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Author: Subject: Everyday Chemistry
mayko
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[*] posted on 19-6-2018 at 13:04
Everyday Chemistry


restarting this thread; hopefully it will be merged when the One, True Thread reappears.

I tried my first vacuum distillation the other day, to clean up some phenol from destructive decomposition of salicylic acid. It was a dark pink, looking like a manganese salt, but definitely smelling like phenol. (I can't tell if the cherry undertones are real, or if it's just an associative memory linked to chloraseptic throat spray).

The distillation was a mixed success. The glassware didn't implode, but I couldn't keep the stillhead warm enough to keep the solid from depositing there... the vapors didn't make it as far as the warm-water condenser :( on the other hand, what I manually scraped out was much cleaner in appearance.

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

[Edited on 4-11-2023 by Texium]




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mayko
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[*] posted on 28-6-2018 at 09:33


Got a bunch of scrap iron sitting in a bucket of muriatic acid, on its way to Fe2O3



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DraconicAcid
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[*] posted on 28-6-2018 at 10:19


I tested some labs for the organic course. You would think a simple acid-base separation of cinnamic acid from benzophenone would be trivial, right? Sodium cinnamate is pretty insoluble in water, and benzophenone has too low of a melting point to crystallize. Bah.



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Sigmatropic
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[*] posted on 28-6-2018 at 11:15


Oxidized an alcohol to the carboxylic acid but couldn't fully get rid of the sideproducts. I'm feeling rather down with all these byproducts in the system.
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[*] posted on 28-6-2018 at 12:35


Still ain't worked up the Benzyl Acetate I made; waiting on a new see funnel. They have a short life span at my house. First post from my mobile!




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[*] posted on 28-6-2018 at 12:49


I made some concentrated aqueous ammonia and KNO3 a few days ago. I also made some 13% NaClO from Ca(ClO)2. I also bought some drain cleaner sulfuric acid called Cleamen 420 which is a colorless, odorless, transparent, viscous liquid and measured its density as 1.835 g/cm^3.

[Edited on 28-6-2018 by CobaltChloride]
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[*] posted on 28-6-2018 at 13:28


Quote: Originally posted by mayko  
restarting this thread; hopefully it will be merged when the One, True Thread reappears.

.


So what happened to the original thread mods, anybody ?




Borosilicate glass:
Good temperature resistance and good thermal shock resistance but finite.
For normal, standard service typically 200-230°C, for short-term (minutes) service max 400°C
Maximum thermal shock resistance is 160°C
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roXefeller
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[*] posted on 28-6-2018 at 17:45


Quote: Originally posted by mayko  
Got a bunch of scrap iron sitting in a bucket of muriatic acid, on its way to Fe2O3


I need to get some of that going. Looking for a handy way to light a tenaciously wet barrel fire, in style. Got the aluminum, but I don't think I ever bought iron oxide.
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JJay
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[*] posted on 29-6-2018 at 23:00


I cleaned and organized glassware. I also organized some of the chemicals.



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[*] posted on 5-7-2018 at 13:50


I started a stripping run of a gallon of Klean Strip Premium. I ended up going through an entire sack of ice so I stopped after about two liters. The can still smells like DCM, so I'll try to finish it ths weekend.



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DraconicAcid
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[*] posted on 5-7-2018 at 20:01


Tested different versions of the piperine extraction from black pepper lab.



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[*] posted on 5-7-2018 at 20:54


Tested bromine in silica to see if it will absorb

Studied about internal oxidtion on such as light sensitive potassium ferrioxalate and ammonium permanganate

[Edited on 6-7-2018 by symboom]

[Edited on 6-7-2018 by symboom]




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[*] posted on 6-7-2018 at 10:47


Quote: Originally posted by JJay  
I started a stripping run of a gallon of Klean Strip Premium. I ended up going through an entire sack of ice so I stopped after about two liters. The can still smells like DCM, so I'll try to finish it ths weekend.


I had success distilling DCM just with cold tap water, 30 cm Liebig condenser @ 400ml/h




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[*] posted on 6-7-2018 at 11:30


Quote: Originally posted by TheMrbunGee  
Quote: Originally posted by JJay  
I started a stripping run of a gallon of Klean Strip Premium. I ended up going through an entire sack of ice so I stopped after about two liters. The can still smells like DCM, so I'll try to finish it ths weekend.


I had success distilling DCM just with cold tap water, 30 cm Liebig condenser @ 400ml/h


I did it with that exact setup when I was first starting out, but I don't think it's as efficient as using ice water with a 30 cm Dimroth, and I had horrible nosebleeds the next day after trying it with a Liebig. Also, I didn't have a convenient tap the other day.




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[*] posted on 7-7-2018 at 00:36


Quote: Originally posted by JJay  
Quote: Originally posted by TheMrbunGee  
Quote: Originally posted by JJay  
I started a stripping run of a gallon of Klean Strip Premium. I ended up going through an entire sack of ice so I stopped after about two liters. The can still smells like DCM, so I'll try to finish it ths weekend.


I had success distilling DCM just with cold tap water, 30 cm Liebig condenser @ 400ml/h


I did it with that exact setup when I was first starting out, but I don't think it's as efficient as using ice water with a 30 cm Dimroth, and I had horrible nosebleeds the next day after trying it with a Liebig. Also, I didn't have a convenient tap the other day.


It could be faster, but I had a closed system (not counting vacuum nozzle, and no vapor came out of it.




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[*] posted on 13-7-2018 at 12:30


A few weeks ago I went rockhounding at an old zinc mine and picked up some glossy black rocks which I thought were sphalerite, hoping to isolate zinc from them. Yesterday, I began to crush the rocks up with a hammer and the powder was red which I thought was strange, but I do not know a lot about minerals so I figured it was nothing and kept going. It was not until I noticed rock fragments sticking to a nearby magnet that I realized the mineral was hematite, not sphalerite. A little disappointed, I cleaned up the hematite and instead made a small dot of copper metal by the carbothermal reduction of basic copper carbonate recovered from the inside of some old copper pipes. I have some malachite and azurite fragments from the same mine and once I get my technique down I want to try and smelt them.

[Edited on 13-7-2018 by Plunkett]
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[*] posted on 13-7-2018 at 12:50


Rock is always useful. I mean you are not searching for anything in rock. Whole rock is something. All elements we need. Like H, He, Li, Be, B, C, N, O, F, N, O, F, Ne...whole periodic table. That's what changed my perception about life. I noticed everything is elements. It would be stupid to just try to extract one element and throw processed rock away. When doing something, do it completely. Do not steal minerals from Mother Nature, she will punish you.

Or this whole post in one sentence: TAKE IT OR LEAVE IT.

[Edited on 13-7-2018 by AlexC]
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[*] posted on 13-7-2018 at 14:21


I tried to convince my dean to look for funding for a benchtop NMR spectrometer.



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[*] posted on 13-7-2018 at 17:55


Back in the lab after a bit of absence. Preoccupied with -- well, life stuff.

Huge pile of dirty stuff to clean up from last time all of which had accumulated a decent layer of dust.
I managed to break a beaker and the stem of a take-off adapter. My most common cause of breakages is me cleaning stuff.
I installed a screen in the lab (spare TV) and attached it via HDMI socket to the computer in the office next door. Already it is more useful than I imagined it would be. So nice to be able to look up stuff while working in the lab.

I am half-way through purifying some dioxane I made last night. I managed to get the tarry mess at the end of the synth to boil over and flood the condenser. Twice. But now it is fractionally distilling nicely and it looks like I will have a good product.
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[*] posted on 4-8-2018 at 17:29


I put 100 grams of technical barium carbonate into a 5L beaker and added 1000 mL of 5% cleaning vinegar. Phew! It stinks! After it finishes reacting, I am going to filter, add sodium hydroxide, evaporate off some of the water at low heat, chill, then recrystallize the precipitate and dry it in my desiccator. I'm going to have to read up on suitable desiccants... removing the last water of hydration is very hard, but I'd like to get the product as dry as practical.



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[*] posted on 4-8-2018 at 18:04


I want to ask you guys how do you have time for such a number of experiments in conjunction with life? I have a wife and two kids. They demand most of the time I have outside of work.

How do you guys do it? I used to have a lot of time to myself for stuff like this. It's really got me down lately.




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[*] posted on 4-8-2018 at 18:12


Hang in there, Lotptr. I am in the same position. Basically, I am finding that I need to schedule in some lab time in a chunk and go hard when I get the chance. And accept the fact that it doesn't happen as regularly as I would like.

I got into the lab the other night for a continuation of dioxane synthesis and found that it had been three weeks since my last visit. Distillation took longer than I anticipated and I ended up going to bed at 2:00 am

I can see that in a couple of months work things might be a bit more settled and I might be able to do more. But then again, it is probable that other priorities will sneak in and it will be just as difficult. Ultimately I have to recognise that a bit of me-in-the-lab time is important enough for me to have to schedule it. And I have to accept that much of the time I will have to get my fix by dropping in here and reading.
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[*] posted on 4-8-2018 at 18:33


Quote: Originally posted by j_sum1  
Hang in there, Lotptr. I am in the same position. Basically, I am finding that I need to schedule in some lab time in a chunk and go hard when I get the chance. And accept the fact that it doesn't happen as regularly as I would like.

I got into the lab the other night for a continuation of dioxane synthesis and found that it had been three weeks since my last visit. Distillation took longer than I anticipated and I ended up going to bed at 2:00 am

I can see that in a couple of months work things might be a bit more settled and I might be able to do more. But then again, it is probable that other priorities will sneak in and it will be just as difficult. Ultimately I have to recognise that a bit of me-in-the-lab time is important enough for me to have to schedule it. And I have to accept that much of the time I will have to get my fix by dropping in here and reading.


See that is me right there! Thanks for that j_sum1. I appreciate the advice.




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[*] posted on 5-8-2018 at 00:02


I usually try to run multiple low-maintenance experiments simultaneously while I do other things. I'm planning on using the barium hydroxide to purify the product from a couple of experimental glyoxylic acid synths, but I'll also put some in a bottle so that I have some ready to go next time I want some (it's pretty useful).

Technical grade barium carbonate is almost as cheap as dirt, but it is very impure. I think it's possible to prepare rather pure barium compounds from it, though, if the right steps are taken.





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[*] posted on 5-8-2018 at 10:47


I just finished purifying some phenolphthalein that I made about a week ago. I used phthalic anhydride that I prepared from phthalic acid from hydrolysis of phthalate esters extracted from scrap vinyl, and phenol that I prepared from aspirin from the dollar store. A lot of work but rewarding.

Now I have to prepare some standardized solutions (sodium carbonate, HCl, NaOH, ethanolic KOH)... It is hot in the lab though, so keeping everything 20°C is a chore that I am not looking forward to. Does anybody else feel like any time one task is completed, another 10 get added to the to-do list?
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