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Texium (zts16)
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[*] posted on 19-1-2016 at 21:22


Quote: Originally posted by JJay  
Quote: Originally posted by Detonationology  
Quote: Originally posted by JJay  
Today I tested out my new water pump in a distillation setup with a five gallon bucket. It works well, but the water in the bucket does heat up.

I recommend a styro cooler


LoL
Normally I just use a little 2 gallon bucket for condenser water, but I fill it mostly with ice when I start, and occasionally drain off water and add more ice throughout the distillation. I actually re-freeze most of the water I use afterwards anyway, so very little water is wasted. This is good for me since my house runs on rainwater and there are sometimes months with practically no rain.

Unfortunately school suddenly appeared again and I haven't had much time for chemistry. I did steam distill d-limonene from clementine peels last weekend though. I haven't yet worked it up, but I can see there's a visible amount of oil, so that's a relief.




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[*] posted on 19-1-2016 at 23:17


I've had issues using ice in my condenser water supply bucket, I found that the ice water passing through the condenser would cool the still head and cause no product to come over, everything would just reflux back into the boiling flask, the first time this happen I didn't realise and kept increasing the temperature and made a real mess of things, now I wait until I have product coming over and the condenser water temp starts to warm before I add the ice
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[*] posted on 20-1-2016 at 04:08


Quote: Originally posted by NedsHead  
I've had issues using ice in my condenser water supply bucket, I found that the ice water passing through the condenser would cool the still head and cause no product to come over, everything would just reflux back into the boiling flask, the first time this happen I didn't realise and kept increasing the temperature and made a real mess of things, now I wait until I have product coming over and the condenser water temp starts to warm before I add the ice

That's the first time I've heard of somethig like this happening. Were you distilling something with a high boiling point?
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[*] posted on 20-1-2016 at 04:34


No just nitric acid Oscilllator, it's more of an issue when distilling things with a lower boiling point
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[*] posted on 20-1-2016 at 06:44


Try wrapping your flask and still head in aluminum foil. You'd be amazed at how fast distillate starts coming over as soon as you do.



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[*] posted on 20-1-2016 at 18:24


Made some copper(II) carbonate and lead(II) carbonate on sunday. Also made some 3.5% H2O2 out of the 1.5% stuff by slowly heating it (below 100oC) to drive off the water. Some time I'll have to do a 'run' of something. The only mass-production I've done is of basic Copper(II) carbonate, got 35g in the end. So perhaps some pure HCl, concentrated HOAc, or something else is in order. I've got lots of 30g quantities of things, so I should probably look into the productions I can do with the larger quantities of things I have.



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[*] posted on 21-1-2016 at 16:22


Earlier I made a 1 M sodium carbonate solution and pulverized some TCCA. Right now I am recovering some ethanol and dehydrating some Epsom salts. I think later I might bend some glass to make a test tube distillation apparatus, distill some methanol, dissassemble a lantern battery to get some carbon electrodes and manganese oxide, and do some titrations.
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[*] posted on 22-1-2016 at 08:47
Bariumthiosulphate


Yesterday I prepared some bariumthiosulphate. Starting point was a BaCl2 solution that (unintentionally) contained some bleach (4.5% NaClO) that had been sucked into the solution. To 10ml of this solution I added what I expect to be an excess of Na2S2O3 solution (around 20ml). Seeing the solubility of BaS2O3 (0.2g/100ml@20C), I'd expect a precipitate to form right away, but the solution turned only a bit cloudy. I guess that some sulphur was formed by the action of the hypochlorite on the thiosulphate.
What surprised me, was that no precipitate formed, neither after 15 minutes or so. I decided to heat the tube and when it was around 60C suddenly a bunch of white crystals appeared. I rinsed with water twice and left to dry in a desiccator over calcium chloride (takes time, NaOH is a better desiccant).
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[*] posted on 23-1-2016 at 06:37


Had some wood to burn so I made a little dH2O today


dH2O.jpg - 1MB

the transformer is just as a weight
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[*] posted on 25-1-2016 at 22:47


Today I dehydrated some sodium acetate that I made from vinegar and sodium carbonate.

Oh and a few days ago I titrated some Price First brand vinegar (a Walmart generic) and came to the conclusion that it was 1.01 M.

Tomorrow I am thinking about making some calcium carbonate from sodium carbonate and calcium chloride.
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[*] posted on 26-1-2016 at 07:26


Recently, I was fairly successful in an attempt to make hexachloroethane from tetrachloroethylene using a FeCl3 catalyst. I could probably do better with anhydrous AlCl3 so I am now in the market for some. The yield with FeCl3 was low but I still got about 20g and resublimed it.

https://www.youtube.com/watch?v=yYA43i_DYgc

I am preparing to undertake the thermal decarboxylation of salicylic acid to phenol. I am working on ways to reduce the amount of phenyl salicylate produced. I think I might be able to get a quantitative yield with a new method I have developed. I will find out tonight.

I have also been working more on the muffle furnace but some parts are in the mail from China so I don't think I'll have it operational until early February.

Aside from that, I have found two novel ways to make benzene (neither are documented here!) and I will be attempting at last one of those soon.




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[*] posted on 26-1-2016 at 09:26


Bought a half gallon of "sudsy" ammonia solution from Dollar General, and after a couple false starts managed to get a bubbler rigged out of my drip tip and bubbled NH4 through dilute HCl. I now have some nice ammonium chloride crystals forming.

@prax--don't know WHY took me so long to flash on your youtube channel. Great videos.




Why did i wait so long to by a hotplate stirrer?
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[*] posted on 26-1-2016 at 09:27


I was fortunate enough to be able to rescue two jars of old, wet, oxidized sodium iodide that my school was going to throw away. Since I already have a decent amount of KI (preferable to NaI due to being non hygroscopic), I figured that the best thing to do would be to oxidize all of it to iodine. Three and a half quarts of 3% hydrogen peroxide later, I became the owner of 544 grams of iodine. :D

photo_1453675008252.jpg - 1.5MB

@Praxichys- I look forward to seeing your benzene syntheses, and your method for more efficient phenol synthesis as that's something I'm planning to do soon.




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[*] posted on 26-1-2016 at 09:50


Over the weekend we had a blizzard in the north east US so I continued working on my piperine extraction from black pepper, reclaimed the iodine from a tincture of iodine found in Rite Aid. I also distilled some methanol from "heet" brand fuel line antifreeze.

I also purchased and started studying the old organic chemistry text book I used at Uconn. Got the same exact publication for 5 dollars total, sold it to the book store 8 years ago for 130. I consider that a win lol

Yeah nothing crazy but i am just starting to actually use all the glass i purchased in the past 6 months. I have distilled water and tested the function of all components just never got around to doing chemistry, now that I am I probably wont stop for a while!




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[*] posted on 26-1-2016 at 10:26


:D I liked your video; now to watch the rest of them, but I hope there are less than 1000!
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[*] posted on 26-1-2016 at 13:09


Quote: Originally posted by zts16  
Three and a half quarts of 3% hydrogen peroxide later, I became the owner of 544 grams of iodine.

!!!

Rename immediately to zts48, being 3x luckier than the next man.

Great job.




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[*] posted on 26-1-2016 at 13:37


Quote: Originally posted by szuko03  
just starting to actually use all the glass i purchased

Funny. Today i laid hands on previously unused bits of glass whilst trying to figure out how to chlorinate ethanol.

As this 'hobby' continues, it'll all get used, even the Dean-Stark trap one day (no idea why i ended up with that piece).




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[*] posted on 27-1-2016 at 16:11


Earlier I finished working up some sodium acetate made by reacting simple household products to obtain a near-quantitative yield.

I received my new hood fan in the mail.

Right now I am drying some calcium carbonate that I made earlier from sodium carbonate and calcium chloride.

Later I am thinking about making a high-temperature heating mantle for 25 mm test tubes and possibly doing some small-scale organic oxidations to see if they really work as reported. Also, I'll probably redistill a couple liters of recovered ethanol if I have time.
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[*] posted on 27-1-2016 at 17:19


I just got done putting up the lattice I got from Dr. Bob last night... a tour of my new and improved lab might be on the horizon!



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[*] posted on 28-1-2016 at 08:54


Quote: Originally posted by zts16  
I was fortunate enough to be able to rescue two jars of old, wet, oxidized sodium iodide that my school was going to throw away. Since I already have a decent amount of KI (preferable to NaI due to being non hygroscopic), I figured that the best thing to do would be to oxidize all of it to iodine. Three and a half quarts of 3% hydrogen peroxide later, I became the owner of 544 grams of iodine. :D



@Praxichys- I look forward to seeing your benzene syntheses, and your method for more efficient phenol synthesis as that's something I'm planning to do soon.

That's both awesome and incredibly 'suspicious (not from you, but from most other people :P).




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[*] posted on 28-1-2016 at 10:45


It would be suspicious if I had a half kilo of I2. ;)



Why did i wait so long to by a hotplate stirrer?
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[*] posted on 28-1-2016 at 13:43


Yeah, you were who I had in mind... :P

zts16, is that photo of the I2 or the contaminated NaI? It's a strange color (at least to me). You've got quite the high school...




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[*] posted on 28-1-2016 at 15:10


Quote: Originally posted by The Volatile Chemist  
zts16, is that photo of the I2 or the contaminated NaI? It's a strange color (at least to me). You've got quite the high school...
That is a picture of the final I2 product. And my school is just alright, it's my chemistry teacher who is great. :)

Today during my independent study, I made potassium chlorochromate (based off of ChemPlayer's video) which I will use for selective alcohol to aldehyde oxidations. I also demonstrated to the AP chemistry class how it reacts with sulfuric acid to produce chromyl chloride (under the fume hood, of course!).




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[*] posted on 28-1-2016 at 15:29


Huh, I had no clue it converted to chromyl chloride when acidified. And it definitely sounds like you're on good terms with your teacher. Mine gives me pipettes, and once offered some cobalt(II) chloride to me (as of yet hasn't panned out, and I'm not going to ask; 'tis rude), but definitely wouldn't let me run anything in one of the fume-hoods during study hall :)



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[*] posted on 28-1-2016 at 15:48


Quote: Originally posted by The Volatile Chemist  
Huh, I had no clue it converted to chromyl chloride when acidified. And it definitely sounds like you're on good terms with your teacher. Mine gives me pipettes, and once offered some cobalt(II) chloride to me (as of yet hasn't panned out, and I'm not going to ask; 'tis rude), but definitely wouldn't let me run anything in one of the fume-hoods during study hall :)
Well, it's not just when it's acidified: concentrated sulfuric acid is required, because what's really happening is a disproportionation reaction that produces CrO3 and chromyl chloride. Very cool to see, as the solid turns dark red and orange vapor is evolved.

Also, the independent study that I refer to isn't just a study hall, I actually requested a period for this year which I can use to do stuff in the lab.




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