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Solving for Mass of an Unknown Solution of BaSO4

Advanced Calculus Master

Experiment 1b: Gravimetric Determination of Sulfate Ion

An unknown sample mixture was cooled in a desiccator then measured out into four different
beakers; each measurement was around 0.3 to 0.4g. The sample was then dissolved in distilled
water and diluted HCl. The mixture was heated to boiling and about 10mL of 0.25M BaCl2 was
added to complete the precipitation reaction. The mixture was kept hot for at least 5 more
minutes before being stored for the next lab. After testing again for precipitation, four crucibles
were obtained by the stockroom and measured. Using a vacuum filtration system the mixture
was decanted through the crucible filter, then rinsed with a 6M HCl wash solution. To confirm all
the precipitation had been filtered, two to three drops of 3M H2SO4 was added to the filtrate.
Once confirmed, and clear, the four crucibles were placed in a beaker and covered with a watch
glass and dried in the oven at 120°C for approximately four days. The dried samples were then
measured again. After calculating the sample first delivered into each beaker, and the dry
resulting BaSO4, we calculated using stoichiometry the mass percentage of SO42- for each trial.
The average percent came out to be 58.43% SO42-

Purpose: This experiment aims to determine the mass percent of sulfate ion (SO42) in an
unknown sample using gravimetric analysis. Through this process, students will develop
essential laboratory skills such as accurate weighing, quantitative transfer, washing and drying of
solids, stoichiometric calculations, and applying simple statistical analysis to their results.

Background: Gravimetric analysis is a classical quantitative method where the mass of a

BaSO4^2−(aq)+HCl→BaSO4(s)

Once formed, the barium sulfate precipitate is filtered, washed to remove impurities, dried, and
weighed. Using the stoichiometry of the reaction and the measured mass of BaSO4, the mass of
sulfate in the unknown sample can be calculated.

Materials and Equipment:

Unknown sulfate sample (~2g), dried

Reagents: 6M Hydrochloric acid (HCl), 0.25M Barium chloride (BaCl2​), 3M Sulfuric acid
(H2SO4)

Equipment: Analytical balance (accurate to four decimal places), Drying oven and desiccator, 3
Selas crucibles, filter flask, and filtering apparatus, Hot plate, beaker tongs, stir rods, wire gauze,
and clamps, Graduated cylinders, watch glasses, polyethylene wash bottles, Medicine dropper,
laboratory burner

Methodology:

1.​ Preparation of the Unknown Sample: The unknown sulfate sample is dried in an oven
at 120°C overnight to remove any moisture. Proper drying technique involves placing the
sample in an open weighing bottle covered by a ribbed watch glass to prevent impurities
from entering, while allowing moisture to escape. The dried sample is then cooled in a
desiccator to avoid reabsorption of moisture .
2.​ Weighing the Sample: Using an analytical balance, three 0.3–0.4 g samples of the dried
unknown sulfate are weighed by difference. Each portion is transferred to a labeled 400
mL beaker without direct contact to avoid contamination .
3.​ Dissolving the Sample: Each sample is dissolved in a small volume of dilute
hydrochloric acid HCl in a beaker. The acid aids in dissolving the sulfate salts without
interfering with the precipitation of BaSO4.
4.​ Precipitating Sulfate Ions: A slight excess of barium chloride solution (BaCl2​) is slowly
added to each beaker while the solution is gently heated on a hot plate. This ensures the
complete precipitation of sulfate ions as BaSO4. The solution is kept warm to promote
coagulation and flocculation of the tiny BaSO4 particles .
5.​ Filtering and Washing the Precipitate: The precipitate is filtered using a crucible and
filter flask. The barium sulfate is then washed several times with a dilute acid wash to
prevent peptization, which could otherwise cause the solid to revert into a colloidal
suspension . Using dilute acid instead of water prevents the dissolution of BaSO4.
6.​ Drying and Weighing the Precipitate: The filtered barium sulfate precipitate is dried in
a crucible in a drying oven. After drying, it is cooled in a desiccator to prevent moisture
reabsorption before weighing. The final mass of dry BaSO4 is recorded for each trial.
7.​ Washing the Precipitate: Wash the precipitate with distilled water to remove excess
barium chloride. Use dilute acid instead of water to avoid peptization, which could turn
the solid BaSO₄ back into a colloidal suspension.
8.​ Drying the Precipitate:Place the crucibles with the precipitates in a 400 mL beaker
covered with a ribbed watch glass. Dry the samples in an oven at 120 °C for at least four
hours, or leave them overnight.
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9.​ Weighing the Precipitate: Cool the dried samples in a desiccator for 10 minutes. Weigh
the crucibles with the precipitated BaSO₄ and record the masses accurately to four
decimal places.
10.​Calculating the Mass Percent of Sulfate: Using the mass of BaSO₄ collected in each
trial, calculate the mass of sulfate ion based on the stoichiometric relationship between
BaSO₄ and SO₄²⁻. The mass percent sulfate in the unknown sample is then calculated
using the formula:

Materials and Methods:

1.​ Weighing of Samples: Three samples of the unknown were weighed and recorded.
2.​ Precipitation of Sulfate Ion: The unknown sample was dissolved and reacted with
barium chloride (BaCl2​) to precipitate the sulfate as barium sulfate (BaSO4).
3.​ Filtration and Drying: The precipitate was filtered, dried, and the mass of the dried
barium sulfate was recorded.

Experiment: On the first day of conducting this gravimetric analysis of the Sulfate ion. We
began by taking the dried unknown sample #109 covered by a ribbed watch glass out of
the oven which was set at 120°C. We then transferred the weighing bottle containing the
unknown sample to a CaSO4 desiccator and let the bottle sit with the glass top slightly
opened for 10 minutes. Once the sample was cooled we weighed the bottle on an
analytical balance and recorded the weight to 4 decimal places. We then numbered three
400 mL beakers as 1,2,3 for three 0.3-0.4 gram samples of the unknown. In beaker 1 the
sample weight was .3145g, in beaker 2 the sample weight came out to .4282g, and in
beaker 3 the sample weight was .3441g. The weights may vary from analytical balance to
analytical balance as this is not taking into account the chance for random error from the
instrument used. However this is what was measured in our experiment. To each sample
we added 50 mL of distilled water, then added 2 mL of 6M hydrochloric acid. To add it
we used a 10mL graduated cylinder. At first the sample was not dissolved completely so
we had to add 3-4 drops more of 6M hydrochloric acid to the samples. Then stirred until
the sample had been completely dissolved. After that, it was diluted with about 200 mL
of distilled water.
The sample was then heated to a boil and kept hot for this part of the experiment.It is
important to heat the solution to near boiling to increase the rate of reaction, but avoid
excessive boiling, which could cause the loss of the sample or lead to unwanted side
reactions. Next we obtained 10 mL of 0.25M barium chloride solution in the 10 mL
graduated cylinder. This will be the reagent used to precipitate barium sulfate from the
sulfate ions in our sample. Using a dropper, 2-3 drops of the barium chloride solution was
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added to the hot sample while stirring the solution with a stirring rod. It is important that
the stirring rod is used exclusively for this specific sample.
Barium sulfate is known for its distinctive white, crystalline appearance. Finally the
successful drying and weighing of the BaSO4 precipitate confirms that it was indeed the
result of the reaction between barium ions and sulfate ions. Any other possible
contaminants or side reactions were unlikely to have formed a precipitate under the
conditions used, further supporting the conclusion that barium sulfate was the only
product.
One common question that may arise is why use barium chloride specifically as the agent
for sulfate precipitation. Well barium chloride (BaCl2) is often used as a precipitating
agent in chemical experiments for several reasons, particularly when you're dealing with
the precipitation of sulfate ions (SO42) or other anions that form insoluble salts with
barium ions. BaCl2 is considered the best precipitating agent compared to other options.
Barium chloride is highly soluble in water, which makes it readily available for reaction
with other ions in the solution. This is essential for the complete precipitation of the
sulfate ions and ensures that sufficient barium ions (Ba2+) are available to react. It is also
important to note barium chloride is selective because barium ions specifically form an
insoluble precipitate with sulfate ions (BaSO4). The precipitation of BaSO4 occurs
almost exclusively with sulfate, while barium does not readily form precipitates with
many other common anions in solution outside of Calcium, Strontium, lead (II), silver,
mercury, and mercury(II). This makes BaCl2 a useful reagent when you need to isolate
sulfate ions from a mixture (Barium sulfate - Wikipedia). Because BaSO4 is highly
insoluble, it can be detected at very low concentrations of sulfate ions, which increases
the sensitivity of the experiment. This is especially useful in analytical chemistry when
you need to determine the presence of sulfate ions with a focus on accuracy (Barium
sulfate - Wikipedia).

Possible Alternatives: Possible alternatives that may be used in terms of determining the
presence of the sulfate ions could be calcium chloride, calcium chloride also reacts with
sulfate ions to form calcium sulfate (CaSO4), calcium sulfate is more soluble in water
than barium sulfate, meaning that the precipitation is less complete and might not be as
effective in a quantitative analysis (Calcium sulfate - Wikipedia). Another alternative
could be Sodium carbonate, Sodium Carbonate could be used to precipitate certain ions,
but it would primarily react with metal ions to form carbonates, not sulfate ions. Thus, it
is less effective for the precipitation of sulfate ions specifically. (Sodium carbonate -
Wikipedia). In essence barium chloride is the best precipitating agent in this type of
experiment because it selectively reacts with sulfate ions to form a highly insoluble
precipitate (BaSO4), ensuring a clear separation of the target anion from the solution.
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Data Collected

Sample Number 1, Mass of Sample .3145g, Mass of SO4 .4460g

Sample Number 2, Mass of Sample .4282g, Mass of SO4 .6034g

Sample Number 3, Mass of Sample .3441g, Mass of SO4 .4925g

From this data, calculate the mass percent sulfate for each sample, the average mass percent
sulfate, and the average deviation from the mean to determine the precision of the results.

Mass of precipitate * (1 mol of BaSO4/233.39g of BaSO4) * (96.06g of SO4/1 mol of SO4)

Percent mass of SO4 = mass of sulfate/(mass of unknown sample) * 100%

Calculations

Trial 1

.4460g * (1 mol of BaSO4/233.39g of BaSO4) * (96.06g of SO4/1 mol of SO4) = .1836g

Trial 2

.6034g * (1 mol of BaSO4/233.39g of BaSO4) * (96.06g of SO4/1 mol of SO4) = .2484g

Percent mass of SO4 2484g/.4282g * 100% = 58.00%

Trial 3

.4925g * (1 mol of BaSO4/233.39g of BaSO4) * (96.06g of SO4/1 mol of SO4) = .2027g

Percent mass of SO4 2027g/.3441g * 100% = 58.91%

Average Percent of mass of SO4 = ( 58.37%+58.00%+58.91%)/3 = 58.43%

PRECAUTIONS: Safety: Barium chloride (BaCl₂) is highly toxic, so proper handling and
immediate washing of hands after use is essential. Wear goggles and lab coats at all times.
Vacuum Filtration: Be cautious when using the vacuum filtration setup as the pressure
differences can lead to implosions. Always inspect the glassware for cracks and wear protective
eyewear.
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CONCLUSION:​
The gravimetric analysis experiment successfully determined the average mass percent of sulfate
ion (SO₄²⁻) in the unknown sample as 58.43%. This result was derived through precise weighing,
careful precipitation of sulfate ions using barium chloride, and accurate measurement of the
barium sulfate (BaSO₄) precipitate after drying. The calculated sulfate percentages across three
trials—58.37%, 58.00%, and 58.91%—demonstrated consistent precision, with a small deviation
from the mean, indicating reliable experimental procedures.

The stoichiometric relationship between BaSO₄ and SO₄²⁻, combined with proper drying,
washing, and filtration techniques, ensured the accuracy of the results. The selectivity of barium
chloride as a precipitating agent for sulfate ions minimized interference from other ions, further
supporting the validity of the findings. The precautions taken, such as the careful handling of
toxic reagents and proper use of filtration and drying apparatus, emphasized safety and
methodical laboratory practice.

Overall, the experiment highlights the effectiveness of gravimetric analysis as a classical and
precise quantitative method for determining sulfate content in a sample. The consistency in
results across trials and the rigorous methodology reinforce the experiment's success and its
utility in analytical chemistry for similar applications.
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Works Cited

Hill, John W., and Ralph H. Petrucci. General Chemistry: Principles and Modern Applications.

Pearson, 2014.​

“Barium Sulfate.” Wikipedia, Wikimedia Foundation, 2024,

https://en.wikipedia.org/wiki/Barium_sulfate.​

Lindsay, William L. Chemical Equilibria in Soils. Wiley, 2009.​

Skoog, Douglas A., et al. Fundamentals of Analytical Chemistry. 9th ed., Cengage Learning,

2014.