Sciencemadness Discussion Board - Everyday Chemistry

Everyday Chemistry

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pneumatician - 23-11-2022 at 08:40

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???

DraconicAcid - 14-12-2022 at 16:15

Reacting some of my samarium with sulphuric acid. Yellow.

B(a)P - 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!

Sir_Gawain - 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.

solitanze - 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.

DraconicAcid - 21-12-2022 at 12:39

Going to work up my samarium(III) sulphate.

Rainwater - 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

DraconicAcid - 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]

Potassium dichromate

j_sum1 - 31-3-2023 at 20:25

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]

Admagistr - 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]

j_sum1 - 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.

Admagistr - 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]

DraconicAcid - 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.

Admagistr - 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...

Bedlasky - 2-4-2023 at 03:46

Quote: Originally posted by DraconicAcid

Try to make saturated solution and let it evaporate.

Lionel Spanner - 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.)

Texium - 2-4-2023 at 07:52

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

j_sum1 - 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.

Keras - 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.

j_sum1 - 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.

Texium - 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.

j_sum1 - 10-4-2023 at 15:15

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

Texium - 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...

DraconicAcid - 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.

Rainwater - 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

arkoma - 3-5-2023 at 18:12

https://photos.app.goo.gl/16SA1f7RDucAvtGh6

hey, it`s pretty.

mayko - 7-5-2023 at 19:15

I have some of the green carbonate complex of cobalt III drying on filter paper, it's a wild color to see from cobalt

mayko - 15-6-2023 at 18:31

Quote:

Edit by Texium: Changed title because the "one true thread" will likely never reappear, unfortunately.

[Edited on 4-11-2023 by Texium]

THAT'S NOT TRUE!! tHAT'S IMPOSSIBLE!!!

anyway

There's a season of Trailer Park Boys which opens with Ricky collecting garbage from the park and trying to sell it back to the community. He offers some beer cans to his quasigirlfiend Lucy, saying that they would look great decorating the kitchen. "No, that's cool, thanks, if I need any I'll come get one," she says.

I mention this because I visited a weirdo friend of mine recently. With students out of the dorms, the dumpsters have been rich pickin's, and he proudly showed me his haul. I expected something like kitchen items, books, a television, but no: he had an impressive pile of aluminum cans. He explained to me that an even weirder friend of his used them as disposable pipes to smoke drugs off of before work, and thought he could use a few.

Okay, I said, but they've got paint and plastic on them, do you really want to encourage him breathing those fumes? Can't you just show him how to use a carrot or an apple?

He insisted that there was no plastic coating on soda cans. I long ago learned that he doesn't regard any of the internet as a legitimate source, believing that it has been irreparably corrupted by Vladimir Putin himself. It was show-me-not-tell-me time.

I scrubbed the outer layer of paint off of the lower half of a can of Diet Coke and suspended it from the tab in a beaker. Then I poured a moderate sodium hydroxide solution around it, and left it to fizz overnight.

The next morning, I had a half aluminum can, half plastic bag, still containing the Coke.

When I showed it to my friend, I definitely convinced him of something. I'm not sure of what, precisely, but he clearly felt like he had been lied to his whole life, about the nature of soda cans. He wants me to go on Christiane Amanpour and alert the general public.

And that's my adventure in the intersection of mad science, harm reduction, and the Trailer Park Boys IRL.

fusso - 15-6-2023 at 19:26

Quote:

Edit by Texium: Changed title because the "one true thread" will likely never reappear, unfortunately.

[Edited on 4-11-2023 by Texium]

Can you explain?

j_sum1 - 15-6-2023 at 19:40

Quote: Originally posted by fusso

Can you explain?

The original thread was lost to the aether in some kind of tech glitch.
It is probably retrievable in one of the site backups, but practically, the information it contained is lost.

arkoma - 15-6-2023 at 20:47

day before yesterday, i massacred four innocent 1964 US 25 cent pieces in hot nitric acid. after two recrystallizations, i`ve got most of the blue from the copper out of my AgNO₃, and a bunch of black stains on my fingers. phone broke at the moment so no pics

mayko - 10-8-2023 at 06:35

I got my hands on some iodates/periodates and have been running through some of the experiments on woelen's site.

One thing I found was that the sulfur/periodate mixture is slightly shock sensitive; when wrapped in aluminum foil and tapped with a hammer there was a distinct smell of sulfur dioxide, small points of purple-brown discoloration on the foil appeared, and there were even a few sparks. When I really went Hephaestus on it, I was eventually able to get a hearty snap. The reaction didn't seem to propagate much; there was plenty of the mixture left to burn afterwards.

DraconicAcid - 10-8-2023 at 08:28

I've been trying to get the silver oxide oxidation of vanillin to work for ethylvanillin, salicaldehyde, and other related aldehydes, with limited success. Some of these acids really don't like to recrystallize.

Always lable beakers

Rainwater - 16-8-2023 at 15:21

Doing some cleanup and the permanent marker lableing a wash beaker had wiped off. No biggie, I put the 3 times refined silver nitrate in the cupboard last night and this was only rinse water. Ill just add my current rinse to it(cu+/hcl/k+/h2o2) and neturalize the whole lot later.
Son of a ;>/"& mother ahhhhhhh.
I run to my shelf, pull out my jar from last night, and discover its lable had also wiped off.

mayko - 15-9-2023 at 20:13

I'd never done a vacuum distillation before so I tried cleaning up a small amount of benzaldehyde that was languishing in the organics bin, turning orange and growing crystals. Everything went better than expected! Nice clear and colorless liquid, with ~65% mass recovery from starting material I'm pretty sure is at least 15% benzoic acid. The only problem was that it took a while for the vapor front to make its way through the claisen adapter, and some moisture condensed in the receiving flask.... the last I fixed by putting it in the freezer and pipetting off the ice lumps once everything was frosty :cool:

Sir_Gawain - 26-11-2023 at 17:38

Dioxane, first time.

Oh, the joy.

Phosphorous pentoxide + water = massively exothermic

Sulaiman - 27-11-2023 at 12:25

Disposing of some P₄O₁₀
I slowly added it to running tap water to flush it away as dilute phosphoric acid,
which I believe is OK for the local waste water treatment plant.
I was surprised by how exothermic the reaction is
(more than conc. sulphuric acid or NaOH or KOH)
So much more dangerous than I'd expected,
based only on previous use in a diy dessicator.

DraconicAcid - 27-11-2023 at 21:22

I had my students try a new lab today- bromination of stilbene. It worked well, although it's tough to recrystallize the product (its solubility doesn't change much with temperature, it seems).

Previous years had made 1,3-diphenylpropenone and a methoxyphenyl analgoue, so I figured, why not brominate these? The first one worked well, but the second just gave oily crap. No idea why. Oh, well.

DraconicAcid - 21-12-2023 at 14:02

I've got a paper here (https://tesla.pmf.ni.ac.rs/lgc/articles/40-1992.pdf ) that discusses the synthesis and thermal decomposition of Cu(urea)4Cl2, made by reacting copper(II) chloride with urea in a 1:2 ratio. Elemental analysis said it was 16.9% copper, consistent with the 1:4 adduct.

I reacted copper(II) chloride with urea in a 1:4 ratio under very similar conditions. My product is 24.6% copper, consistent with Cu(urea)2Cl2.

Grrrrr.......

[Edited on 22-12-2023 by DraconicAcid]

beta4 - 1-2-2024 at 14:42

Today after a long time I go back to the lab for making a printed circuit board. Lately I've been busy with other stuff and I'm almost not doing chemistry anymore, but printed circuits are one of the applied chemistry that I still do from time to time, the other being analog photography.

However this time I found my photoresist developer, a sodium hydroxide and metasilicate solution, had crystallized. Likely due to the low temperatures in the lab.

So I'm sitting here, watching crystals slowly dissolve and remembering when I was dreaming of doing complex reactions that I never got around to trying, or failed.

Oh, well, I still have the lab, reagents and apparatus, so maybe someday I'll get back...

beta4 - 3-2-2024 at 02:26

The resulting printed circuit

charley1957 - 3-2-2024 at 07:43

Good looking board, traces nice and sharp, crisp edges, good solder mask. I like it! Is that some kind of oscillator?

beta4 - 3-2-2024 at 15:17

It is an oscillator. More precisely, a Baxandall oscillator [1]. I'm using it to produce a high voltage sine wave to drive the neon tubes I'm making (I've been learning the very basics of glassblowing). Here's the printed circuit with all components soldered and working

[1] Baxandall, P.J. "Transistor sine-wave LC oscillators: Some general considerations and new developments"
https://web.archive.org/web/20211222202712/http://www.sophia...

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