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Determination of sulfate as barium sulfate

Determination of sulfate as barium sulfate

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Published by Saad Ahmed

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Published by: Saad Ahmed on Oct 17, 2012
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10/24/2013

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University Of Karachi
CHEMICAL PROCESS TECHNOLOGY 
 
(Practical file)
 
Syed Saad Ahmed B-0933040B.E 3
rd 
Year Chemical EngineeringSubmitted To:
Ma’am Khehkashan
 
 
CHEMICAL PROCESS TECHNOLOGY 
2012
2
 
Prepared By: Syed Saad Ahmed
| B.E Chemical Engineering
Experiment no. 2
OBJECT:
Determination of sulfate as barium sulfate
APPARATUS AND REAGENTS:
 
250 ml beaker.
 
Bunsen burner, Water bath, Muffle furnace.
 
Crucible.
 
0.2 M barium chloride.
 
Potassium sulfate.
 
Concentrated hydrochloric acid.
THEROY:
A sample containing an alkali sulfate is dried, weighed and dissolved in dilute HCl.Barium chloride solution is added in excess to precipitate barium sulfate, and the precipitate isdigested in the hot solution. The precipitate is filtered through a paper filter which is thenignited and completely ashed. From the weight of the sample and weight of the precipitate, thepercentage of sulfate in the sample is calculated. The precipitation reaction is the following:






 Variations in the acidity, temperature, manner of addition of the precipitant and time ofdigestion markedly affect the filterability of the barium sulfate precipitate and the extent towhich various foreign ions are co-precipitated. Foreign anions such as nitrate, chlorate andchloride are co-precipitated as their barium salts, and the ignited precipitate contains the salt oroxide as an additive impurity. The co-precipitation of chloride can be decreased by slowaddition of the precipitant. Since nitrate and chlorate interfere even at low concentrations, theyshould be removed from the solution before precipitation.
PROCEDURE:
Weight out accurately 0.5 grams of Potassium sulfate and transfer it to 250 ml beaker.Dissolve the solid in about 25 ml of water and add 0.5-1 ml of concentrated
HCl
and dilute toabout 200 ml. Heat the solution to boiling, add drop wise 15-20 ml of 0.2M
BaCl
2
.H 
2
O
. Stir thesolution constantly during the addition. Allow the precipitate to settle for 4-5 minutes. Then testthe supernatant liquid for complete precipitation by adding a few more drops of Bariumchloride solution. If a precipitate is formed add slowly a further 3-5 ml of the
BaCl
2
solution.
 
CHEMICAL PROCESS TECHNOLOGY 
2012
3
 
Prepared By: Syed Saad Ahmed
| B.E Chemical Engineering
Allow the precipitate to settle as before and test again. Repeat this operation until an excess of
BaCl
2
is present. Keep the covered solution hot, but not boiling for an hour on water bath inorder to allow time for complete precipitation. Filter off the precipitated barium sulfate througha weighed sintered glass crucible no. 4 and wash it with hot water until the chloride reaction ofthe washing is negative. Such that the precipitate dry on the pump for 3 minutes. Ignite theprecipitate in a crucible for 15 minutes at 600
o
C in the furnace.
CALCULATION:
Calculate amount of sulfate in Barium Sulfate:
Weight of empty crucible = 14.20 gWeight of empty crucible +
BaSO
4
= 14.78 gWeight of precipitate (
BaSO
4
) = 0.58 gMolecular weight of
BaSO
4
= 233.43 gAmount of
SO
4
in
BaSO
4
= 96.062 g
   
  
 
   
  
 
   
 
 
   
  
 
   
  
 
RESULT:
Amount of sulfate in 0.58 gm of

is found to be 0.2386 grams
THEORETICAL AMOUNT OF SO
4
IN K
2
SO
4
:
Molecular weight of
2
SO
4
= 174.259Molecular weight of
SO
4
= 96.062

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