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pneumatician
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Mood: ■■■■■■■■■■ INRI ■■■■■■■■■■ ** Igne Natura Renovatur Integra **
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if you reduce it to dust?? no more sprinkled around???
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DraconicAcid
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Location: The tiniest college campus ever....
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Mood: Semi-victorious.
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Reacting some of my samarium with sulphuric acid. Yellow.
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
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B(a)P
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Distillation of fuming nitric acid from potassium nitrate and concentrated sulfuric acid.
Measured density 1.54 g/mL +- 0.03 g/mL at 15C, so likely north of 98% concentration.
Pretty happy with that!
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Sir_Gawain
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Tried to make NHN with hydrazine dihydrogenchloride. The freebasing really sucked because I ran out of filter paper. When I began addition of nickel
nitrate a bluish precipitate formed, then changed to light purple. The dried product was only slightly energetic.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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solitanze
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I made a good sized quantity of Mohr's salt, ferrous ammonium sulfate from fertilizers. The pale green crystals are really pretty.
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DraconicAcid
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Going to work up my samarium(III) sulphate.
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
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Rainwater
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Just watched my fireworks sparkle. 3 of 5 were successful.
All burned completely, failures simply did not have effect, only color.
All ammonia perchlorate based, 8g
powdered sugar, 5g
2g sulfur
10g nitrate salts charcoal powder blend
5g of effect
6in long, 1in diameter cardboard tube.
Aluminum nitrate with Iron powder wrapped in magnesium foil
Copper nitrate with wax coated Calcium metal beads.
Tin nitrate wax coated Sodium beads (Fail)
Silver nitrate with wax coated Potassium/sodium beads. (Will do again, machine gun like pops)
Lithium nitrate with wax coated aluminum powder(fail)
Stay safe friends
"You can't do that" - challenge accepted
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DraconicAcid
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Okay, so I worked up my samarium(III) sulphate. Nice yellow powder (gonna have to find a way to get crystals of it).
A bunch of the metal didn't react, so I put it in hydrochloric acid. Immediate, vigorous reaction, and it turned red. Once it settled down, there
was a yellow solution, a bit of still-fizzing metal bits, and some red precipitate. Red?? I thought all samarium(III) compounds were yellow.
Samarium(II) chloride is brown, but isn't water-stable. Insoluble samarium(II) sulphate, maybe?
ETA: Actually, it seems that it should be samarium(II) sulphate:
https://scholarworks.uni.edu/cgi/viewcontent.cgi?article=315...
If so, it should be samarium(III) tomorrow.
ETA: Yep. It's all yellow now.
[Edited on 5-1-2023 by DraconicAcid]
[Edited on 5-1-2023 by DraconicAcid]
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
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j_sum1
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Potassium dichromate
Potassium dichromate
One of my first ever experiments was the aluminothermic reduction of pottery grade chromium oxide to obtain elemental chromium for my element
collection. Product was obviously impure with lots of aluminium products in the mix. Recently I have been attempting to make something useful from
the mixture. Procedure as follows:
Digest with concentrated HCl to make a solution containing Cr(III)
Neutralise and precipitate with sodium carbonate.
Repeated filter and wash steps to obtain Cr2(CO3)3 of acceptable purity. (Stuff is a dog to filter: not as bad as calcium sulfate but close.)
Dry and roast to obtain Cr2O3
React with KNO3 to get potassium dichromate. Cr2O3 + 2KNO3 --> K2Cr2O7 + 2NO.
Dissolve in water, filter and crystallise.
I have had a bit of fun playing with other routes and other oxidisers to target other useful Cr(VI) compounds: sodium or ammonium dichromate of
chromates. The problem with sodium dichromate is separating it from soluble byproducts at sensible yields. Similarly, ammonium dichromate is going
to have high yield loss and impurity issues due to other species that will crystallise out at the same time. Isolation of calcium chromate might be
a good idea, and easy to separate since it has an inverse solubility curve and is quite insoluble anyway. But I have very little calcium nitrate and
so it is not very practical as a recovery method.
I do have a lovely array of bright coloured test tubes for my efforts.
[Edited on 1-4-2023 by j_sum1]
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Admagistr
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@ j_sum1
Neutralise and precipitate with sodium carbonate.
Repeated filter and wash steps to obtain Cr2(CO3)3 of acceptable purity.
Are you sure that chromium (III) carbonate exists??When I precipitated it out of solution, after a short time CO2 was released and undoubtedly Cr(OH)3
was formed. Similarly, aluminium carbonate cannot be prepared...Even in the literature-Remy,Inorganic Chemistry-It is said that carbonates of Al and
Cr cannot be precipitated from aqueous solution because they are unstable and turn into hydroxides when CO2 is released...
[Edited on 1-4-2023 by Admagistr]
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j_sum1
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You are probably right. The dried chromium compound did not produce much gas when tested with acid. So, probably oxide or hydroxide. With some
residual Na2CO3 present.
Carbonate was what I intended and what I wrote above and also in my lab notes. But after testing with acid I proceded as though it was oxide and
reacted with KNO3. I should have spotted my error when writing that post.
K2Cr2O7 solution looks good and is forming nice crystals. I think I have made good use of some waste I had lying around.
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Admagistr
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j_sum1:
K2Cr2O7 solution looks good and is forming nice crystals. I think I have made good use of some waste I had lying around.[/rquote]
Dichromate is visually very beautiful compound ! I plan to reduce it with SnCl2 and
also by its reaction with Na2CO3 to form compound 3K2CrO4.Na2CrO4,which during crystallization produces light flashes(triboluminescence.)
[Edited on 1-4-2023 by Admagistr]
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DraconicAcid
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I now have holmium, samarium, erbium, and neodymium sulphates, from metals or metal oxides from AliExpress. Pretty. I'd like to grow bigger crystals
of them, but not sure how, with their weird decreasing-solubility-with-temperature.
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
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Admagistr
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Quote: Originally posted by DraconicAcid  | | I now have holmium, samarium, erbium, and neodymium sulphates, from metals or metal oxides from AliExpress. Pretty. I'd like to grow bigger crystals
of them, but not sure how, with their weird decreasing-solubility-with-temperature. |
I recommend the production of crystals of holmium compounds, they are in daylight, yellow in the sun light and in some types of artificial lighting
change color to pink, then it look like compounds of erbium...But I do not have practical experience with growing these crystals yet...
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Bedlasky
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| Quote: Originally posted by DraconicAcid | | I now have holmium, samarium, erbium, and neodymium sulphates, from metals or metal oxides from AliExpress. Pretty. I'd like to grow bigger crystals
of them, but not sure how, with their weird decreasing-solubility-with-temperature. |
Try to make saturated solution and let it evaporate.
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Lionel Spanner
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Made methyl acetate last week, using a nice simple Fischer-Speier reaction with a 5:1 excess of methanol and 5 mol% sulphuric acid. It smelt very
pleasant in a solvent-y way, and proved hard to separate from methanol even using extractive distillation and a Vigreux column, though the methanol
will likely be removed in the next step (Claisen condensation with sodium methoxide to form methyl acetoacetate, which has a much higher boiling point
than methanol.)
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Texium
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Yeah for that reaction you shouldn’t have to worry about excess methanol being an issue. Nice.
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j_sum1
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I have done very few steam distillations and decided today was the day.
Steam distillation of dried thyme.
Leaves swelled. Boiling bumped. 500ml flask overfilled. Leaves through everything jamming every crevice of the glassware. Yield low and stopped early.
Clean up a pain. Smell objectionable. And lingering.
Not doing that again. Next steam distil will be orange peel or something else that smells good.
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Keras
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| Quote: Originally posted by j_sum1 | I have done very few steam distillations and decided today was the day.
Steam distillation of dried thyme.
Leaves swelled. Boiling bumped. 500ml flask overfilled. Leaves through everything jamming every crevice of the glassware. Yield low and stopped early.
Clean up a pain. Smell objectionable. And lingering.
Not doing that again. Next steam distil will be orange peel or something else that smells good. |
Next time, buy a Soxhlet extractor. I assure you this is a breeze to use to get nice essential oils. 
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j_sum1
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I have a soxhlet. But is it really suited to steal distillations? I don't see how that would work.
Fact remains that the odour was unenjoyable. And not in a chlorine or ammonia ir other inorganic kind of way.
Something different next time. And don't overfill the flask.
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Texium
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Soxhlet extraction is fun to watch, but it extracts lots of non-volatile compounds that you probably don’t want (chlorophyll, other pigments,
resins, etc). Not sure what essential oils you’re talking about, Keras, but steam distillation should actually yield a cleaner result.
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j_sum1
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Time to rip the top off an old bottle and play with some hexagons.
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Texium
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Thread Topped
11-4-2023 at 08:43 |
Texium
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| Quote: Originally posted by Texium | | Soxhlet extraction is fun to watch, but it extracts lots of non-volatile compounds that you probably don’t want (chlorophyll, other pigments,
resins, etc). Not sure what essential oils you’re talking about, Keras, but steam distillation should actually yield a cleaner result.
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I just posted a more elaborate explanation of this here: https://www.sciencemadness.org/whisper/viewthread.php?tid=15...
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DraconicAcid
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Getting crystals of my neodymium sulphate. Nice pink solutions from hot aqueous solution. From the yellow, cold solution (from coordination of
sulphate, according to woelen) I tried doing vapour diffusion of methanol into the solution. It turned colourless, with very little crystals forming.
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
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Rainwater
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My lye cell anodes finally went out on me. 12 months - 3 days. Whoooo
4 Pt on Ti mesh anodes. Ti mesh cathodes
I want to get it back up and running so i stripped the cell, replaced the tubing, membranes and now am watching the most stubborn 0.1g piece of
platinum, crawl its way into solution.
Figure ill percipitate it with some vitamin c and torch it back onto the titanium mesh until i get enough to electroplate. Friend from down under says
he's got some to send my way
"You can't do that" - challenge accepted
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