Republic of the Philippines

BATANGAS STATE UNIVERSITY

Pablo Borbon Main Campus II
Alangilan, Batangas City

COLLEGE OF ENGINEERING ARCHITECTURE AND FINE ARTS

BS CHEMICAL ENGINEERING

Submitted by:
Rich Corban C. Camacho
ChE - 2104

Submitted to:
Mr. Dave De Ramos

August 2021
 Republic of the Philippines
BATANGAS STATE UNIVERSITY
Pablo Borbon Main Campus II
Alangilan, Batangas City

COLLEGE OF ENGINEERING ARCHITECTURE AND FINE ARTS

BS CHEMICAL ENGINEERING

Precipitation Gravimetry

Precipitation gravimetry, the analyte is converted to a precipitate by the addition of a

precipitant which may ideally should selectively or specifically react with the analyte as this
would make the process easier. After turning the analyte to a precipitate, the solution it is in is
then filtered and freed of impurities and is heated until a constant weight measurement is
achieved.

Application of Precipitation Gravimetry

Precipitation gravimetry is an analytical method that is utilized in identifying the

amount of Mg²⁺ in water and wastewater. Magnesium is precipitated by utilizing (NH₄)₂HPO₄
as the precipitant, since the precipitant does not react selectively, the most significant
interference, Calcium must be separated from Magnesium by precipitating it as CaC₂CO₄.

The procedure for the analysis is as follows, a sample that does not exceed 60 mg of
Magnesium is to be transferred into a 600 mL beaker and is added with 2 or 3 drops of
methyl red indicator, with the volume being adjustable to 150 mL. The solution is then
acidified with the addition of 6 M HCl and 10 mL of 30% w/v (NH₄)₂HPO₄ . The addition of
concentrated NH₃ until the methyl red indicator turns yellow, is then done after constant
stirring and cooling. After 5 minutes of stirring, 5mL of concentrated NH₃ is added and
stirring is continued for 10 minutes more. The resulting solution is then left to stand
overnight. The precipitate is then isolated by filtration using filter paper and rinsing with a
5% v/v NH₃. Dissolving of the precipitate in 50 mL of 10% v/v HCl is done and is
precipitated again following the same procedures. After filtering, the precipitate is heated at
500 degrees Celsius until it turns into a color white, and it is heated again at 1100 degrees
Celsius until a constant weight measurement is achieved.

To clarify, in the procedure, it is important to note that it is important to only have a

60 mg portion of Magnesium as it already produces a substantial amount of precipitate and
adding more could lead to difficulty in filtration and rinsing.
 Republic of the Philippines
BATANGAS STATE UNIVERSITY
Pablo Borbon Main Campus II
Alangilan, Batangas City

COLLEGE OF ENGINEERING ARCHITECTURE AND FINE ARTS

BS CHEMICAL ENGINEERING

Volatilization Gravimetry

Another gravimetric method of analysis is volatilization gravimetry where the sample

is decomposed either thermally or chemically and the change in its mass is measured. A
different way can also be utilized where a volatile decomposition product is trapped and
weighed. It is called the volatilization gravimetry because of the role of the release of volatile
species in this method.

Application of Volatilization Gravimetry

Volatilization gravimetry can be utilized in the determination of Si in ores and alloys.

The determination of Silicon is done by dissolving the sample in acid and making it undergo
dehydration to precipitate SiO₂, but because other insoluble oxides will form, the precipitate
mass cannot be used as a direct measure for the amount of Silicon present.

For the procedure in this analysis a sample that has a value between 0.5 and 5.0 g is
transferred to a platinum crucible together with excess of Na₂CO₃ and is heated until a melt is
formed. The residue that has cooled down is then dissolved in dilute HCl. The solution is then
evaporated to dryness in a steam bath and is also heated for one hour at 110 degrees Celsius.
After the initial dehydration the residue is then moistened with HCl and dehydration is
repeated. Any acid soluble material is removed by adding 50 mL of water and 5 mL of
concentrated HCl. The solution is then brought to a boil and is filtered. After filtration the
residue is washed with high temperature 2% v/v HCl which is then followed by hot water,
which is then evaporated to dryness twice and removing any acid soluble materials using the
same procedure. The two precipitates are then combined and dried and ignited to a constant
weight at 1200 degrees Celsius, after cooling 2 drops of 50% v/v H₂SO₄ and 10 mL of HF.
The volatile SiF4 is then removed by evaporation to dryness on a hot plate and the residue is
then heated to constant weight by igniting at 1200 degrees Celsius.
 Republic of the Philippines
BATANGAS STATE UNIVERSITY
Pablo Borbon Main Campus II
Alangilan, Batangas City

COLLEGE OF ENGINEERING ARCHITECTURE AND FINE ARTS

BS CHEMICAL ENGINEERING

Electrogravimetry

When the product of controlled-potential coulometry produces a deposit on the

electrode that is functional, then we can use the change in that electrode’s mass as the
analytical signal. The difference in the electrode’s mass before and after the process of
electrolysis is a direct measurement of the amount of analyte in the sample.

Application of Electrogravimetry

An application of Electrogravimetry is observed in the determination of certain metals

in alloys. In the Electrogravimetric determination of copper, the procedure is as follows, the
dissolution of the alloy must take place first. For the determination of copper, it must first be
observed that the Pt electrodes are washed with 2M nitric acid and are flushed with distilled
water. The electrodes are then placed in the solution such that they are completely immersed .
The mixer is then turned on and electrolysis is conducted at a range of 3 to 3.5 volts, and after
30 minutes a miniscule amount of urea is added and 20 cubic centimeters of water is also
added. If it is observed that the copper has been isolated, the cathode is to be raised above the
surface of the solution and is flushed with water (distilled). The cathode with copper is to be
washed with acetone or ethanol and is dried for 4 minutes at a temperature of 110 degrees
Celsius and after cooling it is to be weighed. The color of the copper sediment should be pink
in color as a different color could indicate other metals present with the copper or its partial
oxidation.
 Republic of the Philippines
BATANGAS STATE UNIVERSITY
Pablo Borbon Main Campus II
Alangilan, Batangas City

COLLEGE OF ENGINEERING ARCHITECTURE AND FINE ARTS

BS CHEMICAL ENGINEERING

Gravimetric Titrimetry

The main distinction between the mass or gravimetric titrations from other analytical
methods is that the mass of the titrant is used rather than its volume. The buret is then
replaced by a balance and a weighable solution dispenser, which has certain advantages such
as the elimination of glassware calibration and a higher precision and accuracy than volume
measurements. Titration is used in various industries such as the food industry,
pharmaceuticals, and cosmetic industry.

Application of Gravimetric Titrimetry

In the production of wine, gravimetric titrimetry is utilized to ensure the quality of the
wine in terms of its taste, color and texture. The manufacturers monitor the concentration of
different acids such as malic,tartaric or citric that would affect the quality of the wine. The
different acid concentrations are called titratable acidity. The process is done by titrating
degassed wine with NaOH solution at varying rates until it reaches 8.2 pH. Another important
thing to measure is the amount of sulfur dioxide in the wine as it is used to destroy bacteria
that causes unnecessary fermentation and plays a key role in preserving the color of the wine,
this analysis is done by Ripper titration utilizing a color indicator, which is done by the usage
of iodine and a starch indicator to titrate the solution and obtain the amount of concentration
of free sulfur dioxide.

More advanced techniques could also be utilized such as gas or liquid

chromatography but the process of titration plays a vital role in ensuring the quality and
consistency not only in the production of wine but also in the production of other materials
that involve the process of titration.