Sciencemadness Discussion Board - Ag2C2.AGNO3 (DS)

Ag2C2.AGNO3 (DS)

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DrManhattan - 2-12-2018 at 00:22

In this video, they are using a solution of copper sulfate to wash the raw acetylene gas. Has anyone tried this?

https://youtu.be/F_TIVJS-lFc

Yes, i use a copper sulfate solution to purify my acetylene. Without it my batch came out in match head sized chunks and black. Running it through the copper sulfate solution changed it to off white/very light brown powder.

DrManhattan - 2-12-2018 at 00:32

I managed to find out why my caps were failing. I suspected that my SADS was not the problem so i made a cap minus the ETN and it fired fine. So i was thinking that my ETN was the problem. I dissolved a gram in acetone and let it dry out. Once the acetone had evaporated i had nice crystals but they were damp with some sort of liquid so i let it dry out for a few days till it was bone dry, assembled the cap and it fired fine. I guess the silver acetylide was absorbing whatever the liquid was and making it very insensitive to initiation. Strange since the ETN was allowed to dry out for 3 weeks and seemed to be totally dry.

markx - 3-12-2018 at 12:48

I've recristallised with ethanol. Dissolve the maximum amount in near boiling EtOH over a water bath of course and then set to deep freeze to drop out the product. The solution above the precipitate shall contain a lot of yellowish contaminants. Filter the batch and wash with distilled water. Most of the contaminants shall be removed by the solution passing through the filter and the product left behind is of a very nice flaky appearance with no noticeable impurities that could cause problems.

FeedMe94 - 27-3-2019 at 23:31

Quote: Originally posted by MineMan

hmm

What LoL is proposing should certainly work, but the issue is if this goes of the primary is now 4-8 times more powerful resulting in some bad damage.

It is interesting, but LoL, CHP works fine.

75mg of SADS fails to kick off PETN sometimes... so this could be a real help to that.

Well i know its an old post but... Today 85mg SADS failed to detonate hard hand pressed PETN. Should i try the KCLO3 mix ?

MineMan - 28-3-2019 at 09:26

Quote: Originally posted by FeedMe94

Quote: Originally posted by MineMan

Well i know its an old post but... Today 85mg SADS failed to detonate hard hand pressed PETN. Should i try the KCLO3 mix ?

I like using KCLO4 instead. But yes. Add 30 percent. Just grind your KCLO4 as fine as possible. Secondly, use a renforcing cap. Davis describes the glowing benefits of this...

It’s eseentially a strong plug above the primary.

FeedMe94 - 29-3-2019 at 02:42

[/rquote]

I like using KCLO4 instead. But yes. Add 30 percent. Just grind your KCLO4 as fine as possible. Secondly, use a renforcing cap. Davis describes the glowing benefits of this...

It’s eseentially a strong plug above the primary. [/rquote]

I have plenty KCLO4 so i will try it. Also i didnt have good plug above primary a bit of tissue paper to hold the visco fuse

XeonTheMGPony - 29-3-2019 at 03:30

Quote: Originally posted by FeedMe94

[/rquote]

I like using KCLO4 instead. But yes. Add 30 percent. Just grind your KCLO4 as fine as possible. Secondly, use a renforcing cap. Davis describes the glowing benefits of this...

It’s eseentially a strong plug above the primary. [/rquote]

I have plenty KCLO4 so i will try it. Also i didnt have good plug above primary a bit of tissue paper to hold the visco fuse

This is why I glue and crimp, you really really really need that to ensure good initiation when using non Azide primaries, it is a good guarantee and performance enhancer.

If you have the capability Nitro Lacquer makes for a fast simple glue of relative fast drying time.

Update Wiki - New method synthesis

Vpatent357 - 19-6-2020 at 13:45

"Instead of the conventional synthesis of passing acetylene gas through silver nitrate solution, a purer and whiter precipitate can be formed by passing acetylene gas through acetone and adding the acetylene solution drop-wise to a dilute silver nitrate and nitric acid solution at ambient room temperature."

Update Wikipedia

What do you think of that method for prepare SADS ?

[Edited on 19-6-2020 by Vpatent357]

Belowzero - 19-6-2020 at 22:31

This could be interesting it would be much easier to control the particle size.
Passing the gas through directly gives amorphous chunks of different sizes which are somewhat annoying to handle.
Usually higher temperatures give better results but this would force the gas from the solution.
Surely this is less messy than the traditional method.

B(a)P - 22-6-2020 at 01:11

Quote: Originally posted by Vpatent357

"Instead of the conventional synthesis of passing acetylene gas through silver nitrate solution, a purer and whiter precipitate can be formed by passing acetylene gas through acetone and adding the acetylene solution drop-wise to a dilute silver nitrate and nitric acid solution at ambient room temperature."

Update Wikipedia

What do you think of that method for prepare SADS ?

[Edited on 19-6-2020 by Vpatent357]

I tried this method over the weekend. The resulting product was slightly off white with a very even and fine grain size. The yield was 96% based on silver.

Belowzero - 26-6-2020 at 05:53

I tried the synthesis using dissolved acetylene in aceton.

5 grams of acetone was put in a test tube, the testtube was placed in water just above freezing.
A glass pipet was used to bubble the acetylene from a calciumcarbide/water generator, roughly 10 grams.

An attempt was made to weigh the disolved acetylene but my scale was unable to register the weight gained.
Partly due to the spilling of the acetone since the gas generator was hard to control.

.5 gram of silver nitrate was dissolved in 30 gram of boiling water and filtered since something contaminated my silvernitrate and went out of solution.

The nitrate solution was allowed to cool just above room temperature roughly 35 degrees C.
The acetelyne/aceton solution was added to the silvernitrate solution in 3 steps and a white percipitate inmediately formed.

The SADS was transfered to a gravity filtration setup and washed with distilled water and a few ml of acetone.
Yield still has to be measured.

Improvements:
Drip the water into the acetylene generator for better flow control.

A washing bottle(s) to purify the acetylene.

Even this crude attempt results in a far better product than using the 'traditional' method.
The SADS is just slightly off-white, I'll follow up with pictures of the dry material.

[Edited on 26-6-2020 by Belowzero]

B(a)P - 26-6-2020 at 13:46

Quote: Originally posted by Belowzero

5 grams of acetone was put in a test tube

Improvements:
Drip the water into the acetylene generator for better flow control.

A washing bottle(s) to purify the acetylene.

I'll follow up with pictures of the dry material

[Edited on 26-6-2020 by Belowzero]

Nice write up thanks!

You could try using a measuring cylinder instead of a test tube to give you more freeboard.

I have good success slowing the generation of acetylene by adding I've instead of water to the carbide.

Please report back on your yield when your product is dry.

fdnjj6 - 22-7-2020 at 18:31

I have come up with a way better and cleaner synthesis during experimenting. I was frustrated with getting off colored SADS and began runing tests altering temperature, different scrubbers, amount of acetylene, and time. This was using calcium carbide as the acetylene source. I recorded everything and the hot solution resulted in very white SADS BUUUT they were in globs and covered in a black impurity.

My improved synthesis involves bubbling the acetylene into acetone which basically purifies it extremely well. Then I add the acetone/acetylene solution drop wise with good stirring to the AgNO3 and HNO3 solution. A perfectly white precipitate forms. I have had other people on Reddit test it out and they reported perfect results as well.

fdnjj6 - 22-7-2020 at 18:35

Damn it I did not see the other post already. I used the search option to find acetone and since he spelled it aceton, nothing popped up. I figured no one mentioned it yet.

I'm not sure if he figured this out before me but I had figured this out and posted my results on just about every sub reddit I could find that does explosives, months ago. I thought I was the first since no one had ever mentioned it on the internet and it was a discovery I made during my experimentation. Based off of the replies I got on my post, it sounded like I was the first. I'm not sure though since something could've been hidden or someone just never posted about it.

fdnjj6 - 22-7-2020 at 18:38

Sorry to spam but the yields I get are around 100% It is a very efficient reaction. I wash everything with water and acetone to let it dry faster. A day later and it's ready for use in ETN/SADS detonators. It needs to be completely dry. Even samples that look dry often don't detonate properly or at all.

B(a)P - 23-7-2020 at 20:20

Quote: Originally posted by fdnjj6

Damn it I did not see the other post already. I used the search option to find acetone and since he spelled it aceton, nothing popped up. I figured no one mentioned it yet.

I'm not sure if he figured this out before me but I had figured this out and posted my results on just about every sub reddit I could find that does explosives, months ago. I thought I was the first since no one had ever mentioned it on the internet and it was a discovery I made during my experimentation. Based off of the replies I got on my post, it sounded like I was the first. I'm not sure though since something could've been hidden or someone just never posted about it.

I think that @Vpatent357 found the method on Wikipedia, rather than developing it themselves.

Out of interest have you compared performance between SADS from the acetylene dissolved in acetone method vs SADS from the more tradition method? I have found that generally it appears the same, but this is just based on some pretty subjective very small scale testing. When I find a spare day I intend to make some caps with SADS, some from the acetone method and some from the more traditional method. I plan to detonate them on a witness plate to make sure the performance is comparable before I use it to initiate a secondary.

fdnjj6 - 27-7-2020 at 21:21

Haha funnily enough I was the one to edit that section in as soon as I figured it out. I was so ecstatic to have finally discovered something I thought no one had before and so I posted it everywhere I could. I had forgotten that I edited it on wikipedia as well. I should see if I can add it to the sciencemadness wiki as well. If you find my post on Reddit under the explosionandfire subreddit you'll see it was posted in April. If you go to the Wikipedia article you'll see the last edit was in April. I was the one who made the last edit which was where I added in the pure white part. Since I am not a professional and that was (what I believe to be) my own discovery, I didn't add any references. Hence, the big section in the middle of the article with 0 references.

EDIT: I just added my username to the article. I don't know if that's supposed to be done but that way it gives some more credibility since it was initially lacking any references of some sort.

Regarding your post, I didn't see much of a difference. In my initial attempts at making SADS I formed more SA than SADS due to lack to nitric acid and so it didn't form the double salt completely. There I was able to see a lot more carbon left over and it was weaker. Besides that there were no differences besides purity/color.

I believe that the light sensitivity had decreased a fair bit but it still was light sensitive. The main difference really was just color and purity. There were no more black or tan silver salts forming from acetylene impurities. From a technical perspective, since more SADS is there due to lack of impurities you would yield more energy but I think that the power difference is negligible.

[Edited on 28-7-2020 by fdnjj6]

[Edited on 28-7-2020 by fdnjj6]

dangerous amateur - 31-8-2020 at 08:15

The thread is very long, so please forgive me if i overlooked these informations.

I wonder if the amount of surplus acid in the solution is crucial to succes, or has an influence on the results?
Most data points to some a 32% acid solution.

I'm asking because I would like to use silver nitrate, which I have plenty in stock.
Is there any reason why some people prefer silver over its nitrate?

Also since HNO3 is no so easily available these days, I like to save mine as good as possible. Just imagine you have to use the Birkeland process some time in future. What a mess... Nothing to waste here

So - is such a strong solution really necessary to obtain proper results?

Second question:
Considering markxs mixture with KClO3:
Is there a mixing technique that has proven effective?
It's been a while since I worked with DS but I rember it to have a tendency to from granules, or at least little agglomerations... To mix this perfectly homogenous with KClO3 in dry state should be quite enerving.
Careful diapering, squezing...

Or would you rather use a wet process and break the resulting lumps afterwards?

My KClO3 contains a little silicon dioxide based anticake, maybe that helps a little...

markx - 5-9-2020 at 02:30

Acid content in the reaction mixture does have an effect upon the properties of the resulting ds. Higher acid content yields a more energetic product, but temperature control is the most critical parameter. Agglomeration of the product is quite normal, but is easily reversed if product was made under optimal conditions of acidity and temperature. Stronger granulation suggests not optimal reaction conditions....I’ve observed it happening if the temperature “sweet spot” was intentinally missed towards higher values. Manipulating any mixes of primaries is quite unnerving and requires a lot of care towards safety measures. I would suggest to use a wet process with a easily evaporated solvent like alcohol. And do not go overboard with the homogenisation....the reinforcing effects of the oxydiser are clearly observable with less than perfect mixing.

dangerous amateur - 7-9-2020 at 07:18

Thanks for sharing your experience markx.

Yes I know that acid content has some influence, but I hoped to save a little of that precious forbidden stuff.
So it has to be 30%.

Quote:

I would suggest to use a wet process with a easily evaporated solvent like alcohol

A solvent? Or rather a temporary phlegmatizer?

My choice would be isopropanol. This is not likely to dissolve a lot chlorate.

Still, to exactly measure the right amount, I cannot reduce the batches so much. It has to be 1g, I cannot scale smaller amounts with precision.

[Edited on 7-9-2020 by dangerous amateur]

markx - 8-9-2020 at 00:31

Quote: Originally posted by dangerous amateur

Thanks for sharing your experience markx.

Yes I know that acid content has some influence, but I hoped to save a little of that precious forbidden stuff.
So it has to be 30%.

Quote:

I would suggest to use a wet process with a easily evaporated solvent like alcohol

You can experiment with lesser acid content while still exercising temperature control to see if this has a deterioratory effect upon the vigor of the product.

Yes the "solvent" is more of a phlegmatizer if (per)chlorate is used as the sole dopant. Not so much if nitro(ester) compounds are used for the doping purposes. Would not suggest the latter though.....as impressive as the mix is, it still poses a devastating risk upon one's safety. And the sensitivity + stability aspects are rather unknown.

Please try to keep the amounts that you intend to mix as small as possible. One gram range does not nearly qualify as small scale. There are very satisfactory electronic milligram range scales available and their price is ridiculously low. It would be a good idea to invest in one, if further experimentation in such a field is the goal.

dangerous amateur - 8-9-2020 at 05:31

Actually I have a scale with a 1mg resolution. Thats definitely not 1mg precision though.
edit: my scale is very similar to yours. I dont say it's impossible, but I would say forget about the 1mg digit...

100mg + 25mg should be doable, but the margin of error from batch to batch will be considerably.

I believe I could pretect myself adequately, but I hate to have to explain the bang.

Say - what is in your experience the lower limit for reliable initiation of not to hard pressed (lets assume a density of something like 1,1 - 1,2) ETN or PETN?

I had failures with ca 150mg, but that was a long time ago when I did not monitor everything so closely...

From the experience shared in this thread I would use at least 150mg...

Another question:
What is your experience with decomposing DS, especially with long term storage, and when in contact with ETN or KClO₃:
How easy is the acid liberated, and if it is, what will it do - especially considering auto-ignitions or the like.

Storage stability is one thing, safety is another...
I do not intent to store anything longer than necessary, but you never know.

My feeling is to separete the ETN/PETN somehow from the DS...

[Edited on 8-9-2020 by dangerous amateur]

[Edited on 8-9-2020 by dangerous amateur]

markx - 10-9-2020 at 22:09

Quote: Originally posted by dangerous amateur

Say - what is in your experience the lower limit for reliable initiation of not to hard pressed (lets assume a density of something like 1,1 - 1,2) ETN or PETN?

I had failures with ca 150mg, but that was a long time ago when I did not monitor everything so closely...

From the experience shared in this thread I would use at least 150mg...

Another question:
What is your experience with decomposing DS, especially with long term storage, and when in contact with ETN or KClO₃:
How easy is the acid liberated, and if it is, what will it do - especially considering auto-ignitions or the like.

Storage stability is one thing, safety is another...
I do not intent to store anything longer than necessary, but you never know.

My feeling is to separete the ETN/PETN somehow from the DS...

[Edited on 8-9-2020 by dangerous amateur]

[Edited on 8-9-2020 by dangerous amateur]

Depends on a lot of factors and the actual construction of the energetic train. I've had repeated success with as little as 40mg DS, but on the other hand straying from the successful combination regarding any parameters or components can land you in a zone where 150mg is not enough. So I would say use whatever combination works for you. There is really no universal baseline to rely on regarding amounts.

DS seems not to like storage when it is mixed with any additives. Visual darkening proceeds faster even in dark. But in the pure form and kept damp, dark and cool....a few years seems a breeze.

dangerous amateur - 1-10-2020 at 07:28

I'll have to experiment...
Thank you very much for your insight

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