quantumcorespacealchemyst
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chemistry of GOLD, known reactions and techniques
this is a thread for a comprehensive knowledge database of the reactions of Gold, encompassing all available mechanisms such as chemical,
electrochemical and photochemical techniques, beyond the standard approach of aqua regia. in depth detail and safety information included in procedure
is highly ideal, such as; using permanganate with gold and achieving permanganates and if the mechanisms allow for MnO3+ on gold or if the pentoxide
of manganese will precipitate before attaching and detonate in its own water of formation? this is not a prospecting thread.
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j_sum1
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The what???
Is there a specific question in there somewhere?
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DrMario
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As a first contribution, I submit the topic of thiols on gold:
A nice blog post about the nature of gold-sulfur bonds (it asks much more than it answers):
http://syntheticremarks.com/?p=3711
Related to this, a Sigma-Aldrich whitepaper on thiol SAM preparation on gold:
https://www.sigmaaldrich.com/content/dam/sigma-aldrich/docs/...
Finally, an open access review article published in Nature, on the nanotechnology of the gold-sulfur interface:
http://www.nature.com/nchem/journal/v4/n6/full/nchem.1352.ht...
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blogfast25
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Maybe not but you'd be more convincing if you put up some of your own stuff.
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quantumcorespacealchemyst
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just touching on what doesn't work, i will start from the first part of this working. 2.602g KNO3 and 5.700g NaHSO4 boil in 5ml of water from
distilling to evolve gas, which condenses into a two neck flask with an excess of iodine, and gets heat to form vapor with a condenser on it to keep
it contained. the boiling continues with intermittent fiddling of the magnetic stirrer untill the reaction becomes mostly syrupy, evolving much less
gas and with all the tin foil wrapped around the contraption, carries no more droplets over to the receiving flask. the Au in the receiving flask
seemingly does not react. it sits overnight after filling most of the way with 98% H2SOSO4 and through the day until the next working.
the flask with condensers are shown in the pictures before being reset up on the hotplate with .22mm diameter Pt .950 wire running down the condenser
as the positive cathode and also through the second condenser to a foil of Ta as the negative anode which has a covering of Teflon sheet to keep
electrode separation. sealing of joints is from teflon sheet cut to strips. there are miscalculations on the attached picture due to my notebook
having not quite .5cm boxes. the seals work and tinkering will help hopefully. the power source is 2 series 6v Eveready batteries and the hotplate is
on about 120 degrees Celsius after the electrodes are connected. the color change is noticeable as the reaction progresses and the pump breaks partway
through and the build-up of iodine sublimation is visible in the photographs. the reaction is now slighly warm and is still having the electrodes
connecting. Pt electrode down the main condensor is to + terminal and the Ta/Pt one is to - terminal on batteries.
         
the pictures are backwards and the numbers tell the order. this reaction is now resting with no input energy.
at 14/20 joints, the Teflon sheet sealing is 28mm for a double wrap to seal the vessel. with 1:10 taper, the bottom is 24mm if the height is 20mm.
playing with physical wrapping estimates of math and compass gets close, the measuring scale of graph notebook paper is not quite .5cm it turns out.
indentation by pencil tracing, cutting by scalpel/Xacto blade and trimming on wrapping on joints affords an affordable and effective solution to
Teflon joint sleeves. the math on the paper board is funny and i don't remember where it is from now. there was something about multiplying by 3pi for
the circumference. the mm are cm i believe and then there's more to fix up.
[Edited on 30-10-2014 by quantumcorespacealchemyst]
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quantumcorespacealchemyst
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before. after.
 
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quantumcorespacealchemyst
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dissasembled, Ta electrode, filtered precipitate with undisolved gold, mother liquor/acid, brown precipatate and undissolved gold.
the Ta electrode has some of the brown powder on it so it seems the gold gos + and then reduces on the tantalum. i am hoping for auri-iodic acid in
the mother liquor, although it seems that the gold all is out of solution, the iodine is all dissolved save for the sublimed portions, especially the
over collection on the smaller condenser after pump failure.
    
also there is a patina of what looks like gold (i) iodide on another piece of Au that has been sitting in acetone saturated with iodine and with some
H2SO4 added, sitting for 2-3 days. the camera here does not pick up color and detail very well and so i am not posting a picture now.
[Edited on 31-10-2014 by quantumcorespacealchemyst]
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quantumcorespacealchemyst
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ether wash separated
boiled off
washed again
boiled off
Second time the boiling was inside out of the cold in the same Epsom salt bath. it vaporized somewhat with violet vapor and when the apparatus was
disassembled. I do not know if it was organic or HAuI4. Hopefully, the latter. it smelled not of iodine. if there was subliming iodine it was
seemingly intermingled. Currently it is in a desiccator bag with NaOH in another bottle drying.
   
[Edited on 8-11-2014 by quantumcorespacealchemyst]
[Edited on 8-11-2014 by quantumcorespacealchemyst]
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kmno4
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As I understand, it is some kind of dirty equipment exhibition, because it has nothing (so far) to do with "chemistry of GOLD, known reactions and
techniques".
Слава Україні !
Героям слава !
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aga
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Gold is shiny ...
Edit:
.. or not if it's dirty.
Maybe pink as a muddy precipitate.
Wee-coloured as an Ion.
[Edited on 8-11-2014 by aga]
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subsecret
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You produced nitric acid in situ from KNO3 and NaHSO4? Iron wool column packing and HNO3 are a bad idea. Try using glass beads.
Fear is what you get when caution wasn't enough.
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aga
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Nice response:
There's Nothing really here for anyone to comment about.
The photos are great, yet no chemistry or science as such.
Weights, concentrations, times, temperatures, chemical formulae, a question even.
The world knowedge-base of gold reactions is already collated and documented, and available on the t'interweb.
The notion that This Thread would encapsulate All Arcane Gold Knowledge may have been a little ambitious.
Please ask your Chemistry Question(s)
Normal response:
Detritus ?
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blogfast25
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So much abuse of exquisite glassware. Is that the sound of rattling bones, of real alchemists turning in their graves?
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quantumcorespacealchemyst
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the 2.602g KNO3 and 5.700g NaHSO4 were put in a flask and 5ml of water was added. it was boiled until the syrup did not give enough vapor to condense
over through the condensor into the flask with the iodine which was heated to give vapor. there is no steel wool, that is all sublimed iodine.
this reaction is puzzling as the liquid obtained was a violet black one which was washed with diethyl ether again separated and then boiled again
indoors (which is much warmer this time of year compared to around 50F i believe). which gave a violet dark liquid but this time it smells of an odd
smell, with perhaps a bit of iodine smell but mostly some other odd smell. i left it in a bag with some NaOH to dry for three days and it seems to
have colored the bag so it seems the second time evaporating may have decomposed the compound slightly because when the diethyl ether mix was
evaporated the second time it was indoors and the temperature seems to have been higher in the epsom salt water bath than the 99 degrees C outside.
the result was fuming and smelled funny, where as the first time it was not and seemed to have more liquid and not leave iodine haze on beaker walls
or bottle tops (it was stored the first time overnight). the seperated part from the main washings with ether, which is presumably acid is an amber
color so i dont know where the iodine is besides, in HAuI4, dissolved I2 and possibly HI or HIO3? also, i dont know what the HAuI4 decomposes to as http://gold.atomistry.com/auri_iodic_acid.html gives not much information
i do not remember if i posted the calculations, the iodine was in an amount not recorded from the beginning, used as a vapor generator and then
brought into the reaction. the gold is calculated as 0.126g being in the reaction with 0.127g being recovered in powder and some undissolved pieces
(originally 0.353g). calculation of iodine being in HAuI4 is 0.32472440099g. more than that was added by estimation by eye. the amount that sublimed,
stuck to the flask and was removed is unknown although probably at least a gram of a more than gram amount.
the product seems to be contaminated with iodine but if it is from left over from the solution or a decomposition product i do not know and i do not
have a datasheet/page of HAuI4 to reference.
these pictures are the liquid mostly dry after 4 days. the bag with the haze is behind the second picture.
[Edited on 11-11-2014 by quantumcorespacealchemyst]
  
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quantumcorespacealchemyst
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if a person may help me by telling me what books contain the known reactions of gold and the compound properties, please tell me what they are and/or
where to find them. this thread was began for the purpose of concentrating this stuff in one place and was stated to not be about prospecting so that
the ore processing is talked about on ore processing threads and the chemical workings itself are somewhere separate and side by side. initiating the
thread does not mean i have this knowledge, it is to gather it for people of like mind of working with gold (i hope that it can be done for the
platinum group metals, lanthanides and actinides as well). this glassware is available on ebay currently. hopefully the availability becomes greater
and at lower prices. group purchases on quartz glassware may be done from affordable sellers from china on aliexpress or elsewhere. if american/local
(i live in america) sellers can do the same, that will be great, currently the prices of major glass manufacturers are prohibiting to amateurs,
especially in quartz, if they make it at all.
these are not quartz, they are borosilicate 3.3
i used 14/20 diameter/length glassware from ebay here, the last part used adaptors and all of it used teflon sheets that were and hopefully still are
1-2 USD from ebay, cut to shape with an exacto knife.
the idea here is to show what it looks like while it does and doesn't work and to get an idea of what it is. writing doesn't always give enough data
and scientific papers have been known to not be reproduceable.
this is meant to demystify chemistry and my name on here is supposed to be quantumcorespacealchemystery and the ery doesn't fit on the name
application
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Chemosynthesis
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What I believe the members here are clearly trying to convey is that you are not proposing any hypothetical reactions, giving proper scientific
notations of reproducible measurements and conditions, or doing any science. This is strange when you also do not have any questions in your post.
The whole point of this forum is amateur experimentalism, which requires all I just said. Mixing random chemicals together and then claiming it didn't
work is nonsensical. What are you trying to achieve?
The scientific method works on falsifiable hypotheses with reproducible experimental conditions. Getting the glassware (most members here have
glassware and you seem to the only one mentioning quartz) and some chemicals (best to note sources together isn't any more science than sticking the
word "quantum" in your username makes any sense....
Science as a subject and quantum as in quantum chemistry and physics have meanings, and it can be insulting to people who achieved tedious mastery of
coursework on these to sit through misappropriation and devaluation of these, particularly when poor grammar is used. On that last note, if you truly
live in the U.S., please stop using antecedent less pronouns. Unless the reader is psychic, this is an extremely vague and error prone manner of
communicating. Ambiguity is inherently unscientific in that it inhibits efficient replication of experimentation. Scientific discourse should be clear
and concise.
If you had asked for sources of gold chemistry (improperly capitalized in your thread title) in the first post, you may have been pointed in a more
productive direction days ago.
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quantumcorespacealchemyst
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you get no argument from me guy
any people on here who have gold reaction information please post it all up and down this forum AHAHAHAHA
if permanganating gold can be done without explosions, please post that too
and if anyone knows why my goop decomposed indoors but not outdoors, please let me know that too (decomp temp of HAuI4???)
[Edited on 14-11-2014 by quantumcorespacealchemyst]
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quantumcorespacealchemyst
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odd result
the solution that smelt burnt (like a burnt battery or motor, i don't know, exept relating this smell with burnt electronics) had dried/evaporated and
collected mostly on the cloth cover over the beaker. inside was gold powder, this time golden not brown. among the gold powder was a SILVER hued
amount of peices and some dark black/purplish parts. this was washed with ether and all but the about half to two thirds of the gold powder was able
to be poured into a small beaker. the liquid was amber and the first and largest part of it was spilled (splotch in pictures). the majority of it was
salvaged with two pipettes and ether and herding it into the indentation on the surface and pipetting it back to the beaker. between the spill and
salvaging, the peices of gold that were in the beaker were washed into a fritted buchner funnel and washed. the ether from that was used to salvage
the concentrate on the surface (which appears to be iodine in an odd form similar to when iodine in acetone was spilled on the right side of the
surface and is still there).
so the salvaged gold pieces were attempted to be recovered out of the fine frit and only part of them were recovered, the rest are still in the frit
haha. the recovery was done by pouring water through it reverse into the original container. this was soaked up some with a bit of mercury .116g i
think.. the powder after the second recovery, the frit after attempted washing and the mercury bead are in the pictures
the salvaged goop with gunk/dust seems to be only iodine and doesn't dissolve in water (in picture). although it seems a tiny bit of it could be a
compound. the old acetone spill is shown (with the gunk in the beaker and a bottle of supposedly 100 percent acetone, that is saturated with iodine.)
the cloth, smells of burnt electrical stuff and i am convinced is an odd compound that has iodine in it.
the splotches next to the beaker are those from the previous acetone spill and this is puzzling (the top is a microwave oven side (parts, copper and
stuff, desk for now))
there is some gold to work with
this is a mystery to me.
i read that diethyl ether with iodine in it with gold makes AuI which is a pathway i am interested in for reacting with BiI3
http://en.wikipedia.org/wiki/Bismuth%28III%29_iodide
[Bismuth(III) iodide forms iodobismuth(III) anions when heated with halide donors:[10]
2 NaI + BiI3 → Na2[BiI5] ]
the HAuI4 is still not achieved
and if anyone knows if 3:1 HI:HNO3 is effective as aqua regia, please let me know. i am wondering why this experiment has not yielded any iodoauric
acid
      
[Edited on 28-11-2014 by quantumcorespacealchemyst]
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bismuthate
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I'm gonna be honest I don't think that Au2(BiI5) would be stable.
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forgottenpassword
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The open access journal Gold Bulletin contains more information than you probably want to know about gold: http://link.springer.com/journal/13404
If you copy procedures from there you will encounter less problems than through your current method of trying to re-discover the chemistry. People
have made (and documented) their mistakes so that you don't have to.
As regards your numerous spillages: do not think that heavy metal salts are harmless.
[Edited on 28-11-2014 by forgottenpassword]
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quantumcorespacealchemyst
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bismuthate, yea your probably right, i hope it works. i want to see if mercury iodide does complex as well.
forgottenpassword, awesomeawsomeawesome, i am about to delve in to that
dr mario, thank you for those gold/sulphur related links, especially the first.
edit: is HI in place of the HCl in/of aqua regia effective on gold?
[Edited on 2-12-2014 by quantumcorespacealchemyst]
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forgottenpassword
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Be advised that such journals do not remain open access forever, so -- if as seems likely -- you have some peculiar affection towards gold, then
perhaps you should look at downloading the articles for later-retrieval. Take note of the warnings of toxicity, though. Nice, shiny gold compounds can
still be toxic. If you choose to work with silver you could even turn your skin permanently silver -- a condition known as 'argyria'. I don't know of
a similar condition for gold, so don't even try. Your liver would pack-in long before your skin decided to radiate! 
[Edited on 2-12-2014 by forgottenpassword]
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aga
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Blue, Greyish.
No shiny Silver Surfer look with argyria.
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quantumcorespacealchemyst
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it tuns out, the H2SO4 i was using was 2N, nowhere near the 98% o 95% i thought i had (wrote one o those somewhere). that explains my constant
puzzlement about it's peculia properties and failed reactions.
i took some acetone wash of the reclaimed iodine and put some in a container i let sealed that looked like it was growing mold. it had NaOH o i added
it and aluminum. ate it seemed the gunk was dead and it sat awhile, thee was purple condensate.
it seems thee was/is some gold in thee and it made an alloy with the aluminum. i don';'t think it was any iodine.
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