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Author: Subject: Boiling down Sulpuric Acid
Volanschemia
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[*] posted on 19-2-2015 at 01:07


Quote: Originally posted by Oscilllator  
For what it's worth, I use density measurements almost exclusively when trying to determine the concentration of acids and other substances. Sulfuric acid is ideal for a density measurement, because the density of pure sulfuric acid is about 1.8.
A 100ml erlenmeyer flask and a decent scale will tell you the concentration of your acid to within a few %, and you don't have to mess around with titrations and other such shenanigans.


Oh wow! I can't believe I hadn't thought of that. That sounds like a fantastic plan of action, and I think you already have some 0.01g scales don't you Trizocy? A grad cylinder or a burette would be better than an erlenmeyer flask though I would think.




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[*] posted on 19-2-2015 at 02:06


Quote: Originally posted by TheAustralianScientist  
Quote: Originally posted by Oscilllator  
For what it's worth, I use density measurements almost exclusively when trying to determine the concentration of acids and other substances. Sulfuric acid is ideal for a density measurement, because the density of pure sulfuric acid is about 1.8.
A 100ml erlenmeyer flask and a decent scale will tell you the concentration of your acid to within a few %, and you don't have to mess around with titrations and other such shenanigans.


Oh wow! I can't believe I hadn't thought of that. That sounds like a fantastic plan of action, and I think you already have some 0.01g scales don't you Trizocy? A grad cylinder or a burette would be better than an erlenmeyer flask though I would think.


Damn now we are back on density again, it was this the previous forum also recommended me to do :/
Yes i got 0,01g and have aldready done some measurement with density, and here is the result:

I got a 1L bottle of sulfuric acid, on the bottle it stand 60-100%, when i measure it with 50 mL i got 93,34g

93,34g * 2 = 186,68g

186,68g / 100 = 1,8668 g/ml density

And here is the density table for it: http://www.sschemical.com/wp-content/uploads/2013/05/Convers...

The highest % here is 1,8391 g/ml, but my result is 1,8668???


Also they recommoned me to buy a pycnometer, which is the only way to be truly accurate it they said.
With only burette,pippette or a cyilnder i could never pour on the same amount like last time.


Had a expriment with density and freshwater

Quote: Originally posted by me  
I had a brand new fresh 5L water (think its filter water, and yeah! i know that distilled water and filter water is not same, but this was just a experiment on it, gonna try the destilled water when i got some) so i tryed to measure it 20 times, and here was the result: http://pastebin.com/2xSHGNkq - it comes between 48,14g and 48,95g on 50 ml (20-21°C), (average 48,5905g on 50 mL) My standard deviation was 0.27458.


As you see in the link, almost never got the same number.


Thanks
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[*] posted on 19-2-2015 at 05:47


Trizocy, you got higher density due to some error - rather measuring at different temperature or most likely error in volume measurement. But you know what - if you can't take exact volume of acid, how do you expect titration to work for you?
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[*] posted on 19-2-2015 at 07:09


Trizocy-

If the density of water doesn't work out to be 1g/cc with your equipment, either your equipment or measuring technique needs looking at.

For a start: When using the graduate cylinder, you will observe the "meniscus", a curvature of the liquid's surface due to surface tension. How are you accounting for that?

http://en.m.wikipedia.org/wiki/Meniscus





image.jpg - 18kB



[Edited on 19-2-2015 by Bert]




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[*] posted on 20-2-2015 at 02:31


Hmm i think its my measuring technique which must be wrong :)

Anyway, if i gonna measure density, then i could just buy pycnometer.

Pycnometer (25ml) on 0,01g scale. Note down the Pycnometer weight
Pour Sulf acid in the Pycnometer and put the top on, let acid overflow on the pycnometer.
Put back on scale, to measure the mass

Pycnometer weight - Pycnometer full of sulf acid = mass of sulf acid


Volume / Mass = Density :)?

Then you find what tempture it is, and note that down. And so find specific gravity density sulfuric acid. And lookup where you result is = Profit :)?

But one problem, i havent found a legit confirm authority specific gravity, there are too many of them on google, and all have difference measuring :S

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[*] posted on 20-2-2015 at 06:12


Quote: Originally posted by Trizocy  

Pycnometer weight - Pycnometer full of sulf acid = mass of sulf acid


Volume / Mass = Density :)?




Density measurements with Pycnometers are usaually done relative to pure water. So also measure Pycnometer weight when filled with water.

W0 = pycnometer weight
W1 = pycnometer filled with acid weight
W2 = pycnometer filled with water weight

Density relative to water = (W1 - W0)/(W2 - W0)




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[*] posted on 19-3-2015 at 13:23


Hello!

Let's finish this thread ;)
So... Lets continue.

I got a pycnometer now, so i can try to measure the density now

I got 1 Liter of H2SO4, which on the description it stand 60-100% and what i want is to try to find the specific concentration in the bottle.
So what i have done is to measure several times with a 50ml pycnometer, and a temperature meter.

50ml pyconmeter empty: 34,15g
Average 50ml pycnometer with H2SO4: 126,91g (pour in and out several times, and measure it)

Weight of the H2SO4: 92,76g
Temprature: 7,5 cel to 10,5 cel

So how do i calculate it? Tryed to use Chembuddys calculator, but gave me 185% concentration which is not possible :)
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[*] posted on 19-3-2015 at 13:29


You know both the mass AND the volume of this mass of liquid, don't you see it? Just think about the unit's you have and what you're looking for...

92,76g / 50ml = 1,855g/ml. Then it's just a matter of looking this up in a table.

BTW: Well done, a pycnometer is the proper tool for this. I've always had trouble with getting good measurements from hydrometers.

[Edited on 19-3-15 by Fulmen]




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[*] posted on 19-3-2015 at 15:20


It seems to me that you have some VERY concentrated acid, although I think there may be a little error in the calculation.

Azeotropic (98%) Sulphuric Acid has a density of 1.84g/mL so I would say you have overshot a little, but even so, going off that density reading I would say you have at the very least 97%.




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[*] posted on 20-3-2015 at 04:36


Small amount of dissolved SO3 would throw this off wouldn't it?
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[*] posted on 20-3-2015 at 07:55


Hello guys!

Fulmen:
I aldready know that, but here is the problem, my calculation ending up at 1,855g/ml but the highest concentration of H2SO4 is 1,84g/ml so something is wrong here.

TheAustralianScientist:
How can i do a overshoot when i got a pycnometer? ;)?

Hyfalcon:
May u deepen more about u talking about?

Thanks all!

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[*] posted on 20-3-2015 at 08:54


Trizocy,
Are the weighing scales calibrated ?
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[*] posted on 20-3-2015 at 09:48


Nope :(
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[*] posted on 20-3-2015 at 18:14


Remember the pycnometer is only instrument 1 of 2 in the density measuring process. The scales are equally important, so if the scales are off, your calculation of density will also be off.

Calibration weights are fairly cheap, you just need to get the one that your scale requires.




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[*] posted on 21-3-2015 at 02:56


Also density data are given for specific temperature and your picnometer volume depends on temperature as well, also impurities in sulfuric acid can affect density, since 1.84 is given for azeo H2SO4, which must contain only water.. Better to titrate it, but here you'll come to primary standart preparation problem, yes analytic work is hard to do at home.:(
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[*] posted on 21-3-2015 at 05:14


Start by testing a few known chemicals like water, ethanol etc, that will give you an idea of the accuracy.




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