KUMASI TECHNICAL UNIVERSITY

CHEMICAL ENGINEERING DEPARTMENT

NAME;SABINA ANEESIWA NEIZER
TITLE;GRAVIMETRIC ANALYSIS OF A SOLUBLE CHLORIDE
DATE;8TH APRIL,2019
LECTURER;REV.JOHANNES AMI
INTRODUCTION;
Gravimetric analysis is a type of analysis that involves the determination or measurement of weights or
mass. In this analysis, the mass of a product is used to calculate the quantity of original analyte.
An example of this analysis is the determiation of chloride in a compound.
The principle of gravimetric analysis is precipitation,the mass of an ion in a pure compound can be
determined,and later used to find the mass percent of the same ion in a known quantity of an impure
compound.
Quanlitative analysis;
is the type of analytical method that is used to identify the elements(ions). It is also used to identified
the components of a given mixture. (Based on volume).
Quantitative analysis;
is also used to determine the quantities of elements in the compound or compounds of the mixture.
(Based on the mass of a given solid).
Types of this analysis are ;
1. Physical gravimetry
2. Thermogravimetry
3. Precipitative gravimetry analysis
4. Electrodeposition
Gravimetric analysis is a technique through which the amount of an analyte can be determined through
the measurement of mass. The analysis depends on comparing the masses of two componds containing
the analyte.
Gravimetric factor;
Convets grams of a compound into grams of a single element.
Steps that goes on under this analysis are;
1. preparation of the solution
2. Precipitation
3. Digestion(Ostwald ripening)
4. Washing and filtering the precipitates
5. Drying or igniting the precipitate
6. calculation
In this experiment a precipitating agent was used to precipitate the halide ion ,chloride which is the
silver nitrate. Barium chloride is also a precipitating agent used to precipitate sulfate ion.
In all the precipitation reactions ,the product is salt because it is formed by reactions between cations
and anions and the bonding is electrovalent.
Organic precipitating reagents contain functional groups which combine inorganic ions to form
insoluble salts.
Silver ions undergo the following reaction with chloride;
Ag++Cl-→AgCl(white solids)
An excess of silver ions is added so that the chloide concentration at equilibrium will be negligible. If
enough silver nitrate solution is not used,the precipitation will be incomplete ,resulting in a substantial
error and a low value for the % Cl in the sample.
MATERIALS/REAGENTS;
1. 0.01M Nitric acid
2. 1M Silver nitrate
3. stirrer
4. NaCl
5. Beakers
6. Balance
7. Distilled water
8. Crucibles
9. Heat
10. Measuring cylinder
11. Dessicator
12. Oven

PROCEDURE;
1. Porcelain crucibles were prepared byncleaning them and was then put in an oven at 100 o C for
an hour.
2. It was then cooled in a dessicator for 20 minutes and weighed.
3. The procedure was repeated until th emass of each crucible agreed to within 0.3mg.
4. 0.5g of NaCl was weighed into a 250ml beaker and was dissolved with 100ml distilled water.
5. Tht chloride solution was heated to boiling.
6. With constant stirring the silver nitrate was added until precipitation of the silver nitrate was
complete. The silver nitrate was added in small amount was vigorously stirred.
7. It was allowed to settle a bit and some silver nitrate was added without stirring
8. It was then cooled and filtered through a weighed filter paper.
9. The solution was then washed with 25ml of 0.01M nitric acid.
10. The filter paper containing the precipitate was dried in then oven at 120 o C
11. The dried precipitate was cooled in the dessicator and weighed.
DATA AND CALCULATIONS;
Trial 1 Trial 2 Trial 3
Weght of crucibles 52.796g 50.546g 50.234g
Before heating 52.795g 50.545g 49.232g
After heating 51.888g 49.234g 49.632g

Weight of the NaCl=0.5g

volume of beaker =250ml
volume of water=100ml

Trial 1 Trial 2 Trial 3

Weight of filter paper 0.999g 1.053g 0.983g
Weight of filter paper 1.952g 1.962g 1.846g
+ppt
Weight of ppt 0.953g 0.909g 0.863g

Average mass of ppt=(0.953+0.909+0.863)/3

=0.908g
Calculate the % chloride in the sample;
%Cl=(weight of ppt ×GF)/(weight of sampl) × 100
Gravimetric factor;
m(Cl)/m(AgCl)=(35.453gCl/mol)/(54.44gNaCl/mol)
=0.651gCl/gAgCl
mass,m(Cl)=m(NaCl) × GF
=0.908g×0.651g
=0.591g
Finally % Cl in sample;
%Cl=m(Cl)/m(sampl) × GF×100%
=(0.591g)/(0.5g) ×100%
=118.2%
DISCUSSION;
In theory the percentage of chloride in sodium chloride is 60.66% but from the calculation it was found
to be 118.2%. The variation in the percentage of chloride may have been resulted by impurity in the
sample or due to the random errror during experiment.
This experiment is the classical example of the precipitation reaction where the fomation of dielectric
layer of silver chloride stabillized by nitrate ions takes place. Upon the addition of silver nitrate in the
aqueous solution of the salt,the formation of the silver chloride occurs as a colloid. Slightly excess
silver nitrate is added and also nitric acid is added to raise the concentration of the nitrate ion in the
solution for two reasons. The first reason is to prevent the solubility of the silver chloride precipitates
that are formed as precipitate. The second reason is to enhance particle growth and the formation of the
dielectric layer.
The particle formed are formed as colloid since colloids are stable molecules,it is necessary to heat ,stir
and add more nitrate to obtain particle growth by the process of adsorption. The colloid obtained is
made of silver chloride as primary adsorption layer and nitrate ions make up the counter-ion layer to
stabilize the system. Continued heating ruptures the counter ion layer and promotes stabilization by the
nitrate ions produced by the addition of slightly excess silver nitrate and nitric acid. However ,addition
of too much silver nitrate is avoided to prevent the co-precipitation of the silver nitrate. Nitric acid is
used in the reaction mixture as well as to wash the precipitate formed. Washing with the nitric acid
ensures that the preciptate will be preserved because washing with water may dissolve it.
The precipitate obtained was weighed to determine the percentage of chloride present in the starting
sample . This process can be employed quantitatively to determine the purity of the sample. In many
cases,precipitation reaction of silver halides is qualitatively used to identify whether the inorganic
compound consist of halides. In this lab however, the silver nitrate was used to quantitatively
determine the percentage of chloride present in the samples. The known sample of sodium chloride
seems to have impurity because it gave more percentage chloride than theoretically expected. But ,the
identity of unknown sample was unknown and just by analyzing the percentage of chloride ion nothing
can be said about its identity.
REFERENCES;
1. https://www.ulessays.com/essays/gravimetric – determination-of-chloride .php?vref=1
2. Skoog, D.A.;Holler , F. J.;Stanley R.Crouch,fundamentals of Analytical Chemistry,8th
ed.;Thomas books /cole USA,2004