Sciencemadness Discussion Board - Silver Acetylide synthesis

Silver Acetylide synthesis

Phantom - 20-7-2011 at 14:34

I'm about to make some Ag2C2 * AgNO3 and I heard lots of things about it.
Acetylene from CaC2 usually contains hydrogen phosphide and hydrogen sulphide, and sometimes ammonia ?

I found a synthesis which appears to be safe :

http://www.powerlabs.org/chemlabs/acetylide.htm

Any Tips ?

AndersHoveland - 20-7-2011 at 15:27

What would happen if acetylene were bubbled into a solution of tin(II) perchlorate?
Possibly Sn3(C2)2(ClO4)2 ?

http://www.shadowrx.com/forums/showthread.php?t=1516

The WiZard is In - 20-7-2011 at 18:03

Quote: Originally posted by Phantom

I'm about to make some Ag2C2 * AgNO3 and I heard lots of things about it.
Acetylene from CaC2 usually contains hydrogen phosphide and hydrogen sulphide, and sometimes ammonia ?

I found a synthesis which appears to be safe :

http://www.powerlabs.org/chemlabs/acetylide.htm

Any Tips ?

Without eye balling the link you supply, I would suggest an
analogy.

This is like asking if the procedures to get your Bugatti Veyron
up to 240 mph or to raise cobra's is safe? The problem is
not with the procedure — it is with the results.

Dobe written down in books —

Silver[most all] aceylide - very sensitive to mechanical action.

The acetylides must be handled with extreme care in storage
must be kept cool and wet.

djh
---
It is essential that persons having explosive
substances under their charge should never
lose sight of the conviction that, preventive
measures should always be prescribed
on the hypothesis of an explosion.

Marcellin Berthelot - 1892
Explosives and their power - Page 47

The WiZard is In - 20-7-2011 at 18:38

Quote: Originally posted by AndersHoveland

What would happen if acetylene were bubbled into a solution of tin(II) perchlorate?
Possibly Sn3(C2)2(ClO4)2 ?

http://www.shadowrx.com/forums/showthread.php?t=1516

Noted in passing ....

PATR 2700 C79 mentions a ref. to the synthesis of silver
acetylide ... [by] passing a rapid stream of acetylene through
an aq N/10 soln of silver perchlorate contg 10% ammonia.

[Father] Julius A Nieuwland & Richard R Vogt
The Chemistry of Acetylene
Reinhold 1945

Devote 18 pages of Chapter Two - Mettallo-Derivatives of
Acetylene to aceylides, I find not mention of tin.

I would mention once again --

A few explosives such as cuprous acetylide, [all acetylides]
do not form gases

Cu2C2 --> 2 Cu + 2C

because the heat liberated is not sufficient to gasify the products.
In such cases, the explosive effect is due to the rapidity of liberation of heat and its expansive effect on adjacent air.

TM 9-1910
Military Explosives
1955

Phantom - 21-7-2011 at 00:14

You mean silver acetylide is more dangerous when you press few mg to a strw than HMTD?

quicksilver - 21-7-2011 at 08:37

The term "danger" is all relative. There really isn't any "safe". The levels industry goes to minimize inappropriate detonations is pretty in-depth. From shielding, automation (robotics), distance, weigh / size, & composition synthesis; the methods employed are generally plant-based. As soon as this steps to a laboratory environment, no matter the primary, the "danger levels" goes up substantially.
The generality is often in the level of professionalism (& expenditure) within manufacture. So that it could be said that the lower the level of professionalism, the higher the risk from a primary HE. Once the laboratory is the place of synthesis, the danger factor cannot be avoided by composition. If this aspect is maintained, the operator will do all he can to maximize the mechanisms with a plant structure (rather than a laboratory).

Distance is a substantial agenda due to the shock wave issue & by-product fragmentation. Most all modern industrial setting utilize both shielding and distance to maximize this feature. Weight / size is another issue that can be controlled & although this decreases productivity, it also increases the likelihood of a detonation halting the production. in research, the need for larger levels of material is not necessary so that sub-gram units can be controlled more effectively in more simplistic means. But the laboratory is generally the most dangerous place in which to synthesize often due to the demand for glass structures. industry in not impeded by this. In the modern laboratory portable shielding is common place, weights are kept very low, & physical mixing are studied prior to the synthesis being started.

Realistically, anything less is very dangerous no matter the material. The concept of a "gas-less" primary was attractive as originally, gaseous by products of detonation were thought to contribute to shock-wave damage. This is not true, The USBoM has enough background to determine what common materials are more friction, impact, or heat sensitive than others but as a class, Primary HE display those features as a matter of course. The concept of the EBW detonation device was due in most part to the lack of ability to find a "safer" Primary.

EAPyrotox - 28-7-2011 at 10:35

I recently did another batch, but I usually clean in this order:
water => denatured alcohol => acetone,
but this time I added a wash with baking soda and I had bad results (white strains in gray SA + lack of power).

What do you think? is it useful to neutralize SA?

[Edited on 28-7-2011 by EAPyrotox]

Neitz - 5-12-2012 at 11:15

I am as well preparing for my first silver acetylide synth. Now, I wonder, how's with it's properties(different sesitivities). I am still researching it before hand, but when I synth it, I intend to try everything out myself. All the info is kind of scattered, so could someone write or direct me to it's properties and synth hazards?

I already took this article into consideration(http://www.sciencemadness.org/talk/viewthread.php?tid=1031&a...). I intend to first synth Ag2C2 by the powerlab method, and later also Ag2C2*NO3. And for the latter I have a question: do you first disolve AgNO3 in distilled water and then add HNO3 or vice versa and what are the quantities of AgNO3/H2O/HNO3 I should use?

Thanks!

Mailinmypocket - 5-12-2012 at 15:39

Quote: Originally posted by Neitz

I am as well preparing for my first silver acetylide synth. Now, I wonder, how's with it's properties(different sesitivities). I am still researching it before hand, but when I synth it, I intend to try everything out myself. All the info is kind of scattered, so could someone write or direct me to it's properties and synth hazards?

I already took this article into consideration(http://www.sciencemadness.org/talk/viewthread.php?tid=1031&a...). I intend to first synth Ag2C2 by the powerlab method, and later also Ag2C2*NO3. And for the latter I have a question: do you first disolve AgNO3 in distilled water and then add HNO3 or vice versa and what are the quantities of AgNO3/H2O/HNO3 I should use?

Thanks!

Forum member Woelen has a very nice experiment with it that puts powerlab's to shame

See here:

http://woelen.homescience.net/science/chem/exps/silveracetyl...

CaliusOptimus - 5-12-2012 at 18:48

Run your acetylene through a wash bottle of dilute nitric acid before it goes into the silver nitrate solution. It helps to remove traces of other things from the impure calcium carbide, providing a cleaner product. Use a plastic gas tube, and a plastic graduated flask for the reaction. Find as small a tube as you can, tinier tube means smaller bubbles. Filter and wash on a plastic buchner funnel. Wash with acetone for a fast dry at room temp. Handle only in a humid and static-free environment.

Formatik - 7-12-2012 at 05:58

Quote: Originally posted by Neitz

All the info is kind of scattered, so could someone write or direct me to it's properties and synth hazards?

Silver acetylide, moreover its complexes, are extremely sensitive to static discharge (moreso than other primaries). Its complexes are extremely static sensitive even if they are less impact sensitive and worthless as detonants (an example is silver chloride-acetylide made from ammonicial AgCl and C2H2). In that regard silver acetylide is like silver azotetrazolate, but not silver diazoaminotetrazolate which does not posses this extreme static sensitivity. Note there is a big thread decrying the static sensitivity of silver acetylide, feel free to read it.

Neitz - 10-12-2012 at 07:02

Quote: Originally posted by Mailinmypocket

See here:

http://woelen.homescience.net/science/chem/exps/silveracetyl...

Wow, this is great. Thanks guys.

I'm going to try both methods, one for the disalt and the powerlab's method for the Ag2C2 only. I want to compare the two. Will post results

[Edited on 10-12-2012 by Neitz]

Neitz - 12-12-2012 at 10:14

Quote: Originally posted by CaliusOptimus

Run your acetylene through a wash bottle of dilute nitric acid before it goes into the silver nitrate solution.

Is this step needed when you are working with Silver nitrate solution in nitric acid?
Also, for preparation of this solution, it says on the site given:
Easiest is to take a spatula full of silver nitrate and dissolve this in a 5% to 10% solution of nitric acid

Does this mean diluted nitric acid or the mass percentage of the end solution?

Swede - 12-12-2012 at 17:10

It means add the silver nitrate to a solution that is 5 to 10% HNO3.

The washing of the acetylene is recommended when using calcium carbide as an acetylene source, but in the two times I've tried the reaction, I did not do it but still had success.

This stuff is ear-splitting loud. A few grains, sprinkled and spaced out on a concrete floor, will transmit shock to each other, and touching off one xtal on the edge can set them all off. I'd keep the mass low; it's easy to make too much by mistake.

Neitz - 13-12-2012 at 05:55

Yes, of course, with explosives it's always good to remain at small quantities

. I intend to do more series of explosions, where I would always produce a new smaller batch of it, since the synth. is relatively easy.

Also, is there a possibility of glass shrapnel in a premature detonation? Logically if there isn't enough energy for production of gas products, the pressure won't go up, thus no expansion will be present. But I wonder if the sound can shatter it?

Swede - 13-12-2012 at 08:13

Any leftovers should be stored in a small poly vial under water. I'd avoid glass. It is a primary, after all, and will easily shatter glass.

Check regularly to ensure the water does not evaporate off, which it can do even from a sealed vial. It's no fun to find something like that after a few months "high and dry" with no H2O.

Neitz - 13-12-2012 at 08:30

Yeah, I do not mean to store it, I will explore it's properties on the run, producing it as I go. I believe that's much safer than actually storing it. And I believe it packs a better punch when it's fresh

Neitz - 21-12-2012 at 07:54

Ok, I produced my first batch of Ag2C2 and I am not completely sure which is it. I used a really thin tube, so that the batch would be bigger, thus I got a white solution that looks like milk with some small greyish flakes in it. I filtered it and separated the flakes from the milky solution, but there is very few flakes so I don't believe that would be Ag2C2 and I also used diluted HNO3 to purify the gas, so I believe that the white solution is Ag2C2. But the particles are so small that they cannot be filtered. Should I just left this over night to see if it settles down?

In addition, it looks like this:

[Edited on 21-12-2012 by Neitz]

gnitseretni - 21-12-2012 at 12:31

I don't think those pics are big enough

plante1999 - 21-12-2012 at 12:40

No, they are not, why not a 4000 by 3000 picture?

Neitz - 22-12-2012 at 05:22

Indeed, you two have been most helpful. Really, I don't need your opinion on picture sizes, if you don't know the answer, just be quiet.

[Edited on 22-12-2012 by Neitz]

[Edited on 22-12-2012 by Neitz]

CaliusOptimus - 22-12-2012 at 17:00

Use a finer filter.

watson.fawkes - 24-12-2012 at 17:37

Quote: Originally posted by Neitz

I don't need your opinion on picture sizes

If you can't exercise the courtesy to scale down your pictures so as not to trash to formatting, don't expect courtesy in return.