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7/26/2019 Gravimetric Methods of Analysis.pdf
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CAPE Chemistry - Unit 2 Lecture Notes – Gravimetric Methods of Analysis
1 Copyright © 2016 Mark December
Gravimetric Analysis
Gravimetric analysis uses the mass of a sample to determine the amount of one substance that is present
in the sample. The main steps in Gravimetric Analysis are:
Preparation of the solution
Precipitation
Digestion
Filtration
Washing
Drying (in a crucible) or igniting (using a flame)
Weighing
Calculations
Types of Gravimetric Methods
Precipitation Gravimetry
In precipitation gravimetry an insoluble compound forms when a precipitating reagent, or
precipitant, is added to a solution containing the analyte. In order for precipitation to be
successful, the precipitate formed must be:
of low solubility,
of high purity,
of known composition if its mass is to accurately reflect the analyte’s mass,
easy to separate from the reaction mixture, and
free from impurities.
Because precipitation usually occurs in a solution that is rich in dissolved solids, the initial
precipitate is often impure. These impurities must be removed before determining the
precipitate’s mass.
Coprecipitation occurs to some degree in every gravimetric analysis. It cannot be avoided but
can be minimized by careful precipitation and thorough washing.
Surface Adsorption occurs when unwanted material is adsorbed onto the surface of the
precipitate. Washing serves to remove surface material.
7/26/2019 Gravimetric Methods of Analysis.pdf
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CAPE Chemistry - Unit 2 Lecture Notes – Gravimetric Methods of Analysis
1 Copyright © 2016 Mark December
Practice Question:
1. A certain barium halide exists as the hydrated salt BaX2.2H2O, where X is the halogen. The
barium content of the salt can be determined by gravimetric methods. A sample of the halide
(0.2650 g) was dissolved in water (200 cm3) and excess sulfuric acid added. The mixture was
then heated and held at boiling for 45 minutes. The precipitate (barium sulphate) was filteredoff, washed and dried. Mass of precipitate obtained = 0.2533 g. Determine the identity of X.
(RMM BaSO4= 233.4)
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CAPE Chemistry - Unit 2 Lecture Notes – Gravimetric Methods of Analysis
1 Copyright © 2016 Mark December
Questions:
1. A 0.497g sample of a chloride of a group 1 metal is dissolved in water. Excess acidified silver
nitrate solution is added to the solution of the chloride. The resulting precipitate is filtered and
dried to constant mass. The mass of AgCl formed is 0.957g. Deduce which metal is present in
the original chloride. (Molar mass of AgCl = 143.5 g/mol)
2. The treatment of a 0.8g sample of impure KCl with excess AgNO3 solution resulted in the
precipitation of 1.46g AgCl. Calculate the % of KCl in the sample. (Molar mass of AgCl = 143.5
g/mol)
3. Deduce the formula of MgClX from the following information: 0.635g of MgClX reacts with
excess AgNO3. The mass of AgCl formed is 1.914g. (Molar mass of AgCl = 143.5 g/mol)
4. A student is given a 2.94g sample of a mixture containing anhydrous MgCl2 and KNO3. To
determine the % by mass if MgCl2 in the mixture, the student uses excess AgNO3 to precipitatethe chloride ions as AgCl. The mass of the precipitate is 5.48g. Calculate the number of moles
of MgCl2 in the original mixture and the % by mass if MgCl2 in the original mixture. (Molar
mass of AgCl = 143.5 g/mol)
5. When 0.611g of hydrate barium chloride is heated to a constant mass, 0.521g of residue are
formed. Deduce the formula of hydrated BaCl2. [RAM: Ba = 137.3, Cl = 35.5, O = 16, H =1]
6. A student collected the following data in an experiment to determine the number of moles of
water in one (1) mole of MgCl2. nH2O.
Mass of empty container = 22.347g
Initial mass of sample = 25.825g
Mass of sample and container after heating = 23.978g
Use the data above to calculate the number of moles of water lost when the sample was heated
and determine the formula of the hydrated compound.
Volatilization Gravimetry
Another approach to gravimetry is to thermally or chemically decompose the sample andmeasure the resulting change in its mass. For example, the mass of water in a sample can be
calculated by heating the sample and finding the loss in mass from the sample.
Another method in volatilization gravimetry involves the trapping and weighing of a volatile
decomposition product. For example the mass of water in a sample can also be calculated by
heating the sample and collecting the vapour in a solid desiccant. The increase in mass of the
desiccant will be equal to the mass of water in the sample. .
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CAPE Chemistry - Unit 2 Lecture Notes – Gravimetric Methods of Analysis
1 Copyright © 2016 Mark December
The amount of carbon dioxide in a sample of a carbonate can also be determined by
volatilization. Carbonates are decomposed into carbon dioxide which is absorbed by a solid
desiccant such as Ascarite II which is made up of sodium hydroxide in a non-fibrous silicate.
The sodium hydroxide absorbs the CO2 forming sodium carbonate and water.
2NaOH (aq) + CO2 (g) ⇌ Na2CO3 + H2O
Practice Question:
1. A sample of impure calcium carbonate was decomposed with excess hydrochloric acid. The
liberated carbon dioxide, collected in an absorbent was found to weigh 0.88g. Calculate the %
of CaCO3 in the sample.
2. A 8.4g sample of copper (II) carbonate was decomposed with excess sulphuric acid. The
liberated carbon dioxide, collected in an absorbent was found to weigh 2.2g. Calculate the % of
CuCO3 in the sample.