ANALYTICAL CHEMISTRY

SCIE6022

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 SESSION 2
Gravimetric Analysis

DEPARTMENT OF FOOD TECHNOLOGY

FACULTY OF ENGINEERING
2017
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 OUTLINE

• Introduction
• Weight vs mass
• Calibration and care of balance
• Details of gravimetrics method
• Experimental considerations

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 Learning outcomes
• LO1 Explain about sampling, sample preparation and statistical
treatment
• LO2 Evaluate the results given by the used analytical methods
(gravimetry, volumetric analysis, UV-Vis spectrometry, IR
Spectrometry, atomic spectroscopy, electrophoresis,
chromatography, mass spectrometry, electroanalytical methods)

• LO3 Examine which analytical methods (gravimetry, volumetric

analysis, UV-Vis spectrometry, IR Spectrometry, atomic
spectroscopy, electrophoresis, chromatography, mass spectrometry,
electroanalytical methods) are appropriate in the determination of
chemical composition analysis

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 Gravimetric method

• Gravimetric pertains  using mass to perform analysis

 the amount of analyte is determined by the measurement of the mass
of a pure substance containing the analyte.
• Please be careful on the term “Weight” vs. “mass”
• Do you know what would be the difference(s)?
• To perform weight analysis, then we need: BALANCE
• Different examples of laboratory work require different degrees of
precision  different numbers of SIGNIFICANT FIGURES to the right of the
decimal point.
•  delivering different types of the balance in the market

Which balance’s significant

figure (decimals) to use?
Depends on your application,
Choose wisely
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 THE BALANCE

Needs calibration

• Calibration: process to make an equipment to display correct

information.
• Calibration of balance: to make a balance displays the weight of
1 L of H2O is 1 kg, not 0.99 kg or 1.01 kg (depends on the
desired accuracy)
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 DETAIL OF GRAVIMETRIC METHOD

Gravimetric analysis methods proceed with the

following steps :
1. The weight or volume of the prepared sample is
obtained
2. The analyte is either physically separated from the
sample matrix or chemically altered and its
derivative separated from the sample matrix
3. The weight of the separated analyte or its derivative
is obtained. The data thus obtained are then used to
calculate the desired results

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DETAIL OF GRAVIMETRIC METHOD

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 DETAIL OF GRAVIMETRIC METHOD

There are two main types of gravimetric analyses

A) 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) and
weighed.
B) Volatilization
In this method the analyte or its decomposition products are
volatilised (dried) and then collected and weighed, or
alternatively, the mass of the volatilised product is
determined indirectly by the loss of mass of the sample.
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• Calcium can be determined gravimetrically by
precipitation of calcium oxalate and ignition of the
oxalate ion to calcium oxide.
Ca2+ + C2O42- →CaC2O4
CaC2O4 → CaO + CO2 + CO
• The precipitate thus obtained are weighed and the
mass of calcium oxide is determined.

• Volatilization: removal of volatile components of

analyte by heating it

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 DETAIL OF GRAVIMETRIC METHOD

1. Loss on drying
This is an example of a loss through volatilization
(evaporation) under temperature conditions at which
water would volatilize, hence the word “drying.” The
loss can occur by elevating the temperature of the
sample to just above the boiling point of water lthough
a different temperature may be specified) or through
desiccation

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 DETAIL OF GRAVIMETRIC METHOD

2. Loss on Ignition
This is similar to loss on drying, except that an
extremely high temperature, such as that of a Meker
burner or muffle furnace, is used such that changes
other than just moisture evaporation occur, a process
known as ignition

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 DETAIL OF GRAVIMETRIC METHOD

3. Residue on Ignition
The mineral particles and ash that remain after the ignition of
a sample as described above may be important to calculate
and report
The mineral and ash are known as the residue

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 DETAIL OF GRAVIMETRIC METHOD

4. Insoluble Matter in Reagents

As part of a general analysis report, the labels on certified
chemicals that are soluble in water indicate the percent of
insoluble matter present.
This insoluble matter is determined by preparing a solution of
the chemical, which sometimes involves heating to boiling in
a covered beaker and maintaining a higher temperature for a
specified time to effect dissolution

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 DETAIL OF GRAVIMETRIC METHOD

5. Solids in Water and Wastewater

Total solids involve measuring a volume of the water or wastewater into a
preweighed evaporating dish, evaporating the water using a drying oven,
and obtaining the weight of the residue, which includes all solids,
suspended and dissolved

Suspended solids are solids from a measured volume of sample that can
be trapped on a preweighed filter

Volatile solid determination is similar to the loss on ignition discussed

earlier. Either total solids or suspended solids can be analyzed for volatile
solids

For settleable solids , a sample of the wastewater is taken after the

suspended solids are allowed to settle for a specified time. The solids in
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this sample are then measured in a manner similar to that for total solids
 DETAIL OF GRAVIMETRIC METHOD

6. Particle Size by Analytical Sieving

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 GRAVIMETRIC FACTOR

A gravimetric factor
is a number used to convert, by multiplication, the weight of
one chemical to the weight of another. Such a conversion can
be very useful in an analytical laboratory

QS : The balancing coefficient for the common element in the

formula of the substance sought
QK : The balancing coefficient for the common element in the
formula of the substance known 17
GRAVIMETRIC FACTOR

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USING GRAVIMETRIC FACTOR

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 Water content and ash content:
Using the curve of weight vs time

Initial weight A
100 g
Water content = (length of AB) / (length of AD)
= 60/100 = 60%

Start of carbonization,
inside the furnace
Weight after
drying in oven B
40 g

Weight after C
drying in furnace D
10 g Time
(note: NOT to scale)
Ash content = (length of CD) / (length of AD)
= 10/100 = 10% 20
 References

Kenkel, John. (2014). Analytical Chemistry For Technicians. 04. CRC

Press. Boca Raton, U.S. ISBN: ISBN-978-1-4398-8105-7
Harvey, David. (2000). Modern Analytical Chemistry. 01. Mc. Grow Hill
Companies. ISBN 0–07–237547–7

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