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Author: Subject: Everyday Chemistry
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[*] posted on 23-11-2022 at 08:40


Quote: Originally posted by Piroz  
I used my furnance to preparation calcium oxide from old, carbonated slaked lime. I need CaO for preaparation both ammonia and calcium nitrate.

https://youtu.be/d6vDtND4HSU


if you reduce it to dust?? no more sprinkled around???
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[*] posted on 14-12-2022 at 16:15


Reacting some of my samarium with sulphuric acid. Yellow.



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[*] posted on 14-12-2022 at 16:41


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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[*] posted on 15-12-2022 at 08:30


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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[*] posted on 21-12-2022 at 12:10


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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[*] posted on 21-12-2022 at 12:39


Going to work up my samarium(III) sulphate.

SmIIISulphate.jpg - 49kB




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[*] posted on 31-12-2022 at 17:09


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




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[*] posted on 5-1-2023 at 12:15


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]




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[*] posted on 31-3-2023 at 20:25
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.

    Everyday chromium.jpg - 2.7MB

    [Edited on 1-4-2023 by j_sum1]
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    [*] posted on 31-3-2023 at 23:58


    @ 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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    [*] posted on 1-4-2023 at 03:49


    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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    [*] posted on 1-4-2023 at 12:53


    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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    [*] posted on 1-4-2023 at 14:25


    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.



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    [*] posted on 1-4-2023 at 14:55


    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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    [*] posted on 2-4-2023 at 03:46


    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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    [*] posted on 2-4-2023 at 07:10


    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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    [*] posted on 2-4-2023 at 07:52


    Yeah for that reaction you shouldn’t have to worry about excess methanol being an issue. Nice.



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    [*] posted on 7-4-2023 at 23:54


    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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    [*] posted on 8-4-2023 at 00:36


    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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    [*] posted on 8-4-2023 at 02:07


    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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    [*] posted on 8-4-2023 at 08:18


    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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    [*] posted on 10-4-2023 at 15:15


    Time to rip the top off an old bottle and play with some hexagons.


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    11-4-2023 at 08:43
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    [*] posted on 11-4-2023 at 08:46


    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.
    I just posted a more elaborate explanation of this here: https://www.sciencemadness.org/whisper/viewthread.php?tid=15...



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    [*] posted on 11-4-2023 at 13:34


    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.



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    [*] posted on 3-5-2023 at 06:26


    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




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