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Spartan - 18-4-2015 at 03:16

I have never made silver acetylide/nitrate but i have heard that you can get around 3g (maybe a little bit more) silver acetylide/nitrate from 5g silver nitrate. So i think your yields are ok.

Correct Me I Iam Wrong

MineMan - 18-4-2015 at 09:35

I cunsolted one of the senior members on this board, and I was told that no HNO3 is need, as the silver nitrate breaks down in in water and creates HNO3, just make sure you do not have too much water so your HN03 is more concentrated.

In the book "Primary Explosives" the author states the that a hot acidic solution will yield the least sensitive SADS... so it may be good to add a little HNO3 anyways. See the link for the book below... I have full access through a university Library, so feel free to ask more questions.

https://books.google.com/books?id=wfJHAAAAQBAJ&pg=PA305&...

darklight - 26-4-2015 at 22:36

how about nitroglycerin

j_sum1 - 26-4-2015 at 22:56

How about it?

Zombie - 26-4-2015 at 23:57

That darn Nitro... He sooo funeee!

Oh boy! :cool:

Hennig Brand - 27-4-2015 at 13:04

Quote: Originally posted by Microtek  
Does anyone know what the equilibrium moisture content of AN is at say, 20C and 65% RH? I'm asking because I have a lot of AN in solution (from CAN fertilizer) and want to recover it. I know I could just heat it to drive off the water, but I would like to avoid spending more electricity than necessary.


Found the following which is from an old department of agriculture technical bulletin (912) from the set "Technical Bulletin, Issues 901-915". The set of technical bulletins can be downloaded from Google books. The section on ammonium nitrate and moisture content is attached. It also has a lot of information on several other nitrate salts as well as other chemical fertilizers.

"A material is said to be hygroscopic when it absorbs moisture from the air at ordinary temperatures and humidity. This occurs when the pressure of water vapor in the air exceeds that of the saturated solution of the material."



Attachment: Ammonium Nitrate Moisture Content Technical Data.pdf (556kB)
This file has been downloaded 561 times


Relative Hygroscopicities of Soluble Fertilizer Materials.jpg - 136kB Vapor Pressure of Water & Vapor Pressure of Saturated AN Solutions.jpg - 130kB



I remembered seeing the following from the archive "Yarchive" which is regarding the same concept as above for determining when a material will absorb water from the air (or when it will lose water to the air or dry).

"
From: glhurst@onr.com (Gerald L. Hurst)
Newsgroups: rec.pyrotechnics
Subject: Re: KNO3+S+C/Saltpeter(even more;-)
Date: 16 Nov 1995 21:14:25 GMT
Organization: Consulting Chemist
Lines: 110

In article <1995Nov16.152055.17452@cs.rochester.edu>,
nelson@cs.rochester.edu (Randal Nelson) says:

>>>>There's a nice exercise for you budding chemists out there. Erik
>>>>has opined that NaNO3 becomes hygroscopic at about 73% (?)
>>>>relative humidity. How about checking this figure using only
>>>>solubility data and comparing the result with similar calculations
>>>>for KNO3. In other words, see if you can figure out the highest
>>>>relative humidity at which you would expect black powder made from
>>>>the two materials to remain stable at say 0 deg and 30 deg C.
>
>>Calculations like this are naturally subject to errors arising
>>from the nonideality of strong solutions, so how would you
>>check the results experimentally using only materials you can
>>buy over the counter, not including a hygrometer?
>
>>>>OK, I'll furnish the solubility data:
>>>>
>>>>Soly in g of KNO3 in 100 g H2O is 13.9 (0 deg), 21.2 (10 deg),
>>>>31.6 (20 deg) and 45.3 (30 deg).
>>>>
>>>>The corresponding values for the sodium salt in g are:
>>>>
>>>>73.0 (0 deg), 80.8 (10 deg) , 87.6 (20 deg) and 94.9 (30 deg)
>>>>
>>>>Jerry
>
>OK, since I havn't seen anyone take a shot at this.
>
>You can make a first approximation based on the molar fractions
>of the ionic solutions. For example, take NaNO3 at 20 degrees.
>100 gm of water is 100/18 = 5.56 moles. 87.6 gm of NaNO3 is
>87.6/85 = 1.03 moles, which in solution is twice that number, or
>2.06 moles of ions. The molar percentage of water is then
>5.56 / (5.56 + 2.06) = 72.9%, which, to a first approximation is
>the vapor pressure as a fraction of the 100% relative humidity pressure,
>and hence the humidity at which a saturated solution will pull moisture
>from the atmosphere. This agrees with Erik's figure.
>
>For KNO3, 31.6 gm is 31.6/101 = .313 moles = .626 moles of ions,
>giving a molar fraction for water of 5.56/(5.56+.616) = 90.0%.
>Pretty sticky conditions.

YES! Very nicely done, and probably not too far from reality.
Sodium nitrite has a slightly higher molal solubility than
the nitrate and is known to maintain RH at 66 percent
@ your 20 deg, versus 69.5 percent calculated by the method
you used. We might expect the value for KNO3 to be even more
accurate because of the lesser solubility.

Your answer explains why NaNO3 is not as well suited for
commercial black powder. Although the relative humidity
occasionally climbs over 90 percent in some parts of the
country, it spends a lot more time under this figure. If
BP is anything like AN then it probably dries out at least
as fast as it gets wet from atmospheric moisture and
that means your powder is probably going to be dry when you
go to use it unless your timing sucks.

70 percent humidity is another scene entirely. In the Dallas
area, the humidity tends to rise every summer evening to well
over 60 percent so that if you have spilled AN around, it
will be in liquid pools every morning when you come to work,
but dry out by mid morning and then reliquify as you're heading
home. SN is just about 10 RH units better, so it also spends
a fair portion of its time absorbing moisture, if not in
Dallas, then in Houston :) If you happen to live in Reno,
then you could probably get away with an AN-based powder,
at least most of the time.

As a matter of mainly academic interest, it might be noted
that the solubility of KNO3 increases more rapidly with
temperature than does that of NaNO3. The steeper slope
of the curve means that difference in the hygroscopicity
of the two salts grows narrower at high temperatures and
both salts become increasingly deliquesent, i.e absorb
moisture at lower RH.

If you want to determine the exact RH at which KNO3 and
NaNO3 become deliquescent, the easiest method would be to
put an excess of the well wetted solid salt in a jar
with much a much smaller weighed quantity of either
carefully dried CaCl2 or a strong aqueous solution
of known concentration of CaCl2. THe CaCl2 will slowly
absorb moisture from the wet nitrate, forming a solution
which becomes more dilute with time until equlilbrium
is reached. If the nitrate is still wet at this point,
the solution above it must must have the same vapor
pressure (i.e. the same RH) as the now diluted CaCl2
solution, and that value can be obtained by calculating
the CaCl2 concentration from the weight gained by H2O
absorption and looking up the corresponding RH in the
convenient tables of such values in the CRC or Lange's
handbook.

There are also tables for H2SO4 and NaOH, but I originally
suggested that the materials could be purchased "over-
the-counter" and I now suggest that CaCl2 may be a bit easier
and safer to purchase and handle. There are any number of
other common substances with known solution vapor pressures,
but you might have to look farther than he CRC to find them.

Lest you accuse me of being too academic (or as Beavis might put
it: "Fancy Schmantzy"), allow me to mention that I have used the
method outlined above to determine the parameters for building
an explosives manufacturing facility (using H2SO4) and to
gather data on emulsion explosives for a patent battle between
a couple of major corporations. In both cases, I employed Mason
jars for the experiments. The plant (Kinepak) worked fine, and
we won our case :)

Jerry"


[Edited on 28-4-2015 by Hennig Brand]

nitro-genes - 29-4-2015 at 12:12

2 Ag+ + HCCH --> Ag2C2 + 2H+, so the HNO3 is formed by the reaction anyway, you only need a little to promote complex formation. IIRC, there are more complexes of Ag2C2/AgNO3, something like AgC2*AgNO3 but also AgC2*6 AgNO3. Maybe hot and more acidic solutions promote the latter? Would have to check PATR again...

[Edited on 29-4-2015 by nitro-genes]

Non-Ketone Organic Peroxides

Detonationology - 6-5-2015 at 06:10

Can anyone shed some light on the possibility of making organic peroxides from substances other than ketones (acetone, MEK, etc.), such as from alcohols or aldehydes? I am aware that HMTD is an organic peroxide, but are there more accessible chemicals or fuels that can be made into peroxides?

Loptr - 6-5-2015 at 06:35

Here is a site that lists some peroxide forming chemicals.

http://blink.ucsd.edu/safety/research-lab/chemical/storage/p...
http://safetyservices.ucdavis.edu/snfn/safetynets/snml/sn23/...

[Edited on 6-5-2015 by Loptr]

Detonationology - 6-5-2015 at 06:51

Wow, this is exactly what I was looking for :D Thank you sincerely Loptr

I made tetrazene,but it looks like not sensitivity for hammer hit

smithdotyu - 17-5-2015 at 03:56

Hi all；
I made some tetrazene use Aminoguanidine sulfate + NaNO2 。
I used phosphoric acid to catalyst.make the PH at 5~6 and the temperature
is 50C。

finally I get 1gram tetrazene, and wait it dry,it's orange color，I try to burn it，it burning not fast like HMTD or NHN，slow and make sounds like ’pa、pa、pa‘

In the book they sad tetrazene is sensitive，but i use hammer to hit it，it not explosive 。should I would add some KClO3 to it？

hissingnoise - 18-5-2015 at 01:37

You have most likely obtained guanyl azide ─ a consequence of the presence of mineral acids in the reaction mixture!

Take a long look at Davis's prep. in COPAE?

Ok, dont slam, newbie to the scene needs help

havenochoice - 31-5-2015 at 08:35

Ok, first off, i am new here and the reason for my post is confusion!
I got the bug because i made my first ever batch of black powder last week from materials purchased, and it actually worked!!!!
I am just an individual and not a university of chemical engeneer so i cant get access to other chemicals only those that are buyabale by the general public.

Black Powder:
75% Potassium Nitrate ( got online from the USA, havent got a clue how it got through customs as you cant buy it here! ).
15% Charcoal.
10% Sulphur.

Now here is where my problems begain.....

I tried to create some AP, i know your all against this but it was the only thing i could make as other materials are not allowed to be purchased here!
So....
I had Acetone, Hydrogen Peroxide (9% strength as its the highest strength you can get here, i searched for the 30% but just could not get any ), HCL (33%), and lastly Sodium Bicarbonate.

I mixed the Acetone & HP, cooled it to 4C and then slowly added the HCL catalyst keeping it bellow 8C. I waited a few hours then mixed in the Sodium Bicarbonate to neutrualize the reaction....So far so good,BUT, then a few hours later my eyes started streaming and wouldnt stop, i am guessing the acid had befome gasous. Now i am let with a slimy talc like substance.....I tried exploding a 3mm square sample via a rocket hobbyists fuel cap but the AP did not ignite. Have i ruined the mixture somehow? or will this become combustable once dried? Should i allow it to become dried out?

I also tried to make some ANFO or rather tried to yet again buy ingrediants to make ANFO but i can not get Amonnium Nitrate no matter where i go, so instead i managed to get Urea and some disel as i read Urea could be used instead of Amonnium nitrate.BUT, once again this would not detonate....

In essence i am asking would AP (primary) UFO (secondary) detonate? Or am i missing something obvious to eveyone else and not myself because i am too close to see it?
Will the AP be safe to allow to dry out, and will it then become explosive?
And would UFO work or have i missed something again, maybe Nitric Acid, but that acid is impossible to get, could something other be used that actually is purchasable ( god only knows what that would be it seems everything is illegal! )...

Ps... i am not a mad terroist, i am actually just some one who thinks knolage should be avaliable to everyone and why shouldnt people be allowed to know everything? Its only if they then use that knoladge for illegal gains should they be rightly arrested, not just for wishing to expand they mind....Sorry for the speech, just sick of being accused of being bad just because i believe in freedom of knowladge!

PHILOU Zrealone - 31-5-2015 at 09:09

ANFO is not easy to detonate.
You need confinement and good detonator ...wet CTAP (cyclotriacetonperoxyde) will certainly not do the job.

Urea may be subtituant for Ammonia but then you need to nitrate it to get Urea nitrate (UN).
So UNFO may replace ANFO to get your UFO to fly ;) and that's an INFO :P.

UNFO will also need a good confinement and detonator.

There is no need for sodium bicarbonate to neutralise the CTAP...simply filter and wash with cold water.
The bicarbonate may have induced some decomposition of your CTAP yielding chloroaceton...reson why you cried ... yes it is a lacrymator.

Due to your lack of knowledge and chemical education I really think you should stick to black powder...you will arm yourself or others trying to play with CTAP at this stage.

Knowledge is the power, but to be knowledgeable, you need to read and understand fully what you are playing and dealing with.

First read, then read ... and read even more. Start small and never think you masterize the stuff...it will always remind you one day or another who is the real boss...it's statistical and darwinian so always imagine the worst case scenario...the stuff exploding or detoning right now.

[Edited on 31-5-2015 by PHILOU Zrealone]

greenlight - 31-5-2015 at 09:36

Philou is right good confinement and a decent detonator, even a booster maybe for ANFO and dry AN before mixing.
Urea nitrate is annoyingly quite hygroscopic and can be detonated on its own without fuel oil fairly easily.

I don't know what happened with your AP synth, it sounds correctly done and shouldn't be that hard to mess up.
I would definitely use the Sodium bicarbonate wash especially if using HCL as catalyst just because it would remove all traces of residual acid in the final product which you don't want in something like that (decomposition/increased sensitivity) but that's just me.
It is less sensitive when wet but not useable until dry really.

I agree with PHILOU, you should keep to the BP for now til you have read ALOT of information on energetics and understand how they work and their properties. Not knowing what your doing, especially when trying to manufacture and use something sensitive like AP, could end very badly as sensitive primaries are pretty unforgiving if you treat them the wrong way.




[Edited on 31-5-2015 by greenlight]

Hennig Brand - 31-5-2015 at 09:57

Urea nitrate is not hygroscopic, but it does require careful washing and drying after synthesis from what I have seen to avoid decomposition. AP is quite volatile and not a terribly efficient initiator, but I doubt it is out of the range of normal sensitivity as compared to the primaries in common usage . I would always try to err on the side of caution though and not make assumptions about sensitivity and keep the quantities low.

Amos - 31-5-2015 at 10:19

If you've obtained potassium nitrate already, all your are missing is some sulfuric acid that you can use to make much more stable and reliable explosives, such as ETN, Picric Acid, and nitrocellulose.

greenlight - 31-5-2015 at 19:02

Wow I thought Un was hygroscopic.
I made it when I was very young and I remember it was a bitch to get 100% dry. Maybe I hadn't washed it enough, it was so long ago I forgot what I did.

Hennig Brand - 1-6-2015 at 07:47

Yeah, it is not hygroscopic from what I remember. However, from what I have witnessed it easily decomposes if much heat is used in attempts to dry it and especially in the presence of acidity which catalyzes the decomposition. When UN decomposes it produces nitric acid which catalyzes further decomposition. It may seem when heating UN that it is very hygroscopic, and that it will never dry, but it is the presence of acidity and the water the acidity strongly holds onto that keeps it wet. It will become seriously degraded before it ever dries out if anything more than very gentle heating is used to dry it, because it will simply keep decomposing. UN that has been significantly decomposed by aggressive drying techniques involving heat has lousy explosive properties also, speaking from experience. I would advise washing the acidity from the crystals as much as possible after synthesis with ice cold water, or some other solvent that the UN is only slightly soluble in, and then blottering away the moisture as much as possible by placing the crystals on a stack of absorbent cloth of some kind before using moving air and no excessive heating to dry the material.


[Edited on 1-6-2015 by Hennig Brand]

AN/AL with not fine AL powder

Antoine - 3-6-2015 at 23:17

Hello! The aluminium powder would to be fine to make AN/AL?
I make my powder with a piece of aluminium and with a sheet of fine sandpaper.

greenlight - 4-6-2015 at 03:55

Yes, the finer the better.
If your using small particle sandpaper and it is coming out like dust you should be good.
Grind the AN so it is fine as well and make sure it is dry before mixing.



[Edited on 4-6-2015 by greenlight]

Antoine - 4-6-2015 at 04:33

Yes, it´s a fine dust of aluminium. Thanks you!:)

AN/AL détonation with tatp

Antoine - 4-6-2015 at 04:35

Antoine - 4-6-2015 at 04:38

Sorry, I send my message but I don´t finish it
So, CAN I detonate a 100g AN/AL charge with 1g of tatp in copper pipe?
Thanks! :D

greenlight - 4-6-2015 at 04:52

You can edit message in top right corner..
You should post these types of Q's in the short question/quick answer thread in energetic materials section.
I think 1 gram AP in metal tube should ensure detonation.

Bert - 4-6-2015 at 05:18

Quote: Originally posted by Bert  


Hi Antoine- Welcome to sciencemadness.org!

Please read this FAQ about posting, it will help you decide where and how to bring up topics that interest you, and explain why I moved your threads to beginnings or merged your thread into an existing thread.

Posting on topics

Remember: It is nearly ALWAYS better to post in an existing thread than to start a new one!

Posting- And You...

You should look at the library. In particular, I think you are going to be interested in the Tenney L. Davis and Phokion Naoum books.

The sciencemadness.org library

Plastifier for AN/AL?

Antoine - 4-6-2015 at 09:40

Does anyone now how to make AN/AL plastic? Thanks

greenlight - 4-6-2015 at 19:19

I am fairly sure there is no way your going to be able to plasticize AN/Al at home.
Even if you could the 10%-15% inert binder/plasticizer would make an already not very powerful explosive even less powerful.

PHILOU Zrealone - 5-6-2015 at 04:23

Use Nitrocellulose/nitroglycerin as plasticiser for the AN/Al...it should work and boost the things up.

But beware of headaches

[Edited on 5-6-2015 by PHILOU Zrealone]

dangerous amateur - 5-6-2015 at 08:14

For AN/Al you will need dark aluminium. Anything else will give inferiour performance or will not work at all with small charges.
You cannot make this yourself. You need to buy it somewhere.

For plastification, try this:
https://www.youtube.com/watch?v=EkrsYfFUEIE

Hennig Brand - 5-6-2015 at 08:18

That is exactly how I plasticize it as well Philou, it is essentially aluminized ammonia gelatine dynamite. Maybe with very small amounts of NG & NC it wouldn't be specified as dynamite anymore. It can be very rubbery depending on the content of NG & NC.

greenlight - 5-6-2015 at 08:48

Wow, I never knew you could plasticize AN based explosive.
And using an energetic material to plasticize it sounds good.

MineMan - 6-6-2015 at 08:40

What do you use as a solvent when you mix the AN/AL/NC together...? Nitro methane, I have tried (as Yoda would say). But I used smokeless powder, it did not dissolve well, so a gel it was, instead of plastic (as Yoda would say again!)

Hennig Brand - 6-6-2015 at 10:16

I use a little acetone and sometimes a little heat to prepare the NC & NG gelatine first then mix in the finely powdered and well mixed ammonium nitrate and fuel (whether the fuel is fine aluminum , corn starch or whatever). The vapor pressure of NG at ordinary temperatures is very low while the vapor pressure of acetone is very high, so most of the acetone can be easily and fairly quickly evaporated away with the loss of very little NG.

can sulfanilic acid be used to make explosives?

idrbur - 5-7-2015 at 01:11

Yesterday i read about sulfamic acid and come to know that it contain nitrate.
So can it be used to make explosive???

hissingnoise - 5-7-2015 at 01:39

The potassium salt of sulphamic acid is nitrated in the synthesis of ammonium dinitramide!

Boffis - 5-7-2015 at 14:30

Sulphanilic or sulphamic acid? You have sulphanilic (sulfanilic) acid in your title and sulphamic (sulfamic) acid in the question beneath.

In one of the threads in the energetic sub-forum there is a reference to an old GB patent for the preparation of picric acid from sulphanilic acid, I don't have a copy but it was probably posted in that thread. Try using the search engine instead of starting a new thread every time you have a question.

is it possible to make acetone peroxide in this way??

idrbur - 7-7-2015 at 16:07

I want to make acetone peroxide . I also have homemade peroxy disulfuric acid(h2s2o8) which gives h2o2 and di sulfuric acid (h2s2o7) on hydrolysis . So can i use this mixture instead of h2o2 and few drops of h2so4 for making acetone peroxide.

[Edited on 8-7-2015 by idrbur]

PHILOU Zrealone - 8-7-2015 at 09:48

Quote: Originally posted by idrbur  
I want to make acetone peroxide . I also have homemade peroxy disulfuric acid(h2s2o8) which gives h2o2 and di sulfuric acid (h2s2o7) on hydrolysis . So can i use this mixture instead of h2o2 and few drops of h2so4 for making acetone peroxide.

[Edited on 8-7-2015 by idrbur]

Disulfuric acid is HO-SO2-O-SO2-OH a kind of anhydride
Its hydrolysis leads to sulfuric acid!
HO-SO2-O-SO2-OH + H-OH --> HO-SO2-OH + HO-SO2-OH
= 2 (HO)2SO2 or H2SO4

copper sulfate from ammonium sulfate

Antoine - 11-7-2015 at 15:35

Hi! I have a question, I've got a lot of ammonium sulfate and I need copper sulfate. how can i made copper sulfate from ammonium sulfate?
Thx :)

Zyklon-A - 11-7-2015 at 17:44

This is purely hypothetical, based however on a similar process know to work.
Add it to a stoichiometric ratio of copper (II) hydroxide and heat it.

(NH4)2SO4 + Cu(OH)2 --> 2 NH3 + 2 H2O + CuSO4

The one problem I can see with this is the ammonium sulfate may boil (decompose) before the copper hydroxide dissolves in the melt, preventing the ions from exchanging.

DraconicAcid - 11-7-2015 at 18:44

Quote: Originally posted by Zyklon-A  
This is purely hypothetical, based however on a similar process know to work.
Add it to a stoichiometric ratio of copper (II) hydroxide and heat it.

(NH4)2SO4 + Cu(OH)2 --> 2 NH3 + 2 H2O + CuSO4

The one problem I can see with this is the ammonium sulfate may boil (decompose) before the copper hydroxide dissolves in the melt, preventing the ions from exchanging.


I'd do it in solution, rather than trying to melt the salts.

making nitrobenzene

idrbur - 13-7-2015 at 08:37

I am wishing to make nitrobenzene for many weeks but in my area benzene is not available easily but yesterday i read on wikipedia that it can be synthesised by reacting aniline and KMno4 in specific condition .can anybody explain me the whole procedure from A-Z.
And thanks in advance.

Texium - 13-7-2015 at 08:41

So you're saying you have access to aniline but not benzene? That seems odd.

idrbur - 13-7-2015 at 08:57

You are right we don't have acess to aniline but my friend has and he had given me a little sample and in future we are going to make aniline from indigo.

idrbur - 13-7-2015 at 08:58

You are right we don't have acess to aniline but my friend has and he had given me a little sample and in future we are going to make aniline from indigo.

Molecular Manipulations - 13-7-2015 at 09:25

Using the Sandmeyer reaction you could go from phenylamine to its diazonium ion to benzene or straight to nitrobenzene, but the latter is harder.

PHILOU Zrealone - 15-7-2015 at 12:48

Quote: Originally posted by Antoine  
Hello! The aluminium powder would to be fine to make AN/AL?
I make my powder with a piece of aluminium and with a sheet of fine sandpaper.

Your AN must be very dry and away from air moisture...because traces of moisture allow the protective oxyd layer of the aluminium to be chewed by the NH3 and the HNO3 present in traces in dissociated NH4NO3.
To see what happens...make a saturated solution of NH4NO3 and suspend Al foil schredings into it...after a week or two all the Al will be dissolved as Al2O3 , Al(OH)O and Al(OH)3. If the recipient is closed, pressure will build up inside and crack or expel the cap...probably some hydrogen is formed by the decomposition of the water in contact with the naked aluminium.
2Al(s) + 3H2O(l) --> Al2O3(s) + 3H2(g)

PHILOU Zrealone - 15-7-2015 at 12:54

Quote: Originally posted by Antoine  
Sorry, I send my message but I don´t finish it
So, CAN I detonate a 100g AN/AL charge with 1g of tatp in copper pipe?
Thanks! :D

Is CTAP (cyclo-triacetone peroxyde) stable towards copper, Cu(OH)2 or Cu(2+)?
--> Answer is no; those are not storage advisable!
Peroxydes don't like copper and many transition metals!

Is AN/AL stable towards copper, Cu(OH)2, Cu(2+)?
--> Answer is no; oxydised Cu and metallic Al form a battery in shortcut...thus heating, AN complexes Cu, Cu(OH)2 and Cu(2+) as Cu(NH3)4(NO3)2...

All this is thus not storage advisable, especially if the AN is not well dried and protected from the air.

Better coat the Cu with a varnish/lacker.

PHILOU Zrealone - 15-7-2015 at 13:05

Quote: Originally posted by Zyklon-A  
This is purely hypothetical, based however on a similar process know to work.
Add it to a stoichiometric ratio of copper (II) hydroxide and heat it.

(NH4)2SO4 + Cu(OH)2 --> 2 NH3 + 2 H2O + CuSO4

The one problem I can see with this is the ammonium sulfate may boil (decompose) before the copper hydroxide dissolves in the melt, preventing the ions from exchanging.

The other problem is the formation of CuSO4.xH2O and the complexation of NH3 as Cu(NH3)4SO4...thus more heat and time will be needed to expel fully the NH3 and the H2O.

PHILOU Zrealone - 15-7-2015 at 13:13

Quote: Originally posted by idrbur  
I am wishing to make nitrobenzene for many weeks but in my area benzene is not available easily but yesterday i read on wikipedia that it can be synthesised by reacting aniline and KMno4 in specific condition .can anybody explain me the whole procedure from A-Z.
And thanks in advance.

Benzene can be done by dry distillation of Na benzoate and NaOH...
Same can be done form para-benzene-dioic acid (terephtalic acid) found in OTC PET (Polyethylene-terephtalate) from nearly all soda bottles upon reaction of NaOH...

The Member publication section is thus very instructive for you:
Member publication
benzene
terephtalic acid

Then reaction of benzene with HNO3 (69%) should do the trick...H2SO4 will help to accelerate the reaction up.

Erythritol blackened by black mold

retrofit - 26-7-2015 at 22:09

A recrystallized sample of erythritol is being eaten by some organism. Not all crystals are affected yet. Some are still clear, others are black. It is accompanied by a moldy smell.

I'm looking for tips on how to purify it again, since it's clearly contaminated. Would slow recrystallization from boiling be likely to kill and exclude the organisms/waste products?

What is this

Hawkguy - 28-7-2015 at 21:06

Okay so some of you might have been around when I made my last Erythritol post. Erythritol I bought online (NowFoods brand, Amazon.ca) turned out to be a different sugar I didn't bother to identify. It looks, smells like sugar, but tastes less sweet, and is a lot more soluble in water. I tried nitrating it again today, and made a few observations.

- Not very soluble in Acid, made nitrations difficult.
- Lower nitrates of the sugar produced in first nitration would deflagrate very energetically once melted and exposed to flame. Left behind some Carbon residue. Would decompose, releasing Nitrogen Oxides when heated somewhat gently.
- Second nitration yielded white solid with very low melting point (less than 100 degrees C). Explosive once melted, at a similar scale to DDNP. Would explode after lower nitrates or unreacted sugar boiled off on heating. When melted it would be a yellow oil floating on surface of water. Would form a waxy white solid when cool. If someone shows me how, I can post pictures.

So the point of this post? -> What is it? My interest is dying but some of you might find it cool.

nitro-genes - 28-7-2015 at 21:27

Sounds like erythritol although it could be that it is a mix with other low calory sweeteners, what does the package say? A nitration is not a very effective way of identifying a compound. :)

How was it nitrated?

kecskesajt - 28-7-2015 at 22:39

Lower nitrates could be because of Xylitol.
Try a warmer enviroment for nitration(20C°)
ETN has a very low MP(61C°),not a big surprise.

James Ikanov - 29-7-2015 at 08:53

I'd also speculate Xylitol.

It's the only sweetener I know of that would make sense; it's lower nitrates are less explosive IIRC, and they are also a liquid that tends to make a solution or slurry of the higher nitrates.

However, the higher nitrates are mostly or entirely solid.


Quote:

Would explode after lower nitrates or unreacted sugar boiled off on heating.


Sounds like that could've been bad.

aga - 29-7-2015 at 09:05

Quote: Originally posted by Hawkguy  
So the point of this post? -> What is it? My interest is dying but some of you might find it cool.

Nitrogen Narcosis is a lot less messy.

Praxichys - 29-7-2015 at 11:53

I have NOW Foods erythritol and it works fine for me. You have to use a lot of excess mixed acids to keep the nitration thin enough to stir, otherwise you get incomplete nitration. Grind the crystals into a fine powder in a coffee grinder or a mortar first, then bake it at 100C for a few minutes, spread thinly on a metal pan. It should be like flour when you add it to the acids. A good final consistency for the mixed acids and erythritol is like that of creamed corn or porridge. Pre-chill some extra sulfuric acid. Use it to dilute the mix if it gets too thick and sticky. This soup needs to sit at 15-20C for about an hour, with occasional stirring after adding all the erythritol for good results.

Crash it into five times its volume of ice water and filter immediately. Transfer the wet ETN directly into a saturated solution of sodium bicarbonate and shake, venting often. Filter the crude product.

Wash the product thorougly in plain water after neutralization. The lower nitrates and erythritol are very soluble in water and are easily removed. Recrystallize from warm acetone by making a saturated solution of ETN and acetone in a 50C water bath with stirring. Add acetone slowly at 2 or 3 minute intervals until everything is dissolved. It is extremely soluble so you will not have to use much. Crash the hot solution into fifteen times its volume in ice-cold water, and filter immediately while cold.

I guarantee it's pure erythritol. It's food-grade and the only listed ingredient. They would be in big trouble if it wasn't.

http://www.nowfoods.com/Erythritol-1-lb.htm

[Edited on 29-7-2015 by Praxichys]

kecskesajt - 30-7-2015 at 05:56

My 6$/kg erythritol works just fine.
My procedure is like this:
Pour H2SO4 to the HNO3.Add a thermomether.Cool under 15 C°.Start adding erythritol 0.5 gramms per 2 mins, keeping the temp bellow 20 C°.After adding,keeping the temp. at 20 C° for 2 hours.After it,keep the temp at 30C° for another hour.After this add to 3 times of volume ice-slush.Stir for 10 mins.Filter it,wash with water, saturated NaHCO3, water again.Let it dry for 3 days at room temp.After this,recrystalise from hot 80/20 Alcohol/Acetone solution.Add some NaHCO3.Pour it into 3 times of volume of ice-slush water.Stir rapidly for 5 mins.Filter it.It will make the volume of ETN much bigger.
Use Alcohol or Alcohol/Acetone,ETN is highly soluble in acetone,will make your yield bad.
My yield is between 70-85%.

[Edited on 30-7-2015 by kecskesajt]

James Ikanov - 31-7-2015 at 11:44

Related to the above two posts but not in the exact same line of question.

I recently nitrated an off the shelf erythritol sweetener that also contained small quantities of "Reb A". During the mixed acid process I noted that the solution became very visibly... red/orangey.

I'm not sure if it's related but could the nitration of these trace ingredients affect the final product significantly?

I've noted that my crystals are generally flake like and yellow compared to granular and white as I've previously read them described.

If it's any help I used about 100g of powdered ammonium nitrate in 125ml solution of sulfuric acid with 35g of sweetener.

It's one of those generic brand "Stevia leaf" sweeteners.

I was perhaps foolish to assume that the other ingredients small percentage of the overall product would not affect the outcome.


While I'm at it, I'll just go ahead and ask a few "stupid" questions.

1) I see continuous references to oxygen balance and I think I roughly or conceptually understand that that equates to a more effective chemical reaction for the same amount of reactants... but is there a specific advantage beyond this, such as more rapid gas production or greater explosive brisance? Further, is there a reliable way to calculate the Oxygen balance of a given composition?

2) How reliable is RE factor of TNT? AN is listed on wikipedia as having a VOD of about 2500 IIRC, yet an RE of about 0.42, yet Blackpowder, with a "VOD" (I use the term loosely) of only 600 has about a 0.55? Is it a difference in density or what? How does one even measure RE?

3) Aside from the stickied compendium of energetics, are there any other general reading resources related specifically to energetic materials?
For better or for worse I've found that I more easily absorb material explicitly related to energetics. I've found it as kind of a helpful carrot for learning in small parts about chemistry, as most of the compounds are at least somewhat related and the reactions generally follow the same rough pattern(rapid and literally explosive change to state of matter). I'm not looking to be spoon fed so much as a source relating energetics to the rest of chemistry, though perhaps that is a tall order....

Thanks for any help you can give.

Hennig Brand - 31-7-2015 at 12:07

Not exactly sure how "small quantities" of impurity translates to a mass fraction or percentage, but in general pure reactants are always preferable and some impurities can cause big problems for some reactions and product(s) even in small quantities. Erythritol can be obtained cheaply and in high purity.

1) Taken from the Wiki page on oxygen balance:

"
Oxygen balance (OB, or OB%) is an expression that is used to indicate the degree to which an explosive can be oxidized. If an explosive molecule contains just enough oxygen to form carbon dioxide from carbon, water from hydrogen molecules, all of its sulfur dioxide from sulfur, and all metal oxides from metals with no excess, the molecule is said to have a zero oxygen balance. The molecule is said to have a positive oxygen balance if it contains more oxygen than is needed and a negative oxygen balance if it contains less oxygen than is needed; the combustion will then be incomplete, and large amount of toxic gases like carbon monoxide will be present. The sensitivity, strength, and brisance of an explosive are all somewhat dependent upon oxygen balance and tend to approach their maxima as oxygen balance approaches zero.

The oxygen balance is calculated from the empirical formula of a compound in percentage of oxygen required for complete conversion of carbon to carbon dioxide, hydrogen to water, and metal to metal oxide.

The procedure for calculating oxygen balance in terms of 100 grams of the explosive material is to determine the number of moles of oxygen that are excess or deficient for 100 grams of a compound.

OB% = (-1600 / Mol. wt. of compound) * (2X + (Y/2) + M - Z)

where

X = number of atoms of carbon, Y = number of atoms of hydrogen, Z = number of atoms of oxygen, and M = number of atoms of metal (metallic oxide produced).

In the case of TNT (C6H2(NO2)3CH3),

Molecular weight = 227.1

X = 7 (number of carbon atoms)

Y = 5 (number of hydrogen atoms)

Z = 6 (number of oxygen atoms)

Therefore
OB% = (-1600 / 227.1) * (14 + 2.5 - 6)
OB% = −74% for TNT

Because sensitivity, brisance, and strength are properties resulting from a complex explosive chemical reaction, a simple relationship such as oxygen balance cannot be depended upon to yield universally consistent results. When using oxygen balance to predict properties of one explosive relative to another, it is to be expected that one with an oxygen balance closer to zero will be the more brisant, powerful, and sensitive; however, many exceptions to this rule do exist. More complicated predictive calculations, such as those discussed in the next section of the explosive materials article, result in more accurate predictions."

2) RE (Relative Effectiveness) depends on the application and can be a quick and easy way to get a good approximation of what would be a suitable charge size to use in a certain application. It is a method used by the military and keep in mind they typically use a large excess of explosives per shot.

3) Check out the forum library. A good place to start is "The chemistry of Powder and Explosives" which is free to download. There are many great texts on explosives, many of which can be found online quite easily.


[Edited on 1-8-2015 by Hennig Brand]

James Ikanov - 31-7-2015 at 12:37

Based on the labeling I'm estimating the amount of "Reb A" to be roughly 0.045 grams per gram of sweetener at maximum.... but, the labeling could be misleading.

I reached this conclusion because the ingredients are listed as 2g per packet, with 2g of erythritol in each packet. The labeling usually goes out to at least 0.1 grams, meaning that there is less than 0.1g per 2g of erythritol.

I am aware that there is much purer erythritol available, and there are a wide number of reasons I chose to use this particular sweetener, partly logistical and also simply for curiosity's sake to see if it was possible. It might save me some trouble if I can simply go to the grocery store rather than wait two weeks for each shipment. Perhaps even some money. That said if it negatively effects the end product then it's not really worth it I suppose.

After doing some reading I found a rough look at what REB A consists of and I must say I'm very interested in a more proffesional analysis of what might occur if it was nitrated.... everything about this structure based on my limited knowledge of chemistry screams that it's potentially something that could cause serious interference or adopt it's own explosive properties....

https://en.wikipedia.org/wiki/Rebaudioside_A


And again, thank you for the information!

Edit: after drying my crystals I took a small sample and burned it under the tip of a propane blowtorch. Something interesting that I haven't seen or heard specifically described happened: as the ETN deflagrated, the flame was a very distinct blue and then slowly flashed a bright, almost "aluminum burning" white before disappearing entirely. It was more like watching a very fast thermite.

Is this a common occurrence or no? I'm curious if the small amount of Reb A may have actually significantly altered the properties of my ETN batch.


[Edited on 31-7-2015 by James Ikanov]



[Edited on 1-8-2015 by James Ikanov]

kecskesajt - 1-8-2015 at 21:22

I want to preform a reaction:

From the past days,I made quite a large amount of benzoic acid.
I want to sulphonate to benzene sulphonic acid.
If I add benzoic acid to cc. H2SO4, and heat it to 60 C°, will it get decarboxylated and sulphonated or just sulphonated to benzenesulphonic acid?
And add nitric acid of course to get nitrobenzene.
----------------------------------------------------
Is there any OTC ways to get higher nitrated form of benzene like di or tri nitro benzene?
I don't have dicromated nor TNT.

PHILOU Zrealone - 2-8-2015 at 11:11

@James Ikanov ,

Rebaudioside is <5% in stevia/erythritol. I use the 99% Erythritol - 1% Stevioside blend from Carrefour big departement store in Europe.

If rebaudioside is nitrated it will display the properties of nitrated suggar --> bad stability for storage.
If a few% in ETN, then stabilisation will be lower...and even 1% might be a trouble...yellow color may mean decomposition (NxOy). So recrystalization is a must!

ETN is overoxygenated (positive OB) then it will burn blue to white since all the carbon and hydrogen in the molecule will find oxygen in the molecule to fully burn. Aromatic fuels and explosives usually display negative OB and are underoxygenated...carbon/sooth usually remains after burning what renders the flame yellow and fuliginous.

[Edited on 2-8-2015 by PHILOU Zrealone]

battoussai114 - 2-8-2015 at 11:38

Would you rather boil a solution of acetate with excess acetic acid, or try to separate different acetates?
I've used excess acetic acid to get zinc acetate from some leftover zinc carbonate I had and now I need to get the acetate... but I'm still divided between having my house smelling like vinegar or trying to exploit the solubility of the zinc and some other acetate to separate them.

aga - 2-8-2015 at 13:12

There are times when it's better to just let it go ...

(this not a reference to farting in a lift)

iloveloli - 11-8-2015 at 02:09

I have a question about lead(ii) azide. I mix lead(ii) nitrate solution and potassium azide solution together. The potassium azide solution contain a little bit N2H4. Then i get a pink powder.
I took really little of the power and burn it. it explode and make a loud sound.:o:o
I didn't dry it as it is too terrible........
what is it? i don't thing it is just PbN6.

PHILOU Zrealone - 11-8-2015 at 04:34

Quote: Originally posted by iloveloli  
I have a question about lead(ii) azide. I mix lead(ii) nitrate solution and potassium azide solution together. The potassium azide solution contain a little bit N2H4. Then i get a pink powder.
I took really little of the power and burn it. it explode and make a loud sound.:o:o
I didn't dry it as it is too terrible........
what is it? i don't thing it is just PbN6.

What makes you think that it is more than just Pb(N3)2?
Did you tried it alone as comparison?

N2H4 doesn't complexate with lead (Pb(2+)) like it does with Ni(2+), Zn(2+), Co(2+), Cu(2+),... with such cations unsoluble sensitive complexes may form like Ni(N2H4)3(NO3)2.

N2H4 nitrate (N2H5NO3) is very soluble and deliquescent.

nitro-genes - 11-8-2015 at 05:47

Never seen a pinkish colour for lead azide, what was the source of the potassium azide and lead nitrate? Since you mention hydrazine present, I assume it was synthesized? The pH was presumably much higher when free hydrazine or KOH was present, which might have precipitated a form of basic lead azide (Does it exist?), alternatively, it may have formed a double salt :D. The obtained yield may give some information, or careful destruction of a well measured amount using acidified nitrite and measure nitrogen gas formed. If a double salt has formed, start some extensive testing of the compound and patent it ASAP! :D

[Edited on 11-8-2015 by nitro-genes]

nitroglycerin from h2so4 and kno3

Antoine - 18-8-2015 at 01:55

Hi, I've got a little question, it is possible to make nitroglycerin from potassium nitrate and sulfuric acid instead of nitric acid?
sorry for my poor english :D

kecskesajt - 18-8-2015 at 03:32

It was discoussed many times in this webpage.

gdflp - 18-8-2015 at 08:20

Search the website, this has been discussed many times in this thread.

Bert - 20-8-2015 at 15:52

Does anyone have hands on experience with a mixture of 70:30 Potassium chlorate:cupric thiocyanate?

It is said to be a flame sensitive primary explosive, is there a VoD published anywhere?

PHILOU Zrealone - 21-8-2015 at 02:04

Quote: Originally posted by Bert  
Does anyone have hands on experience with a mixture of 70:30 Potassium chlorate:cupric thiocyanate?

It is said to be a flame sensitive primary explosive, is there a VoD published anywhere?

Good finding Bert,
I have like 50kg of KSCN and NH4SCN... I knew it was of a certain value for energetic materials.

I don't know the VOD nor the power; I haven't done it yet.

From what I know:
-Cyanides and thiocyanates are good ways to store energy thus energetic fuels. Energy output will be greater than with other more common fuels.
-Stoechiometric intimate mixes of chlorates with those must be brisant especially with the non hygroscopic ones (unsoluble) and/or with heavy metal ones (Ag, Cu, Hg).
-Copper may be an activator of sensitivity of chlorate...I had chlorate based black powder stabilised with CuCO3, Cu(OH)Cl and/or CaCO3/CuCl2 smelling chlorine after a while; the basic nature of those compounds was to catch acidity of the sulfur and avoid formation of HClO3; the copper was for green-blue flame color.

--> So Cu(2+)/Cu(+) may be catalyst of decomposition; lowering the activation energy.
--> Great care must be taken with handling, with quantities and with storage (never in hard casing like hard plastic, glass or iron)! Check on a regular basis the smell and look of it.
If stored, store away from chemicals, flamable compounds or damageable valuable stuffs ... just in case of a bad event!

Maybe the unstability comes from Cu(ClO3)2?
Copper chlorate tread
Cu(ClO3)2

About the stability of the ingredients...
It seems Cu(SCN)2 is in the line of Cu(CN)2 and unstable towards water...
Cu(CN)2
Cu(SCN)2

[Edited on 21-8-2015 by PHILOU Zrealone]

Bert - 21-8-2015 at 09:30

I asked this question as some 15 year old devices composed of this were among a store of old special effects supplies I removed from a venue for safe destruction off site-

The devices are essentially an electric match head coated with this composition, bound with a nitrocellulose lacquer. They were designed to initiate shock tube, such as NonEl or NoMatch.

I believe they have degraded due to age (and probably atmospheric moisture, they were not stored in a sealed container with dessicant).

A couple went BANG! very nicely, most just give a sad little spit.

Where does the Oxygen come from?

MadCompSci - 1-9-2015 at 20:16

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

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

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

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

franklyn - 1-9-2015 at 22:03

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

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

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

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

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

Microtek - 1-9-2015 at 23:32

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

phlogiston - 1-9-2015 at 23:36

If oxygen from any other source participates in the reaction, they should include it. Otherwise it is simply wrong.
Quote:
5O2 + 4KNO3 + 2C6H4O6 -> 12CO2 + 4H2O + 2N2 + 2K2CO3


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

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

Fulmen - 2-9-2015 at 00:41

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

PHILOU Zrealone - 2-9-2015 at 05:06

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

Metacelsus - 2-9-2015 at 05:17

The correct equation is:

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

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

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

Bert - 9-9-2015 at 15:36



In explanation of the circumstances leading to this question:
Quote:

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




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

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

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

Edit:

It's gone totally Pousse-café!

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

Also the layers are STRATIFIED IN TEMPERATURE.

Sitting in a 40C water bath:

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

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

Bottom layer: 35C.

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

[Edited on 10-9-2015 by Bert]

[Edited on 13-9-2015 by Bert]

James Ikanov - 9-9-2015 at 21:28

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

How long has it been mixed like that, and under what conditions?

PHILOU Zrealone - 10-9-2015 at 05:26

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

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

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

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

James Ikanov - 11-9-2015 at 22:22

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

Am I missing something here?

PHILOU Zrealone - 12-9-2015 at 02:54

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

Am I missing something here?

Fractionally crystalization not distillation.

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

Did you test the poured unfrozen liquid?

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

James Ikanov - 12-9-2015 at 18:27

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

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

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

Mr.Greeenix - 14-9-2015 at 04:45

TKX-50

dichloroglyoxime is the starting material for TKX-50.

i found a good prepartion method for it!?

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


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

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

thanks

PHILOU Zrealone - 14-9-2015 at 06:36

Quote: Originally posted by Mr.Greeenix  
TKX-50

dichloroglyoxime is the starting material for TKX-50.

i found a good prepartion method for it!?

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


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

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

thanks

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

Maybe they mean dichlorofuroxan or dichloroglyoxime

Mr.Greeenix - 14-9-2015 at 11:51

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

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


roXefeller - 17-9-2015 at 09:23

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

Attachment: US5476967.pdf (706kB)
This file has been downloaded 422 times

Higher density dopes for active base dynamites?

Bert - 19-9-2015 at 00:31

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

Off the top of your head-

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

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

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

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

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

[Edited on 19-9-2015 by Bert]

TATP detonator? WHy?

Grantr - 19-9-2015 at 16:35

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

If the stuff is so unstable why are people using it? It seems to be a death wish.

KesterDraconis - 19-9-2015 at 19:29

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

ecos - 20-9-2015 at 03:19

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

Off the top of your head-

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

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

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

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

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

[Edited on 19-9-2015 by Bert]


I like this question !

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

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

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

Tabun - 20-9-2015 at 03:35

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

Gargamel - 20-9-2015 at 10:45

Quote:

TATP detonator? WHy?


Same as HMTD:

-precursors are relatively easy to get

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

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

That's what makes it popular with many hobbyists.
It's a more dangerous shortcut to successful blasts.

NeonPulse - 20-9-2015 at 15:41

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

Marvin - 20-9-2015 at 16:17

Bert,

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