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UNIVERSITY OF ZIMBABWE

Name: MUTETE RONALD


Reg. no: R164545P
Program: CHH
Course: HCH104
Experiment no: 3
Date: 03 OCTOBER 2017

Title: standardization of AgNO3 solution and determination of chloride


by Mohr’s titration method.
Aim: to determine the percentage of chloride in the given sample.

Objectives
1. To standardize AgNO3 solution using sodium chloride.
2. To determine the percentage of chloride in the given sample using
precipitation titration.
MUTETE RONALD | R164545P

THEORY
Volumetric(titrimetric) analyses, consist essentially in determining the volume of a solution of
accurately known concetration which is required to react quantitatively with the solution of the
substance being determined. The solution of accurately known strength is called the standard
solution. Among these is the precipitation reaction which depend upon the combination of ions
other than hydrogen or hydroxide ion, to form a simple precipitate as in the titration of silver ion
with a solution of chloride ion. (Vogel, 1961)
In the Mohr titration, Cl- is titrated with Ag+ in the presence of CrO42-(chromate dissolved as
K2CrO4)
Titration reaction: Ag+ +Cl- → AgCl(s)
Endpoint reaction: 2Ag+ + CrO42- → Ag2CrO4 (s)
The AgCl precipitates before Ag2CrO4. The colour of silver chloride is white, dissolved in CrO 42-
is yellow, and Ag2CrO4 is red. The AgCl endpoint is indicated by the first appearance of red
silver chromate. Reasonable control of CrO 42- concentration and pH is required for silver
chromate precipitation to occur at the desired point in titration. (Harris C.D, 1991)
Fractional precipitation- if an ion is added to a solution containing two ions which may form a
precipitate with the added ion, that substance will precipitate first whose solubility is exceeded.
In the Mohr titration, silver ion is added to a solution which contains a relatively high
concentration of chloride ion. The two solubility products are:
[Ag+] [Cl-] = 10-10 and [Ag+] [CrO42-] = 9 × 10-12.
A precipitate of silver chloride forms as soon reagent is added, but silver chromate des does not
begin to precipitate until the concentration of silver ion reaches a point at which silver chromate
begins to appear is then, taken as the endpoint of the titration. (Pierre and Haenisch, 1954)
It is not always possible to prepare a standard solution so that its concentration is known to the
necessary degree of reliability. In such a case, a solution of approximately the desired
concentration is prepared and the exact concentration is the established by a determination
known as standardization. The reference substance used in the standardization is often known as
the primary standard. This substance must be of known purity. (Flaschka, et al)
A standard solution (or a standard titrant) is a reagent of known concentration that is used to
carry out a volumetric titration. The titration is performed by slowly adding a standard solution
from a burette or other liquid-dispensing device to a solution of the analyte until the reaction
between the two is judged complete. The volume or mass of reagent needed to complete the
titration is determined from the difference between the initial and final readings. It is sometimes
necessary to add an excess of the standard titrant and then determine the excess amount by back-
titration with a second standard titrant. (Skoog, et al.2013)

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Mohr’s determination of chloride experiment
MUTETE RONALD | R164545P

PROCEDURE

Standardization of AgNo3 solution


Reagent grade of sodium chloride of 0.2g was accurately weighed. The salt was transferred to a
100cm3 volumetric flask, dissolved in distilled water and then diluted to the mark mixing well.
Molarity of the solution was calculated. Volume of 25cm 3 of the solution was pipetted into
250cm3 conical flask, followed by the addition of 1cm 3 of indictor using a graduated pipette. The
portion was then slowly titrated with AgNO3 whilst swirling the flask, to the first colour change
from the yellow colour of the solution. Whenever the endpoint was reached, the flask was shaken
well, and whenever the colour change reverted, the titration was continued until a permanent
faint reddish-brown tinge was obtained. Calculation for molarity of the AgNO3 was done.

Determination of Chloride
A mass of 0.2g of the chloride sample was accurately weighed. The salt was transferred to
100cm3 volumetric flask, dissolved in distilled in water and diluted to the mark. The solution was
mixed well. Volume of 25cm3 portion of the solution was pipetted into 250cm 3 conical flask,
followed by the addition of 1cm3 of indicator. The solution was then slowly titrated with AgNO 3
whilst swirling the flask, to the first colour change from the yellow colour of the solution.
Whenever the endpoint was reached, the flask was shaken well, and whenever the colour change
reverted, the titration was continued until a permanent faint reddish-brown tinge was obtained.
The percentage of chloride in the sample was calculated.

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Mohr’s determination of chloride experiment
MUTETE RONALD | R164545P

RESULTS AND CALCULATIONS

Standardization of AgNO3 solution


Table 1: weighing reagent grade sodium chloride

Mass of sample + empty container/g 2.5350


Mass of empty container/g 2.3132
Mass of sample/g 0.2218

Table2: standardization titration

1st 2nd 3rd


3
Final reading/cm 9.60 19.20 28.70
Initial reading/ cm3 0.00 9.60 19.20
Volume used/cm3 9.60 9.60 9.50

Average titre= (9.60+ 9.60) ÷ 2


= 9.60cm3

Determination of chloride
Table 3: weighing chloride sample

Mass of sample + empty container/g 2.5396


Mass of empty container/g 2.3132
Mass of sample/g 0.2264

Table 4: titration chloride sample with AgNO3

1st 2nd 3rd


3
Final reading/cm 27.50 37.50 47.50
Initial reading/cm3 17.70 27.50 37.50
Volume used/cm3 9.80 10.00 10.00

Average titre= (10.00 + 10.00) ÷ 2


= 10.00cm3
Molarity of the solution of reagent grade sodium chloride:
Molarity = number of moles/ volume in dm3
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Mohr’s determination of chloride experiment
MUTETE RONALD | R164545P

 Number of moles(NaCl)= mass/Mr


= 0.2218÷58.443
=3.8 × 10-3mol
Therefore, molarity =3.8 × 10-3 ÷ (100/1000)
= 0.038M

Molarity of AgNO3 solution:


AgNO3 + NaCl → AgCl(s) + NaNO3(aq)
The reaction is 1: 1 ratio, therefore moles of NaCl= no. of moles of AgNO3.
Molarity= number of moles/ volume in dm3
= 0.003795 ÷ (9.6/1000)
=0.395M

Percentage of chloride in the sample


Ag+ + Cl- → AgCl(s)
1:1 reaction ratio, therefore moles of Ag+ = number of moles of Cl-

 Number of moles= concentration × volume in dm3

= 0.395 × (10/1000)
= 0.00395mol

 Mass of chloride= number of moles × Mr

= 0.00395×35.453
=0.14g
Therefore, percentage of the chloride in the sample= (mass of chloride/mass of sample) × 100%
Percentage = (0.14 ÷ 0.2264) × 100%
=61.84%

DISCUSSION
In this experiment, the amount of chloride in the given unknown sample was determined by
Mohr titration, a direct and accurate method for chloride determination. Procedures for the

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Mohr’s determination of chloride experiment
MUTETE RONALD | R164545P

experiment were strictly followed, and results obtained successfully. The percentage of chloride
obtained in the unknown sample was quite high, 61.84%. This is evidence that the practical was
run correctly with very few or insignificant errors to discuss.
Since a certain amount of excess Ag2CrO4 is necessary for visual detection for the endpoint, the
colour is not seen until after the true equivalence point. Titration error could have arisen because
excess Ag+ is needed to form a detectable amount of red precipitate, however the error is avoided
by the standardization of AgNO3 that was done during the first stages of the practical. This
further proves that the results obtained are reliable, notwithstanding all other possible sources of
errors in the practical.
All titrations were carried out, at about the same temperature (room temperature) since the
solubilities of silver chloride and silver chromate depend on temperature. The whole practical
was done in a very short time period such that, temperatures in the laboratory can never have
fluctuated with wide ranges, enough to distort the precipitation reactions. To prevent the
occlusion of silver chromate in the silver chloride precipitate, continuous swirling of the flask
during the titration was done vigilantly to obtain a sharp and reproducible end points.
However, some systematic and human errors might have been conceded in the running of the
practical. Silver chloride decomposes according to:
2AgCl ÷ Ag(s) + ½ Cl2 (g)
in the presence of light. Regardless of this, no measures were taken in the practical to protect the
silver chloride from light. It is therefore possible that some of the precipitated silver chloride was
decomposed by the effect of uv-radiation and thus distorting the endpoint. The Mohr’s
experiment theory suggests that the practical be carried out at neutral pH of around 6.9-10. A
suitable pH can be achieved by saturating the analyte solution with sodium hydrogen carbonate.
However, nothing was done to make sure, the pH does really stay in this optimum range. Errors
like overshooting beyond the endpoint and might have happened. Contamination of reagents was
also possible because of the use of shared reagents like silver nitrate and potassium chromate
indicator, were other students might not be very careful in preventing contamination.

CONCLUSION
Molarity of the solution of AgNO3 = 0.395M
Percentage of the chloride in the unknown sample = 61.84%

REFERENCES

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Mohr’s determination of chloride experiment
MUTETE RONALD | R164545P

1. Vogel I. Arthur, 1961, A Textbook of Quantitative Inorganic Analyses, 3rd edition, Longman
Publishing, London, page 40
2. Harris C. Daniel, 1991, Quantitative Chemical Analyses, 3rd edition, W.H freeman and
Company, New York, page 172
3. Pierre C. Willis, Haenisch L. Edward, 1954, Quantitative Analyses, 3rd edition, John Wiley
and Sons. Inc., New York, page 293
4. Flaschka A. H, Barnard J. A, Sturrock E.P, 1980, Quntitative Analytical Chemistry, 2nd
edition, Willard Grant Press, Boston, Massachusetts, p133
5. Skoog D, West D, Holler J, Crouch S, 2013, Fundamentals of Analytical Chemistry, 9th
edition, Brooks Cole, Belmont, USA, page 303.

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Mohr’s determination of chloride experiment

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