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JJay
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[*] posted on 20-11-2017 at 03:38


Coffee grinders are super handy, but they overheat too easily IMHO. I burned out a couple before I switched to a blender

It looks like you are making some benzene, which is a lot of fun. You'll be the envy of the entire family around the Thanksgiving turkey with a nice bottle of benzene :D

I just took a nice warm dish of molecular sieves out of the oven.




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[*] posted on 29-11-2017 at 21:53


Finally did a bit of chemistry today even though I probably shouldn't have since I have finals coming up, mainly testing out my new-old Rotovap on some simple stuff. I recrystallized some copper (II) chloride that I made years ago that was getting dusty and used it to pull off the water at about 60 C. Worked great and after about 15 minutes it was dry enough to flake off of the sides of the flask easily with minimal encouragement. After that I used the Rotovap to distill some DCM paint stripper (no vacuum necessary) just to separate it from the goop, did the aqueous workup to remove methanol, and dried it over CaCl2. I have about 300 mL of DCM now, so that's nice. All this took about an hour and a half.

In summary, Rotovaps are awesome. If you're tired of distilling off solvents or standing over a hot plate for hours, I'd highly recommend keeping an eye out for a good deal on one. I know that I'll continue to get a ton of use out of mine in the future.




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WangleSpong5000
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[*] posted on 30-11-2017 at 11:06


Just undertook my first ever distillation! Just a simple distillation of tap water. Boring I know but a logical first choice I think. Went off without a hitch although stupid me had cleaned everthing with a bit of acetone and the recieving flask still had a tiny puddle of unevaporated acetone so yeah... guess I'll just have to re-distill it... :D

That was fun! Now to try something a bit more interesting...
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[*] posted on 30-11-2017 at 15:07


Quote: Originally posted by WangleSpong5000  
Just undertook my first ever distillation! Just a simple distillation of tap water. Boring I know but a logical first choice I think. Went off without a hitch although stupid me had cleaned everthing with a bit of acetone and the recieving flask still had a tiny puddle of unevaporated acetone so yeah... guess I'll just have to re-distill it... :D

That was fun! Now to try something a bit more interesting...
Certainly a better idea than my very unadvisable first distillation- elemental bromine!

https://www.sciencemadness.org/whisper/viewthread.php?tid=26...




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WangleSpong5000
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[*] posted on 30-11-2017 at 18:38


Quote: Originally posted by zts16  
Certainly a better idea than my very unadvisable first distillation- elemental bromine!

https://www.sciencemadness.org/whisper/viewthread.php?tid=26...


A safer idea sure but a better one? Nah... it's far more fun when it's somewhat risky and/or interesting... + risk is interesting by default... there's an equation in there somewhere lol...

Ok so for my second distillation I distilled some OTC paint stripper which was about 60% DCM, 10 - 30% ethanol, 1 - 10% naphtha hydrocarbon mix, 1 - 5% aqueous ammonia and the remainder: a bunch of god knows what additives... the stuff was like thick snotty goo but the DCM (and I'm assuming the ammonia) boiled off and condensed well quick. It's a little cloudy though which I guess is the ammonia?


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[*] posted on 30-11-2017 at 19:17


Quote: Originally posted by zts16  
Quote: Originally posted by WangleSpong5000  
Just undertook my first ever distillation! Just a simple distillation of tap water. Boring I know but a logical first choice I think. Went off without a hitch although stupid me had cleaned everthing with a bit of acetone and the recieving flask still had a tiny puddle of unevaporated acetone so yeah... guess I'll just have to re-distill it... :D

That was fun! Now to try something a bit more interesting...
Certainly a better idea than my very unadvisable first distillation- elemental bromine!

https://www.sciencemadness.org/whisper/viewthread.php?tid=26...

Definitely better than distilling bromine in an untested homemade distillation apparatus. I learned my lesson; never again.

https://www.sciencemadness.org/whisper/viewthread.php?tid=61...
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WangleSpong5000
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[*] posted on 1-12-2017 at 14:44


Quote: Originally posted by Plunkett  

Definitely better than distilling bromine in an untested homemade distillation apparatus. I learned my lesson; never again.

https://www.sciencemadness.org/whisper/viewthread.php?tid=61...


lol yeah I think you're right on that one... still cool though... :D
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[*] posted on 1-12-2017 at 15:19


My plan today is to make some chloroform. Decided to test the concentration of my newly bought bleach with H2O2... saw Nile Red doing this test in his chloroform vid and decided to give it a try. Was ignorant of this procedure up until recently and at this point in my chemistry travels the more stoichiometry the better! It's been a while since Uni and I'm pretty rusty on the basics frankly...

So it turns out the 4% bleach is 3.8%... it's brand new so I assumed it hadn't degraded significantly yet... so yeah thats currently cooling in the freezer and when it's cold enough we'll get crankin!

Later I'll distill the remainder of my paint stripper for the rest of the DCM and at some point I'll re distill the DCM from last night...

Might go to the local hardware store soon and buy some PVC solvent and try my hand at getting the small amount of THF out of it...

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JJay
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[*] posted on 9-12-2017 at 21:21


I am currently making some nitric acid. I chickened out and added 50 mL of water. (101.1 grams Spectracide, 50 mL municipal water, 60 mL Rooto). I brought it to a boil very slowly as lots of red-orange fumes gassed off into the ventillation, and then things cleared up and started distilling. Right now I'm not sure if I just can't smell the toxic nitrogen oxides or what, but the inside of my fume hood smells like nitrous oxide and nothing else.




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[*] posted on 9-12-2017 at 21:42


Made some Ni(OH)2 today, and attempted NiCrO4 (which failed, apparently it's far too soluble in water to just precipitate all out when I mix a Chromate and Nickel(II) sulfate in water...got a tiny bit of brown powder though.) and attempted the hydrolysis of some di-n-butylphthalate for the second time...I guess I'm just not heating it enough, idk.. but this is ridiculous...



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JJay
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[*] posted on 9-12-2017 at 22:25



Here's my yield of nitric acid. I think I have around 70-80 mL here.

I went very slow with the distillation, and it was actually fairly unremarkable except for the beginning and the end. At the beginning the apparatus was filled with scary red fumes while the reaction mixture boiled and basically nothing condensed. At the end, the reaction mixture started foaming furiously and then crystallized with a huge puff of nitric acid vapor that threatened to overwhelm the condenser when I removed the heat.

I could distill the product again, but since this is such a small batch, I think I will just titrate it and use it as is unless it turns out to be exceptionally impure for some reason. It's plausible that it could contain a little bit of sulfuric acid.

In the near future I am going to break out my barium carbonate and prepare some barium chloride and barium nitrate.

IMG_20171209_210519.jpg - 466kB

[Edited on 10-12-2017 by JJay]




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[*] posted on 10-12-2017 at 10:14


Quote: Originally posted by LearnedAmateur  
Quote: Originally posted by NEMO-Chemistry  
Made basic copper carbonate from home made copper nitrate and have no idea how!! I was making copper nitrate, no carbonate involved that I am aware of...... But the sludge looks just like basic copper II carbonate.


That's really strange, how did you go about making it? I've always just bubbled in NO2 to water with a piece of copper pipe in it. Solution skips green (excess HNO3) and goes progressively darker blue like CuSO4 synthesis - once the bubbling has stopped then the tube is removed, solution sits for a week or so in an old salsa jar and I get either nice seed crystals or large, kinda irregular crystals the size of coins. These are removed, dried, dissolved to saturation in DIW and recrystallised using a seed, and the original solution is reused.


Sorry it took so long to come back to this, you said a couple of things that got me thinking. So i have been trying to find out where I go wrong.

I have tried the following with 68% Nitric Acid, 50% Nitric acid, 30% Nitric acid.
Somewhere on the board is a pic (i cant find it now) of a flask of emerald green Copper nitrate. I have put more water in and yet the colour never changes, the flask contains an excess of copper wire.
copper wire.

Its been months now and every once in while I take a small sample and add water to the sample and top the flask up with water. At no point has the colour changed. Whats really odd is the Nitric acid I have used each time is from different sources!

The one flask with the sludge, is a real baffle though. I filtered it and dried in a desiccator for around 3-4 months.
I have just weighed it on my new balance 4.2127g

Seems a huge amount considering the flask is only 500ml capacity. I will check in the week and try and work out what the sludge is. The acid is from a good source, the copper from freshly stripped cable, so everything should be fairly pure. The acid is water clear as well.

I have a small sample of the solution that I added Sulphuric acid too (98% reagent grade), its the only flask with crystals in (small like sugar and green). All other flasks have copper wire still in and no crystals at all.

Really odd, last time i did this i got both copper Nitrate and copper sulphate crystals form, after that the desiccator wouldnt give any more up, you just get blue condensation in the desiccator after a few months.

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[*] posted on 11-12-2017 at 02:47


Over the last 10 days or so I've done a few things. Mostly a bunch of distillations and some other basic stuff.

Distilled some vodka for the ethanol and attempted to distill some hardware HCl which was a disaster! Still waiting for my glass thermometer to be delivered so I've been using the temperature probe on my hot plate magnetic stirrer... which is made of metal... *facepalm* turned the surface of the probe lovely a lovely greedy black... lesson learned.

Looked into the various ways one can attain glacial acetic acid... decided to freeze some 5% vinegar as I found the method interesting and was curious of the results. Decided on reacting sulfuric acid with sodium acetate to attain glacial acetic acid though I haven't done this yet, so to prepare I made some sodium acetate... smelled horrible boiling the solution down... do people actually like that smell?

Found a brilliant thread on this site relating to a method of attaining anhydrous ethanol. Think I'll buy a hydrometer on Wednesday... and a vacuum pump or water aspirator...

Looking into all sorts of things at the moment. Mostly basic stuff I guess but it's been a while since I've been in the lab and even when I was I only a first year anyway so I never did end up doing that many experiments. Lots of time for that now!
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JJay
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[*] posted on 14-12-2017 at 23:31


I put some mineral oil into a jar and then took some of my sodium out of its vacuum sealed package to store under the oil. I quickly realized that the chunk of sodium was actually just slightly too big to fit into the jar and had to cut it. Fortunately, this was not the first time I had ever handled sodium, so I managed to get it sliced into chunks and placed it into the jar with no problems, after which I wiped down the work area with cleaning vinegar.

Quote: Originally posted by WangleSpong5000  
Decided on reacting sulfuric acid with sodium acetate to attain glacial acetic acid though I haven't done this yet, so to prepare I made some sodium acetate... smelled horrible boiling the solution down... do people actually like that smell?


I personally do not like the smell or taste of acetic acid (or sodium acetate), but some people do. I've tried reacting vinegar and baking soda and boiling it down before but usually I just dehydrate sodium acetate trihydrate.

In the near future I am going to clean my sodium by cutting off the oxide/hydroxide crust and shoot a YouTube video of sodium reacting with water.





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[*] posted on 19-12-2017 at 15:19


I did my first fischer esterification today. I started with sodium benzoate, converted it to benzoic acid and then reacted it with methanol to make methyl benzoate. All of the procedures I found use diethyl ether for extracting the methyl benzoate but I do not have any ether so I used naptha camp fuel instead. I am waiting for the naptha to evaporate but my garage already has a nice fruity smell to it.
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[*] posted on 19-12-2017 at 16:59


Ethyl lactate has a nice coconut-like smell to it. Lactic acid can be hard to source, but PLA plastic scraps from 3D printing are polylactic acid, and could theoretically be hydrolyzed to get lactic acid.



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[*] posted on 21-12-2017 at 19:53


I finally got around to weighing out some samples of my unknown concentration nitric acid in volumetric flasks, labeled the flasks, and partially filled the flasks with distilled water. I have been super busy, but I will hopefully have time to run a titration in the next couple of days.


[Edited on 22-12-2017 by JJay]




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[*] posted on 22-12-2017 at 16:55


Last night I did something that fascinated my kids, the experiment with making liquid filled gels out of sodium alginate and calcium chloride. We made chocolate topping beads ant they loved them. My eldest daughter has taken after me and has a huge interest in chemistry and science in general with a huge thirst for knowledge. I try to encourage it as much as possible.
Myself yesterday i made KNO3 by way of mixing the molar amounts of CaNO3 and K2CO3 on a 2 mole scale. Filtered off the calcium carbonate, reduced the volume of the solution, allowing it to cool which precipitated the needle like crystals of KNO3

0D7E168D-0825-4258-96A2-886896FE0708.jpeg - 1.3MB




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[*] posted on 23-12-2017 at 15:06


Been producing EtOH and working on compounding different propellant powders so I can do some tests and post data in NEMO's black powder question thread.



Why did i wait so long to by a hotplate stirrer?
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[*] posted on 23-12-2017 at 15:12


Holy Fuck it's arky !

Glad to see you around and messing with stuff after the bike accident.




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[*] posted on 23-12-2017 at 15:18


Producing aga's favorite substance, huh? Too bad the only alcohol I distill is denatured ethanol. :(



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[*] posted on 28-12-2017 at 02:25


Back from a few days away Christmassing. After traffic and unpacking it was time to break in the new lab. Something simple -- distillation of hardware store acetone (Diggers). I decided to go for a fractionation. mostly as a height test. I needed to check that I could fit a lab jack, mantle, 300mm vigreux, still head and thermometer in the space. The answer, only just.

Mantle is not doing well. Switch seems loose and rattly. Something is shorting in the heating element (the result of a spill a while back.) It blew the RCD when I cranked it up a bit. On my list of things to do has to be disassembling and fixing the mantle.

Continued with a hotplate. Something has me confused though. The acetone came over 8° below BP. I am not aware of any azeotropes that would do that. I can't think of a sensible reason however. It would be sad if my thermometer was that inaccurate. Tails smelled heavy an oily a bit like toluene. I am confident therefore that the product I obtained is an improvement.

Anyway. Lovely to be legitimately writing in this thread.




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[*] posted on 28-12-2017 at 05:27


Quote: Originally posted by j_sum1  
Back from a few days away Christmassing. After traffic and unpacking it was time to break in the new lab. Something simple -- distillation of hardware store acetone (Diggers).


I was under the impression that this particular brand of acetone was pure. The msds says that it is... then again we all know the situation with diggers methylated spirits so this doesn't surprise me.

Why is this do you think? I assume it has sometime to do with industry regulations regarding chemical grades. As hardware store chems are (i assume technical grade?) at the lower end of the grading scale they may not have to declare small amounts of other chemicals. This is pure speculation on my part though...

What do you lot think?




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[*] posted on 28-12-2017 at 05:34


"Pure" on an msds does not mean the same as "pure" to a chemist. Diggers has products that are 100% petroleum distillate according to the msds. But that really tells us nothing about the composition. In this case, acetone is the product that they manufacture and pure means they add nothing else. It is still worth cleaning.



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[*] posted on 28-12-2017 at 18:18


I tried making ammonium oxalate! I think I succeeded- I decided, in my boundless wisdom, to make use of my massive store of urea rather than ammonium carbonate.

I do not recommend what I did- use thermal decomposition to bubble ammonia gas into a solution of oxalic acid- the suckback is considerable and effectively quenches the reaction before completion. I don't have any apparatus for gas bubbling, so I made a trap with a round bottom flask and some distillation adaptors. It worked OK- the suckback collected in the RBF, but some of it still managed to make it's way into the ammonia generating flask.

Ammonium oxalate crystals are very pretty, though.




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