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Author: Subject: The Short Questions Thread (4)
ninhydric1
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[*] posted on 17-12-2017 at 17:24


Would this thermometer adapter:

https://www.ebay.com/itm/Glass-Thermometer-Adapter-With-Thre...

be OK for nitric acid distillation?




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CharlieA
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[*] posted on 17-12-2017 at 17:30


I don't know if the little red cap can stand up, but they are easily enough replaced. Perhaps you could wrap the thermometer with silicone plumber's tape where it is in plastic bushing. I guess that in the long run, I would consider the plastic part to be expendable.
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JJay
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[*] posted on 17-12-2017 at 17:44


If it has a Tygon o ring, it should be OK. If it has a rubber o ring, it will be destroyed.



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[*] posted on 17-12-2017 at 18:15


They require an o-ring to seal correctly. The o-ring needs to be compatible with what is being distilled which in the case of nitric acid requires a floroelastomer. That item does not say what the o-ring is made from or if it has an o-ring.

So its not suitable unless you are happy to bodge it with PTFE plumbers tape.
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ninhydric1
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[*] posted on 17-12-2017 at 18:40


Hmm... then I might get a glass stem tube thermometer adapter then, just to be safe.

I'm asking because I have a nanshin distillation apparatus with a thermometer adapter similar to the one I linked. It indeed has an O-ring, but of unknown composition. Is there any method for determining if it's a fluoroelastomer as wq48 mentioned? Or if you have distilled nitric acid with a nanshin thermometer adapter, if it is able to hold out against nitric vapors?




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[*] posted on 24-12-2017 at 09:39
Thiourea disposal


Does anyone have experience disposing of thiourea? I can't seem to find anything on it anywhere.

I'm thinking

Thiourea + 4 H2O2 + 2 NaOH --> Urea + 5 H2O + Na2SO4

First, thiourea is oxidized to thiourea dioxide, which is hydrolyzed to urea and sulfoxylic acid. The latter is then oxidized all the way to sulfate, with NaOH to neutralize the H3O+ left over (and to keep the pH high enough for hydrolysis of of thiourea dioxide to take place).

Any better ideas?




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[*] posted on 28-12-2017 at 05:44


Any ideas on how to separate copper particles and copper hydroxide?



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ninhydric1
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[*] posted on 28-12-2017 at 12:56


Add acetic acid or dilute HCl. This should react with the copper hydroxide to form a soluble copper salt. Allow to settle and decant the blue solution, or filter out the copper (if you can). Add excess NaOH (or KOH) solution to the decanted, clear solution in order to precipitate the copper(II) hydroxide.

If the copper is in nanoparticle form, the easiest way would probably dissolve it using HCl/H2O2. Then you could use a single-displacement with Al or Zn to form copper metal using a portion of the prepared CuCl2 in solution.




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[*] posted on 28-12-2017 at 13:07


Don't use HCl on copper- it will react if there is oxygen from the air dissolved in solution. Better to use dilute sulphuric or acetic.



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[*] posted on 30-12-2017 at 21:41


Hello everyone. I recently got a job and am now making a little extra cash for chemistry. I have decided that I would like to buy a full face gas mask. I decided to go with a full face design because of high visibility and, even when not in use, it can act as a full face shield. Finding a decent gas mask is not entirely the problem. My main issues are in finding a good filter that will filter out all of the "nasties" that I may work with. I have a fume hood so the only time I would honestly use it would be for very hard to detect gasses and fumes like phosgene, silicon tetrachloride, carbon monoxide, hydrogen cyanide and despite its smellyness in low concentrations, hydrogen sulfide. If I ever work with these items, I want to be sure that if they escape my fume hood, they will not kill me. So, with that being said, I cannot trust my own knowledge on air filters. All this leads to the big question, do any of you have good suggestions for filters? The gas mask I am looking at, takes 3M filters (which I assume refer to the size). Price is not an issue (at least not a big one anyway) because it is likely that I will only use the filters on occasion when I decide to work with Exceptionally dangerous gasses. I know that I have seen threads on this topic before but I simply cannot find them. I look forward to hearing back from you guys! :)

By the way, I uses a bayonet type connection according to the manufacturer.

[Edited on 31-12-2017 by TheNerdyFarmer]
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JJay
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[*] posted on 30-12-2017 at 23:10


The manufacturer disclaims any liability for home use, but these cartridges otherwise look as though they were designed for home chemistry: https://www.homedepot.com/p/3M-Professional-Multi-Purpose-Re...

I've used them, and they are fantastic for everything I've thrown at them (not sure about ammonia). They hold up pretty well but do not have unlimited capacity and degrade in a humid environment to the point where heavy sulfur dioxide fumes can be smelled through the respirator after several hours of use.




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ninhydric1
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[*] posted on 31-12-2017 at 13:15


Is isopropanol OK for stabilizing chloroform?



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[*] posted on 5-1-2018 at 08:36


I think so, but I will defer to those who are wiser and more knowledgeable when it comes to possibly producing phosgene.

Can Portland cement be used to dry alcohols? It is cheaper and easier to find than calcium oxide.

[Edited on 5-1-2018 by JJay]




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[*] posted on 5-1-2018 at 08:55


you could probably get away with using portland cement but I wouldnt recommend it, you have have to add a lot more due to all of the silicates and other impurities. How much alcohol are you trying to dry and how dry do you need it? there might be other cheap easily accessible desiccants.
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[*] posted on 5-1-2018 at 09:09


I'd like to dry unlimited amounts of it to 99.99999% water free :) What cheap and easily accessible desiccants are known to work well?

I recently tried drying some with magnesium sulfate... I have no idea how well it worked yet but will run some tests later... I found numerous posts suggesting magnesium sulfate as a dessicant for alcohols but few claims that people had tried it and found it worked well.




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[*] posted on 6-1-2018 at 18:01


Does anyone routinely pyrolyse NaHSO4 to produce SO3? I am considering alternate routes to concentrated H2SO4. I do have some in stock and I have a good supplier. It is just that it is expensive whereas bisulfate is dirt cheap where I live.

I know the theory but with something like SO3 I would love advice from experience.




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[*] posted on 11-1-2018 at 19:28
Ball milling magnesium.


Hello everybody. I have plans to make a ball mill. In fact, 50 lead balls came in the mail for it today. My main reason to build one is to make things like magnesium powder. There is one problem though. Doesn't magnesium react with the oxygen (and some nitrogen at elevated temp) in the air? If this is true, when I put crude magnesium shaving in the mill, will I just end up with a bunch of magnesium oxide when I take it out? If so, how would I go about doing this. Perhaps ball milling with a dry solvent such as toluene mixed with the media?
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elementcollector1
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[*] posted on 11-1-2018 at 22:20


I feel like ball-milling magnesium, even under solvent or argon, would be a very bad idea. Wasn't there a thread here a few years back about someone who tried it and got severely injured?



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TheNerdyFarmer
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[*] posted on 12-1-2018 at 03:19


Thes reason I ask, is that I can't find magnesium powder anywhere. Usually I would settle for just shavings, but some reactions require the powder. Any idea on where I could get my hands on a small amount of the powder?
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[*] posted on 12-1-2018 at 05:25


A simple file worked for me but I only needed a few grams. You will not get powder with a file like you would from a ball mill, but you will get finer than shavings. United Nuclear also sells granular magnesium for a decent price.
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[*] posted on 12-1-2018 at 08:07


Quote: Originally posted by TheNerdyFarmer  
Thes reason I ask, is that I can't find magnesium powder anywhere. Usually I would settle for just shavings, but some reactions require the powder. Any idea on where I could get my hands on a small amount of the powder?


I don't know where you are but Ebay sells it.
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ninhydric1
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[*] posted on 30-1-2018 at 17:24


I'm doing some experimentation in zinc acetate decomposition, but the leftover zinc oxide is always contaminated with a brown substance. I'm using a butane gas burner with stainless steel measuring cups as my crucibles, and I'm heating it up to around 400 degrees Celsius. Is the stainless steel oxidizing, forming iron oxides, and how would I prevent it?



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[*] posted on 31-1-2018 at 09:19


Try using zinc oxalate in place of the acetate in an inert gas. Reference: https://www.sciencedirect.com/science/article/pii/S004060310... .

[Edited on 31-1-2018 by AJKOER]
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[*] posted on 31-1-2018 at 09:32


Oxalic acid is one of the two ingredients of 'barkeepers friend' stainless steel cleaner,
oxalic acid (and I think many oxalates) chelate iron and iron oxides from the steel
- hence the colour - I guess.




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[*] posted on 31-1-2018 at 09:47


Quote: Originally posted by j_sum1  
Does anyone routinely pyrolyse NaHSO4 to produce SO3? I am considering alternate routes to concentrated H2SO4. I do have some in stock and I have a good supplier. It is just that it is expensive whereas bisulfate is dirt cheap where I live.

I know the theory but with something like SO3 I would love advice from experience.


No experience on this experiment, but you may think about heating a mix of NaHSO4 with Fe powder in glass covered bowl in an old, disposable, microwave oven with short power burst only. Reference suggests the need for more equipment, see https://www.researchgate.net/publication/250012947_Microwave... also https://www.mri.psu.edu/sites/default/files/file_attach/135.... and more generally, http://aip.scitation.org/doi/abs/10.1063/1.2159078?journalCo... .

Needless to say, procedure can be extremely dangerous especially to eyes, lungs,...

[Edited on 31-1-2018 by AJKOER]
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