CHY610S LAB TWO

Name: Profile Gottlieb

Course: Chemical Engineering
Student Number: 223046922
Lecturer: Mr B. Sililo
Table of Contents
1. Abstract.......................................................................................................................................... 3
2. Introduction ................................................................................................................................... 3
Background ....................................................................................................................................... 3
Purpose .............................................................................................................................................. 3
Aims & Objectives ............................................................................................................................ 3
3. Materials & Reagents ................................................................................................................... 3
Materials ............................................................................................................................................ 3
Reagents ............................................................................................................................................. 4
4. Procedure ....................................................................................................................................... 4
Sample Preparation .......................................................................................................................... 4
Precipitation ...................................................................................................................................... 5
Filtration and Washing ..................................................................................................................... 5
Drying and Weighing ........................................................................................................................ 5
5. Results ............................................................................................................................................ 6
6. Discussion....................................................................................................................................... 6
7. Conclusion ..................................................................................................................................... 6
8. Recommendations ......................................................................................................................... 6
9. Post Lab Questions ....................................................................................................................... 7
References .............................................................................................................................................. 9
 1. Abstract
This experiment determines the amount of sulphate in a solid sample using gravimetric
analysis. Sulphate is precipitated as barium sulphate (BaSO4), separated, dried, and weighed.
The mass of BaSO4 is used to calculate the sulphate content in the original sample. Key steps
include sample dissolution, sulphate precipitation, filtration, washing, drying, and weighing the
BaSO4.

2. Introduction
Background

Gravimetric analysis is a quantitative method that involves isolating and weighing a compound
in a pure form. In this experiment, sulphate ions in a solid sample are precipitated as barium
sulphate (BaSO4) by the addition of barium chloride (BaCl2). The precipitate is then filtered,
washed, dried, and weighed. The mass of the BaSO4 is directly proportional to the amount of
sulphate in the original sample.

Variations in acidity, temperature, the manner of adding the precipitant, and digestion time can
significantly affect the filterability and purity of the barium sulphate precipitate. Foreign ions
can interfere with the precipitation.

Purpose

The purpose of this experiment is to accurately determine the amount of sulphate in a solid
sample using gravimetric analysis. This involves obtaining a high-quality barium sulphate
precipitate, which is essential for accurate quantification.

Aims & Objectives

• To determine the sulphate content in a solid sample.

• To perform gravimetric analysis through the precipitation of sulphate as barium
sulphate.
• To optimize conditions for obtaining pure and filterable barium sulphate precipitates.
• To accurately weigh the final precipitate and calculate the sulphate content.

3. Materials & Reagents

Materials

• Crucibles
• Filter paper (Whatman 40)
• Hot plates
• Desiccator
• 100 mm Watch glasses
• Stirring rods
 • 400 mL Beakers
• Glass funnels
• Wooden funnel holder
• Oven
• Marking paper
• Thermometers
• Burettes
• Rubber policeman
• Burners
• Tripods
• Tongs

Reagents

• Distilled water
• 6 M HCl solution
• 5% barium chloride (BaCl2) solution
• Silver nitrate (AgNO3) solution

4. Procedure
The procedure followed is based on the lab manual, with the specified differences in materials
and reagents.
Sample Preparation

1) A crucible was weighed. A filter paper was weighed. A filter paper and sample were
weighed. 50.1 ml of distilled water was added to the sample.
2) A 100 mm watch glass, a stirring rod, and a 400 mL beaker were washed.
3) The glassware was rinsed with tap water and then with distilled water.
4) The beaker was labelled.
5) The beaker was covered with a watch glass and stored until needed.
6) The unknown sample was transferred to a clean beaker and covered with a dry watch
glass.
7) The sample was dried in a 105−110°C oven for at least one hour.
8) The dried sample was stored in a desiccator until cooled to room temperature.
9) Approximately 0.35 g (+-0.0001 g) of the dried sample was weighed into the prepared
beaker.
10) 50 mL of distilled water and 5 mL of 6 M HCl were added to the sample, followed by
200 mL of distilled water.
11) The beaker was covered with a 100 mm watch glass and stored until the next step.
Precipitation

1) The sample solution was heated to approximately 90°C on a hot plate.

2) 5% barium chloride (BaCl2) solution was added dropwise from a burette. The initial
volume of BaCl2 in the burette was 65.1 ml. The temperature of 20 ml of BaCl2 was
74°C.
3) After approximately 15-20 mL of BaCl2 solution was added, the precipitate was
allowed to settle for 12 minutes. The volume of the mixture during settling was 275 ml.
4) The completeness of precipitation was tested by adding a few more drops of BaCl2
solution. The temperature of the solution prior to this addition was 56°C. Eight
additional drops of BaCl2 were added. The total volume of BaCl2 solution added was
21 ml.
5) The beaker was covered, and the solutions were heated on a hot plate for one hour at
approximately 90°C to aid in the digestion of the precipitate.

Filtration and Washing

1) A glass funnel and a wooden funnel holder were obtained.

2) The funnel was cleaned and supported in the holder above the labelled beaker.
3) An ashless Whatman #40 filter paper was inserted into the funnel.
4) 200 mL of distilled water was heated to 80°C for washing the precipitate.
5) The supernatant was decanted through the filter paper.
6) The precipitate was transferred into the filter paper with hot distilled water, using a
rubber policeman to ensure complete transfer.
7) The precipitate in the funnel was washed with three 5 mL portions of hot distilled water.
8) Each washing was collected separately in a small, clean beaker, and two drops of
AgNO3 solution were added to test for the presence of chloride ions.
9) The filter paper containing the precipitate was removed from the funnel, folded, and
placed in a crucible.
10) The identity of the sample in the crucible was recorded.

Drying and Weighing

1) The crucible was supported on a tripod, and heating was started with a small flame.
2) The flame was moved around to heat all parts of the crucible evenly.
3) The flame size was gradually increased, avoiding strong heating that could ignite the
filter paper.
4) Once the paper was charred, the flame temperature was increased.
5) The flame was moved as needed to heat all parts of the crucible strongly.
6) When all carbon residue was removed, the temperature was maximized by positioning
the tip of the blue cone of the flame just below the crucible wall.
7) The crucible was heated in this manner for ten minutes.
8) The crucible was allowed to cool for a few minutes before being placed in a desiccator
to cool to room temperature.
9) The cooled crucible was weighed.
10) The heating, cooling, and weighing process was repeated until successive weights
agreed to within 0.2 mg.
 5. Results
Weight of crucible: 39.45 g
Weight of filter paper: 0.84 g
Weight of filter paper + sample: 1.53 g
Weight of sample: 1.53 g - 0.84 g = 0.69 g
Volume of distilled water used: 50.1 ml
Initial volume of BaCl2: 65.1 ml
Volume of BaCl2 added: 21 ml
Temperature of 20 ml of BaCl2: 74°C
Volume of mixture during precipitate settling: 275 ml
Temperature prior to adding drops of BaCl2 to test for completeness: 56°C
Time waited for precipitate to settle: 12 mins
Temperature of mixture after one hour: slightly over 90°C

6. Discussion
During the ashing process, the filter paper charred more than expected, and some sample fell
out of the paper into the crucible. Possible reasons for excessive charring include excessive
heating rate where the flame was too large, or the heating was too rapid. A non-specified filter
paper might have been used instead of the specified ashless filter paper, affecting its burning
characteristics. The loss of sample during ashing could have affected the results by
underestimation of Sulphate where the final weight of the precipitate would be lower than the
actual amount. Losing precipitate directly affects final calculations, making the results
inaccurate.

7. Conclusion
The experiment aimed to determine the sulphate content of a solid sample. A procedural error
during ashing resulted in sample loss, likely underestimating the sulphate content. Future
experiments should carefully control the heating rate during ashing and use the correct type of
filter paper. The objectives of determining the sulphate content were partially met, but the
accuracy was compromised by the procedural error.

8. Recommendations
• Carefully control the heating rate during the ashing process to prevent excessive
charring and sample loss.
• Ensure that the correct type of ashless filter paper is used.
• Implement a more careful transfer technique to prevent any loss of precipitate during
filtration and washing.
• Use a larger crucible to provide more space and reduce the risk of sample loss during
ashing.
9. Post Lab Questions
1. Approximately how many mL of 5% BaCl2⋅2H2O solution would be required to
precipitate all the sulphate if we assume that your samples are pure calcium
sulphate? Assume that the density of the barium chloride solution is 1.00 g/mL.

To answer this, we need to use stoichiometry. The balanced equation for the reaction
is: CaSO4(aq)+BaCl2(aq)⟶BaSO4(s)+CaCl2(aq)

The mole ratio of CaSO4 to BaCl2 is 1:1.

o First, calculate the moles of CaSO4:

▪ The molar mass of CaSO4 is 136.14 g/mol.
▪ From the "Results" section, the mass of the sample is 0.69 g. However,
the question asks us to assume the sample is pure calcium sulphate.
We'll use 0.35g as a theoretical value, as the lab manual suggests this
amount.
▪ Moles of CaSO4 = (0.35 g) / (136.14 g/mol) = 0.00257 mol
o Since the mole ratio is 1:1, we need 0.00257 mol of BaCl2.
o The molar mass of BaCl2⋅2H2O is 244.26 g/mol.
o Mass of BaCl2⋅2H2O needed = (0.00257 mol) * (244.26 g/mol) = 0.6277 g
o The barium chloride solution is 5%, meaning 5 g of BaCl2⋅2H2O is in 100 mL
of solution.
o Volume of 5% BaCl2 solution needed = (0.6277 g) / (5 g/100 mL) = 12.55 mL

Therefore, approximately 12.55 mL of 5% BaCl2⋅2H2O solution would be required.

2. If the samples were pure potassium sulphate, would you require a smaller or
larger volume of barium chloride solution than the amount calculated in 1. above?

The balanced equation for the reaction is: K2SO4(aq)+BaCl2(aq)⟶BaSO4(s)+2KCl(aq)

The mole ratio of K2SO4 to BaCl2 is 1:1.

o First, calculate the moles of K2SO4:

▪ The molar mass of K2SO4 is 174.25 g/mol.
▪ We'll use 0.35g as a theoretical value
▪ Moles of K2SO4 = (0.35 g) / (174.25 g/mol) = 0.00201 mol
o Since the mole ratio is 1:1, we need 0.00201 mol of BaCl2.
o Mass of BaCl2⋅2H2O needed = (0.00201 mol) * (244.26 g/mol) = 0.4909 g
o Volume of 5% BaCl2 solution needed = (0.4909 g) / (5 g/100 mL) = 9.82 mL

Comparing this to the 12.55 mL calculated for calcium sulphate, we would require a
smaller volume of barium chloride solution for potassium sulphate. This is because, for
the same mass, potassium sulphate has fewer moles than calcium sulphate, and since
the reaction is 1:1, we need fewer moles of barium chloride.

3. If ordinary filter paper, instead of ashless paper, were used, how would your
experimental results be affected? Would they be too high or too low?
 If ordinary filter paper were used, the experimental results would be too high. Ordinary
filter paper contains cellulose, which, when burned, leaves a residue of ash. This
additional ash would add to the measured mass of the BaSO4 precipitate, leading to an
overestimation of the amount of sulphate in the original sample. Ashless filter paper is
specifically designed to leave a negligible residue upon ignition.

4. Why are the washes of the barium sulphate tested with AgNO3?

The washes of the barium sulphate precipitate are tested with AgNO3 (silver nitrate) to
check for the presence of chloride ions (Cl−). Barium chloride (BaCl2) is used to
precipitate the sulphate, and it's important to ensure that all excess chloride ions are
washed away. Silver nitrate reacts with chloride ions to form a white precipitate of
silver chloride (AgCl):

Ag+(aq)+Cl−(aq)⟶AgCl(s)

The presence of this white precipitate indicates that chloride ions are still present in the
washings, meaning that washing must continue to ensure the purity of the BaSO4
precipitate.

5. Does the solubility of BaSO4 increase significantly as the temperature of the

solution is increased?

The solubility of BaSO4 does increase with temperature, but not very significantly.
BaSO4 is generally considered quite insoluble in water, and while increased
temperature will cause a slight increase in solubility, the change is not large enough to
cause substantial errors in this experiment, especially considering the digestion process
is done at 90ºC, and the washings are done with hot water.

6. What are the most important errors in this procedure?

o Incomplete Precipitation: If not all the sulphate ions are precipitated, the
results will be too low. This can be caused by insufficient addition of BaCl2.
o Loss of precipitate: Any loss of the BaSO4 precipitate during transfer,
filtration, washing, or ashing will lead to a low result.
o Errors in weighing: Inaccurate weighing of the sample or the final precipitate
will directly affect the results.
o Filter paper errors: Using non-ashless filter paper, or losing sample during the
ashing process.

7. From your answer to question 6 above, would you say that the procedure for the
sulphate analysis is likely to give results that are too high or too low?
o Results that are too high are most likely.
 References
• Department of Mining and Process Engineering. (2018). Chemistry 215, CHY 610s
gravimetric sulphate determination practical 1. Namibia University of Science and
Technology.
• Seely, O. (2019, January 15). Gravimetric sulfate determination. LibreTexts.
https://chem.libretexts.org/Ancillary_Materials/Laboratory_Experiments/Wet_Lab_E
xperiments/Analytical_Chemistry_Labs/Gravimetric_Sulfate_Determination