UNIVERSITY OF MINES AND TECHNOLOGY (UMaT),

TARKWA
SCHOOL OF PETROLEUM STUDIES
DEPARTMENT OF CHEMICAL AND PETROCHEMICAL ENGINEERING

A REPORT ON GRAVIMETRIC ANALYSIS OF SOLUBLE CHLORIDE

BY
FELIX YEBOAH
SPE41.014.114.21
CLASS: RP II

COURSE NAME: CHEMISTRY LABORATORY PRACTICES

COURSE CODE: RP 273

COURSE LECTURER: AMI JOHANNES

MARCH 2023
 CONTENT

ABSTRACT ................................................................................................ 2

INTRODUCTION .......................................................................................3
PRECAUTIONS TAKEN DURING EXPERIMENT .................................................. 4
AIM AND OBJECTIVES OF EXPERIMENT ............................................................. 4
APPARATUS AND REAGENTS NEEDED FOR EXPERIMENT ............................ 4

PROCEDURE ............................................................................................. 6
PREPARATION OF NaCl SALT ................................................................................. 6
PRECIPITATION OF NaCl WITH AgNO3 ..................................................................6
FILTRATION AND FINAL WEIGHING .................................................................... 6

RESULTS AND CALCULATION ............................................................ 7

CALCULATIONS .........................................................................................................7

DISCUSSION ........................................................................................... 10
CONCLUSION ............................................................................................................12
RECOMENDATION ...................................................................................................12

REFERENCES ..........................................................................................13

1
 ABSTRACT

In this experiment, sodium chloride salt was used as a test sample to determine the
amount of chloride ions present in it by gravimetric analysis. 0.5g of the salt was
treated with 1M AgNO3 to obtain white precipitate of AgCl. The chloride was initially
formed as colloidal solution. After subsequent heating and the addition of Nitric acid ,
nucleation process was dominated by particle growth and the precipitates separated
out as coagulated mass. This precipitate was filtered, dried and weighed. Then the
average percentage of chloride present in NaCl was determined to be 142.123 ％

2
 INTRODUCTION

Gravimetric analysis derives its name from the fact that the constituent being
determined can be isolated in some weighable form. Chloride ion may be
quantitatively precipitated from solution by the addition of silver ion according to the
following ionic equation:
Ag+(aq)+ Cl−(aq)→ AgCl(s)
The addition of a silver nitrate solution to an aqueous solution containing chloride ion
precipitates AgCl quantitatively .The silver chloride precipitate initially forms as a
colloid, which is coagulated with heat. Nitric acid and a small excess of silver nitrate
aid coagulation by providing a relatively high electrolyte concentration( acidic pH).
The acidic pH eliminates the interference by anions(like carbonate and sulphides).
Otherwise, these anions can form sparingly soluble silver salt in neutral pH. Similarly,
the silver nitrate is also added in little excess to enhance the formation and diminish
the solubility of silver chloride.Moreover, the combined action of moderately high pH
and slightly excess AgNO3 promotes the coagulation of the silver chloride precipitate
by formation of dielectric layer.Finally,the precipitate can be collected on a
previously weighed filter paper, dried, and weighed.
From the mass of the AgCl obtained, the amount of chloride in the original sample
can then be calculated.

3
 PRECAUTIONS TAKEN DURING EXPERIMENT

Dry silver chloride is virtually unaffected by exposure to light. As the analysis is

performed, it is almost impossible to prevent photo-decomposition of the wet silver
chloride precipitate.Generally,the effect is small and can be ignored provided that
exposure to direct sunlight, or extended exposure to fluorescent lights, is avoided. The
simplest way to minimize photo-decomposition is to store the Silver chloride in a dark
space (desk drawer)

Silver nitrate, like other silver salts, is relatively expensive.Use the amount of silver
nitrate solution that you need for the experiment, but try to avoid wasting significant
amounts of silver nitrate solution.

AIM AND OBJECTIVES OF EXPERIMENT

To illustrate typical techniques used in Gravimetric Analysis by quantitatively

determining the amount of chloride in the chloride salt.

APPARATUS AND REAGENTS NEEDED FOR EXPERIMENT

 500ml Beaker
 Wash bottle
 Stirring Rod
 0.01M Nitric acid
 1M Silver nitrate
 Policeman
 Dessicator
 Buchner funnel

4
 Filter paper
 Distilled water

5
 PROCEDURE

PREPARATION OF NaCl SALT

0.5g of NaCl was weighed into three different 500ml beaker and each portion
dissolved using 100ml of distilled water.Each beaker was distinguished with a label
on it.

PREPARATION OF AgNO3
Silver nitrate can be prepared by dissolving silver in nitric acid followed by
evaporation of the solution. .

3 Ag + 4 HNO3 → 3 AgNO3 + 2 H2O + NO

PRECIPITATION OF NaCl WITH AgNO3

NaCl solution was heated to boiling and with constant stirring AgNO3 was added
until the formation of AgCl precipitate was completed.

HNO3 and a small excess of AgNO3 was added to the solution to aid coagulation.
AgNO3 was added in bit until solution became a little more clear. The solution was
then kept in a locker to cool.

The same procedure was performed for the remaining two solutions of NaCl.

FILTRATION AND FINAL WEIGHING

The precipitate was washed with three 25ml portions of 0.01M Nitric acid.
A filter paper was weighed and its mass recorded. It was folded and place it in the
funnel so that one side has three folds and the other side has one fold of paper against
the funnel.
The paper was wet with HNO3 to hold it in place inside the funnel. All the precipitate
and solution from the beaker was transferred onto the filter paper using a rubber
policeman and a wash bottle to wash out the last traces of precipitate.
Filter paper containing precipitate was dried in an oven for 2 hours at 120℃. Finally,
the precipitate was cool in a desiccator and the mass weighed and recorded.

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 RESULTS AND CALCULATION

Trial 1 2 3

Mass of the 0.502 0.502 0.504

NaCl(g)

Mass of filter 0.645 0.661 0.651

paper(g)

Mass of filter paper 3.381 3.384 3.857

+ precipitate

Mass of precipitate 2.736 2.723 3.206

Mass of Chloride 0.6768 0.6736 0.7931

Percentage of 134.821 134.183 157.361

chloride in
precipitate

Table 1 Experimental results

CALCULATIONS

Atomic weight of chloride = 35.453 g/mol

Molecular mass of AgCl = 143.32g/mol
������ ����ℎ� �� �ℎ������
Mass of chloride in precipitate = ��������� ����ℎ� �� ����
× ���� �� �����������

���� �� �����������
Percentage of chloride = ���� �� ���� ����
× 100 %

Trial 1
35.453�/���
Mass of chloride =143.32�/��� × 2.736

Mass of chloride = 0.6768g

7
 0.6768�
Percentage of chloride = 0.502� × 100 %

= 134.821 %

Trial 2

35.453�/���
Mass of chloride =143.32�/��� × 2.723g

Mass of chloride = 0.6736g

0.6736�
Percentage of chloride = 0.502� × 100 %

= 134.183 %

Trial 3

35.453�/���
Mass of chloride =143.32�/��� × 3.206g

Mass of chloride = 0.7931g

0.7931�
Percentage of chloride = 0.504� × 100 %

= 157.361 %

134.821 + 134.183 +157.361

Average percent of Cl = 3

= 142.123%

(�−�)2
Standard deviation=
(�−1)

(134.821−142.123)2 +(134.183−142.123)2 +(157.361−142.123)2

Standard deviation=
(3−1)

8
=13.20

9
 DISCUSSION

For this experiment, sodium chloride was reacted with 1M of AgNO3.However, it is

known in general that the chemical reaction involved in precipitation reactions is a
double replacement or double displacement reaction process as shown in the chemical
equation below.

NaCl (s) + AgNO3 (aq) → NaNO3 (aq) + AgCl (s)

It can be noted that the 0.1 M nitric acid (HNO3) added to the solution was not
included in the chemical equation because of its catalytic role and not a
part of the reactants.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 precipitates formed are formed as colloids. Since colloids are stable molecules, it
is necessary to heat, stir and add more electrolyte (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
precipitates formed. Washing with nitric acid ensures that the precipitates will be
preserved because washing with water may dissolve it .

The precipitate thus 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 consists of
halides. In this lab however, the silver nitrate was used to quantitatively determine the

10
percentage of chloride present in the samples. The known sample of Sodium chloride
seems to have impurity because it gave more percentage of chloride than theoretically
expected.

The calculated mass of chloride was used to determine the percent chloride by
dividing it by the mass of the sodium chloride salt.The values of the obtained
percent of chloride as shown in table 1 are 134.821% for Trial 1, 134.183%
for Trial 2, and 157.361% for Trial 3 which gave an average percent chloride of
142.123%.The variation in the percentage of chloride in the known sample may have
been resulted by impurity in the sample or due to the random error during experiment.

Several situations can cause significant increases or decreases in precipitate mass,and

therefore poor results. Silver chloride slowly photo-decomposes by the following
reaction:

2AgCl(s) + 2hυ → 2Ag(s) + Cl2(g)

Since chloride is lost as chlorine gas, the above reaction causes the results to be low.
The silver metal produced during photo-decomposition is responsible for the violet
colour that develops in the precipitate. If photo-decomposition occurs in the presence
of excess silver ion, the following reaction occurs:

3Cl2(aq) + 3H2O(l) + 5Ag+(aq)→ 5AgCl(s) + ClO3-(aq)+6H+(aq)

This causes the analytical results to be too high.

Obviously, the data in Table 1 are not accurate and not necessarily more precise. The
standard deviation may be used to determine whether a result should be retained or
discarded. As a rule of thumb, you should discard any result that is more than two
standard deviations from the mean. From the experiment, a result of
134.821%,134.183% and 157.361% was obtained and the average percentage of
chloride and standard deviation was determined as 142.123 and +/- 13.20 respectively,
the results should be discarded. This is because s = 13.20 and 2 x( [134.821 - 142.123 ]
= 7.302; [134.183-142.123]=7.94; [157.361-142.123]=15.238), which is greater than
13.20. This result is more than two standard deviations from the mean. Since the
value of the standard deviation is large the experimental results lack precision.

11
 CONCLUSION

There is about ± 23% variation from the average that can be observed from each of
the calculated chloride percentages. This variation may be due to precipitates left
adhering to the surface of the filter paper, rubber policeman, or perhaps some
precipitate fell outside the filter paper which affected the final mass of the precipitate
and consequently influencing the succeeding calculations made. This observed
variation is very significant and affected the results of the experiment. Hence, it
can be concluded that the experiment procedure did go as expected, with loss of
materials and impurity in the sample or due to the random error during experiment.

RECOMENDATION

Filter paper used in experiment may loss weight during the drying process thus,
affecting the mass of the precipitate. Therefore, it is advisable to use crucibles instead
of filter paper in collecting and drying of precipitates.

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 REFERENCES

Farrance, I., & Frenkel, R. (2017). Uncertainty of measurement: a review of the rules
for calculating uncertainty components through functional relationships.

Haynes, W. M. (Ed.). (2014). CRC handbook of chemistry and physics. CRC press,
(49)pp.

Vaughan, N. P., Milligan, B. D., & Ogden, T. L. (2016). Filter weighing

reproducibility and the gravimetric detection limit. The Annals of Occupational
Hygiene,( 331-337)pp.

Dr. Johannes Ami (2021),Chemistry Lab Manual, University of mines and

Technology,Tarkwa,1st edition, (14-15)pp.

Dr. Adel Ahmed Mohammed Saeed, (2020) , Gravimetric Analysis, Aden

University ,(13-37)pp

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