TITLE

The Gravimetric Determination of Chloride

OBJECTIVE

The objectives of this experiment are:

1. List down the important factors which effect the crystallinity/size of precipitate.
2. Describe the steps to be taken to ensure that the precipitates formed are large and easily
filtered and avoid peptisation.
3. Carry out the gravimetric experiment confidently.
4. Calculate the theoretical yield of a product.
5. Calculate the percentage yield of a product.

INTRODUCTION

Gravimetric analysis is a technique through which the amount of an analyte (the ion being
analyzed) can be determined through the measurement of mass or concentration. Gravimetric
analyses depend on comparing the masses of two compounds containing the analyte. The
principle behind gravimetric analysis is that the mass of an ion in a pure compound can be
determined and then used to find the mass percent of the same ion in a known quantity of an
impure compound. In order for the analysis to be accurate, certain conditions must be met:

1. The ion being analyzed must be completely precipitated.

2. The precipitate must be a pure compound.
3. The precipitate must be easily filtered.

An example of a gravimetric analysis is to determine the amount of chloride ion in a

compound. It is one of the most common methods employed in lab. Any inorganic compound
containing halogen can be made into aqueous solution and treated by silver nitrate to obtain
the precipitates of silver halide. In this experiment, chloride was used as the test sample. The
reaction involved is as follows:

𝐴𝑔+ (𝑎𝑞) + 𝐶𝑙 − (𝑎𝑞) → 𝐴𝑔𝐶𝑙(𝑠)

The silver chloride precipitate initially forms as a colloid, which is coagulated with heat.
Nitric acid and a small excess of silver nitrate aid coagulation by providing a relatively high
electrolyte concentration. The solution is kept slightly acidic during the precipitation step to

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eliminate possible interference from anions of weak acids (for example, 𝐶𝑂3 2− ). These anions
form slightly soluble silver salts in neutral solution. Nitric acid is added to the wash liquid to
maintain a high electrolyte concentration and to prevent peptization during the washing step.
(Peptization is the formation of a colloid by dispersion of a precipitate. Colloids pass through
filter crucibles while precipitates do not). The excess acid is volatized during the subsequent
heat treatment. Finally, the precipitate is collected in a previously weighed filtering crucible,
washed, and brought to constant mass at 110°C.

In addition to possible interferences to all gravimetric methods, the presence of any other
halide will cause high results since they produce a silver halide which is even more insoluble
than silver chloride. Also, silver chloride is light sensitive and excessive photodecomposition
will produce erroneous results, according to the reaction:

2𝐴𝑔𝐶𝑙(𝑠) → 2𝐴𝑔(𝑠) + 𝐶𝑙2 (𝑔)

The precipitate becomes violet-purple, due to the presence of finely divided silver metal, and
results will be low. If silver ion, Ag+ is present, in addition to the above, the following reaction
will also occur as a result of the photodecomposition reaction:

3𝐶𝑙2 (𝑎𝑞) + 3𝐻2 𝑂(𝑙) + 5𝐴𝑔(𝑎𝑞) → 5𝐴𝑔𝐶𝑙(𝑠) + 𝐶𝑙𝑂3 (𝑎𝑞) + 6𝐻 + (𝑎𝑞)

If this reaction predominates, the results will be high. To minimize such errors, it is
recommended any unnecessary exposure to light.

The advantages of gravimetric analysis is that, if methods are followed carefully, provides
for exceedingly precise analysis. In fact, gravimetric analysis was used to determine the atomic
masses of many elements to six figure accuracy. Gravimetry provides very little room for
instrumental error and does not require a series of standards for calculation of an unknown.
Also, methods often do not require expensive equipment. Gravimetric analysis, due to its high
degree of accuracy, when performed correctly, can also be used to calibrate other instruments
in lieu of reference standards.

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METHODS

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REFERENCES

http://www.wiredchemist.com/chemistry/instructional/laboratory-tutorials/gravimetric-
analysis

https://en.wikipedia.org/wiki/Gravimetric_analysis

https://www.ukessays.com/essays/biology/gravimetric-determination-of-chloride-biology-
essay.php

http://www.mtsu.edu/chemistry/chem2230/pdfs/Exp%202.pdf

https://www.scribd.com/doc/47085012/Experiment-Gravimetric-Analysis