Experiment 2

Gravimetric Analysis
Introduction
Gravimetric analysis is one of the most important methods of quantitative chemical
analysis. It is based on accurate measurement of the weight of the analyte or some compound
chemically related to it (Reger, Goode, & Bali, 2010). The substance whose composition or
concentration is being investigated is converted to an insoluble, stable and pure compound which
can readily be converted into a form suitable for weighing. The weight of the element is easily
calculated from the knowledge of the formula of the compound and the atomic weights of the
constituent element (Khopkar, 1998). If methods are conducted carefully, gravimetric analysis
provides for exceedingly precise analysis. However, a slight misstep in the procedure leads to
discrepancies in the result. The steps commonly followed in gravimetric analysis are (1)
preparation of a solution containing a known weight of the sample, (2) separation of desired
constituent, (3) weighing of the isolated compound and (4) computation of the amount of the
sample from the observed weight of the dissolved substance.
There are three types of gravimetric analysis namely volatilization gravimetry,
electrogravimetry and precipitation gravimetry. Volatilization gravimetry converts the analyte
into a gas of known chemical composition whereas electrogravimetry separates the analyte by
deposition through the use of an electric current (Skoog, West, Holler, & Crouch, 2014). In this
experiment, precipitation gravimetry was used. It is where the analyte is separated from a
solution of the sample as a precipitate and is converted to a compound of known composition
that can be weighed. Precipitate formation can either be nucleation where colloidal suspensions

are favored or particle growth where a crystalline suspension predominates. Chances of forming
one of this are influenced by the precipitate solubility, temperature, reactant concentration and
the rate at which reactants are mixed. Colloidal suspensions are tiny particles (10 -7 to 10-4 cm in
diameter) which show no tendency to settle nor are they easily filtered.

Unlike colloids,

crystalline suspensions tend to settle spontaneously and has dimensions bigger than colloidal
suspension (tenths of a millimeter or greater). Controlling the particle size could be made by
adjusting the variables in the relative supersaturation equation.

Relative supersaturation=

QS
S

The most common filtering medium is a cellulose-based filter paper which is classified
according to its filtering speed, its size, and its ash content on ignition (Rattenbury, 1966).
Filtering speed is a function of the papers pore size which determines the particle sizes retained
by the filter. The rate of filtering of the filter paper is classified as fast (retains particle size> 2025mm), medium fast (retains particles>16mm), medium (retains particles>8mm) and slow
(retains particles> 2-3mm). Proper choice of filtering speed is important since if the filtering
speed is too fast, the precipitate may pass through the filter paper. A slow filter paper, on the
other hand, may cause clogging of the filter paper.
Filter paper is hygroscopic and is not easily dried to a constant weight. Thus the use of
low ash filter paper is encouraged in quantitative analysis. A quantitative low ash filter paper,
having an ash content of 0.0010% w/w, is pretreated by washing with a mixture of HCl and HF
to remove inorganic material. The filter paper must be removed through ignition before weighing
the precipitate. If the filter paper is not a low ash, the result is a residue of noncombustible
inorganic ash that contributes a positive determinate error to the precipitates final mass. A

determinate or systematic error causes the mean of the data set to differ from the accepted value
influencing the accuracy of the result (Skoog, West, Holler, & Crouch, 2014). A positive
determinate error is then characterized by an increase in the value of the data from the accepted
value.
Furthrmore, when the analyte is converted to precipitate, constant weighing must be
achieved. All solids have a certain affinity to water (hygroscopic) thereby causing an increase in
the weight of the analyte (Reger, Goode, & Bali, 2010). Thus, it is of prime importance that a
sample should be dried to a constant in a crucible of known weight. This is conducted through
the help of a desiccator. A desiccator is an essential piece of apparatus in gravimetric analysis.
The lower compartment is filled with a drying agent. Granular or fused anhydrous calcium
chloride is often used as a desiccant but silica gel is more effective and may be regenerated by
heating at a temperature range of 150C to 180C. Silica gel is impregnated with a cobalt salt.
When the gel is no longer capable of taking up moisture, the cobalt becomes hydrated and so
changes color from blue to pink. Vaseline is applied on the lid of the desiccator so as to make it
airtight and enabling the lid to slid off easily.

References

Khopkar, S. (1998). Basic Concepts of Analytical Chemistry. New Delhi: New Age
international(p) Limited, Publishers.
Rattenbury, E. M. (1966). Introductory Titrimetric and Garvimetric Analysis. Oxford: Pergamon
Press Ltd.
Reger, D. L., Goode, S. R., & Bali, D. W. (2010). Chemistry: Principles and Practice. Australia:
Cengage Learning.
Skoog, D. A., West, D. M., Holler, F. J., & Crouch, S. R. (2014). Fundamentals of Analytical
Chemistry. Philippines: Cengage Learning Asia Pte Ltd.