Sciencemadness Discussion Board - Ag2C2.AGNO3 (DS)

Ag2C2.AGNO3 (DS)

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prometheus1970 - 25-1-2011 at 13:33

I just did a synth for AG2C2 double salt. I dissolved 1 gram AGNO3 in 60ml water with 20 ml HNO3. I then bubbled Acetylene gas (by reaction of CaC2 with water) through said soln. for about 10 min. I definitly got a precipitate, but rather than the fine grayish-white solid I see in most videos, I got a coarser brownish-black material from the reaction. Am I a dimwit? Or will this work just fine (as a primary)?

I wanted to check before I tested a few mg that this is what I think and not uranium nitrate or some other insanely dangerous compound...

[Edited on 1-25-2011 by prometheus1970]

not_important - 25-1-2011 at 14:57

Did you clean up the acetylene before bubbling it through the silver solution? Raw acetylene from CaC2 usually contains hydrogen phosphide and hydrogen sulphide, and sometimes ammonia. A solution of HCl and CuCl2 can be used to remove much of the impurities, but make sure it is kept well acid; the C2H2 is then washed with dilute NaOH and then water. Detail can be found online, especially in chem books from the late 1800s to 1930s.

Rosco Bodine - 25-1-2011 at 21:05

You may find these patents an interesting read

US2483440
US2474869

and equivalents

GB616318
GB616319

Attachment: US2483440 Silver Acetylide Double Salts.pdf (295kB)
This file has been downloaded 1839 times

Attachment: US2474869 Silver Acetylide - Mercury Acetylide complex.pdf (104kB)
This file has been downloaded 1548 times

Attachment: GB616318 Silver Acetylide - Mercury Acetylide complex.pdf (142kB)
This file has been downloaded 1244 times

Attachment: GB616319 Silver Acetylide complex salts.pdf (339kB)
This file has been downloaded 1435 times

zajcek01 - 25-1-2011 at 22:48

Prometheus1970, the material you obtained should work just fine as a primary.

When I use to prepare it, I didn't use any HNO3 or anything.
I just made a solution of AgNO3 in distilled water and bubbled C2H2 in it directly from CaC2 + H2O. The material started to precipitate as greyish powder which latter turned to almost black on light. The precipitate was filtered, washed with some clean water. It had the same initiating properties even after 3 years of storage under water in brown glass container.

If your material is brownish precipitate this might be an impurity.
If your silver nitrate was made by dissolving jewlery in nitric acid, the impurity might be some copper nitrate, from that copper dubble salt. (some sources say it is highly sensitive)

Ag2C2.AGNO3 (DS) synth

prometheus1970 - 26-1-2011 at 06:57

In better light this morning I saw the precipitatewas just grayish black-no brown, after all.

I'm pretty sure, in retrospect that I let the water line in the gas generator get too close to the outlet valve and somCAOH got pushed though the line into the reaction vessel. I test some of the black-gray gravelly precipitate and it burned to ash but with about as much energy as fuse paper. I'll try again soon. My AGNO3 solution was not bluish at all, should it have been? I used reagent grade AGNO3, many of te videos I've seen had a bluish solution to which they add HNO3 before the bubbling part, but I suspect they may have dissolved dimes in HNO3 and got some copper contamination

[Edited on 1-26-2011 by prometheus1970]

hiperion42 - 28-1-2011 at 12:00

PHILOU Zrealone has given some tips for
producing high purity product.

http://www.sciencemadness.org/talk/viewthread.php?tid=1031&a...

prometheus1970 - 29-1-2011 at 16:23

I suspected that the CAC2 in water reaction produced sulfides. The gas generator(afterward) smelled of rotten eggs...

[Edited on 1-30-2011 by prometheus1970]

-=HeX=- - 29-1-2011 at 16:35

Did you do something silly like dry it in the sun? The sample I have sun dried here looks similar to what you describe...

Ag compounds + light = bad...

Though I have had one sun dried sample from Palladium sitting underwater under my bed for ages - still got a bit left in there methinks. It aint been treated to gentle either... i will look at it tomorrow when the alcohol concentration in my bloodstream decreases a bit!

------
"Fire burns, cleans the soul, and momma didn't raise her no dirty boy no sirree"

Jimbo Jones - 30-1-2011 at 07:05

Actually it’s all about the purity of the acetylene gas. I have made two tests. Both of the two starting solutions (2 gr. silver nitrate, 20 ml. distilled water and 7,6 ml. (65 % ) nitric acid – all of them ACS grade) were mixed directly in the reaction vessel (a 50 ml. syringe), which by it self was put in improvised heater (empty box of ice-cream, with hole in the cap). The temperature of the water (according one Russian Lab manual) was around 70 – 80 C. The acetylene gas generator was made from intravenous system tubes and little jar. The water for the generator was delivered from 20 ml. syringe, mounted directly to the jar lid and isolated with some blu-tack. The first sample was treated with raw (smelly) acetylene, but to the second system was added primitive purifying chamber, based on 100 ml. bottle and 37 % sulfuric acid. The yield with the raw acetylene was dark, brawn powder. The semi-clean acetylene produced dirty white powder. After some tests I was able to find that along with the great stability, the second batch also have superior initiation properties.

Hey HeX, any new info around yours micro FAE charges?

http://www.sciencemadness.org/talk/viewthread.php?tid=7762&a...

-=HeX=- - 30-1-2011 at 08:51

The acetylene quality is obviously going to be a factor - put in impure crap, get impure crap out! Basic science

Though the way you dry it (sunlight!!) also is an epic factor and I assume you should wash the stuff with distilled water once filtered...

+++++++++++

Off Topic

Jimbo: I did some more work on the FAE since, and find that yep, something there DEFINATELY detonates. Lifting the same mix with flash just made a fire, wheras when HE is used to 'lift' it it seems to 'CRACK!' like a FAE or something. Hard to explain the noise.

I will be making another soon.

Also, I am slowly developing a theory about how it works, could take some time though. I think the blast causes the double bonds in the diesel (I think theres double bonds somewhere) to crack or something. I cannot word it properly, its just a set of pictures in my head that need transcription onto paper.

prometheus1970 - 30-1-2011 at 20:04

No , no sun drying of my silver nitrate based product, I actually know better than that. The plastic (LDPE most likely) bottle I use as a gas generator is one that comes with saline solution for hospital to use for irrigation, etc. not the sterile stuff that comes in bags. The bottom of the bottle has an inverted cone, like one would use to make a shape charge, so the only way I could be sure the CAC2 would get wet was to fillthe water above the top of the cone and drop the lttle carbide stones in now and then as the bubbling stops then quickly replacing the cap. I drilled a minimum diameter hole in the side toward the top where a clear pvc tube is inserted |(about 5mm ID) then goes into the reaction vessel (a 100ml grad. cylinder)

prometheus1970 - 2-2-2011 at 08:55

When using metallic Ag for Ag2C2.AgNO3 synthesis is it best to dissolve the silver, then separate out the AgNO3 and then redissolve it in purified water, add HNO3, bubble etc.? Or should I just add purified water to the AgNO3 dissolved in the HNO3, then bubble? I can see how separating out the AgNO3 then redissolving it would be better, because you could weigh out how much you wanted to use, but then that may be an unnecessary step if you only dissolve the appropriate amount of silver to begin with. Also, does Ag2c2.Agno3 perform better if pressed?

grndpndr - 3-2-2011 at 12:04

Quote: Originally posted by -=HeX=-

The acetylene quality is obviously going to be a factor - put in impure crap, get impure crap out! Basic science

Though the way you dry it (sunlight!!) also is an epic factor and I assume you should wash the stuff with distilled water once filtered...

+++++++
grndpndr's f up

Along those lines about silver and impuritys.Ive heard and intend to heed warnings concerning copper content in 90% sterling /coin silver.Any Ideas about possible reactions using 85%silver solder the remainder mainly Mn.(Harris safety-silv?)
A search of jewelry silver solder revealed a sterling silver w/Cu
replaced w/germanium? Anyone aware of potential problems using silver w/this impurity?
And, Industrial grade bottled acetylene.Pure enough w/o clean up?I dont want to assume anything if I should try a synthesis of a new(to me) primary.Thanks

[Edited on 3-2-2011 by grndpndr]

quicksilver - 4-2-2011 at 09:45

GENERALLY; bottled industrial welding asses are fairly good becasue they don't stick around in the tanks for decades. Tanks are used, re-filled, etc. It doesn't appear to be an issue. Calcium carbide (IMO) is more expensive; however you can rig up something in a lab that has a "sep-funnel-dripper" and get some fairly decent yields from a few ounces of carbide.
Occasionally the silver doesn't dissolve right away. I am NOT sure why this is but some people add droplets of water to begin the process but I simply let it lay still. I was once told this indicated presence of nickle. Nickle appears to be of little consequence as does tin. Jewelry silver occasionally has 1% Ni or Sn for strength and tarnish resistance, etc. However.....Indian jewelry from mines can have small amounts of arsenic - & that CAN be a serious problem.

If the silver had enough copper to make it an issue; there would be substantial "tell-tale" deep green in the acid (minute quantities of nickel could also make a LIGHT green; but that's an issue with coins or jewelry). What's more, even then if your product is fluffy white snow-like material that would indicate silver not copper. Copper and cuprous acetylide is dark from it's beginning (not after it have been exposed to UV or what have you). Another factor is that copper acetylide is a less effective synthesis; requiring longer exposure levels to the gas. If you are getting white flocks immediately;that sounds like silver. - Copper takes some time.

prometheus1970 - 4-2-2011 at 18:30

I just got a full pound of CaC2. My last synth immediately produced very nice, white, fluffy precipitate. I'm pretty sure it was a matter of pulverizing the AgNO3 crystals and dissolving them in hot water. I was quite pleased with the results of that attempt. Now I'm looking mostly for the least expensive silver nitrate. I've even been in touch with someone at Kodak, telling him that, "my friends and I"(my friends being you guys) would likely buy a few kilos per year if his prices were reasonable. However, he may only be interested in selling on the order of 1000 kilos+. I explained my situation and am waiting to hear back. i just said that my friends and I are into hobby chemistry and, while we would not need tons of the compound, several dozen 100 gram batches may well be sold to me and my ilk. I'll post the results here when I hear back.

[Edited on 2-5-2011 by prometheus1970]

quicksilver - 5-2-2011 at 10:19

Do not be surprised if the price is unaffordable high. Silver took a jump to 27USD awhile back and the cost is directly reflected in the silver market place. I actually kept up with certain chemical prices for some time and silver nitrate was one of them. It is VERY rare for a consistent - price to be lower than market which is still nearly $500 a lb. - If yield costs were not figured in a simple understanding of 16 ounces @ $27 is $432.
Occasionally you can find someone who doesn't know the price and has one unit container, or someone who would flush several small weight containers as they would be old in a university setting perhaps.....but in general: silver nitrate is a serious money maker.

prometheus1970 - 6-2-2011 at 07:34

I was doing similar extensive research for HNO3 and found that, as long as you buy a few metric tons(sometimes minimum order is just 1 metric ton), it only costs about $600.00 per ton. I knew that it was available in bulk, but figured even if I had a way to store hundreds of gallons of the stuff, the price per ton would be like $100,000 or so. It was quite interesting to find that if I had a place to put it and a way to satisfy federal regulations (set up a shell company with a legit need for craploads of nitric acid) I could conceivably buy enough to get me through a long weekend of heavy synthing.

I found a website called "silver nitrate.org" that sells 50 gram batches for $49.00 w/free shipping. sounds like the best deal yet, even bettter than salt lake metals who is also pretty reasonable.

[Edited on 2-6-2011 by prometheus1970]

quicksilver - 6-2-2011 at 12:11

Be very careful of 2 issues.

If it seems to be too good to be true: it usually is.

VERY often silver nitrate is sold in solution.

Some years back I was into collecting all sorts of thing like coins and swords and what not. I got burned on eBay 2x because of the wording and I WANTED it to be a good deal; so I didn't look for idiosyncrasies or unique phrases that should have alerted me to a scam.
I am NOT saying you may have discovered something fantastic but look at the basis of it. IF a noble metal based material that is price adjusted as a world market commodity is selling for "X" - how can a profit be made for selling it at "Y"?

Now it -=IS=- possible that someone knows that AgNO3 is a seriously expensive & highly sought after chemical and MAY have found a very efficient method of production of high yield synthesis.....that's possible. But be careful; as this would also be a standard for very large chemical firms that have seriously large contracts that are VERY competitive.

I say this becasue of another issue that occurred with "pyro-oriented" materials. Sometime back there was a company that adulterated powdered aluminum with carbon & sold it as "Indian dark" aluminum. It actually was ALCAN 808 with about 15% air-float charcoal. hey sold off a hell of a lot and closed up fast. Several LARGE middlemen got stuck with a lot of it. It was really only discovered becasue it's was very poor performance on a very small level (firecrackers).
VERY few westerners make classic firecrackers in the classic method of two bamboo sticks & pulp & rice paper. Someone made some with this material and (naturally) the results sucked. It was examined under a microscope and compared to the classic foil-backed paper dark Al & the distinction was very vivid. By then the "company" was folded and a great deal of money lost. Large special effects firms lost a great deal of money and some folks got stuck with (essentially) unsellable crap. Some folks even tried to keep the public from finding out as faith would be lost on the real thing as it looked THAT good. But it's performance was marginal on a large scale. On a small scale it was obvious. But the real money was on the larger special effects orders & to loose their sales would be disastrous.
Adulterating a product like AgNO3 would not be too tough IF the sales went to small-scale individual purchases for a short duration.
....Buyer beware.

[Edited on 6-2-2011 by quicksilver]

The WiZard is In - 6-2-2011 at 12:51

Quote: Originally posted by quicksilver

Be very careful of 2 issues.

If it seems to be too good to be true: it usually is.

VERY often silver nitrate is sold in solution.

Beware of the I loose money on every item I sell —
I make it up on the postage eBay sellers.

One US buck for 100gms.... http://tinyurl.com/4k2rm5o

prometheus1970 - 7-2-2011 at 06:17

The AgNO3.org site actually sells 40 gram parcels for $49.00. A good price ,but not inordinately great. Salt lake metals sells 50 grams for $62.00. Oops! my bad, I was just going by what seemed to be the best price. Upon doing a little math: AgNO3.org's price is $.81 per gram, Salt Lake Metals is just $.80 per gram. I'm still waiting to hear back from the Kodak guy, but I'm pretty sure he'll just refer me to his supplier, since I'm only interested in (comparitively)small orders. I'll keep you all posted...

prometheus1970 - 7-2-2011 at 06:19

Yeah, I saw the ebay listing for 100 grams buy it now price $1.00, but with shipping cost of $89.00. Ebay is the perfect venue for a scam like that since once you click "buy it now", you're legally bound to do so. Credat Emptor, for sure

[Edited on 2-7-2011 by prometheus1970]

[Edited on 2-7-2011 by prometheus1970]

quicksilver - 7-2-2011 at 12:36

I'm glad you didn't get snookered. -=NOTE: OT remark...=-
I rarely buy from eBay anymore. I know they have all sots of return shit and "protections" but I can live without the hassle and being obligated to really check the shit deep because (IMO) maybe up to 20% of that is in some manner a rip.

I am really into books on energetics. I especially don't like their "politics" about "helping" reduce what they consider inappropriate or suspicious or whatever. People such as that develop "lists" of purchases, etc. I don't need "big brother eBay" attempting to fight crime by censorship.

grndpndr - 10-2-2011 at 14:40

I may be wrong but hold on to your hat last night vI thoughtb I saw spot silver @$33 troy oz.

FWIW Im also quite careful not simply about possible ripoffs from e-bay sellers but EBAYS apparent list keeping and sharing with those(gov agencys) who might have an interest.
Finally FWIW I vehemently disgree with both EBAYs and PAYPALs Politics and political donations.Aiding in controlling thier customers privacy etc thru law. BBs snitches.

prometheus1970 - 10-2-2011 at 15:08

I think I'd have a hard time (emotionally) dissolving silver into HNO3, despite how well I may know that that is the most economical way to AgNO3. I have a feeling that silver prices will soon make a jump and having "wasted"| that much investment quality metal in light of a market rise would make me quite regretful. I think I finally found a good, inexpensive source for AgNO3. I have a tendency to be greedy with new discoveries. Now that I've found that Ag2C2.AgNO3 is a synth with which I have a great deal of success, my natural (misguided) response is to want to acquire just gobs of the reagents so I'll have plenty onhand for quite awhile. It is then that I must remind myself that making/storing large amounts of priaries is a rally bad idea. As of yet I only have .325 grams in stored away

Jimmi_P - 18-6-2011 at 15:24

Quote: Originally posted by quicksilver

. It is VERY rare for a consistent - price to be lower than market which is still nearly $500 a lb. - If yield costs were not figured in a simple understanding of 16 ounces @ $27 is $432.
.

There are only 12 troy ounces in a pound. just thought I would let you know.

About Silver Acetylide/Nitrate (SA.DS) synthesis and improvement

Vpatent357 - 12-7-2014 at 02:37

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]

markx - 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!

NeonPulse - 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.

Vpatent357 - 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]

Manifest - 3-8-2014 at 08:29

Why is it necessary to acidify the solution of Silver Nitrate with nitric acid before bubbling acetylene?

Hennig Brand - 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 1142 times

markx - 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:

Yup, looks about right...

Vpatent357 - 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]

Manifest - 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

markx - 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!

Vpatent357 - 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..

Manifest - 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.

markx - 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 811 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]

caterpillar - 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.

forgotpassword - 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.

markx - 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.

Spirit of Niter - 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.

PHILOU Zrealone - 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]

Spirit of Niter - 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.

PHILOU Zrealone - 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]

@ 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:

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

Spirit of Niter - 19-8-2015 at 18:52

Quote: Originally posted by PHILOU Zrealone

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.

kecskesajt - 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

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:

)

Hennig Brand - 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).

kecskesajt - 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

[Edited on 29-8-2015 by kecskesajt]

Spirit of Niter - 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.

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

markx - 11-10-2015 at 22:40

Excellent visual contrast between the different pH levels! Did you conduct the synthesis at room temperature? Judging from coloration of the product (if the picture was taken shortly after drying was complete) it probably was done at room temperature or close to that.

PHILOU Zrealone - 15-10-2015 at 10:35

My neutral one looks more like your acidic one, so I guess you did one or more mistakes during your synthesis:

-in too strong light (artificial or sun)

-you didn't exhaust the AgNO3 well with acetylen (the unreacted AgNO3 will darken your complex and make it more friction sensitive), this will also lower the yield.

-you didn't wash your filter paper with demi water first (chlorides from bleaching are detrimental due to AgCl formation and reaction with light)

-you didn't wash the precipitate several times with demineralized water to take away all the uncomplexated AgNO3, this allows one to rerun acetylen through the solution until completely exhausted --> increasing yield.

-you had some Ca(OH)2 from your acetylen generator that was taken by the acetylen into your AgNO3 solution....dark AgOH forms immediately and turns into black Ag2O...this also sensitizes the salt.

Spirit of Niter - 15-10-2015 at 19:36

Quote: Originally posted by markx

Excellent visual contrast between the different pH levels! Did you conduct the synthesis at room temperature? Judging from coloration of the product (if the picture was taken shortly after drying was complete) it probably was done at room temperature or close to that.

The syntheses was conducted outdoors under a carport in the shade. It was fairly warm out when I conducted the neutral synthesis and as for the other two the synthesis were done at night. My final products were temporarily stored under a cardboard box in the shade until I did a few tests.

Quote: Originally posted by PHILOU Zrealone

My neutral one looks more like your acidic one, so I guess you did one or more mistakes during your synthesis:

-in too strong light (artificial or sun)

-you didn't exhaust the AgNO3 well with acetylen (the unreacted AgNO3 will darken your complex and make it more friction sensitive), this will also lower the yield.

-you didn't wash your filter paper with demi water first (chlorides from bleaching are detrimental due to AgCl formation and reaction with light)

-you didn't wash the precipitate several times with demineralized water to take away all the uncomplexated AgNO3, this allows one to rerun acetylen through the solution until completely exhausted --> increasing yield.

-you had some Ca(OH)2 from your acetylen generator that was taken by the acetylen into your AgNO3 solution....dark AgOH forms immediately and turns into black Ag2O...this also sensitizes the salt.

-My neutral synthesis was done in a shaded area during the day and the other two at night.

-I wondered if I was passing enough C2H2 through the solutions because I believe my yields could be a little higher.

- I was sure to rinse off the “bleached” filter paper with deionized water. I used deionized water in all three syntheses whenever called for, i.e. the acetylene generator.

-As for your fourth point pleases elaborate a little bit more. Are you saying that I would have to wash the precipitate while still in the initial solution? Followed by passing more acetylene through the solution to achieve a high yield? For the acid synthesis I filtered the precipitate and washed three times; first with 150ml of NaHCO3N (0.15g)/ deionized H2O solution, next with 150ml of deionized H2O, and finally with 100ml of denatured alcohol.

-I don’t doubt that my solutions received contaminants from the acetylene generator. I didn’t bother washing the gas. This was my first time synthesizing Ag2C2 and its double salt. I was merely keeping the experiment simple. At least for now…

PHILOU Zrealone - 16-10-2015 at 10:24

Quote: Originally posted by Spirit of Niter

Quote: Originally posted by PHILOU Zrealone

So you did almost everything wel

.

To me your yield could be improved by passing several times acetylen into the solution with the permeate of the filter. Filtration each time between acetylen session over the same already filtrated precipitate onto the filter.

The fourth point is that you have to wash the filter with the precipitate in it with demi water (a few 5ml) turn a little with a rod in the filter to resuspend the precipitate...this will increase a bit the volume of solution for bubbling acetylen but this recycle all unused/unbound AgNO3 to the complex.

The design is best with a vertical long tube and the bubble at the bottom...this allows a longer contact time (residence time) between acetylen and AgNO3 solution..this also helps flocculation of the precipitate for easier recollection by filtration.

For your acid precipitate only the demi water wash is sufficient.
The basic wash with NaHCO3 will make Ag2CO3 if AgNO3 is still present in your precipitate and will eventually ruin the benefit of the complexated HNO3, it will be neutralised as NaNO3 and leave the complex with your other washes.

The final denaturated ethanol wash is also useless because it introduces unknown denaturant into the equation...simply press between paper towels and leave precipitate to dry in a mild warm and shadow area.

Spirit of Niter - 18-10-2015 at 20:05

I appreciate the helpful tips. I’ll be sure to take note of them for next time. I think later sometime as I get more in depth with experimenting with silver acetylide, I’ll synthesize it’s none explosives complex Ag2C2.6AgNO3.

More Infromation

MineMan - 13-8-2016 at 08:47

Hello All,

I wanted to share some pages that I extracted from the book "Primary Explosives" about SADS. From what I gather the least sensitive product is made from a hot acidic solution (30% nitric acid, or lots of silver nitrate compared to distilled water). I tried this and the product does indeed seem less sensitive!

Attachment: Primary Explosives.oxps (5.4MB)
This file has been downloaded 1078 times

markx - 21-8-2016 at 23:03

Quote: Originally posted by MineMan

Hello All,

I wanted to share some pages that I extracted from the book "Primary Explosives" about SADS. From what I gather the least sensitive product is made from a hot acidic solution (30% nitric acid, or lots of silver nitrate compared to distilled water). I tried this and the product does indeed seem less sensitive!

Yes, hot acidic synthesis is the way to go. Product formed in these conditions was so numb towards mechanical stimuli that it did not go off in my drop tester under a 2kg weight dropped from 60cm. Where as room temperature "neutral" synthesis product (discolored) could be set off with a light tap of a hammer. Electrostatic sensitivity still remains, so care should be taken to handle the double salt at all times!

MineMan - 22-8-2016 at 10:12

Markx... that is amazing, 60cm with a 2kg weight, how many times did you verify this because I still can set mine off with a hammer, but it needs a couple of decent hits!

I put some of my SADS in the way of a bbq pezio spark and it did not ignite... but I believe you.

It could be the "perfect" primary if we can reduce the static sensitivity... I only have a few ideas though...

-Adding 10-20% potassium perchlorate helps the oxygen deficiency and lessens the sensitivity without adversely affecting the power.
-Just use a humidifier while loading this into caps or devices, and then the caps should provide a faraday cage and there is nothing to worry about... although an electric engineer told me once that static just needs a crack the size of a micron to enter.

markx - 23-8-2016 at 12:04

Quote: Originally posted by MineMan

Markx... that is amazing, 60cm with a 2kg weight, how many times did you verify this because I still can set mine off with a hammer, but it needs a couple of decent hits!

I've verified it on 5 batches of product (2-4g) synthesised according to the procedure that I described on this thread earlier. The sweet spot for solution temperature during acetylene administration seems to be around 65C. I have started from metallic silver all the times and used metal from only one batch of silver that I aquired for the purpose. It is not highly pure ( scraped leftover residues from the chamber of vaccum vapor deposition process). It has a definitive copper impurity in it as can be seen from the characteristic blue hint of solution after nitric acid has dissolved the metal. There may be other contaminants that are not visually detectable. So they may or may not have an effect on the final result, but so far it has turned out very satisfactory. But these are just my observations and results that apply for the batches that I have syntesized so far. So please do take them as exactly that and nothing else! I have no intention to suggest that you or anyone else using different materials is guaranteed to have the same outcome. There may be numerous factors that influence the process, so always assume proper safety precautions. This is a very sensitive energetic material and just because certain conditions allow it to be less responsive towards impact initiation does not take away the other hazards of heat, flame and static discharge.

MineMan - 23-8-2016 at 12:42

I am aware of this, thank you for your verification. My product was made at 70-75C and it cannot be set off by metal on metal friction even when the sharp edge of one bar is used against a steel plate (1cm thick) and 30-40 pounds of pressure is administered. Just wish we could find a way to reduce the static sensitivity... what about plasticizing this primary?

PHILOU Zrealone - 23-8-2016 at 13:16

Quote: Originally posted by markx

Quote: Originally posted by MineMan

Markx... that is amazing, 60cm with a 2kg weight, how many times did you verify this because I still can set mine off with a hammer, but it needs a couple of decent hits!

Copper into the mix may be a problem or not...depends on its interaction...
I suppose unsoluble CuC2 do form (copper II acetylide) what is not sensitive nor explosive to my experience (by opposition with Cu2C2 (copper I acetylide) wich is sensitive and explosive).

You could have separated the Cu out of the Ag/Cu mix by cementing the nitric acid Ag/Cu mix with a piece of Cu pipe...all the Ag (and nobler metals) would have precipited as a fine dust leaving a blue solution of Cu(NO3)2 and most of the Cu pipe.
Ag + Cu + HNO3 --> AgNO3 + Cu(NO3)2 + NxOy + H2O
2 Ag(+) + Cu(s) --> Ag(s) + Cu(2+) (as Cu(NO3)2)

PHILOU Zrealone - 23-8-2016 at 13:20

Quote: Originally posted by MineMan

I am aware of this, thank you for your verification. My product was made at 70-75C and it cannot be set off by metal on metal friction even when the sharp edge of one bar is used against a steel plate (1cm thick) and 30-40 pounds of pressure is administered. Just wish we could find a way to reduce the static sensitivity... what about plasticizing this primary?

BTW Thank you for the extraction work out of the book.
I wish I could read the rest of the book

.

I also dream of plasticizing SADS...but the plasticizer needs to be active (explosive) and stable towards SADS.
I hope being able to test some tested possibilities in a near future (by the end of the year)

markx - 29-8-2016 at 08:55

Quote: Originally posted by PHILOU Zrealone

In fact it seems that most of the copper, if not all, remains in solution after the acetylene administration is complete...visually the solution's blue hint is unaltered by the process. So I've not bothered with the purification techniques so far.

I've played around with some energetic mixes to "phlegmatize" SADS, but it seems that diluting this primary will quite sharply render it unresponsive towards flame initiation. Then again out of fear of accident I've used very small amounts and the ratios were vaguely defined to be honest. Another option would be to impregnate a pressed pellet of SADS with a solution of another energetic (of known concentration) to avoid the mixing and friction of the process. Might be worth a shot...

Tricka90 - 7-9-2016 at 01:42

I tried SADS synthesis starting from pure silver metal. I obtained it by extracting silver via cementation from some tablespoons.
pH of my 8.5% w/w silver nitrate solution was slightly above 1 when I start reacting it with acetylene gas, from calcium carbide.
The solution was colorless, so no copper was present, noticeably.
I didn't warm up the solution, but ambient temperature was quite high considering it was a hot summer evening.
I used deionized water for both silver nitrate solution and acetylene gas production.
I washed the product many times with just deionized water, when dry it had a light grey color.

With that procedure I got a very stable product.
Hammer test was satisfying but nothing exceptional.
Friction test was outstanding: it had to put in so much effort to make it detonate by scratching it with an iron hammer on a not so smooth concrete floor and I make it only once.

I didn't know SADS was also sensitive to static discharge. What does it mean exactly? Is there any way to test this kind of sensitivity?

greenlight - 7-9-2016 at 03:07

Here is an answer to your question taken from Introduction to the technology of explosives:

"Electrostatic sparks

There are no widespread standard tests yet for testing the electrostatic or spark sensitivity of explosives. A number of tests have been devised, and perhaps a standard will someday be accepted. In general, secondary explosives are not particularly susceptible to this mode of ignition; however, primary explosives and most pyrotechnics are susceptible. Initiation of an explosive materialby an electrostatic pulse is acheivef if sufficient energy is delivered to the explosive material. Since most explosive materials are not good electrical conductors, the electrostatic pulse must have sufficient potential to overcome the explosive material's low electrical conductivity.
Sandia National Laboratories has developed a uniform test specification for measuring the spark gap sensitivity of explosive-containing components. A 600-pF capacitor charged to 20kV is discharged through the component with 500 ohms in series with the discharge circuit. This test is considere to be equivalent (or in excess) of the discharge that might be obtained from a static discharge from the human body.
In the loose powder test it is measured by discharging a 600-pF capacitor from a pointed electrode through a sample of loose powder (approx 0.2g) to a ground plane.
the voltage is varied until one ignition in ten trials or the voltage limit of the testing equipment is reached."

Theres not much you can do at home to measure the exact sensitivity.

[Edited on 7-9-2016 by greenlight]

MineMan - 7-9-2016 at 10:36

I have my doubts about SADS being as static sensitive as everyone says...

When made properly right temperature, right PH, and the right ratio of Silver Nitrate to to solution it is nearly immune to friction as Tricka stated, infact, if he had heated the solution and made sure that the solution contained 25% nitric acid, the hammer test would have been more impressive. Several times this product has failed to detonate when compressed with a visco fuse also. I have placed small amounts of this product between a pizoelectric spark from a blow torch with no detonation (flash powder had the same results).

What I do know is that the same SADS that refuses to go off with the hardest of hammer blows on steel, will go off with a light tap when placed on a rough hard rock... so perhaps a small static spark can... the sucky thing is, we just don't know... even with spraying everything with static gaurd... static electricity seems impossible to predict... so I am afraid of a false sense of comfort.

SADS works great still with 10-15% potassium perchlorate, maybe this would help reduce it some....?

I believe Bert has a story of his SADS going off unexpectedly just from peeling a label off the container it was kept in. But I don't know how his product was made, if it had been exposed to sunlight and the such.

markx - 7-9-2016 at 22:58

Quote: Originally posted by MineMan

I have my doubts about SADS being as static sensitive as everyone says...

so perhaps a small static spark can... the sucky thing is, we just don't know... even with spraying everything with static gaurd... static electricity seems impossible to predict... so I am afraid of a false sense of comfort.

SADS works great still with 10-15% potassium perchlorate, maybe this would help reduce it some....?

I believe Bert has a story of his SADS going off unexpectedly just from peeling a label off the container it was kept in. But I don't know how his product was made, if it had been exposed to sunlight and the such.

That is exactly the point....static is very deceptive as one can not see, feel or predict its presence with reasonable means. Most excessive mechanical factors can be avoided or alleviated with proper procedures, but static remains the devil in disguise. So all false comfort is to be avoided at all cost in our field of practice

As for testing the static sensitivity in home laboratory...in fact a lot can be done if one has a little electronical inclination and the will to use it. To devise a small power supply that charges a high voltage capacitance to a preset voltage through feedback is not too complicated of a task. This needs to be coupled with a small test chamber that has a means to decrease the standoff between electrodes (either manually or electromechanically triggered) to initiate the discharge of the capacitance through a tiny sample of the compound to be tested. The voltage on the cap can be displayed on a low volt digital voltmeter through a suitable voltage divider bridge. The same can be done for setpoint voltage. There are halfbridge driver ICs with error amp inputs available for pennies and these can govern the whole process.....got my gears turning actually

Tricka90 - 8-9-2016 at 05:29

Yes, static discharge seems like a real pain in the ass due to the fact that it's almost unpredictable.
I think one of the best thing we can do to handle SADS a bit more safely is avoiding the use of materials which can easily accumulate electrostatic charge.
In the following link there's a list of materials which tend to get charged. Paper, cotton, steel and wood seems to be the safest, so I would use those materials to handle, store, let dry and transport SADS. According to the list, the most dangerous thing we can do is touching SADS with bare dry hands or leather gloves while it lies on a Teflon surface...

http://www.school-for-champions.com/science/static_materials...

Tricka90 - 10-9-2016 at 05:41

Hello everyone.
I would like to ask you what quantity of unconfined SADS can, in your opinion, cause serious damage if detonated in the very proximity of one's hand. I think a 20 mg dose is not so dangerous, but what about 100 - 200 mg? Or even a few grams?

MineMan - 10-9-2016 at 08:51

Tricka90, I am disappointed with your question, from your previous posts it seemed like you were learning quite rapidly....

A few grams! 10mg causes a hole in a soda can, 20mg causes shrapnel from that hole to pierce the other side!

I think it would be best if you made a small quantity and experimented with small amounts and then told us what you think.

20mg could/would probably take flesh off the fingers to expose bone, 50mg definitely would. 100-200mg hmmm, ouch. A few grams, I am still flabbergast that you asked this.

KesterDraconis - 10-9-2016 at 15:17

Quote: Originally posted by Tricka90

Hello everyone.
I would like to ask you what quantity of unconfined SADS can, in your opinion, cause serious damage if detonated in the very proximity of one's hand. I think a 20 mg dose is not so dangerous, but what about 100 - 200 mg? Or even a few grams?

Depends on your definition of serious damage. Removing skin and flesh is easy, it won't take many milligrams to do that. Breaking bones (potentially irreparably) would be in the 250mg to 500mg range I think. After that, you are most definitely losing fingers if not the hand.

It also depends on what type of confinement you mean. Even a quarter of a gram if held in your fist and set off is going to basically take your hand. So, the question is really relative. Best advice is to make small batches (about 0.5 grams), keep it far from your hands when you can, and use precaution about flame, heat, impact, friction, static, etc.

[Edited on 10-9-2016 by KesterDraconis]

Tricka90 - 11-9-2016 at 00:26

Thank you for your quick and informative replys.
I'm sorry, I think I didn't make myself clear with my last question: when I asked about detonation "in the very proximity" of one's hand I was intending the explosive to be very near the hand (less than 10 cm) not in direct contact of it, for God's sake

Of course even a few tens of mg can be extremely harmful if exploding right in contact with the bare hand, as you said, but I think (and hope!) nobody would handle a primary this way!
So, do you think those quantities can provoke permanent damage even when detonating at a 5 to 10 cm distance from the hand? I would say 100mg can cause irreparable injuries even at such distances, am I guessing right?
As for a few grams...I asked but I'm frightened to know the answer!

p.s.
I never manufactured (nor I'm planning to) more than a 100mg SADS batch: I think it would be unjustifiably dangerous since that quantity is more than sufficient for conducting the major sensitivity tests and for detonation purposes within certain ranges.

[Edited on 11-9-2016 by Tricka90]

KesterDraconis - 11-9-2016 at 15:45

Quote: Originally posted by Tricka90

Thank you for your quick and informative replys.
I'm sorry, I think I didn't make myself clear with my last question: when I asked about detonation "in the very proximity" of one's hand I was intending the explosive to be very near the hand (less than 10 cm) not in direct contact of it, for God's sake

Yeah, I don't know if its smart, but I don't know it it is smart, but I use soft pieces of straw to scoop or handle primaries, this way, there is little risk of friction or shock, and my hands stay a good 5cm-7cm away at all times. (though frankly, I don't like dealing with primaries, and I've only ever synthesized three, and never actually used one to set off a secondary charge).

Tricka90 - 18-9-2016 at 03:33

Yes, I think it definitely is a good idea.

I read that when making SADS, 10% HNO3 (by weight) should be added to the AgNO3 solution.
So if I have 9ml water should I add 1ml of 65% HNO3 or 1ml of 99% HNO3?
Or maybe the weight of AgNO3 salt itself also has to be consider in the calculations?

[Edited on 18-9-2016 by Tricka90]

Metacelsus - 18-9-2016 at 06:36

If you want a 10% w/w solution, you'll need a total of 9 grams of water and 1 gram of nitric acid. You can calculate the volume amounts using the density and the concentration of your nitric acid.

Tricka90 - 18-9-2016 at 07:15

Thank you Metacelsus, so if my calculations are correct I will obtain 10gr of 10%HNO3 solution by mixing 8.46gr H2O and 1.54gr 65%HNO3. That's the correct ratio to obtain the best SADS, is that correct? (of course I will also add AgNO3 then).

MineMan - 18-9-2016 at 12:46

you really want around a 25-29% HNO3... read the paper I attached a few weeks ago...

Tricka90 - 19-9-2016 at 07:18

I downloaded and read several times the paper you attached, it is very informative on the subject but the author doesn't express himself about the optimal percentage of HNO3 in the AgNO3 solution, he only says it has to be "slightly acidic". It does say that ignition temperature of SADS increases up to 280°C when 28% HNO3 solution is used but it's still not clear what is the optimal concentration that optimizes the most and most important SADS parameters.

[Edited on 19-9-2016 by Tricka90]

MineMan - 19-9-2016 at 08:21

Hmm. I thought he says as close to 30 percent as possible. After 30 percent a different undesirable form is made.

I could be mistaken. Anyways please report back on your results!

Tricka90 - 19-9-2016 at 08:34

In the paper you attached he doesn't define any limit about HNO3 concentration. He however advise against using more than 10% w.w AgNO3 concentration because in that case the formation of silver acetylide–hexanitrate would occur.
Talking about AgNO3 concentration, what do you think is optimal? It seems 5 to 10 % w.w range is ok.

MineMan - 19-9-2016 at 11:00

I don't know. If you read that paper several times you know just about what I do....

Tricka90 - 30-9-2016 at 23:51

Do you think that passing too much acetylene gas through the AgNO3 solution would cause any problem?

MineMan - 1-10-2016 at 10:51

No...

but I don't think you need any more than 3 minutes of time.

Tricka90 - 2-10-2016 at 00:29

Thank you MineMan.

What's your yield for SADS? I get about 0.4g SADS for 1g AgNO3 and I think that's pretty bad...

[Edited on 2-10-2016 by Tricka90]

MineMan - 2-10-2016 at 16:16

I think my yield is pretty close to yours maybe about .6.... instead of .4

Tricka90 - 25-10-2016 at 06:13

Since it seems like many forum members are having an hard time obtaining fairly pure white SADS I would like to share some tips on optimizing the whole process to get a powder as white as the one you can see in the attached picture (still wet), even when "dirty" acetylene gas (the one readily produced from calcium carbide and water reaction) is used.
I'm not an expert, so I'm just gathering all the rules that lead to the attainment of the pure product in the picture below (I'm supposing you're already familiar with the entire procedure).

- The following proportions between the reagents are recommended: 8.7ml H2O, 1.3ml 65% HNO3, 700mg AgNO3, 1.5g CaC2 in 40ml H20. More than 450mg net SADS will easily be obtained

- AgNO3 solution must reside inside of a narrow and tall cylinder when reacting with acetylene gas.

- AgNO3 must be as pure as possible, no copper derivatives are allowed, the best choice is nitrating very pure Ag

- H2O for both AgNO3 solution and gas generator must be bidistilled

- AgNO3 solution must be kept in the 65 to 70 °C temperature range during the whole reaction with acetylene

- A mechanical filter such as cotton or, even better, chemically unreactive cigarette filter must be firmly placed inside the tube which transports acetylene gas. When strongly blowing into the tube, air should come out with difficulty

- All the reactions must be performed with very soft light

- Acetylene gas should not react through AgNO3 solution for more than 4 minutes. More than that will produce just some tens of mg more of SADS but purity will decrease dramatically

- Filter must be washed before filtering the powder, which must be copiously washed with bidistilled water as well.

- Drying time must be reduced to a minimum (less than 24 h if possible) and performed in a clean, slightly warm, dry (of course

) and dark location. Water shouldn't be allowed to stay in contact with SADS for many hours so the powder must be spread out on a surface capable of absorbing water while not allowing for SADS to stick. Filter papers from chemistry stores are optimal.

I didn't add any book reference or justifications for any of the rules I listed, so if you're interested feel free to ask.
Hope this helps, have a nice day.

MineMan - 25-10-2016 at 09:01

Nice product,

I really like your tip about no more than 4 minutes. My best batch of SADS did not go off with hard grinding in a mortar and pestle. See if yours is the same

nitro-genes - 27-10-2016 at 11:47

Looks like an excellent product indeed and detailed write up, SADS when properly made is a very useful initiator with excellent properties. I must say, from my own experience (using very similar process) I used to get a snow white product, with pearl gloss with most batches of calcium carbide, though one particular batch of carbide was a really dark grey (with granular black lumps in between) and no matter how careful the synthesis was performed, the first bubble of acetylene produced immediately resulted in a dark brown precipitate. The crude carbide product can contain many impurities, some of which cannot be removed easily and likely form a complex with Ag+ as well. Looking for a visually clean batch of calcium carbide may reallly be of help due to differences in batch puritity.

Tricka90 - 28-10-2016 at 00:45

Thank you MineMan and nitro-genes, I'm happy you like the product.

@MineMan: The tip about avoiding long time exposure to acetylene gas isn't my idea, I read it in Matyas' Primary Explosives book where it's stated that if acetylene is passed for enough time, simple Ag2C2 may start forming.
In practice, if you carefully pay attention to the colour of the precipitate during its formation from the beginning to the end, you'll see that it gradually assumes a more grey and brownish tinge as the reaction proceeds.

@nitro-genes: I agree with you, having high purity calcium carbide is key, if even the first precipitate formed is not fairly white it is a clear indication that acetylene should undergo a purification process if high quality SADS is to be obtained.

MineMan - 28-10-2016 at 11:48

Looking forward to the det tests!

markx - 28-1-2017 at 06:23

Right....finally i've gone and and done it out of pure curiosity: dilution of SADS with KClO₃. A rather perilous and unknown path in the general direction of "courting disaster"

The SADS was a fresh batch from a procedure I've described earlier on this same thread and formed at exactly @ 65C. A potent sweet point for the pure stuff. Now to see if one can further enhance the performance with the aid of potassium chlorate. The chlorate is also from DIY electrosynthesis origin and has been meticulosly recristallised and ball milled to a fine powder. I presume it is quite pure in reasonable framework.

Sample mixtures of 100mg each were weighed in proportions to account for resulting dilutions that contained 0, 15, 20, 25, 30, 40 50 % of KClO₃. The samples were homogenised in the dry state very carefully with a plastic pestle in stainless steel vessel until presumed to be well mixed.

"Organoleptic" evaluation of performance was then commenced by picking up a small amount of the respective sample on the tip of a wooden safety match and then being lit with a butane torch. Resulting sound effect and the degree of shattering of the wooden match was used as a relative scale to assess the potency of the sample. Amount of samples tested was not strictly equal, but I tried to get the maximum amount of every mix to stick on the match tip without it falling apart or off under it's own weight. So they are more or or less comparable in terms of amount. The scales could not pick up the amount of sample so it must have been on the order of about 1mg.

So the results were quite interesting and in some ways unpredictable. What struck me with the greatest amazement was the fact that all of the mixtures up to 50% chlorate content by mass remained detonable in the tiniest of amounts just like pure double salt. Of course the power of the mixtures started to steer down starting from about 25% of chlorate content and upwards. At 50% chlorate content the mix was basically unable to damage the tip of the match and only scarred the surface, leaving a sooty stain. I do think that even above 50% chlorate content the mixture will still remain detonable, but as the performance had dropped below any practically acceptable level, did not go any further with the dilution this time.
The sweet spot of dilution mixtures seems to lie quite predictably in the range between 15-20% chlorate content by mass.

These samples caused by far the most damage to the wooden match and were characterised by a sharp and unbelievably strong sound even in these tiny amounts. I can not assure that the 15-20% dilutions are far superior compared to pure double salt in terms of "match shattering" performance, but they definately are not inferior according to the results at hand.
Of course nothing is known about the stability, sensitivity or viable storage time of these mixtures yet. So I will assume the worst at the moment and so should everyone else.

PHILOU Zrealone - 28-1-2017 at 10:39

Nice idea to mix KClO3 with SADS.
Next step AgClO2 /SADS

or AgNO2/SADS

It seems there is a SADS/SANC variant using Ag perchlorate instead of nitrate --> SAPC.
Maybe Ag chlorate can do aswel --> SACC :cool:

Your testing is a bit rough/arsh/primitive...would be better to get a sand crushing test with 10-50 mg of the various mixes...result would be more relevant, comparable to each other and of better scientific value.
Also not using very much material and not so costy.
Eventually the sand may be extracted with HNO3 to recover the silver nitrate

.

Also the % mixes into your study must hold a little more steps:
0, 5, 10, 15, 20, 25, 30, 35, 40, 45, 50
Then it would be perfect.

I have played a few days ago with snap it everywhere bangers (the tiny paper bags containing 4 to 5 grit stones (3mm diameter) and covered with silver fulminate)...the favourite sport of my brother and I is to open the bag cautiously and to boost the charge (when un-boosted you can snap it between your fingers without risk or pain) with 1-5 mg SADS/SANC...it turns then into an interesting detonating device...making your ears ring when trowed into a room...it makes a white thunderball (5-10 cm diameter) with a loud report...against a white wall it makes a radiant spot of black silver.
Of course when boosted it can hurt the fingers when snaping.
If you let the bag fall from 1m it detonates (propelling the grit onto the ground...so better wear glasses.

You can make booby traps with it, if someone walks onto it bang...under the wheels of a car with tape...bang when the wheel rol onto it.

The fun is that it is upgradable by joining more bags together...but caution...the power increases to the power 3 when doubled.

Also for storage...into cotton whool...no big quantity into the same place...and no rude handling.

[Edited on 28-1-2017 by PHILOU Zrealone]

markx - 28-1-2017 at 11:38

Quote: Originally posted by PHILOU Zrealone

Nice idea to mix KClO3 with SADS.
Next step AgClO2 /SADS

or AgNO2/SADS

It seems there is a SADS/SANC variant using Ag perchlorate instead of nitrate --> SAPC.
Maybe Ag chlorate can do aswel --> SACC :cool:

So many options on conducting a bit of pyrotechnical mischief

I do admit that the approach was insistently primitive, but I was not in the mood to mess up my perfectly good saturday afternoon with a coupious amount of unknown primary energetic mix going sideways on me and then having to explain the lot to the intern at the ER

To my defense I can say that at least I'm not drawing any far reaching conclusions from the "results".
But there is promise to the claim of sustainabilty if these dilutions hold up to the test of time in terms of stable and prolonged function. Only time will tell....
In the meantime one can do a more refined spectrum scan in the range between 10-20% chlorate content and refine the assessment method for brisance of the samples. I fear that quartz sand would be a medium of too high hardness for this mix, especially if one tests amounts in the range of 50mg as would be used in the intended initiation devices and hence it would possibly distort the results since resolution between the samples might be too small and overlapping. So what I would opt for is a nice soft limestone fraction in the range of say 250 microns with a very narrow particle size ditribution. Lucky me that my assistant has to handle and characterize the quality control of about 2 shipments of 30 tons of the stuff every week at work

I guess there is more on the topic coming in near future...

Laboratory of Liptakov - 29-1-2017 at 13:33

Interesting testig of SADS - KClO3. However for more precise results always is good metal plate. If all energy is discharge to plate, thus without hole, is measurement pretty precise. For 1 mg estimate Alu can Cola or 2 - 3 layers of this material. In metal arises impact with a memory and it is possible easy measurement. Impact without hole, this is important. All energy must be discharge to metal. Without spend in hole. Best is annealing metal, aluminium or copper. Both have a good memory on the shockwave. Thickness can be 0,1 to 0,5 mm for very small samples about 1 mg to 10 mg of EM.
........LL.......... :cool:

markx - 30-1-2017 at 10:02

Thanks to the moderately affordable luxury of a chinese mini lathe I've been tinkering on the setup of sand crushing test equipment....

First one is going to need a sample forming set...like the one below:

Which is put together like that:

Allrighty then....let's weigh a sample into the tube:

Compact it moderately to fix it in the tube:

Attach the fuse holder and a lenght of visco:

And we have a sample ready for testing and evaluation....of course for that we are going to need a sand cell to contain the evaluation medium.

Like the one below...the "nr 36" cell....yup, looks aboot right:

Can be dissasembled for easier filling and amptying of sand and test samples:

So for further steps one is going to lower the sample into the cell and add a preweighed fraction of evaluation medium to cover the sample (granulometry must be known and tightly conrolled). Then assemble the cell and light the fuse. After the "pop", disassemble cell, remove sand and separate sample parts: fuse holder, end cap, etc. Weigh the sand to be sure none has been lost and perform sieve analysis to evaluate how much sand has been reduced in grit and relate that to the "potency" of the sample. This should give better scientific value than comparing mangled match tips

PHILOU Zrealone - 30-1-2017 at 10:36

Really nice setup markx!

Where did you bought it and for what price?

Would be nice to get a standard procedure and setup between forum members.

markx - 30-1-2017 at 11:22

I did not buy it....made it all from scratch today at work

Bits and pieces picked up from workshop metal scrap dumpster and adding a little value and function...

Laboratory of Liptakov - 31-1-2017 at 01:06

Oh my God...super science aparatus for international research of all primary materials. Los Alamos Laboratory device. I am waiting on the first results.......... :cool:

....LL

markx - 31-1-2017 at 02:34

Update.....

The "nr 36" cell is officially complete and ready for testing:

It was missing the bottom in last post, so I had to "fabricooble" one

And a dedicated sample holder that threads in dead center:

Turned out pretty good.....it's awesome how much possibilites open up if one owns a small lathe and a welding apparatus

As for the testing medium I'm going to use 250/100 micron limestone sand fraction and brisance shall b related to the amount of fraction passing through 100 micron sieve after testing. One can accumulate several repetitions on a single sieve and get an averaged and more representative result for the mesured sample mix. This prevents the extra work of sieving each sample and averaging afterwards.

The sand bulk in drying process....porosity makes it hard to get the moisture out, but it's moving along and shall be ready to use tomorrow:

[Edited on 31-1-2017 by markx]

PHILOU Zrealone - 31-1-2017 at 13:06

Wow! You work fast and ingeniously!

I'm more than eager to see first results.

Sand will dry faster in a kind of tumble drier or into a fluidized bed (warm air from under through the sand that is lifted up (fluidized) a little and fall back down).

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