Name: Shenique Campbell PAGE: ……

EXPERIMENT NUMBER: 5 DATE: March 13, 2021

DETERMINATION OF WATER OF CRYSTALLISATION IN FeSO 4•xH2O

INTRODUCTION:
The aim of this experiment is to find the value of x in the hydrated salt, FeSO4•xH2O,
using two methods – gravimetric analysis and a redox titration. The accuracy of the two
methods is to be evaluated at the end of the experiment.

BACKGROUND:
1. Explain why each method can be used to determine the value of x in the hydrated iron(II)
sulfate.
Gravimetric:
Gravimetric analysis is a class of lab techniques used to determine the mass or concentration of a substance by measuring a change
in mass. Volatilization gravimetry involves separating components of our mixture (hydrated iron(ll) sulfate) by heating or
chemically decomposing the sample. The heating or chemical decomposition separates out any volatile compounds (water), which
results in a change in mass that we can measure.
Redox titration:
Redox titration (also called an oxidation-reduction titration) can accurately determine the concentration of an unknown analyte
(unknown concentration of iron (II) ions (Fe2+)) by measuring it against a standardized titrant (Potassium Permanganate
(KMnO4)).

2. Predict which of the two methods will be more accurate in determining the value of x in the
hydrated iron(II) sulfate.
Redox Titration

MATERIALS:
List the materials and equipment needed for this experiment.
Electrical Balance, Hydrated Iron(II) Sulfate, Oven, Crucible, Paper Towel.

RISK ASSESSMENT:
Based on the procedure, identify any hazards associated with the experiment.
State how these hazards can be reduced.

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Chemical/Apparatus Hazard Risk Precaution
Oven Heat: close oven racks can High Proceed with caution when
cause burns with contact with placing and removing the
skin crucible.
Iron sulphate Irritant: to the eyes, skin & Low Wear safety glasses
respiratory system (goggles)
Avoid contact with skin.

PROCEDURE:
Method I – Gravimetric Analysis
1. The crucible was weighed and the mass recorded.
2. Between 1.30g and 1.80g of hydrated iron(II) sulfate crystals was added to the crucible and the new mass recorded.
3. The crucible containing the hydrated salt was placed in the oven and heated for 2-3 hours.
4. The crucible was allowed to cool.
5. The crucible and its contents were weighed.
6. Steps 3 -5 was repeated.
DATA:
Design tables to collect the data
Method I – Gravimetric Analysis
Before Placed in the Oven After Placed in the Oven
Mass of crucible (g) Mass of crucible and hydrated salt (g) Mass of crucible and anhydrous salt (FeSO4) (g)
17.63 18.99 18.51

ANALYSIS:
A. Mass of hydrated salt (FeSO4•xH2O):
= Mass of crucible and hydrated salt - Mass of crucible
= 18.99g – 17.63g
= 1.36g
B. Mass of anhydrous salt (FeSO4):
= Mass of crucible and anhydrous salt (FeSO4) - Mass of crucible
= 18.51g – 17.63g
= 0.88g
C. Mass of water:
= Mass of hydrated salt (FeSO4•xH2O) - Mass of anhydrous salt (FeSO4)
= 1.36g – 0.88g

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= 0.48g
D. Number of moles of FeSO4
Using molar mass of FeSO4 to be 151.91gmol-1
= Mass of FeSO4/ molar mass of FeSO4
= 0.88g/ 151.91gmol-1
= 0.0058mol
E. Number of moles of H2O:
Using molar mass of H2O = 18gmol-1
= mass of H2O/ molar mass of H2O
= 0.48g/18gmol-1
= 0.0267mol
F. Dividing by the smallest mole ratio
FeSO4 H2O
=0.0058mol/0.0058mol = 0.0267mol/0.0058mol
=1 = 4.6
= 5 rounded to the nearest whole number.

DISCUSSION:
Questions to guide the discussion and conclusion:
 What could have caused the value you calculated in each method to differ from the expected value?
 What assumptions did you make in your analysis?
 Which method was better to determine the value of x?
Justify your answer with data.

Gravimetric analysis is a class of lab techniques used to determine the mass or concentration of a substance by measuring a
change in mass. The chemical we are trying to quantify is sometimes called the analyte. Volatilization gravimetry involves
separating components of our mixture by heating or chemically decomposing the sample. The heating or chemical decomposition
separates out any volatile compounds, which results in a change in mass that we can measure. Using this method, the water of
crystallisation was determined to be 5. However, this value is 2 less than the expected value 7. Various conditions may have affected
this value which are as follows:

 The storage temperature of the sample.

 Amount of sample and surface area of the sample in contact with the air and heat in the oven, which varies by using
containers of different diameters.

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 The sample was not given enough time for the water to evaporate.

Additionally, it was also assumed during the experiment:

 All mass lost from the sample is from evaporated H2O, as opposed to some other decomposition process.
 All the water is coming from the dehydration of (FeSO4•xH2O).

Compared to the redox method where the value for the water of crystallisation was determined to be 7 as opposed to the gravimetric
where it was determined to be 5, the redox method was better to determine the value of x. The redox method required a shorter time
and obtained more accurate results based on the calculations for the expected value of x.

CONCLUSION: Restate your results

The redox method is more accurate compared to gravimetric analysis in finding the water of crystallisation for hydrated
iron (II) sulphate as the value obtained was closer to the expected value 7.

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