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CHRIS25
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Yes, that's what came out the bottom, the alchohol a little yellow.
‘Calcination… is such a Separation of Bodies by Fire, as makes ‘em easily reducible into Powder; and for that reason ‘tis call’d by some
Chymical Pulverization.’ (John Friend, Chymical Lectures London, 1712)
Right is right, even if everyone is against it, and wrong is wrong, even if everyone is for it. (William Penn 1644-1718)
The very nature of Random, Chance development precludes the existence of Order - strange that our organic and inorganic world is so well defined by
precision and law. (me)
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CHRIS25
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Testing for Potassium chloride Tartaric acid presence
Hallo, I have a filtered white crystaline mass which I believe is potassium chloride, but I want to know whether this really is KCL or whether it has
any tartaric acid in it, it smells of surgical spirits, but I do not want to just throw it away and start again, I want to test so that I can learn
and establish what has been happening. If someone could advise please.
‘Calcination… is such a Separation of Bodies by Fire, as makes ‘em easily reducible into Powder; and for that reason ‘tis call’d by some
Chymical Pulverization.’ (John Friend, Chymical Lectures London, 1712)
Right is right, even if everyone is against it, and wrong is wrong, even if everyone is for it. (William Penn 1644-1718)
The very nature of Random, Chance development precludes the existence of Order - strange that our organic and inorganic world is so well defined by
precision and law. (me)
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vmelkon
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1. Flame test for potassium
2. Dry your solution slowly to have large crystals. Check out the crystal structure.
3. Add to some baking soda and see if it fizzes (acid test)
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CHRIS25
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Ok, thankyou. Right, I added white powder to sodium bicarbonate, it fizzed. Also that had a PH of 8. I then added some to distilled water. The KCL
obviously did not dissolve, but the solution was PH3.
So the methanol idea does not work in the slightest. How then can I separate the KCL from the Tartaric acid. Simply add distilled water and filtrate
I suppose? Why then did some suggest the alchohol method - it did not work.
[Edited on 1-11-2012 by CHRIS25]
‘Calcination… is such a Separation of Bodies by Fire, as makes ‘em easily reducible into Powder; and for that reason ‘tis call’d by some
Chymical Pulverization.’ (John Friend, Chymical Lectures London, 1712)
Right is right, even if everyone is against it, and wrong is wrong, even if everyone is for it. (William Penn 1644-1718)
The very nature of Random, Chance development precludes the existence of Order - strange that our organic and inorganic world is so well defined by
precision and law. (me)
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CHRIS25
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Potassium chloride is supposed to be Soluble.....
Whatever I have does not dissolve. At least not noticeably. I passed de-ionized water through it twice and the PH of the water is 3, indicating
tartaric acid. But the white mass does not dissolve, otherwise I would have not been able to get a clear solution from the filter. Now this white
crystalline powder is supposed to be KCL with a solubility of the top of my head 200-280g per 100mLs. Coming from potassium bitartrate and mixed with
HCl I don't see the logic here.
The original suggestion to isolate tartaric acid was via alchohol because KCL does not dissolve in alchohol but tartaric acid can be dried out
after filtration definitely does not work at all.
I am sure there is a logical explanation to all this, but I can not see it. I really need some help.
‘Calcination… is such a Separation of Bodies by Fire, as makes ‘em easily reducible into Powder; and for that reason ‘tis call’d by some
Chymical Pulverization.’ (John Friend, Chymical Lectures London, 1712)
Right is right, even if everyone is against it, and wrong is wrong, even if everyone is for it. (William Penn 1644-1718)
The very nature of Random, Chance development precludes the existence of Order - strange that our organic and inorganic world is so well defined by
precision and law. (me)
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Nicodem
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Threads Merged
2-11-2012 at 04:43 |
CHRIS25
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I have an unknown product which was supposed to be Tartaric acid crystallizing out of solution as the solution was left to evaporate over many days.
This was what I did:
CaCo3+C4H5KO6 gives C4H4CaO6+CH4K2O6+h2O+CO2: Then:
CaCL2+CH4K2O6 gives2KCl+CH4CaO6: Then:
H2SO4+C4H4CaO6 gives CaSO4+C4H6O6
Method: 250mLs of warm water and added cream of Tartar, potassium bitartrate and dissolved. Then:
Added 15g Calcium carbonate. Then:
Filtered the calcium Tartrate precipitate and collected this into a beaker and added 25mLs of 98% sulphuric acid dissolved in 75mLs of de-ionised
water. Then:
Waited until all the precipiate had settled to the bottom whilst still keeping the solution warm at around the 75c temperature. Filtered this
precipitate and poured de-ionised water over it several times to collect the solution in the beaker. Allowed to cool and evaporate. But after three
days I decided (after checking whether anything would decompose) to heat the solution gently for a number of hours and indeed I reduced the 300mLs to
60mLs and then removed from the heat and allowed to cool.
Observations about the the last part: The solution was very clear, after many hours of heating there was just water vapour coming off; then there
suddenly appeared, after I left the solution un-attended for two hours, a room full of obnoxious gas, a foggy cloudy gas hanging, I had to ventilate
the room quickly. The solution was now a light yellow colour and with white, fog like material settling at the bottom. I had earlier on, before
heating noticed fine crystal-like structures that dissolved upon heating and then re-appeared upon cooling, but now that has all gone. Also the PH
is now at this moment at 11, whereas when I first did a litmus test at the end of the whole double displacement, when I poured water over the calcium
sulphate and collected the solution, and before the first heating, the PH was at 1. After trying to research out everything I can about tartaric
acid and sulphuric acid I have no clue now what I have or why the PH change. Grateful for some insight or pointers please.
There is a part at the end of this video that is inconsistent, or at least, confusing. http://www.youtube.com/watch?v=Bt36jpk02Pk
He quotes in the video the following: "Filtrate while is still hot. Wash many times the sulfate that contains still quantities of tartaric acid and
add the washing water to the philtrate. Let it evaporates for 6-10 days, than you will collect large crystals of tartaric acid".
If you follow this, as I did, and wash the calcium sulphate as he says you end up with huge amounts of wash water in your beaker, which is not shown
on the video. Secondly a Filtrate IS the solution after the mass has been filtered, so what he mistakingly says next is to then wash all the wash
water that you have just used to wash the Sulphate....which obviously I did not do. So I would be grateful if someone could clear up this confusing
explanation please.
[Edited on 8-11-2012 by CHRIS25]
[Edited on 9-11-2012 by CHRIS25]
‘Calcination… is such a Separation of Bodies by Fire, as makes ‘em easily reducible into Powder; and for that reason ‘tis call’d by some
Chymical Pulverization.’ (John Friend, Chymical Lectures London, 1712)
Right is right, even if everyone is against it, and wrong is wrong, even if everyone is for it. (William Penn 1644-1718)
The very nature of Random, Chance development precludes the existence of Order - strange that our organic and inorganic world is so well defined by
precision and law. (me)
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CHRIS25
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After two failed attempts I decided to follow my own calculations according to the stoichemetry. Believing that he might have a reason for way off
calcuulations I did the reaction a third time according to strict stoichemetry.
Working with 37.5g Potassium bitartrate
That would be 10g of CaCO3 not 15
11.1g of CaCl2 not 15
and then 9.8 mLs of H2SO4 and 15 mL water not 25mLs and 75 mLs water.
This third attempt also failed, the yield was practically the same as the last two times - about 0.2g of crystals still in solution - since
evaporation will take at least two weeks especially if, after he suggests, you keep pouring water over the sulphate to flush out the tartaric acid in
the filter, Any suggestions. I could buy the stuff tomorrow but I don't really want to give up on this one just yet.
‘Calcination… is such a Separation of Bodies by Fire, as makes ‘em easily reducible into Powder; and for that reason ‘tis call’d by some
Chymical Pulverization.’ (John Friend, Chymical Lectures London, 1712)
Right is right, even if everyone is against it, and wrong is wrong, even if everyone is for it. (William Penn 1644-1718)
The very nature of Random, Chance development precludes the existence of Order - strange that our organic and inorganic world is so well defined by
precision and law. (me)
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CHRIS25
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Registered: 6-4-2012
Location: Ireland
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Well, success! Spoke too early. I have a nice collection of tartaric acid crystals. I was fooled, because after I noticed crystals forming last
week they disappeared after about 5 days - and the solution turned from a free flowing watery solution into a mildly thick viscous light cream
solution with no sign of crystals and I assumed that this had failed. But after another two days a whole load of tartaric acid crystals appeared with
almost complete evaporation.
‘Calcination… is such a Separation of Bodies by Fire, as makes ‘em easily reducible into Powder; and for that reason ‘tis call’d by some
Chymical Pulverization.’ (John Friend, Chymical Lectures London, 1712)
Right is right, even if everyone is against it, and wrong is wrong, even if everyone is for it. (William Penn 1644-1718)
The very nature of Random, Chance development precludes the existence of Order - strange that our organic and inorganic world is so well defined by
precision and law. (me)
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ErgoloidMesylate
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Mood: Freedom of thought is priceless - You can't afford it
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Tartaric acid prep - OTC
Quote: Originally posted by CHRIS25  | | Well, success! Spoke too early. I have a nice collection of tartaric acid crystals. I was fooled, because after I noticed crystals forming last
week they disappeared after about 5 days - and the solution turned from a free flowing watery solution into a mildly thick viscous light cream
solution with no sign of crystals and I assumed that this had failed. But after another two days a whole load of tartaric acid crystals appeared with
almost complete evaporation. |
That calcium method tends to form a nasty sludge. A cleaner prep, I have permission to detail, that guaranteed was not done by me, but was an adaption
from a science journal. It uses 91% isopropyl, which may dissolve some of the ionic salts, but the precip should leave those in solution, and spit out
the tartaric. It uses a vacuum (water aspirator vacuum is sufficient).
10 grams cream of tartar
50 ml distilled water
Stir to dissolve as much as possible.
10ml of concentrated hydrochloric acid
Stir for one minute
Vacuum to reduce volume to 10 ml
Should be yellowish at this point, and have some crystals floating around in it.
100 ml of 91% isopropyl to dissolve.
Anything that does not dissolve should be filtered out at this point.
Now use vacuum to reduce to 50 ml.
The tartaric acid should precipitate and should be filtered out.
Cannula transfer and cannula filtering is used for lysergic synth Compressed air and remove co2
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