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B.

Schematic Diagram

I. Constant Mass of Crucible


II. Gravimetric determination of Sulfate
III. Drying and Charring Process
Experiment 2
GRAVIMETRIC DETERMINATION OF SULFATE AS BARIUM SULFATE
A. INTRODUCTION

The objective of this experiment is to experimentally analyze an unknown analyte


via a precipitation reaction. This is most likely to be done by properly using relevant
techniques in precipitation and gravimetric analysis to collect and weigh the precipitate.
After the collection of data, analysts must be able to calculate the percentage by mass of
SO4-2 in the unknown sulfate solution through the aid of stoichiometry.

Gravimetric analysis is an analytical method used in determining the amount of a


substance accurately from an aqueous solution by selective precipitation. Through
filtration, the precipitate is separated from the filtrate or the remaining aqueous
solution and is then weighed after the process. The next general procedure in
gravimetric analysis is washing, followed by drying and/or ignition. If the chemical
formula for the precipitate is known and the precipitation reaction is complete, then the
mass of the substance in the original sample can be known.

In this experiment, sulfate solution and BaCl 2 solution will be utilized in analyzing
the concentration of sulfate from a sample solution. Sulfate is quite common in nature
and may be present in natural water with concentrations ranging from a few to several
thousand milligrams/liter. These are of considerable concern because they are indirectly
held responsible for two serious problems in handling and treatment of wastewater:
odor and sewer corrosion. This is a result from the reduction of sulfates to hydrogen
sulfide under anaerobic conditions.

A precipitation reaction occurs when a sulfate-containing solution is mixed with


barium-containing solution. This reaction forms barium sulfate, which precipitates as
very fine particles. For easier analysis, this precipitate undergoes digestion or
precipitate ageing, which happens when a freshly formed precipitate is left, usually at a
higher temperature, in the solution from which it precipitates. This results to a cleaner
and bigger particle which will be an advantage in weighing and filtration process.

The experiment will start off when a constant mass of crucible is observed, followed
by the determination of the mass of the sample. Then, a pre-weighed sample of the
unknown sulfate will be dissolved in water. A 50% HCl solution is then added to the
solution with 4.5 to 5 pH to increase the solubility of the BaSO4, which will result to a
decrease in the rate of precipitation. After that, aqueous barium chloride is added to the
sulfate solution which will then result to the precipitation of sulfate ions as barium
sulfate. This will be digested for about one hour to minimize error from the spilling of
precipitate.
In an aqueous solution, sulfate ion undergoes the following reaction with barium:
Ba2+(aq) + SO42-(aq) → BaSO4 (s) Ksp = Ba2+SO42− = 1.1x10−10 at 25 C

This barium sulfate precipitate is gathered through filtration, dried and weighed.
In the procedure, barium chloride is added in excess and the precipitation reaction goes
to completion. With this being stated, it can be assumed that all of the sulfate is
transferred from the original sample to the precipitate. After reaching a constant weight,
determination of the concentration of the sulfate as % BaSO4 can now be performed
using stoichiometry. This also yields to the mass of sulfate in the original sample since:

mass of sulfate in the precipitate = mass of sulfate in the unknown sample

Using the balanced chemical equation for the precipitation reaction, the moles of the
precipitate can be obtained by the equation:

moles = mass/molar mass

Then, the moles of analyte can be calculated from the balanced chemical equation using
the mole ratio of analyte: precipitate. From this, the mass of the analyte can be obtained
by the equation:

mass = moles x molar mass

The percent by mass of analyte in sample is also given by:

mass analyte
by mass= x 100
mass of sample
To obtain the best results, collected BaSo 4 crystals should be as large as possible.
This is mainly because larger crystals do not generally pass through the filter paper and
it also minimizes the amount of impurities adsorbed onto the crystals due to smaller
surface area. These large crystals are achieved through decreasing the rate of
precipitation, which is done by the slow addition of BaCl 2 solution to the sulfate solution
while continuously stirring the solution. Addition of HCl solution also contributes to the
decrease in the rate of precipitation.
Formulas to be used:

d́=
∑ di
n

x́=
∑ xi
n
C. Data Blanks
I. CONSTANT MASS OF THE CRUCIBLE
Table 2.1 Taring of crucible and cover
Condition Trial 1 Trial 2

Initial mass of crucible w/ lid, g

Mass of crucible w/ lid after 1st


heating, g

Mass of crucible w/ lid after 2nd


heating, g

Mass of crucible w/ lid after 3rd


heating, g

Mass of crucible w/ lid after 4th


heating, g

Mass of crucible w/ lid after 5th


heating, g

Constant mass of crucible w/ lid,


g (m1)
I. GRAVIMETRIC DETERMINATION OF SULFATE
Table 2.2 Constant weight of crucible and precipitate
Condition Trial 1 Trial 2

Mass of crucible and precipitate, g

Mass of crucible and precipitate


after 1st heating, g

Mass of crucible and precipitate


after 2nd heating, g

Mass of crucible and precipitate


after 3rd heating, g

Constant mass of crucible and


precipitate, g (m2)

Table 2.3 Determination of Sulfate


Condition

Volume of sample, mL

Mass of crucible and cover (from table


2.1, m1), g

Mass of crucible and precipitate (from


table 2.2, m2), g

Mass of barium sulfate, g (m2 – m1)

% Barium sulfate

x́ ± d́

% sulfate

x́ ± d́
References:
(n.d.). Retrieved from http://users.metu.edu.tr/chem223/Sulfate.pdf.
Libretexts. (2019, June 5). 7: Gravimetric Analysis (Experiment). Retrieved from
https://chem.libretexts.org/Bookshelves/Ancillary_Materials/Laboratory_Experi
ments/Wet_Lab_Experiments/General_Chemistry_Labs/Online_Chemistry_Lab_
Manual/Chem_11_Experiments/07:_Gravimetric_Analysis_(Experiment).
Stubbings, J. (n.d.). Gravimetric Analysis Tutorial. Retrieved from
https://www.ausetute.com.au/gravimetric.html.