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Author: Subject: Everyday Chemistry (provisional)
JJay
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[*] posted on 5-8-2018 at 22:25


Here's the barium acetate solution that was left behind after gravity filtering. It has a slight sulfurous odor, and it is obviously impure. I'm not exactly sure what the brown color is... I believe that iron (iii) acetate is rather insoluble. There were iron filings in the barium carbonate; they stuck to the stirbar.

My plan is to add some sodium hydroxide solution, which should precipitate barium hydroxide octahydrate. Heating to boiling and doing a hot filtration will hopefully get rid of any carbonates. I'll probably recrystallize the product a few times for purity then dry it to the monohydrate in a warm oven (easier than using a desiccator).

IMG_20180805_220721.jpg - 153kB

I have some disgusting and toxic barium waste sludge that I have to dispose of. I'm pretty sure I should not put it down the drain. Right now it is just sitting in a container while I figure out what to do with it.




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[*] posted on 8-8-2018 at 04:37


Today I prepared ethyl benzoate from benzoic acid, dry ethanol and sulfuric acid on 0.5 molar scale. For some reason the reaction boiled out of control, flooded the condenser and made a wintergreen-smelling volcano inside my lab. Of course this happened when I left the reaction unmonitored for a few minutes. Only a small portion of the reaction mixture was lost though, and I ended up with 58 % of ester of density 1.04 g/ml, which is fine considering the starting materials are cheap.

This will be used to make triphenylmethanol by reaction with phenylmagnesium bromide.
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JJay
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[*] posted on 9-8-2018 at 02:45


I made some nitric acid from hardware store chemicals. I haven't titrated it yet, but I'm guessing it is about 50% concentration.

nitric.jpg - 112kB

When doing the distillation, I ran a PVC hose from the takeoff outside, and it's a good thing I did - when the potassium bisulfate started to crystallize, it almost all crystallized at once, giving off a lot of heat and overwhelming the condenser, sending boiling hot nitric acid vapors through the hose. I'd never done a nitric acid distillation on this scale before, but I suspected that might happen, so I was prepared.

I didn't get a chance to finish my barium hydroxide because the nitric acid distillation took too much of my attention, but hopefully, I'll get to that tomorrow.





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[*] posted on 9-8-2018 at 03:10


Does anyone know what happened to the old thread? I found a link to it but apparently it "doens't exist".

Anyway, today I made some 2,3-dimethoxybenzaldehyde from ortho-vanillin and methyl iodide, with potassium carbonate in acetone. Then I condensed the product with 2-cyanoacetamide to give 2-(2,3-dimethoxybenzylidene)-2-cyanoacetamide as nice white needles.

Interestingly the product has strong blue fluorescence under long wave UV light. With the 3,4-dimethoxy pattern, the fluorescence in turqoise instead. And with the 4-dimethylamino pattern, the fluorescence in bright orange. I'll probably make a thread at some point with more details.



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[*] posted on 9-8-2018 at 21:24


About 2 months ago somebody had a topic about disappearing threads and falling post counts... Shortly after that the Everyday Science thread disappeared, along with a handful or more other threads. It was probably missed quickly because of its sticky status.

In the OP, no one seemed to know what was going on, but it wasn't exactly the mod lounge. I remember JJay or jsum_1, streety or symboom, aga, maybe coppercone were all there. I can't find it anymore, maybe deleted because I found a duplicate thread from 2015. Pretty sure its simply something to deal with until the forum software is upgraded.

I'm moving into a new lab space! so I'm not exactly working every day on chemistry. Or any day for now. :(
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JJay
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[*] posted on 10-8-2018 at 01:16


I don't know what happened to it, and I'm not going to speculate. I had probably at least 50-100 posts on that thread.

I did not do any chemistry today because my Internet was down for much of the day, and I didn't have the necessary references. But I will be back at it in full force tomorrow.




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[*] posted on 10-8-2018 at 11:55


Quote: Originally posted by j_sum1  


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.


That is some tarry ass stuff too, but amazingly comes out of the glass easy. Finally bought a small (100ml) boiling flask for the pursuit of my esters.

Medical hassles keep me out of the lab, kids are grown! (In hospital right now, just had surgery. Again *sigh*)





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JJay
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[*] posted on 19-8-2018 at 21:14


I made a nice little batch of chloroform with the last of my bleaching powder in three runs. I don't recommend doing this unless you have a surplus of bleaching powder, but you can add 100 mL of acetone to 300 grams of standard pool grade calcium hypochlorite and 1.5L water in a 3L flask in an ice bath with mechanical stirring with a reflux condenser (add acetone slowly or the mixture might boil and foam excessively, filling the condenser with suds. if that happens, dump ice water through the condenser to avoid making a big mess). Once the reaction stops, you can distill off the chloroform on a water bath. It is possible to do the reaction without mechanical stirring by shaking the flask and cooling it repeatedly until shaking doesn't make it warm up, but that is an enormous pain.

The crude product (which is what I have here) will be wet and probably contaminated with acetone. I'm going to wash mine with concentrated sodium bisulfite solution, dry it over potassium carbonate, distill it, stabilize it with 1% ethanol, and store it with the rest of the lab chloroform.

chloroform.jpg - 90kB

Now that I've used up the last of my calcium hypochlorite, I think I'm going to stick with making chloroform with chilled liquid bleach. It's much less work that way.



[Edited on 20-8-2018 by JJay]




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[*] posted on 30-8-2018 at 00:36


Earlier I set up a hot filtration apparatus and did a dry run (I've never actually done a hot filtration before). Right now I'm boiling down some crude barium hydroxide solution. It likely contains a little less than a mole of barium hydroxide, so I'm going to try to get the volume down to about 200 mL then filter and refrigerate. I'm hoping for white crystals. I have a bucket filled with dilute sulfuric acid that contains the waste and the paper towels used to do the cleanup.

Oh and I'm also running a fractional distillation and slowly evaporating a solution on a steam bath.

distillation.jpg - 101kB

[Edited on 31-8-2018 by JJay]




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[*] posted on 31-8-2018 at 02:46


I made 400 grams of 60 % nitric acid by distillation from sodium nitrate and sulfuric acid. I tried to increase the strength of the acid to reach around 65-70 %, but this seems impossible without a fractionating column.
The product will probably be used to make some o- and p-nitrotoluene.

I'm also purifying cinnamaldehyde from cinnamon bark oil using sodium metabisulfite. The goal is to form the bisulfite adduct, remove the rest of the organics by filtration and the deprotect the cinnamaldehyde using a base. I wish I had an overhead stirrer because the bisulfite adduct forms a thick slurry that is difficult to stir.

I'll post a thread when I'm done.

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[*] posted on 31-8-2018 at 19:21


I did a hot filtration of crude barium hydroxide solution and then washed the filter cake and beaker with about 100 mL of boiling water. Unfortunately, a small amount of silty material (likely barium carbonate) made it through the filter paper and cotton ball. Right now the solution is cooling. I'm hoping that the silty material will go through the filter paper just as easily when I filter off the barium hydroxide, but I imagine I'll have to recrystallize.





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[*] posted on 18-9-2018 at 18:15


Turned some manganese sulfate into manganese carbonate



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JJay
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[*] posted on 19-9-2018 at 05:39


Getting ready to run some distillations....

distillations.jpg - 109kB




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[*] posted on 20-9-2018 at 19:02


Quote: Originally posted by mayko  
Turned some manganese sulfate into manganese carbonate


I made a slurry in water and added HCl and it's a chloride now.

one cool thing is that after additions of HCl, when the effervescence died down, there was a clear stratification of the translucent acidified layer and the murky lower layer still containing suspended carbonate. There seemed to be points of reaction between the two, visible as a spot of bubbling on the dark surface. They seemed to have some interesting dynamics: some of these upwelling spots persisted for a while, some extinguished quickly, and some grew into a large foaming for a moment




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[*] posted on 23-9-2018 at 15:42


I've been converting oxalic acid to formic acid all weekend. It's a cute little reaction cycle catalyzed by glycerine, in which a glyceryl oxalate ester is formed, the ester is decarboxylated to a glyceryl formate ester, and the ester is hydrolyzed and the formic acid distilled off. Several literature sources call for thorough drying of the glycerine beforehand, but it's not obvious why, and NurdRage didn't make any special mention:

https://erowid.org/archive/rhodium/chemistry/formic.acid.htm...
https://www.youtube.com/watch?v=ceL-I0azPH8 (with a guest appearance from Gary the Bug)

Anyway, I'm coming up on ~100 mL of distinctly anty-smelling crude product




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[*] posted on 23-9-2018 at 15:53


I've been thinking about doing that too. I have to wonder if there isn't an easier way, though... something like hydrogen peroxide and methanol....

Oh and I've been purifying solvents all weekend. I finally managed to clean my sep funnel by putting some abrasive cleaner and a handful of coins into it and swirling it around. There was a waxy coating clinging to the walls, and now the funnel has that sparkling new glassware look to it.

[Edited on 23-9-2018 by JJay]




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[*] posted on 23-9-2018 at 20:21


Currently dissolving a neodymium magnet in sulfuric acid. Also made a few mL of crude methyl salicylate. Also mixed 50 mL of a lacquer thinner with 50 mL of water to determine the toluene/DCM concentration. Will start separating the components of the thinner next week when I have time, as toluene is unfortunately not sold as a pure product anymore where I live.



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[*] posted on 24-9-2018 at 12:42


Quote: Originally posted by JJay  

Oh and I've been purifying solvents all weekend.


That's what i'm doing now - I had 20L of various waste solvents, most of which mixtures of methanol/water eluent waste from my HPLC.
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[*] posted on 24-9-2018 at 17:39


Screwed up and made a pretty hefty amount of bismuth oxynitrate. Went and hydrolyzed my bismuth (III) nitrate I'd made by dissolving metallic bismuth in nitric acid.

Damn. Would dissolving it in concentrated HNO3 push the equilibrium back the other way and allow me to recover the nitrate?

Edit: I believe my new strategy could be to dissolve it in weak nitric acid solution, and neutralize with sodium carbonate to get bismuth (iii) oxide, followed by digestion in HCl and reduction with aluminum to yield metallic powdered bismuth, filtered, added to conc. nitric acid, and evaporated. Phew! That's one heck of a round-trip if I can't just add it back to conc. nitric acid....

[Edited on 25-9-2018 by weilawei]
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[*] posted on 25-9-2018 at 08:40


Anyone on here ever thought about making some Xylyl Bromide? Found some Sodium Bromide solution at the store the other day, when I ran Chlorine through it I got some nice dark droplets of Bromine. I destroyed that sample obviously but am considering making some Xylyl Bromide by just mixing Xylene/ Bromine in reflux and irradiating (patent says a lamp should be sufficient).

I know that there will be a couple brain cells lost in the experiment but it seems like a pretty interesting chemical overall. I've made and tested a couple other similar chemicals before and had a lot of fun, like chloropicrin or iodoacetone.



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[*] posted on 29-9-2018 at 17:29


I removed a couple of centimeters from my 20 cm thermometer tube so that it will fit into a 3 L flask. I am not very experienced at glassblowing, but I managed to get the end to seal without doing too bad of a hack job.

I also constructed a large gravity filtration apparatus by drilling numerous small holes into the bottom of a 3.75 L ice cream bucket. The bottom of the pail is exactly the same size as a coffee filter. It works pretty well except the bucket is a little too flexible to hang without the sides caving in and reducing capacity. I'm going to try it with a more rigid pail.




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[*] posted on 30-9-2018 at 12:36


Just distilled out DCM and toluene out of a refinisher. Will do a fractional distillation when I have time to separatye the two.



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[*] posted on 1-10-2018 at 00:11


Quote: Originally posted by JJay  
I also constructed a large gravity filtration apparatus by drilling numerous small holes into the bottom of a 3.75 L ice cream bucket. The bottom of the pail is exactly the same size as a coffee filter. It works pretty well except the bucket is a little too flexible to hang without the sides caving in and reducing capacity. I'm going to try it with a more rigid pail.


For my diy heating mantle I bought some glass fibre cloth
https://www.ebay.co.uk/itm/0-03mm-Ultra-Thin-Fiber-Glass-Fab...
It is very fine mesh, it has unbroken threads / no loose bits, it is surprisingly strong, and resistant to heat, acids etc.
I think that it may make an excellent filter material,
with or without mechanical support.

It also looks suitable as a simple mechanical membrane for an electrochemical cell.
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[*] posted on 1-10-2018 at 00:15


It worked OK, but it still takes forever to filter calcium salts.

I was thinking about doing that with some ceramic paper, but it's a little on the expensive side to use for filters... interesting idea, though.




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[*] posted on 1-10-2018 at 09:24


I put some more solvents in bottles. I probably ought to recycle my waste toluene.... At some point today, I plan to recrystallize some sodium carbonate.



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