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prometheus1970
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Ag2C2.AGNO3 (DS)
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]
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not_important
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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.
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Rosco Bodine
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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 1243 times
Attachment: GB616319 Silver Acetylide complex salts.pdf (339kB)
This file has been downloaded 1435 times
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zajcek01
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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)
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prometheus1970
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Ag2C2.AGNO3 (DS) synth
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]
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hiperion42
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PHILOU Zrealone has given some tips for
producing high purity product.
http://www.sciencemadness.org/talk/viewthread.php?tid=1031&a...
.....ejuu....................................................................Ffg..............................g.............
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prometheus1970
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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]
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-=HeX=-
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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"
If you give a man a match he will be warm for a moment. Set him alight and he will be warm for the rest of his life.
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Jimbo Jones
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Actually itβs 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 β 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 β 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...
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-=HeX=-
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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.
If you give a man a match he will be warm for a moment. Set him alight and he will be warm for the rest of his life.
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prometheus1970
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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)
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prometheus1970
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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?
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grndpndr
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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] |
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quicksilver
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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.
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prometheus1970
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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]
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quicksilver
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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.
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prometheus1970
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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]
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quicksilver
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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]
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The WiZard is In
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| 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.
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. |
Beware of the I loose money on every item I sell β
I make it up on the postage eBay sellers.
One US buck for 100gms.... http://tinyurl.com/4k2rm5o
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prometheus1970
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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...
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prometheus1970
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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]
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quicksilver
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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.
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grndpndr
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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.
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prometheus1970
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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
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Jimmi_P
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| 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.
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