Gravimetric analysis

Lecture 7

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
Tech
 Definition
• Gravimetry encompasses all techniques in
which you measure mass or a change in
mass.
• Measuring is the most fundamental of all
analytical measurements and gravimetry is
unquestionably the oldest analytical
technique.
• Quantitative estimation by weight.

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
Tech
 Introduction
• Gravimetric analysis is a group of analytical
methods in which the amount of analyte is
determined by the measurement of the
mass of a pure substance containing the
analyte.
• Gravimetric methods can also be defined
as quantitative methods based on the
determining the mass of a pure compound
to which the analyte is chemically related.

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
Tech
 Types of gravimetric analysis

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
Tech
 Types of gravimetric analysis
Precipitation – analyte must first be
converted to a solid (precipitate) by
precipitation with an appropriate reagent.The
precipitates from solution is:
- filtered;
- washed;
- purified (if necessary);
- weighed.
2021 spring semester, Vilnius Tech Lecturer Ingrida Bružaitė
 Types of gravimetric analysis

Volatilization – in this method the analyte or

its decomposition product are volatilised
(dried) and then collected and weighed or
alternatively, the mass of volatilised product
is determined inderectly by the loss of mass
of the sample.

2021 spring semester, Vilnius Tech Lecturer Ingrida Bružaitė

 Example of precipitation
• Calcium can be determined gravimetrically
by precipitation of calcium oxalate and
ignition of the oxalate ion to calcium oxide.
• Ca2+ + C2O42- → CaC2O4(s)
• CaC2O4 → CaO(s) + CO2 (g) +CO(g)
• The precipitate thus obtained are weighed
and the mass of calcium oxide is
determined.
2021 spring semester, Vilnius
Lecturer Ingrida Bružaitė
Tech
 Example of volatilisation

Example:
- Water can separate from most inorganic compounds by
ignition, the evolved water can then be absorbed on any one
several solid desiccants.
- The weight of water evolved may be calculated from the
gain in weight of the absorbent.
- Not all insoluble precipitates are well suited for gravimetric
analysis.

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
Tech
 Criteria of successful determination

2021 spring semester, Vilnius Tech Lecturer Ingrida Bružaitė

Criteria of successful determination

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
Tech
 Advantages of gravimetric analysis

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
Tech
 Disadvantages of gravimetric
analysis
• There are potential problems with
gravimetric analysis that must be avoided
to get good results.
• Proper lab technique is critical;
• Careful and time consuming;
• Scrupulously clean glassware;
• Very accurate weighing.

2021 spring semester, Vilnius Tech Lecturer Ingrida Bružaitė

 Steps in gravimetric analysis
after the sample has been dissolved, can be
summarized as follows:
- preparation of the solution,
- precipitation,
- digestion,
- filtration,
- washing ,
- drying or igniting ,
- weighing and finally calculation .
2021 spring semester, Vilnius
Lecturer Ingrida Bružaitė
Tech
Preparation of analyte solution

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
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 Precipitation process

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
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 Digestion of the precipitate

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
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 Filtration

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
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2021 spring semester, Vilnius
Lecturer Ingrida Bružaitė
Tech
2021 spring semester, Vilnius
Lecturer Ingrida Bružaitė
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 Filtration

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
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 Washing

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
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2021 spring semester, Vilnius
Lecturer Ingrida Bružaitė
Tech
 Drying or ignition

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
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2021 spring semester, Vilnius
Lecturer Ingrida Bružaitė
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 Weighing

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
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 Steps in a Gravimetric analysis

https://www.youtube.com/watch?v=q9Yz5rEh3
CI#t=71

2021 spring semester, Vilnius Tech Lecturer Ingrida Bružaitė

 Calculation

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
Tech
 Calculations in gravimetric analysis

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
Tech
Exercise no.1.
Calculate gravimetric factor (GF) for the
conversation in the table:
No. Analyte mw or aw Precipitate mw
1. P 31 Ag3PO4 419
2. K2HPO4 174 Ag3PO4 419
3. Bi2S3 514 BaSO4 233.4
4. Al 27 Al2S3 150

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
Tech
2021 spring semester, Vilnius
Lecturer Ingrida Bružaitė
Tech
 Calculations in gravimetric analysis
In gravimetric analysis, we are generally
interested in the percent composition by
weight of the analyte in the sample,that is:
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑎𝑛𝑎𝑙𝑦𝑡𝑒 (𝑔)
𝑎𝑛𝑎𝑙𝑦𝑡𝑒 % = 𝑥100
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 (𝑔)

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
Tech
 Calculations in gravimetric analysis

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
Tech
Exercise No.2.
A 0.5962 g sample of iron ore is dissolved in
perchloric acid (HClO4). All iron present is
oxidized to Fe3+. The solution is filtered to
remove solid matrix materials and made
basic with addition of ammonium hydroxide.
The iron precipitates as the Fe(OH)3xH2O gel.
The precipitate is collected in a cistern crucible
and ignited to produce Fe2O3 . What is the wt.
% of iron in the sample if the analysis produced
0.3210 g Fe2O3?
2021 spring semester, Vilnius
Lecturer Ingrida Bružaitė
Tech
2021 spring semester, Vilnius
Lecturer Ingrida Bružaitė
Tech
Exercise No.3.
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 (200mL) and
excess sulfuric acid added. The mixture was then
heated and held at boiling for 45minutes. The
precipitate (barium sulfate , mw = 233.3) was
filtered off, washed and dried. Mass of precipitate
obtained = 0.2533 g. Determine the identity of X.

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
Tech
2021 spring semester, Vilnius
Lecturer Ingrida Bružaitė
Tech
Exercise No.4.
Calculate the weight of Mn ( aw = 55g/mol )
in 2.5 g of Mn3O4 ( mw = 229 g/mol ) ?

2021 spring semester, Vilnius

Lecturer Ingrida Bružaitė
Tech
2021 spring semester, Vilnius
Lecturer Ingrida Bružaitė
Tech