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JJay
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[*] posted on 28-12-2017 at 21:25


I am going to finally get around to titrating my nitric acid this evening after I put my equipment away. Most of my glassware items have a box that they belong in, but I have a dozen or so that do not... sometime later this week I am going to shop around for polystyrene sheets to make boxes to hold some of those pieces.



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JJay
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[*] posted on 29-12-2017 at 18:06


My nitric acid titrated at 48%.



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[*] posted on 29-12-2017 at 18:41


Prepared some zinc carbonate for a higher purity when it comes to preparing zinc compounds. I need some zinc acetate for a nanoparticle project of mine, but zinc chloride would be a useful compound for future organic chemistry reactions I might perform. I'm also going to need some silver nitrate, so I'm preparing for my first nitric acid distillation.



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[*] posted on 29-12-2017 at 19:26


Today, i tried my hand at making magnesium silicide and silane gas. I am making this for a future project which i plan on posting on here soon. Anyway, for the most part it failed. Only the outside of the reaction mixture actually reacted and all of the inside remained unreacted. It did, however, react to form some silane gas. I think that one reason that it didn't work well was that my magnesium was more like very fine small shavings rather than powder. (any ideas on how to make the powder? I was thinking perhaps ball milling in mineral oil, then washing the remaining mixture with acetone or toluene to get rid of the mineral oil. Secondly, I used a small butane torch to heat up the mixture. Butane is certainly capable of getting hot enough but the problem was in the size of the flame. Since I was using a small torch, the flame was only able to cover a small portion of the test tube at a time. Anyway, next time i think i am going to try propane because i have a propane torch that has a larger flame. I believe my next project will be to dry some methanol that i have with magnesium shavings/ribbon. (If anyone has a good source of reasonably affordable, quality 3A molecular sieves, or owns some that they want to sell, please U2U me). Molecular sieves would be ideal.. but sometimes you just gotta make do :P.

[Edited on 30-12-2017 by TheNerdyFarmer]
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[*] posted on 1-1-2018 at 18:13


Took my first shot at pulling lithium out of batteries today; 1 of the two was a success :)
the other.... well.........




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[*] posted on 5-1-2018 at 19:31


Attempted making nitric acid via the Tdep method using bisulfate. The process is a foaming nightmare and painfully slow. I don't think I'll be doing it again.



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[*] posted on 5-1-2018 at 23:03


Did you get any nitric to come over?
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[*] posted on 5-1-2018 at 23:33


Well I haven't tested it yet but something came over woth a whole lot of NO2. I think it is RFNA but there may be some water in it.

The reaction ate my favourite stir bar. I guess it wasn't PTFE like I thought.




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JJay
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[*] posted on 9-1-2018 at 13:37


I checked three different stores and couldn't find any distilled water, so I'm distilling some water....



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JJay
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[*] posted on 9-1-2018 at 15:09


I figured that since I'm boiling some water I might as well calibrate my wildly inaccurate alcohol thermometer. I used a couple of data points in a boiling point calculator with the barometric pressure at the nearby airport and found that it is off by 4.8 degrees at 100 C!

I guess that's what you get for $1.75 with free shipping from China....




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JJay
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[*] posted on 11-1-2018 at 13:33


I'm distilling some muriatic acid to obtain pure azeotropic HCl for use in synthesis and as an acidimetric primary standard. I'll be monitoring barometric pressure carefully.

...

Now I have two 500 mL bottles of HCl, one labeled "20.2% (lab)" and one labeled "20.244% (lab best)."

[Edited on 12-1-2018 by JJay]




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[*] posted on 13-1-2018 at 22:07


Distilled some hardware store toluene and then removed remaining water using a Dean Stark trap and Dimroth condenser.

There is something oddly satisfying about watching vapour fronts and condensation in a nice bit of glassware.




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[*] posted on 14-1-2018 at 01:52


Quote: Originally posted by JJay  

Now I have two 500 mL bottles of HCl, one labeled "20.2% (lab)" and one labeled "20.244% (lab best)."
[Edited on 12-1-2018 by JJay]


20.244% is an incredibly precise number




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[*] posted on 14-1-2018 at 06:21


Quote: Originally posted by JJay  
I'm distilling some muriatic acid to obtain pure azeotropic HCl for use in synthesis and as an acidimetric primary standard. I'll be monitoring barometric pressure carefully.

...

Now I have two 500 mL bottles of HCl, one labeled "20.2% (lab)" and one labeled "20.244% (lab best)."

[Edited on 12-1-2018 by JJay]


How did you measure the pressure that accurately?
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JJay
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[*] posted on 14-1-2018 at 10:21


The last digit is estimated using basic measurement theory (i.e. linear regression).



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[*] posted on 14-1-2018 at 12:12


Made some chloroform via haloform reaction, but might've made a chloroform-acetone azeotrope instead. Might need to do some washings or maybe a distillation.



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[*] posted on 14-1-2018 at 19:12


I made some solid iodine for the first time with potassium iodide, sodium bisulfate, and hydrogen peroxide. When I replenish my sodium bisulfate and potassium iodide, I will do this on a larger scale.
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[*] posted on 17-1-2018 at 05:19


Failed attempt at oxidising toluene to benzaldehyde. Well, not quite failed. There was a faint whiff of something almond-like mixed in with a mL of fairly sharp-smelling yellow oil at the bottom of the flask.
Procedure being followed was on the first page of the stickied thread -- involving iron and copper catalysis. Posted details were a bit sketchy and there were good reasons for it not working well.
I have videoed it all and will edit it into something for my yt channel. Later I can do a (hopefully successful) follow up.

All good fun though.




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[*] posted on 19-1-2018 at 02:19


I made some benzaldehyde by refluxing benzyl alcohol with 10% nitric acid and a few grams of sodium nitrite for a few hours. This produced an orange liquid that smelled strongly of cherries. It formed a thick mass of brown powder with sodium bisulfite solution. The powder bleached to a tan color with a 3% hydrogen peroxide wash. I stirred the bleached powder with saturated sodium carbonate and obtained a dark brown liquid. It vacuum distilled to produce crystal clear benzaldehyde! The yield was not great, but the process was very easy and satisfying.

CycloKnight's posts describe a method of oxidizing toluene with manganous-ammonium alum. It ties up several pieces of equipment but works well.
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[*] posted on 19-1-2018 at 02:56


Hmm. I chose toluene as the starting point since I have toluene but I do not have benzyl alcohol. Also I wanted to try something new.

CycloKnight's method involves electrolysis as well. While this is within my capabilities I was hoping to tackle something new to me and with fewer variables.

Happy with what I accomplished and I will see if I can make some improvements.




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[*] posted on 19-1-2018 at 10:23


Just finished filtering and washing some quite pure paracetamol crystals from IPA to be used in new and possibly exciting endeavours - pearly white and devoid of any coloured impurities despite the strongly yellow solution. Currently air drying but I intend to weigh up tomorrow and compare the yield to the amount present in the original tablets, I estimate I have between 3 and 5 grams from 10 tablets.

So out of a potential 5000mg (10 x 500), 4390mg +/- 10mg were recovered with a bit of solution to spare. Going to recrystallise again and hopefully get some larger crystals, at least 1-2cm as opposed to the maximum of 5mm; upon closer inspection and mixing the two batches, the second lot definitely had a slight hint of yellow but it was only noticeable in certain light types, this should almost certainly be gone in the final crop.

[Edited on 20-1-2018 by LearnedAmateur]




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[*] posted on 19-1-2018 at 10:58


As part of an experiment for my next video, I got to saw through a block of dry ice with a wood saw. Cuts just like wood does! Just have to be careful the solid CO<sub>2</sub> "sawdust" doesn't get on your skin!

Interestingly it also produced some little bits of dry ice that were crystal clear, instead of the usual white. Looked just like regular ice!
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[*] posted on 20-1-2018 at 16:10


Made some acetic acid from sodium acetate and sulfuric acid. Although I initially started pouring the sulfuric acid in the flask with the sodium acetate, I noticed it started boiling due to the heat of the reaction. So I attached the flask to the distillation apparatus and replaced the thermometer adapter with an addition funnel, to add the rest of the acid dropwise. After that I put back the thermometer and started distilling.

Next up, I'll be making copper acetate.
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[*] posted on 21-1-2018 at 13:31


Made sodium methoxide yesterday. It was pretty easy and ran smoothly. I’m going to be using it as a catalyst in preparation of methyl ricinoleate. I have used KOH and NaOH but these didn’t allow for a phase separation like the methoxide is supposed to do.

76BBA474-6FE8-42EC-979F-CE861C3E2331.jpeg - 2MB




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[*] posted on 23-1-2018 at 09:48


Mainly to test a new 2000ml flask with a bubble in the glass wall
and a new (used) dual hotplate (1.5 kW and 1.0 kW nominal)
I set up a simple experiment;

Ambient, equipment and liquid temperatures all 20oC
On the 1.5 kW hotplate element I put a 5l aluminium pot containing 2l sunflower cooking oil
I clamped a new, washed 2l rbf containing 1l (+/- 0.25ml) of clear tap water (999.9g +/-0.2g) in the oil
a 0 - 110 oC Thermometer was clamped to measure water temperature
and a 0 - 250 o thermometer for the oil.

To start this mini-experiment, the hotplate was plugged in and turned to MAX.
. Power input = 240V x 6.0A = 1440 W (actually measured, true rms)
. the thermostatic temperature controller began to operate at 13 mim, oil = 111 oC, water = 48oC
. after 30 min.oil = 167oC, water = 101oC, water just boiling
. after 40 minutes of boiling, 70 minutes total elapsed time, heating was stopped and the flask removed and rapidly cooled under running tap water.

During the last 20 minutes of water boiling, the oil temperature reached a fairly constant 176 oC due to the operation of the thermostat.

Almost exactly 540 ml of cloudy water remained in the flask.

Based on water evaporation at 2257 J/g
the effective heating power was 432 W (87 minutes per litre of water evaporated)

I could bypass the inbuilt thermostat to get more heating power
but even with thermostatic regulation the temperature difference across the RBF wall was 75 oC
which is already a little high.

[Edited on 23-1-2018 by Sulaiman]




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