FACULTY OF APPLIED SCIENCES

ANALYTICAL CHEMISTRY (CHM421) LAB REPORT

TITLE : DETERMINATION OF Fe IN A FERUM SOLUTION

BY

GRAVIMETRIC ANALYSIS

EXPERIMENT NO :8

NAME : ORNELLA LYNN JOSEPH

MATRIC NO. : 2020983037

GROUP : AS2464B

DATE OF EXPERIMENT : 9TH NOVEMBER 2020

DATE OF SUBMISSION : 14TH DECEMBER 2020

LECTURER’S NAME : DR KHAIRIL ANUAR BIN JANTAN

ABSTRACT

In this experiment, we are going to conduct calculation to find the ferum’s percentage
from a solution containing ferum. The method of filtration is used to determine the mass of
ferum. In this part, gravimetric analysis is completed through the usage of filtration method in
order to get the filtrate then proceeded to pour the filtrate into a crucible which then is
inserted in a furnace to be heated at 300°C overnight. The purpose of heating process is to
make sure the filter paper is completely burnt to obtain the precipitate only. Last but not least,
the precipitate is weighed to conduct the calculation for the percentage of ferum in a ferum
solution. Based on the experiment being carried out, the weight of precipitate obtained is
20.2513g whereas the weight percent % (w/v) obtained for this experiment is 56.65 %.

OBJECTIVE

1. To obtain the ferum’s percentage in a ferum solution.

INTRODUCTION

The method of volatilization and precipitation are both the general types of
gravimetric analysis in which the definition of gravimetric analysis is where based upon the
measurement of mass that can be generalized into two kinds. For the method of precipitation,
the quantitative determination of a substance consist of ion isolation in solution through a
reaction of precipitation, filtering, washing of precipitate so it is free from contaminants,
precipitate conversion to a product with a known composition and lastly weighing of
precipitate and determine the mass by differences. The quantity of original ion can be
determined based on the mass and known composition of the precipitate.

In order to have a successful determination, the substance needed must undergo a

complete precipitation process. Generally, most precipitation determinations are of such low
solubility that losses from dissolution which can be neglected. For instance:

Fe2+ ⟶ Fe3+

Fe3+ + O2- ⟶ Fe2O3

Solubility of Fe2O3 will be further reduced by Fe3+ excess that is added which pushes the
equilibrium to the right side. The product weight should be in known composition. So, the
calculation for mass of Fe in the solution can be conducted as Fe2O3 is a stable compound.
PROCEDURE

A. Precipitation
25 mL of ferum solution is pipetted into a 400 mL beaker then added with 25 mL
distilled water. Then, the beaker is covered with a watch glass. The solution is heated
until it boiled. 1 mL of concentrated HNO3 is added drop by drop. After that, solution
is continued to be heated until it became clear and proceeded diluting the solution
with 200 mL distilled water and it is boiled again. The beaker is transferred to the
bench and the solution is slowly added with 1:1 NH4OH then stirred until excessed.
This can be noticed when no more precipitate formed and steam odour can be
smelled.

B. Preparing a crucible
Crucible is cleaned and heated for 10 minutes. Then, it is cooled in a desiccator and is
correctly weighed.

C. Filtering and washing the precipitate

Precipitation underwent filtration through decantation by using method of
precipitation for gravimetric analysis without stirring the solution so it made sure
most of the precipitate could stay in the beaker. Then, the precipitate is washed with
30 mL warm 1% NH4NO3 solution. The solution is poured into a filter funnel while
leaving behind most of the precipitate. This process is repeated for three times and
finally all the precipitates are quantitatively transferred into the funnel. Lastly, using
warm distilled water, the precipitate is washed and the filtrate for chloride is tested
with acidic silver nitrate solution.

D. Drying and weighing the precipitate

The filter paper containing the filtrate is transferred into a crucible and is placed
inside a muffler furnace to be heated at 300°C overnight. The position of crucible is
recorded by using a piece of paper inside the furnace. When the process is done, the
crucible is cooled and the mass of precipitate is weighed. Lastly, the percentage of
ferum in the given solution is calculated.
RESULT

Weight of empty crucible = 39.9747g

Weight of crucible + precipitate = 60.2260g

Weight of precipitate = 20.2513g

CALCULATION

Mole of Fe3+ in sample = 25 mL (1 L/1000 mL) x (60.4 Fe/1 L) x (1 mol Fe/55.85)

= 0.02704 mol Fe

Mole of Fe2O3 (experimentally) = mass of solid Fe2O3 x molar mass of Fe2O3

= (20.2513 g) / (159.69 g/mol)

= 0.1268 mol

Based on equation:

2Fe2+ + 3/2 O2- ⟶ Fe2O3

2 mol Fe3+ : 1 mol Fe2O3

Mol of Fe3+ = 0.1268 mol x 2

= 0.2536 mol Fe

Mass of Fe3+ = mol of Fe x molar mass of Fe

= 0.2536 mol x 55.85 g/mol

= 14.1636 g

Weight percent % (w/v) of Fe3+ = Mass of Fe3+ (g)/ Volume of solution (mL) x 100%

= (14.1636 g/ 25 mL) x 100%

= 56.65 %
DISCUSSION

For this experiment, the determination of Fe in a ferum solution by gravimetric

analysis is done to obtain the percentage of ferum from the ferum solution. Gravimetric
analysis is a classic technique for assessing the mass of an analyte by precipitation and is
known to be more accurate than titrimetric analysis which is a form of quantitative analysis
used to assess the concentration of a product in a solution by the addition of a norm (titrant)
and to track the chemical reaction effects. This is because, titrimetric analysis is more to
depending on personal skills which is more likely to get more errors while gravimetric
analysis depends only on the heating process which have less errors and obtained good result
when it is heated completed.

Based on the equation, iron (II) ion is oxidized to iron (III) in order to form the
precipitate which is Fe2O3. The colour that is formed is intense brown colour when reacted
with NH4OH. Hence, the addition of NH4OH is to make it easier in distinguishing the
presence of visible colour. The amount of analyte from sample solution is found by relating
the mole ratio between theoretical mole of Fe in the sample which is 0.02704 mol and the one
obtained experimentally that is 0.2536 mol Fe. Therefore, the weight percent % (w/v) of
ferum obtained is 56.65 %. On the other hand, the amount of Fe contains in 20.2513g of
Fe2O3 is 14.1636 g.

In order to avoid errors or accidents, the steps must be taken carefully. For instance,
all the work that involves NH4OH must be conducted inside the fume cupboard so that the
smell of compound is not distributed in the lab. As for the precipitation process, it needs to be
done in chronological order where the steps are followed according to the gravimetric
analysis steps. This is due to lessen the outcome of analysis that is not desirable and to
achieve better result.
CONCLUSION

In conclusion, the weight and the percent weight % (w/v) of the precipitate can be
obtained accurately through the use of gravimetric analysis which in this experiment is
filtration. Hence, the ferum’s percentage found in a ferum solution is 56.65 %.

REFERENCES

1. Conductometric titration: An alternative to gravimetric analysis. (2019, February 11).

Vernier. Retrieved from, https://www.vernier.com/vernier-ideas/conductometric-
titration-an-alternative-to-gravimetric-analysis/
2. Hargis, L. G. (1988). Analytical chemistry: Principles and techniques. Pearson
College Division.
3. Gravimetric analysis. (n.d.). Retrieved from,
https://ion.chem.usu.edu/~sbialkow/Classes/3600/overheads/Gravimetry/gravimetric.
html
APPENDICES