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Author: Subject: Opinion on distillation kit purchase
Dark Alchemist
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[*] posted on 10-12-2015 at 02:06
Opinion on distillation kit purchase


http://vi.raptor.ebaydesc.com/ws/eBayISAPI.dll?ViewItemDescV...

OK I'm new to distillation kits will this be OK for distilling nitric acid and sulphuric acid? it will need to stand up to open flame contact.

If not I'm going to have to make one and really haven't a clue were to start could someone give me a list of parts needed for a basic set up.
Also what does the vacume feature mean? Does it have to be used?




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[*] posted on 10-12-2015 at 05:34


Although good quality glassware will stand up better to flame contact, you should still never distill using a direct flame. Uneven heating will crack the glass. Sulfuric acid is best distilled with an air bath and nitric acid is distilled using a hotplate. The vacuum feature simple means that it allows you to hook it up to a vacuum for vacuum distillation.

The kit seems OK, but I would prefer one with 300mm fractionating column and 300mm condenser, rather than the 200mm in the kit offered by your seller.
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[*] posted on 10-12-2015 at 05:42


Nitric acid: yes
Sulfuric acid: maybe (needs to reach much higher temperatures)

The vacuum doesn't have to be applied.

List of parts for vacuum distillation (all ground-glass):
Flask
Still head/Thermometer adapter
Thermometer
Condenser
Vacuum adapter
Receiving flask

The kit also has a Vigreux column, which is useful for fractional distillation.




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[*] posted on 10-12-2015 at 15:13


If it helps I intend to use it for making nitric through H2SO4 nitrate salt probably KNO3 simple distillation so the only thing that needs boiling will be The HNO3 produced.

I'm still learning proper lab procedure and equipment ect and since I'm just starting out (its only been a few months) I don't have a heating mantle.
Now you already said no open flame so could I use an electric stove element?
And how do I clean up the mess left over from the reactants
Also I will be using H2SO4 boiled till white fumes from car battery's approx what concentration is this at? I have been told around 98% is that true?

What is the difference between white fuming red fuming and yellow fuming? I have heard all these terms thrown around but am pretty shure there all the same concentration just with impurity's like NOx gas dissolved in.

Finally this might seem a silly question but google has not satisfied me in its awnsers regarding this.
when people say acid is diluted to 68% do they mean for exsample 68mls nitric 32mls water as in volumetric or is it molar if so because again still learning these things about how much water to nitric acid ratio by volume please do I use to get fuming down to the 65-68% range. Because I do not seem to be able to find a chart that says so and so acid in so and so concentration has 7mls to a mole or whatever and even if I could how many moles of water to acid is 68% ? Confused

Sorry if this seems silly this is just a build up of my frustration at simple things. Oh well still learning


[Edited on 10-12-2015 by Dark Alchemist]




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[*] posted on 10-12-2015 at 15:55


I have heard that a hot air gun -- the kind that is used for stripping paint is a reasonable heat source for lots of different things. In the absence of a mantle, I would go that way.

68% nitric acid is on a mass basis.




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[*] posted on 10-12-2015 at 16:12


So it is moles ?
Or do you mean grams?
PS thanks for the heat gun idea.

[Edited on 11-12-2015 by Dark Alchemist]




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[*] posted on 10-12-2015 at 16:48


Wait so tell me if this sounds right 2205 grams of fuming + 234 grams water will give me roughly a 63% concentration of nitric acid? If moisture and contaminants are taken into consideration?

Recalculated dies this sound right ?
4.284 grams RFNA
4.36 grams H20
=68% HNO3 ?

[Edited on 11-12-2015 by Dark Alchemist]

[Edited on 11-12-2015 by Dark Alchemist]




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[*] posted on 10-12-2015 at 18:21


Mols not moles. You had better learn about two things really quickly. Dimensional analysis and stoichiometry. If you didn't take highschool chem sign up for chem 1a or the equivalent at any college. Mols are not grams! mols are the way we find the number of grams to react with another substance. If, for example you wanted to react NaOH with HCl to make NaCl and water you wouldn't want to mix say 9 grams NaOH with 9 grams of HCl.
an Avogadro number of Na would weigh the amount shown on any decent periodical table (another essential). so 6.23X10*23 atoms of sodium would weigh 23 grams. You don't need the Avogadro # but you need to know the atomic or molecular weight of the atom or molecule. So 9 grams of NaOH = how many mols?

Back to the kit; Vigeraux columns are popular with glassware makers and or OK for holding back foam but not much else. So little improvement on the surface area. I would buy the parts you need instead. I would use a Snyder column or some kits come with two condensers one of which has little bumps to hold column packing. A short column with little rings or glass balls of anything to make more surface will serve better than a fucking Vigeraux. Look up theoretical plates but don't bruise your brain about it.

9 g* mols NaOH/40g/mol = 0.23 mols I can't show you how this looks on paper but that is a simple d.a.
HCl is about 18g/mol so 0.23 mols would be 18*0.23 = 4 g. In a proper d.a this would all be on one line. (I should really write one out on a graphics program and paste it here but it's late and I'm going home besides you need to do a lot of these until they become second nature. Your interest i chemistry is laudable but please don't try to skip the basics.

[Edited on 11-12-2015 by chemrox]




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[*] posted on 10-12-2015 at 18:40


No no I think you misunderstood me I understand what a mol is.
What I'm asking is when making 68% nitric from 84% is am I using grams or mols as a percentage?
For example is it as simple as adding 16 grams of water to 100 grams 84% fuming?
Or do I need to figure out molar percentages and then covert those to grams?

Thank you for the advice on the dist kit by the way.
Sorry if I came across as ignorant but there is difference between an ignorant man who refuses to acknowledge the truth and an eager man trying to understand the truth.



[Edited on 11-12-2015 by Dark Alchemist]

[Edited on 11-12-2015 by Dark Alchemist]

[Edited on 11-12-2015 by Dark Alchemist]




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[*] posted on 10-12-2015 at 19:25


The law of dilution

c1v1 = c2v2

So, if you have 84% and you want say, 150mL of 68% then,
c1=0.84
c2=0.68
v2=150

calculate v1. This is the amount of nitric acid to measure out. Then make up to 150mL with water.




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[*] posted on 10-12-2015 at 20:50


Thank you that's exactly what I needed!!!

[Edited on 11-12-2015 by Dark Alchemist]




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