972, to A. S. Balchan and G. R. Cowan, a spanning or transverse shock wave is introduced into non-diamond carbon positioned in a metal container cylinder, by the progressive collision of the container cylinder and a surrounding coaxial metal driver cylinder, which is propelled by a detonation, the shock wave moving axially through the non-diamond carbon at a velocity equal to the collision velocity, or the detonation velocity of the explosive surrounding the driver cylinder. The detonation velocity preferably i in the range of about from 3000 to 6000 meters per second, most preferably about from 4000 to 5000 meters per second. At the same time, to achieve optimum yields, the detonation pressure of the explosive needs to be sufficiently high to accelerate the driver cylinder over the short distance between colliding cylinders at a sufliciently high velocity to produce the cylinder-spanning shock wave"

in the same patent (US3823044 A) they added:

"Although the desirability of employing ANFO mixtures in a process of this kind is great when factors such as safety, economy, and convenience are considered, the ANFO mixtures heretofore known which detonated in the required velocity range did not develop a sutficiently high detonation pressure to afford optimum yields in the process. Heretofore, higher detonation pressure could be achieved only at the expense of increasing the detonation velocity to a value outside the required range."

As normal ANFO cannot generate the required pressure for converting carbon to diamond they made a special ANFO mixture for increasing the pressure of detonation. This ANFO mixture is suitable for diamond synthesis via the coaxial metal tube described above. Also from US3823044 A:

"The ANFO detonating composition of this invention, which comprises AN in the size blends specified above as well as the previously specified amount of densifying agent, has a bulk density of at least about 1.00 gram per cubic centimeter, and an ideal detonation pressure, calculated for a composition containing 10% densifier, ranging from about 35 kilobars at a detonation velocity of 4000 m./sec. to about 60 kilobars at a detonation velocity of 5000 m./sec., these pressures and velocities being suitable for the diamond synthesis process described in US. Pat. 3,667,911, the disclosure of which patent is incorporated herein by reference"

After all this explanation, members should be more scientific when they criticize experiment done by an expert like Dr.Van ROMERO. Learn to read and search before replying randomly.

Dany.

Bert - 7-4-2014 at 12:33

Yay! Documentation!! Referances AND pertinent quotes from same!!! Patent information!!!!

This is the best documented thing posted here in a while-

Dany, you are not like the rest... You make me happy.

Not like some of the others, who make tiny plastic baby Jesus cry, and kill many kittens.

I still think Jaime and Adam are fucking entertainers not scientists, and the show is "infotainment" at best- But their guest was legit, it would appear.

[Edited on 7-4-2014 by Bert]

DubaiAmateurRocketry - 7-4-2014 at 13:40

Do you think the tetrasodium salt of tetranitroaminoethane actually have a detonation velocity of 10.9km/s ? This is so much higher than ONC. around 30% by weight of this explosive produces Na2O, and it will react with CO2 to produce sodium carbonate, so there are only few gas moles left, how is 10.9km/s possible?

DubaiAmateurRocketry - 9-4-2014 at 04:59

Has anyone tried synthesis of hydroxylazide? (N=N=N-O-H) Hydroxylazide must be a strong acid and will give the anion azidooxide -1.

It may be synthesized from reduction of Nitrylazide(N=N=N-NO2) or Nitrosylazide (N=N=N-N=O)

Or maybe It can be synthesized from H-O-Cl + NaN3 > H-O-N=N=N + NaCl?

PHILOU Zrealone - 14-4-2014 at 02:14

Has anyone tried synthesis of hydroxylazide? (N=N=N-O-H) Hydroxylazide must be a strong acid and will give the anion azidooxide -1.

It may be synthesized from reduction of Nitrylazide(N=N=N-NO2) or Nitrosylazide (N=N=N-N=O)

Or maybe It can be synthesized from H-O-Cl + NaN3 > H-O-N=N=N + NaCl?

HOCl splits like HO(-) and Cl(+); NaN3 splits like Na(+) and N3(-)... so how would you join Na(+) and Cl(+) or HO(-) and N3(-)? You should get tiny amount of Cl-N3 and NaOH and finally NaOCl + HN3.

Dornier 335A - 14-4-2014 at 02:40

Yes, hypochlorous acid and sodium azide solutions react to form extremely explosive chlorine azide gas.
Woelen has done it: http://www.sciencemadness.org/talk/viewthread.php?tid=10581

FeRe - 14-4-2014 at 09:20

For example Tatp is a static sensitive explosives. For its is able to go off through static discharge, a human is needed ?(can it just go off through a human who has enough static electricity) I mean can it go off itself through static discharge when it is in a tube.

Dany - 14-4-2014 at 10:50

FeRe, you are asking this question because you synthesized TATP and you are afraid that the tube will go off by itself or between your hand...wright? a small advice boy, stay away from peroxide and sensitive explosive, your parent need you and you need to keep your hand safe...

Dany.

DubaiAmateurRocketry - 14-4-2014 at 11:53

HOCl splits like HO(-) and Cl(+); NaN3 splits like Na(+) and N3(-)... so how would you join Na(+) and Cl(+) or HO(-) and N3(-)? You should get tiny amount of Cl-N3 and NaOH and finally NaOCl + HN3.

Thanks, I realized it too after I commented.

What do you think will happen upon NO2+ nitration on hydroxylamine? Will it yeild N-hydroxydinitramide? I final product seems stable, I am worried about one intermediate compound - N-hydroxynitramide.

FeRe - 14-4-2014 at 11:57

Quote: Originally posted by Dany

FeRe, you are asking this question because you synthesized TATP and you are afraid that the tube will go off by itself or between your hand...wright? a small advice boy, stay away from peroxide and sensitive explosive, your parent need you and you need to keep your hand safe...

Dany.

No I didn't I just wanted to explain myself with this example. You can replace tatp with lead azide or other static sensitive primaries. I know peroxides are dangerous. Someone can help me in this question ?

[Edited on 14-4-2014 by FeRe]

PHILOU Zrealone - 15-4-2014 at 12:10

Thanks, I did not find its sensitivity until the referrence.

What about the Hyponitrite 2- anion? Again dihydroxylammonium hyponitrite seems interesting with perfect OB (NH3OH)2(N2O2). The hyponitrite anion seems more stable than the nitroxylate.

Also what do you think about nitrosyl hyponitrite anion? the hydroxylammonium salt will be a isomer of ADN - N4H4O4, however this compound might be denser due to the hydrogen bonds, and maybe more sensitive.

http://pubs.acs.org/doi/abs/10.1021/jp204967h?journalCode=jp...

[Edited on 30-3-2014 by DubaiAmateurRocketry]

The making of hydrazinium or hydroxylamonium exotic oxonitrogen salts will be ruled by the oxydoredox potential of the anion vs the cation...disproportionation reaction may result with destruction of both cation and anion.
Hydroxylamonium nitrite or hydrazinium nitrite (precursor of HN3) are good examples, just as ammonium nitrite which exists but is unstable and turns into N2 and H2O.
NH4NO2 --> N2 + 2H2O
So the existance of an alkaline salt (Na/Li/K) is not per se meaning that an NH4, NH3OH or N2H5 salt could be done.

Not strictly related to nitroxylate or to hyponitrite... on the organic side there exist cupferron made by reaction of aromatic hydroxylamine with NH3 and nitrite ester...
Ar-NHOH + R-O-N=O + NH3 --> Ar-N(ONH4)-N=O + R-OH
This group of compounds has not been very much studied as energetic group.

Edited:
Just imagine that you have 1,3,5-trichloro-2,4,6-trinitrobenzene... the chlorine atoms are activated for substitution:
-reaction with water provides trinitrophloroglucidol
-reaction with NaN3 provides trinitrotriazidobenzene
-reaction with NH3 provides trinitrotriaminobenzene
-reaction with H2N-NH2 provides trinitrotrihydrazinobenzene

So maybe that reaction with hydroxylamine will provide a way to trinitrotrihydroxylaminobenzene (C6(NO2)3(NHOH)3)
--> Has someone info on that compound?
(see THATNB.jpg file joined)
The later could then be reacted with ammonia and a nitrite ester to provide 1,3,5-trinitro-2,4,6-(N,N',N"-trinitroso-trihydroxylamino)-benzene triammonium salt (C6(-NO2)3(-N(ONH4)-N=O)3 or C6H12N12O12).

Maybe this triammonium salt could precipitate valuable primaries with heavy metals, or with alkalies (Li, Na, K, ...).(see TNHATNB.JPG file joined where M = heavy metal like Ag, Hg, ...)
Maybe the triammonium salt could exchange ammonium for hydrazinium (C6(-NO2)3(-N(ON2H5)-N=O)3 or C6H15N15O12) or for hydroxylamonium (C6(-NO2)3(-N(ONH3OH)-N=O)3 or or C6H12N12O15)
(see TNHATNB.JPG file joined where M = NH3OH or NH3-NH2)....

[Edited on 16-4-2014 by PHILOU Zrealone]

PHILOU Zrealone - 15-4-2014 at 12:18

Quote: Originally posted by BobD1001

I purchased a quantity of Formaldehyde from Elemental about 6 months ago. I received it in an opaque HDPE container, and it has since been stored along other similar liquids within a storage cabinet in my semi-temp controlled garage. The minimum temperature this cabinet will see in the winter is approximately 55* F. Upon taking inventory today, I noticed a thick layer of white residue on the bottom of the bottle. At first I thought the bottle was losing its integrity and becoming porous, but I quickly realized that it was in fact a white solid at the bottom of the container. A quick search reveals that this is most likely Paraformaldehyde forming due to the colder temperatures. My question is, upon warmer temperatures will this redissolve to reform the formaldehyde solution, or will it require more elevated temperatures. Here is a link to a picture of the bottle and its bottom layer. Link

No paraformaldehyde won't redissolve by temperature increase.

PHILOU Zrealone - 15-4-2014 at 12:34

Can this be nitrated?
http://en.wikipedia.org/wiki/Dihydroxyacetone

And, can someone help me find synthesis of dinitroethane? or trinitroglycerin? Just interested to see the impact sensitivity and other properties of these liquid EM since the ONO2 group give much more impact sensitivity than NO2 group. I have searched on spinger and WOL, but not much related contents are shown. Thanks.

Dihydroxyaceton is not nitratable directly it is a strong reductor because in equilibrium with 2,3-dihydroxy-propanal...it has the ability to polymerize into dark polyphenolic stuffs (see its use as artificial suntanner).
Just as aceton (propanone) is unstable towards HNO3, so would DHA.
It could be nitrated by a derivated way via war gas lacrymator dichloroaceton and reaction with silver nitrate saturated solution...
Cl-CH2-CO-CH2-Cl + 2 AgNO3 --> O2N-O-CH2-CO-CH2-O-NO2 + 2 AgCl (s)
The molecule might suffer hydrolysis behavior (and unstability-explosive runaway) because of the cetonic group and enol-ceton equilibrium. This effect is seen in nitrosuggars (nitrate esters of suggars).

Dinitroethane can be 1,1 (geminal) or 1,2 (viccinal)... synthesis is pretty easy using the conventional synthesis pathways of nitroalcanes. I suppose you want the 1,2-DNE.
R-Br or R-I + AgNO2 (or LiNO2/NaNO2/KNO2 in DMF).

Trinitroglycerin is a confusing name for nitroglycerin; I suppose you meant 1,2,3-trinitropropane.

There is indeed very little info on those nitroalcanes of the family H-(CHNO2)n-H.

Edited:
Stil they are of much interest because surprisingly at a certain point of n, the linear polynitroalcanes (with one NO2 per carbon unit (cf nitromethane, 1,2-dinitroethane, 1,2,3-trinitropropane) surpasses in density equivalent lenght polymeric H-(CHONO2)n-H (with one ONO2 per carbon unit (cf methyl nitrate, EGDN, NG, ETN, XPN, MHN) by much; and polymeric H-(CHNHNO2)n-H (with one nitramino per carbon unit (cf methylnitramine, EDNA, propantrinitramine)) by a little.
So in theory it can lead to the highest density CHNO explosives this not counting with the fact each CH-NO2 unit:
-can react with formaldehyde to make (-C(CH2OH)(NO2)-)n which can be nitrated to make perfect OB polymer related to nitro-isobutyl-trinitrate ester and 2,3-dinitro-2,3-dimethylol-1,4-butanediol tetranitrate ester (O2NOCH2-(-C(CH2ON2)(-NO2)-)n-CH2ONO2)
-can react with nitrous acid to introduce a nitroso group in the place of the hydrogen increasing by much the density.
One should not pernitrosate the compound in a way to get perfect OB and some H bondings...1 nitroso per 3 unit would be optimum.
-(CHNO2-CHNO2-CHNO2-)n + HNO2 --> (-C(NO)NO2-CHNO2-CHNO2-)n + H2O
Pernitrosated compound would be denser but would be overoxygenated and would require some extra dense fuel to burn.

[Edited on 16-4-2014 by PHILOU Zrealone]

PHILOU Zrealone - 16-4-2014 at 08:41

10900 m/s? Is this even real? Tetranitroaminoethane's tetrasodium salt have a calculated detonation velocity of 10.9km/s at its crystal density! and it is reported to have a VoD of 9570 at only 1.84g/cm3 I am trying to find for information if this is true. The tetraammonium, hydrazine, hydroxylammonium salt of this also seems interesting.

I frist saw this russian paper.
Download link(press the pdf) = http://yadda.icm.edu.pl/yadda/element/bwmeta1.element.baztec...

I then searched for the english name and this paper poped up. This is a review, the tetrasodium salt of tetranitroaminoethane is on the last page.

quoted from a post slightly below:
Do you think the tetrasodium salt of tetranitroaminoethane actually have a detonation velocity of 10.9km/s ? This is so much higher than ONC. around 30% by weight of this explosive produces Na2O, and it will react with CO2 to produce sodium carbonate, so there are only few gas moles left, how is 10.9km/s possible?

The name is confusing tetranitroaminoethane should more be like ethynyltetranitramide, tetranitraminoethane or 1,1,2,2-tetra-nitramino-ethane (2(O2N-NH-)2CH-CH(-NH-NO2)2).

It is kind of a dimer of methylenedinitramide (CH2(-NH-NO2)2) and as such it will display higher detonic performances data (d, VOD, brisance).

True that 9570 m/s at a density of 1,84 g/ccm seems a little too high, but maybe does the value come from calculations what might account for overestimation.

Tetrasodium salt and other ammonium, hydazinium or hydroxylamonium salts will be energetic, no doubt...

But for the tetrasodium salt it is hard to tell the VOD because it is not a CHNO explosive...the presence of the Na will increase the density by a lot but the sodium will be a dead weight in the end of the explosion process (as you said Na will take some oxygen and maybe catch some CO2 under cooling and equilibration- this requires time and detonation is out of equilibrium reaction)...
However during the detonation process itself at the temperature of explosion sodium will behave like an ionised gas (a plasma) and will for sure contribute to the shockwave (just like water what also displays explosive behaviour over 2000°C by splitting back to its elements H2 and 1/2 O2). Sodium is linked to nitrogen and so during detonation maybe some metalic Na gas is produced (this happens with NaN3) so the heat of burning of Na contributes to the temperature of explosion but less so than the original hydrogen atom.

(CH(NNaNO2)2)2 --> 2 CO2 + 2 Na2O +H2O + 4 N2 + 1/2 O2

So in the balance you have density increase vs heat of explosion loss.

As a side note in the second document at the end...the reaction is a nuclear reaction because the russians or the chineses reacted the tetranitramino-ethane with calcium hydroxyde (Ca(OH)2) and they got the tetrasodium salt... so they turned calcium into sodium.

Even if there is a translation error, chemistry remains chemistry.

TheAlchemistPirate - 16-4-2014 at 10:51

Hey guys I have lately been having troubles with distilling nitric acid, and was wondering if an oil bath is what I need. Basically, I have tried synthesizing it by heating H2SO4 and KNO3 at 100 degrees C on my hot plate, but every time I do it the acid starts condensing on the sides of the boiling flask(round-bottomed). I also noticed that when I moved the flask to one of the corners it started pressurizing, and almost shattered the stopper that popped out because of it.
My theory is that Im heating it too much in order to make up for the lack of ambient heat around the flask. Anyways, I wanted to know how I can fix this problem. If I were to place a stainless steel bucket filled with mineral oil on the hot plate would that work? Or will I have to spend another 200$ on a heating mantel? I haven't seen anywhere on google or youtube where anyone has done this.

DubaiAmateurRocketry - 17-4-2014 at 02:40

Thank you PHILOU Zrealone for anwsering my question in this detail. Interesting, a polymer with positive oxygen balance would be extremely interesting.

http://www.sciencemadness.org/talk/viewthread.php?tid=27095&...

In this post last reply, I uploaded a file on easily nitrating HTPB. Also for dinitroethane, is the carbon too acidic for use in propellant additives?

Also, what do you think about the nitronium cation nitration on HONH2? Will it yeild HON(NO2)2 ?

Davin - 18-4-2014 at 22:03

Has anyone tried synthesis of hydroxylazide? (N=N=N-O-H) Hydroxylazide must be a strong acid and will give the anion azidooxide -1.

Generally, the best reagent for the addition of an oxygen atom to a nitrogenous system is hypofluorous acid, HOF, prepared by the bubbling of a 10% F₂ in N₂ mixture through H₂O/MeCN at -10 ^oC. Reaction with sodium azide did not seem to work, but I only tried a few times.

Would be amazing to undergo a cycloaddition with a nitrile giving a tetrazole-1-oxide, but alas it does not seem to exist.

DubaiAmateurRocketry - 18-4-2014 at 23:14

Quote: Originally posted by Davin