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Organic : Experimental errors
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(1 recommendation so far) Message 1 of 7 in Discussion 
From: MSN NicknameP_5z3  (Original Message)Sent: 10/11/2004 6:06 PM
I started out with a hydrated salt (CuSO4 �?/SPAN>H20), but after heating it turned into an anhydrous salt. What are some experimental errors that might have occurred??
 
Thank you


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 Message 2 of 7 in Discussion 
From: MSN Nickname·Steve·Sent: 10/11/2004 6:39 PM
Hi, and welcome to the group.  In my experience, errors in this lab result mainly from:

1) Incomplete drying, resulting in a higher final weight than it should be, and

2) loss of solid during heating (from splattering of the solid while it is heated, like popcorn popping!) or during handling, resulting in a lower final weight than it should be.

And of course the accuracy of the result is also limited by the accuracy of the balance used to make the weighings, and the care used in handling the balance (unless you used an electronic balance).
 
 
Steve

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 Message 3 of 7 in Discussion 
From: MSN NicknameP_5z3Sent: 10/11/2004 7:00 PM
hey...thx for the experimental errors!!
but, would it the accuracy of the balance be a human error?? Because human errors are not valid for the lab report... (gladly appreciate it though)
 
While heating the hydrated copper sulfate, would the evaporation of the impurities affect the water mass?
 
I got 6 water molecules in my calculation...so would the crucible lid being tightly closed and the crucible being too close to the bunsen burner be reasons why the water molecules did not evaporate resulting in higher water molecules??
 
Thank you so much for your answers!!  

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 Message 4 of 7 in Discussion 
From: MSN Nickname·Steve·Sent: 10/12/2004 12:36 AM
If you used a beam balance, then, depending on its condition, it could be the cause of inaccurate weighings.  Some of our old ones are rusty and the arm does not swing freely, causing some readings to be a little high and others low.  But, if your balance was in good condition, and was capable of measuring to at least 0.01 g, then it is probably not to blame, unless you were weighing very small quantities like a few tenths of grams.  But also, some students are just more patient and careful using the balances and get better weighings as a result.  But that's a "human" element.

There probably are not any volatile imputites in the hydrated CuSO4, so the extra loss in weight that caused you to get a slightly high amount of water may be due to a loss in weight another way, such as spattering out or oozing out of the crucible during the heating.  Did you stir the contents with a stirring rod to break up lumps?  If so, some material likely stuck to the stirring rod and would be lost that way.  Probably the sample itself was of good purity.  If you were weighing very small amounts of compound, in the tenths of grams range, then inherent weighing uncertainty in any general purpose lab balance could cause an error of plus or minus an H2O in your calculated formula.

It's also possible that overheating could cause some decomposition of the CuSO4.  This would cause an excessive loss of weight:

"The pentahydrate is 100% isolable only in temperatures lower than 30 degrees celcius. The light blue trihydrate non-isolable form can be obtained around 30°C. White monohydrate form is available at 110°C, while the anhydrous form can be isolated near 250°C. The decomposition slightly starts at 250 degrees, while complete decomposition occurs around 600 degrees...

The reaction is as follows: CuSO4 (aq) ==> SO2(g) + CuO(s)

If you smelled any SO2 fumes, that's what happened!  In a hot Bunsen burner flame, you are getting near 600°C.
 
 
One more thing, on the "human" side again - be careful not to round numbers too much during calculations.  I've seen students round off numbers like 1.14 g to 1.1 g, or worse, 1.42 g to 1 g. This really affects the calculation!  This rounding may be justified "mathematically" speaking, but it's best to not round numbers during calculations, just round off the final answer at the end, to avoid accumulating "roundoff error".  Use a formula weight of 159.609 g/mol in your calculation, not 160, etc., just to be on the safe side!
 

Steve

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 Message 5 of 7 in Discussion 
From: MSN NicknameP_5z3Sent: 10/12/2004 2:21 AM
hiii....How does the decomposition of the CuSO4 affect the loss of weight?...like what does the decomposition of the compound have to do with the mass?
 
Thank you!!

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 Message 6 of 7 in Discussion 
From: MSN Nickname·Steve·Sent: 10/12/2004 3:10 AM
I believe the high temperature decomposition reaction would be
 
2CuSO4(s)   -->  2CuO(s)  +  2SO2(g)  +  O2(g)
 
So, there would be additional loss of weight due to the loss of gaseous SO2 and O2, just as the weight decreased when the H2O was driven off.  This would give a greater weight loss after heating, resulting in a higher calculated amount of water in the hydrate.  The remaining solid decomposition product, cupric oxide, is a nearly black solid, so if any formed, even in small amount, it would darken the remaining anhydrous CuSO4 and be very evident.  But if your anhydrous product was still near white, then it's probably safe to say that high temperature decomposition did not occur.
 
Steve

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 Message 7 of 7 in Discussion 
From: MSN Nickname·Steve·Sent: 10/14/2004 7:27 PM
I tried using CuSO4 with my chemistry class in lab today, and indeed, decomposition was quite a problem if the crucible was heated too strongly.  In those cases the anhydrous solid was quite blackened, especially on the bottom and around the edge, and the weight loss was in some cases more than twice what it should have been.  So I think there is a very good chance this is what happened with yours also.  Clearly, CuSO4 requires gentle heating!
 
Steve

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