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VladimirLem - 8-10-2013 at 09:07

Hi there

I think this forum needs some thread like this...it really sucks always to start new threads or post in (old) threads, which are often only a bit related to the question...

well so i start and hoping no mod/admin dislike my idea :(

i allways read from qeople using hexamine dinitrate at the RDX symnthesis but i've never seen a more hygroscopical comound like this and even a friend who had alot of expierience at chemistry is desperat at not getting HDN dry...anyone have an (efficient) idea how to get that dry?




bfesser - 8-10-2013 at 09:10

<strong><a href="viewthread.php?tid=25055">The Short Questions Thread (4)</a></strong>

I see no harm in an EM-specific short question thread.

DubaiAmateurRocketry - 27-12-2013 at 17:42

Actually, I want to point out that a short question thread especially for EM is very favorable because one can receive much better quality/useful reply/anwers when people who are into energetic materials ask and answer in the same place.


DubaiAmateurRocketry - 27-12-2013 at 17:50

Okay let me start the first question here, sorry for double posting.

When I was almost purchasing Hydroxylammonium salt where I would ion exchange for hydroxylammonium perchlorate, a member, Anders Hoveland pointed out it has an impact sensitivity of 2J !!!! Impossible I thought, since its patented so much and synthesized on such large batches in their patents, so I wonder if his claim is true. I have a hard time finding its sensitivity. I guess its so insensitive it does not need such a scale to measure it ? I havent seen an explosive so sensitive and having OB of over +40 at same time.

Thank any one who can help this. dar.

Dany - 27-12-2013 at 19:19

US patent 2768874, indicate that hydroxylammonium perchlorate has an impact sensitivity of 15 which according to the patent represent the distance in centimeters a 2 kilogram weight was required to fall in order to produce 50% shots (determined on Bureau of Mines impact machine). However, as it is known the value of sensitivity of energetic material can vary considerably between different test and configuration.

Dany.

Attachment: US2768874A.pdf (50kB)
This file has been downloaded 560 times


Dany - 27-12-2013 at 19:43

DAR,

i will give you some examples of impact sensitivity of certain type of explosives taken also on the same machine (Bureau of Mines impact machine) so as to be able to compare with the sensitivity of hydroxylammonium perchlorate.

First the testing machine is fully described in Military Explosives (TM 9-1300-214 ARMY TECHNICAL MANUAL) chapter 5 (section 5-6) and the values are also extracted from this manual:

Mercury fulminate: 5cm
Tetracene: 7 cm
HMX: 32 cm (for 20 milligram sample)

You should be careful when comparing the sensitivity with your hydroxylammonium perchlorate since as i mentioned the sensitivity can vary even on the same apparatus, one factor may be the crystals morphology of the explosive being tested.

Dany.

DubaiAmateurRocketry - 27-12-2013 at 20:57

Wow Thank you dany! I will synthesize a gram or less and see its sensitivity next few month. Still surprised at the high sensitivity. 15cm and 2kg is around 3 joules (similar to ETN) However I expect it to have only a moderate VoD. I might also synthesize a gram of Hydroxylammonium dinitramide from KN(NO2)2 and Hydroxylammonium perchlorate/sulfate(i'm pretty sure they will ion exchange). What surprised me is they obtained the dry form of the salt.



From This Article


Does Ammonium perchlorate and Potassium dinitramide ion exchange for Ammonium dinitramide ? It seems all okay but ADN's solubility is far higher than Ammonium perchlorate. In papers they used Ammonium sulfate, however I think just for more economic ? However I have few kg of AP sitting here and dont want to buy more ammonium sulfate.


[Edited on 28-12-2013 by DubaiAmateurRocketry]

roXefeller - 27-12-2013 at 21:32

Vlad, did your friend try washing in acetone or ethanol and then low temp dessicator? I know this is the canned internet method but I'm curious if his results didn't live up to expectations.

Dany - 28-12-2013 at 03:03

DAR,

The specific impulse of hydroxylammonium perchlorate(NH4ClO5)/hydrazine (optimal mixture) is approx. Isp=262 s, see [1] page 244.

other interesting physical properties for NH4ClO5 is found in [2]. for example, the crystal density of NH4ClO5 is 2.06 g/cm3 and heat of formation @ 298 °K HOF= -66.5 kcal/mol.

Dany.


Attachment: [1].pdf (595kB)
This file has been downloaded 1056 times

Attachment: [2].pdf (537kB)
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[Edited on 28-12-2013 by Dany]

DubaiAmateurRocketry - 28-12-2013 at 08:29

Yes thank you dany, not only the specific impulse is higher, Hydroxylammonium perchlorate(HAP) also have much higher density than AP. from PROPEP code HAP give nearly 10s higher than AP if directly replaced. This is a very high increase. unfortunately its impact sensitivity is too high.

The [1] paper seems to have undercalculated many explosives. paper [2] seems to treat HAP as a normal compound without sensitivity. It wont even ignite in pressure slightly lower than ambient pressure. I'm still in doubt in the real impact sensitivity of HAP and I will set up my own 2.5kg steel ball weight dropper to test it in the coming few month. Only if my shipping goes cross the strict boarder of Dubai though.

Do you know the impact sensitivity of potassium dinitramide(KDN)? My search engine have ammonium dinitramide overlaping it and most papers I found only use KDN as a intermediate for ADN and does not provide any impact sensitivity for KDN.

Dany - 28-12-2013 at 09:18

Quote: Originally posted by DubaiAmateurRocketry  
Do you know the impact sensitivity of potassium dinitramide(KDN)? My search engine have ammonium dinitramide overlaping it and most papers I found only use KDN as a intermediate for ADN and does not provide any impact sensitivity for KDN.


Yes, this article is very useful (see table. 2)

Dany.

Attachment: Article.pdf (621kB)
This file has been downloaded 678 times

[Edited on 28-12-2013 by Dany]

DubaiAmateurRocketry - 28-12-2013 at 10:45

Quote: Originally posted by Dany  

Yes, this article is very useful (see table. 2)

Dany.

[Edited on 28-12-2013 by Dany]



Ahh I see, over 20 J is a very nice and safe for handling. Thank you.

DubaiAmateurRocketry - 29-12-2013 at 06:43

In this paper

http://onlinelibrary.wiley.com/doi/10.1002/(SICI)1521-4087(199906)24:03%3C159::AID-PREP159%3E3.0.CO;2-0/abstract

The conversion of ethylene glycol bis-chloroacetate to ethylene glycol bis-azidoacetate was done using DMSO. can it be repeated with DMF ? or is there some special reason for the use of DMSO ? other than tocxity ?

Dany - 29-12-2013 at 07:03

Quote: Originally posted by DubaiAmateurRocketry  
The conversion of ethylene glycol bis-chloroacetate to ethylene glycol bis-azidoacetate was done using DMSO. can it be repeated with DMF ? or is there some special reason for the use of DMSO ? other than tocxity ?


DMF and DMSO are classical solvent for SN2 reactions like the one encountered here. The choice of the solvent should be optimized to meet the requirement of high yield products, minimum time reaction and minimum side products. This is done during the course of the study, however, this is not written in the scientific paper. what you see in these article is the final result of the optimizing procedure done by the author of this study. This is not necessarily the best result that can be obtained, other way can be explored to achieve better results. So maybe the authors used the DMF and found that is inferior to DMSO for carrying this reaction.

Dany.

DubaiAmateurRocketry - 29-12-2013 at 13:02

Thank you dany.

Any one know why many energetic compound's deutrated form has been synthesised ?

Another question. Does Ammonium perchlorate ion exchange with Potassium dinitramide to form KP and ADN ? Almost all papers that says ADN from KDN uses ammonium sulfate.

What about this ? NH4ClO4 + KNO3 = KClO4 + NH4NO3. KClO4 is less soluable however ammonium nitrate is more soluable so .. is this reaction possible ?


[Edited on 29-12-2013 by DubaiAmateurRocketry]

Metacelsus - 29-12-2013 at 15:33

Quote: Originally posted by DubaiAmateurRocketry  

Any one know why many energetic compound's deuterated form has been synthesized ?


For NMR, maybe? (Although that usually involves deuterated solvents . . . Maybe they want to eliminate the signal from certain protons for some reason?)

[unfounded speculation] For some strange, classified application in nukes??? [/unfounded speculation]

Dany - 29-12-2013 at 16:38

DAR,

isotopically labelled explosive where synthesized for detonation experiment like the explosive nitromethane. Deuterated nitromethane shows interesting properties over normal nitromethane. For example, the critical diameter of deuterated nitromethane in glass is more than double the critical diameter of normal nitromethane see:

http://library.lanl.gov/cgi-bin/getfile?00789342.pdf

also 14C labeled HMX has been synthesized for biodegradation studies see:

http://onlinelibrary.wiley.com/doi/10.1002/%28SICI%291099-13...

Dany.

NexusDNA - 31-12-2013 at 08:23

I have a question that has been bugging me for some days... is there any type of hand protection that can successfully prevent them from tearing apart by, say... as low as a gram of a HE?

I know EOD (bomb squad) doesn't use gloves for mobility, but also they deal with *much* more a gram of them explosives.

If there is, any availability for the amateur?

Turner - 31-12-2013 at 08:43

Heavy finger weighted gloves maybe?

Dany - 31-12-2013 at 09:26

Quote: Originally posted by NexusDNA  
I have a question that has been bugging me for some days... is there any type of hand protection that can successfully prevent them from tearing apart by, say... as low as a gram of a HE?

I know EOD (bomb squad) doesn't use gloves for mobility, but also they deal with *much* more a gram of them explosives.

If there is, any availability for the amateur?


Working with explosive and high energy density materials are not suitable for beginners in the field of science and chemistry. before handling these materials, you should have good theoretical background on the sensitivity of these materials and what are the danger encountered during the handling. PhD student working on energetic materials subject must handle different type of explosive. If a student synthesize a new compound, nothing is known about it's properties so synthesis is realized on small quantities (100-200 milligrams). Synthesizing Bigger quantity are permitted only after a series of test (friction sensitivity, shock sensitivity, thermal analysis...) on the new compound are realized. During the handling, the student wear Kevlar gloves, and work is performed behind a safety shield. Anti-static materials are used to avoid any electrostatic discharge that can trigger detonation. For more on these protective gloves read this paper:

http://publik.tuwien.ac.at/files/PubDat_169519.pdf

Remember, that the best safety is to work with small amounts <250 milligrams. With small amount, it is likely (but not sure) that you will not loose a finger, a hand or a head...

Dany.



[Edited on 31-12-2013 by Dany]

NexusDNA - 31-12-2013 at 15:25

Thanks Dany. But as the paper suggests, even 1g of lead azide will tear steel-core kevlar gloves. Maybe we should work with our feet!

And happy new year to all of you!

[Edited on 31-12-2013 by NexusDNA]

Dany - 31-12-2013 at 15:44

Quote: Originally posted by NexusDNA  
Thanks Dany. But as the paper suggests, even 1g of lead azide will tear steel-core kevlar gloves. Maybe we should work with our feet!

And happy new year to all of you!

[Edited on 31-12-2013 by NexusDNA]

This example illustrate how crazy are some members here. Some have worked with grams of very sensitive peroxide explosive! You cannot handle this large quantity of peroxide (or other sensitive explosive) and say "i have the control of what i'm doing".

The reason of why any material can resist a detonation is the following:

when an explosive detonate near a material (the explosive is considered attached to this object with no space between them) the detonation wave that spread over the explosive charge has a velocity between 4-10 km/s and pressure in the range of 200-450 kbar. The Thought steel will yield (this mean will bend or fracture) when subject to a stress of 10-15 kbar so at 200-400 kbar rang the strength of any material can be neglected and the material is treated like a fluid. This why the branch of studying the detonation physics is fluid dynamics.

happy new year for you and all other members.

Dany.

[Edited on 31-12-2013 by Dany]

Happy New Year

roXefeller - 31-12-2013 at 17:41

Stay safe all you western hemisphere pyrotechnicians. Don't come back with sad stories.

Peroksit - 1-1-2014 at 08:01

why doesn't egdn is completely used instead of ng by dynamite factories?
couldn't the dynamite just go from egdn ?

[Edited on 1-1-2014 by Peroksit]

Dany - 1-1-2014 at 08:15

EGDN has similar detonation properties as NG (although less dense 1.49g/cm3 for EGDN vs 1.59 g/cm3 for NG). EGDN has partially replaced NG in explosive industry the main advantage is that the freezing point of EGDN is lower than that of NG (-20°C for EGDN vs 13°C for NG).

Dany.

[Edited on 1-1-2014 by Dany]

DubaiAmateurRocketry - 1-1-2014 at 09:27

We've been talking of tetrazoles and tetrazines a lot, now what about 4 member or 8 membered nitrogenous rings? diazete dioxide and its derivatives seems good. Also what about other nitrogen hydride cations other than NH4+ and N2H5+ ? Diazene and triazene seems more dense than NH4, N2H5. Can they be protonated to form salts? I also found that hydrazoid acid can be protonated too.

[Edited on 1-1-2014 by DubaiAmateurRocketry]

DubaiAmateurRocketry - 2-1-2014 at 17:29

I want to make NTO, however to start from less steps, I want to start from 2,4-dihydro-3H-1,2,4triazol-3-one. However the 2,4-dihydro is not availible as a commercial product but 2,1 dihydro is..

http://www.chemdoor.com/yp/show_2747_46371.html

Their structure is striking similar except with 1 NH group in on position 4 rather than position 1.

So will I get the exact same final product if I nitrated it ? Will it change to 2,4 form ? Would be happy to know. Thanks !

Turner - 2-1-2014 at 18:38

How do we know how dangerous casting ETN is? The only accidents I know of from ETN heat explosion where when it was rapidly heated (hot plate or glass w/ flame)

Has ETN ever detonated from slow heating by something like a water bath? It may become more sensitive when molten, but if it is undisturbed, I don't see how it would explode for no reason? Is melting 50g of ETN more prone to explosion than 1g melting under the same conditions (water bath).

Because I think a cast of ETN and RDX would have amazing brisance over TNT based casts.

DubaiAmateurRocketry - 2-1-2014 at 19:01

Never never cast ETN. Why would you even handle anything with sensitivity under 20cm of HD50?

ETN is very badly reputed in this form, see some member's severe injuries from ETN.

Lost almost 2 hand/ scared all over for life from ETN

[Video] Lost hand with few grams of sensitive explosive

Few miligram of ETN, and that is what can happen to you.

Sthe person above had just few miligrams... and that happened to him. If 1 piece was toward his eyes he could have been blind..So..... Just Don't... Cast it and you will be on the news.


[Edited on 3-1-2014 by DubaiAmateurRocketry]

DubaiAmateurRocketry - 2-1-2014 at 19:16

Where can I find a full synthesis of HMX starting from Hexamine ? The one that uses paraformaldehyde and Acetic anhydride ? Is there any paper on perfecting this method ? And also RDX ?

[Edited on 3-1-2014 by DubaiAmateurRocketry]

Turner - 2-1-2014 at 19:41

google "HMX synthesis" you'll find quiet easily.


That is not the response I was looking for Dubai, the fact of the matter is, ETN can no doubt detonate when subject to thermal shock. Just as NG can.

"Cast and you will be on the news" I've casted ETN before, in a straw in a hot water bath. I may do some tests w/ molten ETN, test friction and shock sensitivity.

My question is, is ETN more prone to detonate when it is molten in large amounts?


I think I would be leaving too powerful of a composition by never trying cast ETN in reasonable amounts (10-50g taking great care of course to not expose it to thermal shock but slow melting and solidifying away from where it would cause damage if it did explode.

How about cast ETN/RDX compositions? 75/25 RDX/ETN at cast density would probably surpass pressed HMX or even HMX plastique in terms of brisance.




Dubia:

http://web.mit.edu/semenko/Public/Military%20Manuals/RogueSc... I think that is what you're looking for. If you do try it report how it works, and then video detonation.




[Edited on 3-1-2014 by Turner]

[Edited on 3-1-2014 by Turner]

Turner - 2-1-2014 at 20:07

Also look, this guy was very professional with everything he did and took extraordinary safety precautions, 13g Cast ETN: http://www.youtube.com/watch?v=m496k0l1XIk

Because, when doing burn tests with ETN it always melts way before deflagrating, has it ever popped when exposed to open flame?

I would only ever dare cast ETN that has been recrystalized and absolutely no left over acid.



That video is quiet violent, I wonder if the Nitrocellulose coating on the fuse burned down too fast? Once when I was testing out some Visco fuse I ordered, it looked like the NC deflagrated down the fuse very fast while the core burned, maybe not. I've used that fuse 5-8 times w/ no problem though


DubaiAmateurRocketry - 2-1-2014 at 20:19

alright then try casting it behind a blast shiled. or at least fune hood + faceshield + thick lab coat.

and dont try too much. cast it in water, so if it explodes its less fatal. ETN is sensitive.

thx for hmx synthesis ive seen that. is there any.other ? this one is spending too mich acetic anhydride. I remember there are less step methods with slightly less yield.

roXefeller - 2-1-2014 at 20:26

You could also gain excellent brisance by just using liquid, unadulterated NG, but it also has complexities in handling and a longer storied history of accidents. This is why EM researchers spent so much time getting extremely powerful materials that come nearly insensitive to use as base charges. At some point you have to trust the Tradition of our predecessors and not get too headstrong for the sublime things that you are warned against.

roXefeller - 2-1-2014 at 20:35

Quote: Originally posted by DubaiAmateurRocketry  
thx for hmx synthesis ive seen that. is there any.other ? this one is spending too mich acetic anhydride. I remember there are less step methods with slightly less yield.


Have you seen this one.

Attachment: cyclic and linear nitramines.pdf (726kB)
This file has been downloaded 615 times


roXefeller - 2-1-2014 at 20:48

Quote: Originally posted by DubaiAmateurRocketry  
Where can I find a full synthesis of HMX starting from Hexamine ? The one that uses paraformaldehyde and Acetic anhydride ? Is there any paper on perfecting this method ? And also RDX ?

[Edited on 3-1-2014 by DubaiAmateurRocketry]


Here's a cut from Chemistry and Technology of Exp. Vol3 (page 110)

pg110_CATOEv3.png - 33kB

DubaiAmateurRocketry - 2-1-2014 at 21:58


thank you roxfeller

what are other nitrogen-oxide anions other than NO2 N3O4 NO2 NO NO3

[Edited on 3-1-2014 by DubaiAmateurRocketry]

roXefeller - 6-1-2014 at 20:15

I kinda suppose the answer to be 'no', but do you suppose that the paraformaldehyde from campa-chem could ever be washed clean enough to be suitable for the rdx synthesis?

Motherload - 12-1-2014 at 01:53

What's wrong with blue RDX ??
Try washing with MeOH.

They only sell the Eco friendly crap here now.
Can trioxane be used instead of paraformaldehyde ?

Can DEGDN really be co-nitrated ?

DubaiAmateurRocketry - 12-1-2014 at 02:03

Diethylene glycol dinitrate(DEGDN) is low in sensitivity therefore I would like to have a mixture of trimethylolethane trinitrate(TMETN) with DEGDN to decrease the sensitivity of TMETN.

however on this page.

http://web.mit.edu/semenko/Public/Military%20Manuals/RogueSc...

Megalomania's guide on DEGDN specified very clearly, that DEGDN can not be nitrated like others, it will decompose in acids. So it is carried out in a inert solvent, such as dichlorofluoromethane.

However on this page.

http://web.mit.edu/semenko/Public/Military%20Manuals/RogueSc...

DEGDN is co-nitrated with TMETN without any solvent. Will DEGDN decompose ?

Dany - 12-1-2014 at 05:19

Quote: Originally posted by DubaiAmateurRocketry  
Diethylene glycol dinitrate(DEGDN) is low in sensitivity therefore I would like to have a mixture of trimethylolethane trinitrate(TMETN) with DEGDN to decrease the sensitivity of TMETN.

however on this page.

http://web.mit.edu/semenko/Public/Military%20Manuals/RogueSc...

Megalomania's guide on DEGDN specified very clearly, that DEGDN can not be nitrated like others, it will decompose in acids. So it is carried out in a inert solvent, such as dichlorofluoromethane.

However on this page.

http://web.mit.edu/semenko/Public/Military%20Manuals/RogueSc...

DEGDN is co-nitrated with TMETN without any solvent. Will DEGDN decompose ?


DAR,

this is copy-pasta from Military explosive (TM 9-1300-214)

"-DEGDN can be manufactured with a yield of approximately 85 percent of the theoretical by adding diethylene glycol to mixed acid containing approximately 50.3 percent nitric acid, 44.7 percent sulfuric acid, and 5.0 percent water. The temperature of the mixture is kept at 10° to 15°C. The spent acid is very unstable and fumes off if heated or allowed to stand for a few hours. The separated DEGDN is purified by washing with successive portions of water, dilute sodium carbonate solution, and water until neutral. The purity of the product is dependent mainly on the purity of the diethylene glycol used in the manufacturing process.

-DEGDN is so insensitive that mixing with another nitrated compound is required to produce a useful explosive. DEGDN alone, however, does explode in the pendulum friction test. The explosion temperature test value for DEGN is 237°C"

this is also a patent US1936020 for the nitration of diethylene glycol.

Dany.

dangerous amateur - 12-1-2014 at 08:46

Short question from me:

from the wikipedia article on Ammonium sulfate:

In November 2009, a ban on ammonium sulfate, ammonium nitrate and calcium ammonium nitrate fertilizers was imposed in the former Malakand Division—comprising the Upper Dir, Lower Dir, Swat, Chitral and Malakand districts of the North West Frontier Province (NWFP) of Pakistan, by the NWFP government, following reports that they were used by militants to make explosives. In January 2010, these substances were also banned in Afghanistan for the same reason.

Why did they ban the sulfate?
it must be a big PITA to make AN from the sulfate and maybe KNO3 or something, AN is much more soluble.
What's the Warlords use for it?

[Edited on 12-1-2014 by dangerous amateur]

Dany - 12-1-2014 at 09:01

In war time every substance become precious for people doing explosives/energetic materials. Maybe it is difficult to make ammonium nitrate form the sulfate, but Al-Qaeda terrorist have mastered how to extract KNO3 form sheep and other animals excrement to make black powder. the KNO3 may be used to make ammonium nitrate when combined with the ammonium sulfate. Maybe they should ban sheep in Afghanistan :D. It is impossible to stop making explosive since many of the materials used for their fabrication has a dual uses and many of these chemical is simple to synthesized. So even you ban a large amount of chemical you still not able to stop bomb manufacturing.

Dany.

dangerous amateur - 12-1-2014 at 09:12

Quote: Originally posted by Dany  
So even you ban a large amount of chemical you still not able to stop bomb manufacturing.

Dany.


No doubt about that.

But I'm still wondering. If I was so poor as these guys I would have had other troubles than making nitrates out of shit...

Turner - 12-1-2014 at 10:06

I wonder if someone can perform an exchange type reaction with ammonium sulfate (or other NH4+ ion containing salt) and a nitrate salt like Potassium Nitrate or sodium nitrate in Large amounts.

if someone had 200 lbs of ammonium sulfate fertilizer, and 200 lbs of sodium nitrate fertilizer, they could theoretically have that amount of ammonium nitrate.

DubaiAmateurRocketry - 12-1-2014 at 10:11

Dany,

Ahh that patent is very helpful, thanks a lot.

Quote: Originally posted by Dany  

-DEGDN is so insensitive that mixing with another nitrated compound is required to produce a useful explosive. DEGDN alone, however, does explode in the pendulum friction test. The explosion temperature test value for DEGN is 237°C"


where did you find that ? I wish i can see any sensitivity of DEGDN mixtures with another high explosive such as BTTN or NG

roXefeller - 13-1-2014 at 20:07

Quote: Originally posted by DubaiAmateurRocketry  
Where can I find a full synthesis of HMX starting from Hexamine ? The one that uses paraformaldehyde and Acetic anhydride ? Is there any paper on perfecting this method ? And also RDX ?

[Edited on 3-1-2014 by DubaiAmateurRocketry]


I just noticed this while reading the Urbanski text (vol 3 pp 117):

Quote:

This observation also appears to explain why an excess of paraformaldehyde should have a harmful influence on the yield of cyclonite. In particular, Winkler noticed that the addition of formaldehyde to a hexamine solution in aqueous acetic acid causes the decomposition of hexamine which proceeds at a rate depending on the ratio of formaldehyde to hexamine.


Are you really intending to add paraformaldehyde and Ac2O to a hexamine/nitric acid process?

As far as blue RDX, the blue will probably come out when all is done for purification, but the cyclic polymerization can sometimes be finnicky. Hence the oft quoted low yields, the waste acid is full of linear nitramines that never polymerized. I'm hoping that impurities after washing won't hinder this polymerization.

roXefeller - 13-1-2014 at 20:16

Quote: Originally posted by Turner  
I wonder if someone can perform an exchange type reaction with ammonium sulfate (or other NH4+ ion containing salt) and a nitrate salt like Potassium Nitrate or sodium nitrate in Large amounts.

if someone had 200 lbs of ammonium sulfate fertilizer, and 200 lbs of sodium nitrate fertilizer, they could theoretically have that amount of ammonium nitrate.


This is getting a bit taboo for the forum. Lab work can be scaled up (the essence of chemical engineering) but why are you hypothesizing 200 lbs of AN (I don't think your stoich works out), and why here? That's alot of solution to be sloshing around and drying.

DubaiAmateurRocketry - 31-1-2014 at 05:51

Does hydroxylammonium-5-amino-tetrazolate exist ? Any papers/ information of it ?

How to I obtain ammonium nitrate form a solution ? I have around 100ml of water dissolving around 5 gram of AN and it did not precipitate even when I put it in my fridge(around 5 degree C)



[Edited on 31-1-2014 by DubaiAmateurRocketry]

Turner - 31-1-2014 at 15:31

You will need to evaporate all the water, boil the solution down, and then put it in an oven to evaporate the rest, you will end up with dry ammonium nitrate.

underground - 31-1-2014 at 16:06

Quote: Originally posted by DubaiAmateurRocketry  

How to I obtain ammonium nitrate form a solution ? I have around 100ml of water dissolving around 5 gram of AN and it did not precipitate even when I put it in my fridge(around 5 degree C)



Use a Desiccator Bag

Metacelsus - 31-1-2014 at 16:20

That is a relatively dilute solution. I recommend boiling it down first, then cooling it. From Wikipedia, its solubility at 0 C is 118 g per 100 g water.

From personal experience, boiling down ammonium nitrate solutions is difficult. They transition directly to molten ammonium nitrate, and it is difficult to tell when this occurs. Decomposition is a problem (basement filled with dense white smoke:(). I recommend not boiling all of the water off.

[Edited on 1-2-2014 by Cheddite Cheese]

DubaiAmateurRocketry - 1-2-2014 at 16:06

Alright thank you, Ill just wait for the hot summer of Dubai and then leave it outside then :D

I wonder if hydroxylammonium-5-amino-tetrazolate, [NH3OH]+ [CN5H2]- or dihydroxylammonium nitriminotetrazolate [(NH3OH)2]2+ [CN6O2]2- exist or ever synthesized.

Turner - 1-2-2014 at 16:39

You don't need to wait for your AN. Boil the solution down slowly, I don't know how dilute it is although. Once you notice slight white smoke coming from it that smells a little different (not steam). And then pour this liquid while hot onto a tray. You will notice long crystals begin to form as the solution cools, this is AN, but in order to evaporate all of the water, gently and carefully heat, you may use an oven if you have to but don't get it too hot, this wouldn't be so dangerous. You will end up with dry, white ammonium nitrate in a granular form.

Peroksit - 5-2-2014 at 11:24

Did anybody hear a mixture of AN/Red Phosphorus ? I seen a patent which about the mixture. Red phosphorus is for increase its sensivity for weak blasting caps. This mixture will be stable or safe ?


[Edited on 5-2-2014 by Peroksit]

Motherload - 5-2-2014 at 13:52

I wouldn't touch any mixture with Red Phosphorous in it.

DubaiAmateurRocketry - 12-2-2014 at 11:37

Does anyone have or can find a full guide on the synthesis of Diethylene glycol dinitrate (DEGDN)? An experimental part in a paper is also good.

I just can not find its actuall synthesis be stated in a paper except on some websites that Ive been told to contain false information.

Omnipresent75 - 15-2-2014 at 13:08

I saw a demonstration online, where potassium persulfate was made by following procedure:

45,6 G of ammonium persulpfate dissolved in 100 ml of water

30 G of potassium chloride dissolved in 100 ml of water

Mix the solutions, cool it in fridge, filter crystals out and rinse them with water

Said to yield 54 G K2S2O8, and a leftover solution of Ammonium Chloride.

I scoured the WWW for more info on this proces, and found none. Which is why i hope someone here will enlighten me, as i´m out of options.

Is it a Hoax?

Thanks!

[Edited on 15-2-2014 by Omnipresent75]

DubaiAmateurRocketry - 15-2-2014 at 13:21

That sounds like a reasonable reaction, check the solubility rules, potassium persulfate should precipitate from the solution.

Omnipresent75 - 15-2-2014 at 13:26

what i don´t understand is why i can´t find anyone else mentioning this reaction.??

Turner - 15-2-2014 at 17:58

Looks like any other salt ionic exchange reaction whatever the word for that is.

PeeWee2000 - 16-2-2014 at 17:35

I thought almost all alkali metal and ammonium compounds were very soluble or did my AP Chem teacher steer me wrong? I think the words you might be looking for are Salt Metathesis Reaction or Double Displacement Reaction. You probably cant find it because specific simple reactions like this aren't highly discussed. You might read this for more info on the reaction http://en.wikipedia.org/wiki/Double_displacement_reaction

Zyklon-A - 16-2-2014 at 17:51

I don't know why you asked this in the EM Short question / quick answer - Thread.
But no not all group 1 salts are very soluble, although many are, for instance sulfates, which are rarely soluble.

DraconicAcid - 16-2-2014 at 18:08

Quote: Originally posted by PeeWee2000  
I thought almost all alkali metal and ammonium compounds were very soluble or did my AP Chem teacher steer me wrong?


The key word being "almost". There are a few alkali metal compounds with low solubility (KClO3 and K2PtCl4 come to mind). If you're working with concentrated enough solutions, you can precipitate out compounds that are fairly soluble, as long as the reactants are more soluble.

Omnipresent75 - 16-2-2014 at 19:08

Thanks for answering my question, silly as it apparently was.;)

roXefeller - 16-2-2014 at 19:32

Zyklonb, I love the diversity of elements and compounds you have listed...
Latest acquired element(s): Lithium, Gold and Cadmium.
Next element(s) to acquire: Sodium, potassium.
Latest acquired compound(s): Sodium Hydroxide, Acetone.

You just never expect to see group I alkali metals alongside hardware store lye and acetone. Then gold and cadmium thrown in to round it out. :D

The amount of primary-booster needed

underground - 17-2-2014 at 04:09

Cause i do not want to open a new topic for only a short question, that i want to ask is:

The amount of primary-booster that is going to detonate an amount of secondary explosive like ANNMAL or ANFO always is going to be the same ? or it must be increased as the secondary explosive increases ?

For example, 3gr of ETN and 500mg of HMTD can easily detonate an amount of 300gr of ANNMAL - ANFO. Now if the ammount of ANNMAL - ANFO changed to 300kgr, the 3gr of ETN and 500mg of HMTD would be enough ?

[Edited on 17-2-2014 by underground]

Zyklon-A - 17-2-2014 at 06:05

@roXefeller, Haha, yeah, well I haven't been trying to get elements in any order.... Also I don't have much budget to go just for a collection, all my chemistry budget goes into buying useful chemicals (like Sodium Hydroxide, Acetone) and equipment, not something that will sit on a shelf and never be used.;)

goldenoranges - 17-2-2014 at 11:38

Quick Question: Is Red Phosphorus banned in the USA? I can't find it on Ebay, Amazon, or United Nuclear.

Is there a synthesis tutorial on this site?

I know if it isn't banned, it is probably watched, as it is one of the ingredients for a few nerve agents and drugs. (just to clarify, that is not what I want it for)

[Edited on 17-2-2014 by goldenoranges]

elementcollector1 - 17-2-2014 at 11:58

Banned, due to extensive use in methamphetamine manufacture.
Curious - what is your intended use, then?

goldenoranges - 17-2-2014 at 12:15

Motherloads "wizard balls" got me interested in making them :D

http://www.sciencemadness.org/talk/viewthread.php?tid=28972#...

I saw when I tried searching for a synthesis you can make it out of urine? I am not sure if the person was being serious or joking. I also see some websites offering it, but it seems sort of fishy...
http://www.hottdealss.com/Red%20phosphorus.html

I am searching for a synthesis in the ullmann's encyclopedia of industrial chemistry, which is a great resource for information on chemistry.


roXefeller - 17-2-2014 at 12:35

You should be looking at this thread. https://www.sciencemadness.org/whisper/viewthread.php?tid=65

I believe the urine thing did happen some time ago. You'll see that phosphorus sources are common, reduction to elemental isn't so. And from talking to the ironworkers in Idaho who worked in the molten phophorus plants, rather 'exciting'.

goldenoranges - 17-2-2014 at 12:50

hmm yeah, it is harder than I originally thought it would be to get a hold of it. Thanks for that link though, it is an interesting way of getting calcium sulfate!

Motherload - 17-2-2014 at 15:59

Goldenoranges .... Don't make those "Wizzard Balls" they sound cool but they are dangerous.
I have burnt my self badly with them. That's why I won't touch any mixtures of RP with oxidizers.
If you think AP is sensitive .... Variants of Armstrongs mixes are waaay worse.

goldenoranges - 17-2-2014 at 16:08

Oh, ok. I thought it would be like the old strike anywhere matches in a ping pong ball, but faster, but never mind if its that dangerous, and expensive for the RP. Druggies are really pissing me off, they get all the chemicals banned and hard to get/expensive.

Zyklon-A - 17-2-2014 at 16:17

I have semi related question. Since both RP and iodine are used to make methamphetamine, why is iodine easer to get? Sure it's still kind of illegal, but you can still buy it. It's on United Nuclear (you can only get an ounce though.) I wish it was the other way around, since iodine is easer to make too. Not that I would ever even consider making methamphetamine.

elementcollector1 - 17-2-2014 at 16:22

Mainly because its other uses are far more economically useful and less replaceable than RP - although that hasn't stopped the DEA from trying to phase out iodine.

Zyklon-A - 17-2-2014 at 17:16

Ok, thanks. That makes sense... Another reason that I just though of is because they know that iodine is easy to make, so if cooks could buy RP, and make iodine...

Bert - 17-2-2014 at 17:18


http://www.deadiversion.usdoj.gov/21cfr/cfr/1310/1310_02.htm...

Red phosphorous and arsenic sulfide (As4S4, realgar) are hard to come by these days. Considering how many people lost bits and pieces to pyro using these with Potassium chlorate, it might not be such a terrible thing.

I did see a supplier of oil paint pigment materials selling realgar a short while back. For an insane price-

Ah yes. He's got cinnabar (HgS) too?

http://www.masterpigments.com/index.php?p=products


goldenoranges - 17-2-2014 at 17:53

Haha, who wants to buy this and distribute it? Minimum order is 19 metric tons :P It would be hilarious if it managed to get by customs, and you actually ended up with it! The DEA would freak out if they ever found out.

http://www.alibaba.com/product-detail/Phosphorus-for-Match-I...

EDIT If anybody sees this within the next 10 minutes, and is interested in astronomy/asteroids/cool things, here is a live feed of one passing by earth.
http://events.slooh.com/stadium/potentially-hazardous-astero...

[Edited on 18-2-2014 by goldenoranges]

GoldGuy - 17-2-2014 at 21:52

Anybody know why RPis always used instead of white phosphorous? Aside from the volatility of WP, why isn't it just used instead of RP?

Motherload - 17-2-2014 at 21:58

RP doesn't need special handling as WP does.
RP can be acquired from the striking surface of match books/boxes.

Zyklon-A - 18-2-2014 at 07:26

It isn't always used instead, some people use white phosphorous as well. But the main reasons are, it spontaneously ignites in air, and it's quite toxic as well, also the heat from skin can cause premature ignition. It's cool for science demonstrations (eg. burning in pure oxygen), but dangerous and hard to get.
Is it true that white phosphorous turns into a different allotrope over time?

DubaiAmateurRocketry - 18-2-2014 at 09:05

Does Nitrogen gas expand more at high temperature or Carbon monoxide? I know they're very similar in molar masses but does one gas expand more or less? Expansion of gases sometimes are not perfect, for example CO2 can obtain different volumes with same pressure.

Bert - 18-2-2014 at 10:31

http://www.molecularsoft.com/help/Gas_Laws-Real_Gas.htm

Plasticizing MHN?

NeonPulse - 18-2-2014 at 21:57

I was wondering if anybody knows if MHN can be safely plasticized in the same manner as PETN or ETN using polybutene? i dont see why not, except the sensitivity being greater than ETN-PETN may be a cause for worry. if i choose to do so i want to do it as safely as possible and being sure that it wont go off in my face. any answers would be greatly appreciated.

plasticizers

underground - 18-2-2014 at 22:18

Can i dissolve any polubutylene/polyisobutylene material with any solvent, add then the EM and the motor oil, and let then the solvent to evaporate ? will it work or it just need a resin-hardener mix ?

Quote: Originally posted by underground  
Cause i do not want to open a new topic for only a short question, that i want to ask is:

The amount of primary-booster that is going to detonate an amount of secondary explosive like ANNMAL or ANFO always is going to be the same ? or it must be increased as the secondary explosive increases ?

For example, 3gr of ETN and 500mg of HMTD can easily detonate an amount of 300gr of ANNMAL - ANFO. Now if the ammount of ANNMAL - ANFO changed to 300kgr, the 3gr of ETN and 500mg of HMTD would be enough ?


Does anyone have the answer ?

Motherload - 18-2-2014 at 23:20

I was wondering if anyone has ever tried ETN/NC composite ?
Say 70% ETN + 30% NC with Acetone as solvent
Or even replace say 5% NC with synthetic oil to make flexible.

TheOddEngie - 19-2-2014 at 04:21

can TNP be made from salicylic Acid sulfuric acid and ammonium nitrate i have not seen any reports of it being done with ammonium but just checking so im not wasting my time i dont see why it wouldnt work though?

Bert - 19-2-2014 at 04:43

It works, but Sodium nitrate has a reputation for working better-

See: " Rosco's Good Old Country Recipe for Picric Acid "

http://www.sciencemadness.org/talk/viewthread.php?tid=4457&a...

A few moments searching on the site would have shown you that-


[Edited on 19-2-2014 by Bert]

goldenoranges - 20-2-2014 at 05:57

AN NM SA is a good explosive. My question, ANNMSA+AL, would that be a better one? As in more sensitive? I realize the aluminum would dissolve creating hydrogen, but it would still be there, right?

TheChemiKid - 20-2-2014 at 16:20

I can make either Acetone Peroxide or Picric Acid, which is more stable? I think Picric is more stable, but if there is not a big difference, I would prefer to make AP.

Motherload - 20-2-2014 at 16:41

There is a BIG difference in stablilty and performance aswell.
There is numerous threads about the stability of AP.
Picric acid would be a much better choice.

Zyklon-A - 20-2-2014 at 18:40

Stick with Picric Acid.

DubaiAmateurRocketry - 22-2-2014 at 05:39

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

Dornier 335A - 22-2-2014 at 08:54

Fedoroff doesn't mention any other salts than the nitrate, perchlorate, sulfate, acid sulfate and hydrochloride. It is however claimed that hydroxylamine will form salts with most strong acids. My guess is that other salts can be prepared from hydroxylammonium sulfate solution and a barium salt. Hydroxylammonium sulfate seems pretty simple to prepare too.

DubaiAmateurRocketry - 28-2-2014 at 10:52

The universe is hypothesized to start from big bang, a singularity. Which means the density is infinite. So according to all equations to calculate Detonation velocity I know of, the VoD of big bang will be infinite m/s since the density is infinite?

nitro-genes - 5-3-2014 at 09:35

Finally remembered my password! :)

@ undergound

Can i dissolve any polubutylene/polyisobutylene material with any solvent, add then the EM and the motor oil, and let then the solvent to evaporate ? will it work or it just need a resin-hardener mix ?

Yes, this is how it is commercially produced as well, best way is to dissolve PB/PIB in solvent, add plasticizer/motoroil, then add EM and stirr gently. You can also add the EM to water and stirr while adding the binder/plasticizer/solvent mix, this will give an even coating of the EM crystals.

In general , you don't need to increase the detonator strength with increasing amounts of secondary.

Metacelsus - 5-3-2014 at 14:51

Quote: Originally posted by DubaiAmateurRocketry  
The universe is hypothesized to start from big bang, a singularity. Which means the density is infinite. So according to all equations to calculate Detonation velocity I know of, the VoD of big bang will be infinite m/s since the density is infinite?


The laws of physics as currently known do not apply to those conditions.

underground - 6-3-2014 at 03:57

Quote: Originally posted by nitro-genes  

Yes, this is how it is commercially produced as well, best way is to dissolve PB/PIB in solvent, add plasticizer/motoroil, then add EM and stirr gently. You can also add the EM to water and stirr while adding the binder/plasticizer/solvent mix, this will give an even coating of the EM crystals.


Very good!!! So with any source of PIB (like rubber PIB gloves) a SAE 10 motor oil and a solvent, a really good plasticizer can be made for any EM!! Have you got any info about that or any DIY guide ?

Quote: Originally posted by nitro-genes  

In general , you don't need to increase the detonator strength with increasing amounts of secondary.


Very interesting, so that means that a 100kgr, and over of ANFO, can fully be detonated with only 4-5gr of ETN ?? !!


[Edited on 6-3-2014 by underground]

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