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Gravimetric Analysis 2

Gravimetric analysis is a quantitative analytical technique where the analyte is determined by weighing the precipitate or pure compound formed after a chemical reaction. There are different types including precipitation gravimetry, volatilization gravimetry, and electrogravimetry. The key steps involve preparing the test solution, precipitating the analyte, digesting and filtering the precipitate, drying or igniting it, and weighing to calculate the composition. Gravimetric analysis provides precise results but is limited to analyzing one element at a time.

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145 views25 pages

Gravimetric Analysis 2

Gravimetric analysis is a quantitative analytical technique where the analyte is determined by weighing the precipitate or pure compound formed after a chemical reaction. There are different types including precipitation gravimetry, volatilization gravimetry, and electrogravimetry. The key steps involve preparing the test solution, precipitating the analyte, digesting and filtering the precipitate, drying or igniting it, and weighing to calculate the composition. Gravimetric analysis provides precise results but is limited to analyzing one element at a time.

Uploaded by

Madhuri poulkar
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Gravimetric analysis

Gravimetric Analysis

It is the technique in which determination of amount of

analyte through precipitates or pure compounds


It is quantitative analysis in which the end product is weighed

and from that weight composition of analyte is determined.


Hence gravimetric analysis is based upon the measurement of

the weight of a substance of known composition which is


chemically related to the analyte
Types of Gravimetric Analysis:

Precipitation Gravimetry: This involves chemical


precipitation of the constituents.
Volatilization Gravimetry: In this method, the constituents are
decomposed due to volatilization at a suitable temperature
Electrogravimetry: This involves the electrochemical
reduction of the metal ions at the cathode and simultaneous
deposition of the metal ions at the cathode
Thermogravimetry: In this type, the sample is heated and with
the change in temperature changes in mass of the sample are
recorded
Principle
Principle of gravimetric titration :
Based on the conversion of ion/element /compound
which have low solubility into precipitates and this
precipitates separated by from mother liquid filtrate
and weight (pure compound ) so we can determine
ions /compounds presents in compound.

 Bacl2 + H2SO4 BaSO4 + 2HCL


analyte ppt agent precipitate
Advantages of Gravimetric Analysis

If the methods are followed carefully, it provides

exceedingly precise analysis.


It is used to determine the atomic masses of many

elements to six-figure accuracy.


It provides a little room for instrumental error and does

not require a series of standards for calculation of an


unknown.
Disadvantages of Gravimetric Analysis

It usually provides only for the analysis of a single


element, or a limited group of elements, at a time.
 Comparing with Modern method it is a
traditional combustion analysis.
Steps involved in Precipitation Gravimetric
Analysis

Preparation of the test solution


Precipitation
Digestion of precipitate
Filtration and Washing of precipitate
Drying and / or ignition of precipitate
Weighing
Calculation
Preparation of the solution
Solid sample must be dissolved in a suitable solvent.
Some form of preliminary separation may be
necessary to eliminate interfering materials.
The Purposes of Solution Preparation
1. To maintain low solubility of the precipitate.
2. To obtain the precipitate in a form suitable for
filtration.
3. Proper adjustment of the solution condition may also
mask potential interferences.
Factors that Must be Considered when Preparing the
Solution
Volume of the solution during precipitation
Concentration range of the test substance.
The presence and concentrations of other constituents.
Temperature
pH
Formation and Properties of Precipitates
Analyte + Precipitating Agent Precipitation

Super saturation
Three steps are involved in precipitation:
1) Supersaturation:- The solution that contains greater concentration of
solute than that corresponding to the equilibrium solubility at the given
temperature is called as supersaturated solution.

2) Nucleation:- When a more stable phase is formed from the metastable


phase of super saturation is called nucleation.

3) Precipitate Particle Growth:- Growth of particle of precipitate continuous


after the nucleation. In this, small ions come together to form a larger
precipitate particle .
Digestion of Precipitates
A precipitate allow to stand in presence of liquid from

which it is originally precipitated, large crystals grow


at cost of small once this process is called digestion or
Ostwald's ripening.
In this process small particles get dissolved &

reprericipated on surface of larger crystals


Washing of Precipitate
Gravimetric precipitates need to be washed to remove
any impurities that may have been precipitate along with
the main precipitate.

Properties of liquids :-
1) Washing liquid should be inert to the main precipitate
2) Washing liquid must be volatile
Ex ammonium salt are mostly use washing liquid
Dilute ammonium oxalate solution is used to wash calcium
oxalate ppt
Another ex is dilute ammonium nitrate is used to wash iron
hydroxide
Filtration of precipitates
The process of separation of precipitates from the
parent liquid is called as filtration the primary aim of
the filtration to get the precipitate and the filtering
medium quantitatively free from the solution
Various system used for the filtration are:
Filter paper
Porous fitted plates made of resistance glass e,g.
pyrexof silica
Drying and ignation
Drying is the term used when temperature is below
250 c and the ignation above 250 and below 1200 c
Drying is possible for the precipitates on the filter
paper ,gooch crucible,sintered glass or porocelain
crucibles.
Ignation is done by placing the crucible in muffle
furnace or by using appropriate burner.
After the drying crucible and precipitates placed in
desiccator for 30 min and weighted.

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