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Author: Subject: Ag2C2.AGNO3 (DS)
Vpatent357
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smile.gif posted on 12-7-2014 at 02:37
About Silver Acetylide/Nitrate (SA.DS) synthesis and improvement


1/ Do you think it is bad to wash SA.DS with a solution of sodium bicarbonate (NaHCO3), it will not initiate the decomposition? (leaching silver nitrate salts)
as the wash water is already bad for SA.DS but acid HNO3 in SA.DS maybe could be bad too.. I think
My washing:
100 ml 5% NaHCO3 => 100ml H2O => 50ml ethanol => 50ml acetone
is good?

2/ What the good concentrations of silver nitrate and nitric acid to produce the best possbile double salts (NOT with silver acetylide–hexanitrate Ag2C2·6AgNO3)?
i ear about less 10% wt. for AgNO3 but for acid .. (i use 60% ​​HNO3)
My solution proposed:
1gr silver dilute in 3ml HNO3 60% and add 10ml demineralized water (reaction at 80-90°C)
Good proportions?

3/ It's really useful to use a small Amount (~ 3%) of Iron (III) nitrate - Fe (NO3) 3 in the solution to prevents any precipitation of free silver (as HNO3 already does) which should increase the purity of the product?
http://www.google.com/patents/US2483440 patent US2483440

4/ Silver acetylide have a oxygen balance OB = -26.7%, add % of KCLO3 or other components can adjust/improve efficiency as mercury fulminate? (MF ob = -11.2%)

5/ I am looking for all possible ways to reduce static ESD sensitivity. I thought of adding 1% graphite or 1% conductive carbon black .. give me your opinions

[Edited on 12-7-2014 by Vpatent357]
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[*] posted on 20-7-2014 at 04:55


Quote: Originally posted by Vpatent357  
1/ Do you think it is bad to wash SA.DS with a solution of sodium bicarbonate (NaHCO3), it will not initiate the decomposition? (leaching silver nitrate salts)
as the wash water is already bad for SA.DS but acid HNO3 in SA.DS maybe could be bad too.. I think
My washing:
100 ml 5% NaHCO3 => 100ml H2O => 50ml ethanol => 50ml acetone
is good?

2/ What the good concentrations of silver nitrate and nitric acid to produce the best possbile double salts (NOT with silver acetylide–hexanitrate Ag2C2·6AgNO3)?
i ear about less 10% wt. for AgNO3 but for acid .. (i use 60% ​​HNO3)
My solution proposed:
1gr silver dilute in 3ml HNO3 60% and add 10ml demineralized water (reaction at 80-90°C)
Good proportions?

3/ It's really useful to use a small Amount (~ 3%) of Iron (III) nitrate - Fe (NO3) 3 in the solution to prevents any precipitation of free silver (as HNO3 already does) which should increase the purity of the product?
http://www.google.com/patents/US2483440 patent US2483440

4/ Silver acetylide have a oxygen balance OB = -26.7%, add % of KCLO3 or other components can adjust/improve efficiency as mercury fulminate? (MF ob = -11.2%)

5/ I am looking for all possible ways to reduce static ESD sensitivity. I thought of adding 1% graphite or 1% conductive carbon black .. give me your opinions

[Edited on 12-7-2014 by Vpatent357]



I have come to the conclusion that the following process produces a satisfactory SADS with good stability (towards visual degradation under light and the preservation of initiating ability at least):

2g of metallic silver is added to 10ml of 65% HNO3 + 10ml of distilled water. Silver will dissolve with diffisulty in concentrated nitric acid, hence the dilution with H2O. The mixture is heated in a water bath to speed up the reaction.

(If one has silver nitrate available the previous steps can be skipped and a stoichiometric amount of the salt used directly in combination with nitric acid to acidify the solution.)

Next the solution of silver nitrate and nitric acid is placed in a thermostated water bath at a temperature in the range of 65-70C. Stirring is used if possible (magentic or overhead, both work fine). Another 10ml of distilled water is added to the solution and the solution temperature is let equlilibriate (a thermometer in the reactor is of great help).

The acetylene gas generator is set up and once the temperature has equlibriated the flow of gas is led to the reactor. A syringe needle works very well as a bubbler. I find it is of great help to cool the gas generator with ice inserted directly into the generator fluid. This will help to keep the acetylene formation reaction calm and stable over a prolonged time. The generator can be constructed from a 500ml pet bottle. I have not found to be neccessary to use any additional scrubbing or filtering for the gas. Too much trouble and no difference in product properties. Just keep the gas generator ice cold and the fluid from entering the gas line and the SADS reactor. Keeping things simple is always the best approach for practical applications (well...on the majority of occasions).

Keep the acetylene gas flowing into the silver nitrate solution for several minutes until no more visible percipitate is formed. The precipitate is snow white and voluminous if all is going correctly. The reaction temperature has a profound effect on the product properties with 65-70C being (in my experience) the optimum range. If one drifts from this temperature range, the product will be discolored, have inferiour initiating properties and have a raised sensitivity towards degradation under light. E.g at 85-90C the product will have visibly larger cristals, discolour even in relative darkness and have greatly reduced brisance with a profoundly sooty residue after detonation. At 20-30C the product will dicolour already in the reaction vessel after about one minute of gas flow and will again have inferiour stability against light and relatively reduced brisance (viually and audibly observed). But the product from the optimum 65-70C temperature range will be snow white, stable towards light (it will slightly discolour in sunlight though) and have greatly superiour brisance....a small tab picked up to the tip of a safety match and lit will shatter the wood leaving a pencil like fibrous mess and basically no sooty residue.

After the preciptation is complete I filter the product, wash with coupious amounts of distilled water and store it in the fridge, damp in a ziploc baggy on the same filter paper. If needed, the proper amount is removed from storage and dried on paper in realtive darkness at room temperature. It has remained stable stored either damp or dry over 6 months with no visible discoloration or degradation in properties. Although it would be best to make and use it as needed, as opposed to keeping an old batch on storage for future uses.

I would not advise to wash the product with alkaline neutralising agents like bicarbonate or god forbid ammonia solutions....it will most likely shift the equilibrium towards the formation of silver precipitates or the removal of the nitrate from the double salt. Don't quote me on that, but generic reasoning tends to make me think in that direction. Neither do I think that the addition of ferrous compounds will improve the odds of a more stable product. Again I would observe the path of simplicity...the more components you will have in a system, the more likely are unexpected unfavorable interactions. We are talking about a primary here and hence I would stick to known routines if it is to be stored for use in a further experiment involving secondary energetics. But of course if one wants to just experiment on the SADS alone, regarding mixtures with KClO3 or other OB improvement additives or the ESD sensitivity issues, then go ahead. But cautiously and using small amounts!




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[*] posted on 20-7-2014 at 15:20


I have made this compound a few times in the past but never thought to cool the acetylene generator or use ice instead of water. None of the synthesis methods I followed mentioned it. Would this stop the Brown ppt that forms in the gas line? The brown impurities settled on top of the bubbles leaving the reaction mixture couldn't help for getting a nice clean product either. A small sample that I had was stored in the dark dry and fairly cool 20-25℃ but over a 6 month period it still got progressively darker mostly on the exposed surface though.it still seemed to retain its power. I did make it outside at night and it was fairly clean when stored an off white color. Another time bottled acetylene was used instead of the carbide and this result was much more satisfactory, being very white and staying this way until it was all used.the power was still seemingly the same but less residues were left on the detonation surface. If you can get it bottled gas is the way to go. Also it was suggested to me to pass the acetylene through a washing solution of diluted nitric acid first giving a much cleaner gas for use in this synthesis although I never did try that.



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[*] posted on 1-8-2014 at 15:23


I made videos on the sensitivity of silver acetylide Double salts,
take a look there :)

=> http://www.youtube.com/channel/UCBPOcEPXHNnolfp5ADDM5qw/vide...

and put a little graphite not change the sensitivity of compound to the static discharge test :/

[Edited on 1-8-2014 by Vpatent357]




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[*] posted on 3-8-2014 at 08:29


Why is it necessary to acidify the solution of Silver Nitrate with nitric acid before bubbling acetylene?
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[*] posted on 3-8-2014 at 10:42


Silver Acetylide: Ag2C2
Silver Acetylide Double Salts: Ag2C2.AgNO3

The nitric acid is supplied in excess to make sure the double salt is formed.

I guess the number of silver nitrate groups can vary in double salts. I have attached a journal article which might be of use.



Attachment: Structural Variation in Novel Double Salts of Silver Acetylide with Silver Nitrate.pdf (126kB)
This file has been downloaded 455 times





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[*] posted on 5-8-2014 at 22:48


Just for illustration...the appearance of optimised reaction condition SADS and the damage it did on the tip of a totally innocent, yet expendable safety match:

DSCF0119.JPG - 2MB DSCF0121.JPG - 2MB

Yup, looks about right...




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[*] posted on 6-8-2014 at 09:04


Thanks for your help markx,

I recently got the same result, crystals SADS white snow, a great purity :)
I want to explode ANNMAL I now looking for a secondary explosive fairly easy synthesis and 100% safe to handle,
ETN is too sensitive for me, PETN may be suitable but must have PE and concentrate NA, order PE online may seem suspect ..
I thought about Nitrocellulose Blasting Cap, but I do not know if it is viable,

Cap: 300mg SADS => 700mg wet pressed NC in syringe => 10g ANNMAL

[Edited on 6-8-2014 by Vpatent357]




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[*] posted on 6-8-2014 at 10:30


ETN is not as sensitive as you might think, you're only going to be working with tiny amounts anyway.
People have casted ETN without problems.

Here's a guy that made a blasting cap from it. SADS is more sensitive than ETN.
https://www.youtube.com/watch?v=zkfiKlYDxno
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[*] posted on 7-8-2014 at 02:07


Quote: Originally posted by Manifest  
ETN is not as sensitive as you might think, you're only going to be working with tiny amounts anyway.
People have casted ETN without problems.

Here's a guy that made a blasting cap from it. SADS is more sensitive than ETN.
https://www.youtube.com/watch?v=zkfiKlYDxno


I implore you, please do not attempt the construction method portrayed in the video without proper blast shields and personal protection. It is very dangerous practice to be honest. Metal containment and tools that apply strong forces to a primary explosive in contact with the secondary charge is best to be avoided in amateur practice. For starters I would suggest light plastic containment (like a straw or light foil tube) hand compacted with the secondary charge of choice...recristallised ETN is excellent for that purpose. Use a wooden dowel for compaction, not a metal rod. Strong compaction is not needed, it will only increase the risks during assembly and make initiation more difficult, creating the need for a bigger amount of primary. The primary charge should be constructed separately, e.g. in a separate plastic tube on top of a pyrotechnic composition which can be lit via a safety fuse or e-match. Then the primary and secondary parts of the initiation device can be joined together prior to use, with a few mg of loose secondary inbetween them. This way one can avoid strong forces during assembly and lower the risk of an accident considerably. For hand compacted ETN with a few mg of loose ETN on top, the initiation is reliable upwards from 20mg of SADS in direct contact with the loose part of secondary. I use 40mg now, just to be sure. More than that is just overkill and waste of primary material. I would suggest to first work out a reliable and replicable design for the initiation device with proper testing and assurance on how it behaves. Once you feel confident in its performance and reliablility, then move on to mating it with your secondary test charge of choice. Be safe and do not rush things!




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[*] posted on 7-8-2014 at 12:10


I agree with that too, I find it very dangerous, in the future I already count separate primary and secondary and use cap-placer system,

I saw a YT video [HERE] where the guy was using 200-300mg SADS to set off activated ammonium nitrate charges.

What do you think? Activated ANNMAL is there a viable secondary? and even in small amounts?
It seems have a good sensitivity, and spare me a secondary synthesis as ETN..




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[*] posted on 7-8-2014 at 13:31


Will do, thank you for your warning.
I will use a straw, I was just trying to explain to Vpatent that ETN is not as sensitive as he might think.
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[*] posted on 5-10-2014 at 23:24


For the people who are in command of the russian language:


Attachment: bagal-init.djvu (3.7MB)
This file has been downloaded 238 times


There is a very interesting section on SADS (pages 424-434). Further information can be uncovered following the refereces in the respective section of the book.
I was very surprised to see the impact sensitivity data....79cm drop height with 500g weight. Quick testing of my own product in the drop hammer device confirmed the low impact sensitivity of SADS obtained from acidic heated solution. To my amazement a 6mg sample packed in foil did not detonate under 2kg weight dropped at a height of 60cm....not even after a multitude of attempts. It was also impossible to get it to detonate by directly hitting with a 300g hammer...the sample would flatten and disintegrate after numerous blows on a steel anvil, but did not explode. That kind of impact resistance is more akin to nitramine type of secondaries like rdx. For example ETN goes off at around 30cm in my drop test, making it more than twice as impact sensitive as the "primary". As the flattened foil sample was retrieved from the drop tester and heated with a butane torch it immediately detonated. I really see the need for a proper experiment series covering the properties of this primary....we might see some very unexpected results regarding the various types of sensitivity of this substance.

[Edited on 6-10-2014 by markx]




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[*] posted on 6-10-2014 at 03:36


I did read this book in a library, when I was young. What is interesting, this guy do not tell bad words about TATP, except one- this compound is too volatile.



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[*] posted on 8-10-2014 at 09:23


Maybe he meant Silver Fulminate.

Is it possible to make SADS without Nitric Acid? I ordered 20g of Silver Nitrate.
I could make some but it's a pain and it's pretty dangerous distilling with those fumes.
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[*] posted on 10-10-2014 at 02:49


Quote: Originally posted by forgotpassword  
Maybe he meant Silver Fulminate.

Is it possible to make SADS without Nitric Acid? I ordered 20g of Silver Nitrate.
I could make some but it's a pain and it's pretty dangerous distilling with those fumes.


In my undestanding it is possible to make a product inclining towards silver acetylide in composition from "neutral" solution of silver nitrate. I have not practically tried it, but from experimental descriptions the product from neutral solution is not very much inferior compared to the acidic one in terms of initiation ability. Although it displays more sensitivity towards mechanical influences.
I'm assuming that reaction temperature has a similar effect as with strongly acidic solution, hence I would suggest conducting the synthesis at 65-70C. After all, silver nitrate is by character an acidic salt, forming a low ph solution when combined with water. Therefore the product from a solution with no extra acid should be similar to the one from acidified reaction. Just try it with small amounts and report your findings....as always, the real experiment results will reflect the true nature of things.




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[*] posted on 16-8-2015 at 09:03


I've been doing an extensive amount of research on silver acetylide and its double salt and I can't seem to find the answer to one question.
Why will introducing acetylene into a basic solution result in simple Ag2C2 while Ag2C2.AgNO3 is precipitated from a neutral or acidic solution?
I would appreciate it, if someone could explain this or point me in the right direction to a post or document that will enlighten me.




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[*] posted on 16-8-2015 at 12:03


Quote: Originally posted by Spirit of Niter  
I've been doing an extensive amount of research on silver acetylide and its double salt and I can't seem to find the answer to one question.
Why will introducing acetylene into a basic solution result in simple Ag2C2 while Ag2C2.AgNO3 is precipitated from a neutral or acidic solution?
I would appreciate it, if someone could explain this or point me in the right direction to a post or document that will enlighten me.

In basic media (except maybe with NH3), Ag(+) will precipiate as AgOH (or Ag2O)...
AgNO3 -aq-> Ag(+) + NO3(-)
Ag(+) + OH(-) --> AgOH(s)
2 AgOH(s) --> Ag2O(s) + H2O(l)
So you get coprecipitate of Ag-C#C-Ag and AgOH/Ag2O.

With NH3 you get complications as sensitive AgNH2, Ag2NH and Ag3N may form.

In neutral media precipitation of Ag2C2 do form a litlle HNO3...so medium becomes acidic
AgNO3 + H-C#C-H --> Ag-C#C-Ag(s) + 2 HNO3

In neutral and acidic media AgNO3 remains stable and may complexate the precipitating Ag-C#C-Ag to form the double salt!

[Edited on 16-8-2015 by PHILOU Zrealone]




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[*] posted on 16-8-2015 at 18:42


Quote: Originally posted by PHILOU Zrealone  

With NH3 you get complications as sensitive AgNH2, Ag2NH and Ag3N may form.
[Edited on 16-8-2015 by PHILOU Zrealone]


I didn’t know that synthesizing with an NH3 solution could possibly co-precipitate other explosive compounds. I’m going to look further into those compounds.
Thank you


Quote: Originally posted by PHILOU Zrealone  

In neutral and acidic media AgNO3 remains stable and may complexate the precipitating Ag-C#C-Ag to form the double salt!
[Edited on 16-8-2015 by PHILOU Zrealone]


If I understand correctly…

In acidic and neutral (which also becomes slightly acidic) solutions the AgNO3 remains stable because AgNO3 forms in an acidic solution, whereas AgNO3 is not stable in a basic solution and won’t form the SA.DS complex.




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[*] posted on 19-8-2015 at 06:16


Quote: Originally posted by Spirit of Niter  

Quote: Originally posted by PHILOU Zrealone  

In neutral and acidic media AgNO3 remains stable and may complexate the precipitating Ag-C#C-Ag to form the double salt!
[Edited on 16-8-2015 by PHILOU Zrealone]


If I understand correctly…

In acidic and neutral (which also becomes slightly acidic) solutions the AgNO3 remains stable because AgNO3 forms in an acidic solution, whereas AgNO3 is not stable in a basic solution and won’t form the SA.DS complex.

@ Spirit of Niter,
You almost got it
"because AgNO3 forms in an acidic solution"
It is not the AgNO3 that forms, it is already present when bubbling H-C#C-H into it ... and AgNO3 remains stable in neutral or acidic media allowing it to complexate with the precipitating Ag-C#C-Ag to form the SADS.

----------------------------------
@ all SM readers,

On further thinking :cool::D;)
1°)Apparently a similar compound could be obtained with AgClO4...
Would be nice to compare the two complex salts

2°)One may think to alternatives:
AgClO2 (already explosive on its own)
AgClO3
AgIO4
AgIO3
AgNO2 (unsoluble)
AgC(NO2)3
AgN(NO2)2

3°) Also Mercury does display explosive acetylides...
So to be investigated valences I and II...
Hg nitrate
Hg nitrite
Hg chlorite (already explosive on its own)
Hg chlorate
Hg perchlorate
Hg iodate
Hg periodate
Hg nitroformiate
Hg dinitramide




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[*] posted on 19-8-2015 at 18:52


Quote: Originally posted by PHILOU Zrealone  

@ Spirit of Niter,
You almost got it
"because AgNO3 forms in an acidic solution"
It is not the AgNO3 that forms, it is already present when bubbling H-C#C-H into it ... and AgNO3 remains stable in neutral or acidic media allowing it to complexate with the precipitating Ag-C#C-Ag to form the SADS.


In my last post I should have worded my statement a little better.
Yes, of course the AgNO3 is already present and doesn’t form. What I was trying to convey was that because AgNO3 itself crystallizes in an acidic solution it’s going to remain stable when placed back in an acidic solution. That’s all…
Thank you for your response.




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[*] posted on 29-8-2015 at 03:56


I made SASD but instead of a nice TICK,a grain of a salt explodes like a pop-pop :o
A size of a half matchhead ignited explodes and makes my ear ring.
Is it normal or too powerful?
(Side note: I can't download any file from this page :mad: )
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[*] posted on 29-8-2015 at 07:42


Yes, even an amount of SADS very much smaller than the head of a paper match head will detonate unconfined when lit and make an extremely loud, sharp, sound (painful to ears).



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[*] posted on 29-8-2015 at 07:55


So I'm lucky, because what I saw on youtube,the guy get a bigger amount of it and ignited but the wood spatula didnt had any injury.
http://m.youtube.com/watch?v=Q6nVkAvVrSQ
Imagine,if there was a little wood burning :o

[Edited on 29-8-2015 by kecskesajt]
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[*] posted on 11-10-2015 at 12:13


Earlier last month for the first time I experimented with silver acetylide and its double salt complex. I went about with three synthesis routes, the basic, neutral, and acidic solutions.

Ratios
Basic solution
30g NH4OH
1.5g AgNO3
3g CaC2 in 150ml of deionized H2O

Neutral solution
30g deionized H2O
1.5g AgNO3
3g CaC2 in 150ml of deionized H2O

Acidic solution
27g deionized H2O
3g HNO3
1.5g AgNO3
3g CaC2 in 150ml of deionized H2O

Yields
Basic solution
.34g of simple Ag2C2

Neutral solution
.42g of Ag2C2.AgNO3

Acidic solution
.61g of Ag2C2.AgNO3

Everything seemed to turn out successfully. I recorded flame, friction, and impact tests of all three batches. However, I don’t have anything uploaded so here are some pretty pictures.;)


DSCF0554.JPG - 3.3MB DSCF0564.JPG - 2.9MB

[Edited on 10/11/2015 by Spirit of Niter]




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