Name: Sittie Ayenah D. Dimaporo Instructor: Divine Angela G. Sumalinog, Ph.D.

Section: 1 CHE-B Date Experiment Performed: July 4,2019

Group No.: 4 Date Experiment Submitted: July 5, 2019

Experiment 5: Determination of Chloride using Mohr Method

ABSTRACT

Argentometric titration and Mohr’s method are the chemical processes used in the
experiment to test for the presence of chloride ions in a solution that involves a silver nitrate
solution. An indicator, potassium chromate is added to the analyte before it is titrated with silver
nitrate as the precipitating agent. Standardization of AgNO3 is conducted in order to compute the
AgNO3 concentration which will be vital in calculating the Cl- concentration of the unknown
sample. When the analyte is titrated with AgNO3, it forms a silver chloride precipitate, the
endpoint is marked when a brick red precipitate of AgCrO4 is formed. Three trials were
performed in order to gauge the accuracy and precision of the obtained Cl- concentration, which
is 0.0216 M, based from the theoretical value of 0.016 M. Due to personal error and method
error, a 35% error was calculated, but this can be counteracted by practicing good titration
techniques.

INTRODUCTION

Precipitation titrations are based upon reactions that yield ionic compounds of limited
solubility (Korkmaz, 2001). It requires a suitable precipitating agent in order to determine
halides like chlorides, bromides, and iodides present in a solution. The use of AgNO3 as a
precipitating agent is also known as argentometric method in which the application of the Mohr’s
method in the experiment will most likely obtain actual values. The process of the Mohr’s
method involves the use of AgNO3 as a titrant in the presence of an indicator like K2CrO4 in order
to determine the chloride ions in the solution. The precipitating agent will react with the
unknown chloride-containing solution to form AgCl as a precipitate in which at this point, all the
chloride ions will be used up.

The reaction is represented by,

+ -
Ag + Cl → AgCl (s)

The excess silver ions will then react with the indicator that will form Ag2CrO4 which
will exhibit a visible brick-red precipitate that will serve as the endpoint of the titration. The
objective of the experiment is to determine the amount of chloride ion concentration that exists
in a solution of an unknown sample by titrating it with AgNO3.

MATERIALS AND METHODOLOGY

Before starting the experiment the materials used such as the Pocari Sweat; graduated
cylinder; volumetric flask; pipette; AgNO3 solution; K2CrO4; and titration setup were prepared.

The solid AgNO3 was dried for 1 hour at 100 C and cooled, and 8.5 g of it was dissolved
in a 100 ml distilled water. It was transferred into a 500 ml volumetric flask and filled to mark
with distilled water. In a 200 ml distilled water, 1.00 g of K2CrO4 was dissolved and stored in a
reagent bottle.

A 50 ml solution of 0.1 M NaCl was diluted into a 250 ml volumetric flask, and was then
filled to mark with distilled water. In an Erlenmeyer flask, 10 ml aliquot of diluted NaCl solution
was pipetted into it, adding 50 ml of distilled water and 1 ml of chromate indicator. The NaCl
solution was then titrated with the AgNO3 solution until the first hint of red precipitate appears.
Two more trials were made in the standardization of AgNO3 solution.

A 50 ml of Pocari Sweat sample was then diluted into a 250 ml volumetric flask, and
filled to mark with distilled water. In an Erlenmeyer flask, a 10 ml aliquot of the diluted sample
was pipetted into it, 50 ml of distilled water, and 1 ml of chromate indicator was then added. The
sample was titrated with AgNO3 solution until the first hint of red precipitate appears. Two more
trials were made in the determination of chloride ions of the unknown sample.
RESULTS AND DISCUSSIONS

Table 1. Standardization of AgNO3 solution

Molarity of NaCl solution (M) 0.1 M

Trial 1 2 3

Initial Volume of AgNO3 (mL) 45.3 42.9 40.8

Final Volume of AgNO3 (mL) 42.9 40.8 35. 3

Volume of AgNO3used (mL) 2.4 2.1 2.5

Molarity of AgNO3 (M) 0.0833 0.0952 0.0800

Average Molarity of AgNO3 (M) 0.0862

Table 2. Chloride Content of Unknown Sample

Trial 1 2 3

Initial Volume of AgNO3 (mL) 38.8 mL 37.7 mL 37.3 mL

Final Volume of AgNO3 (mL) 37.7 mL 37.73 mL 36.8 mL

Volume of AgNO3 used (mL) 0.6 mL 0.4 mL 0.5 mL

Molarity of Cl- in sample (mmol/mL) 0.0259 0.0172 0.0216

Average Molarity of Cl- in sample (M) 0.0216

Standard deviation 0.004310

Relative Standard deviation 19.95%

Theoretical Molarity of Cl- in sample 0.016

Percent error (%) 35%

 The data as presented in Table 1 shows three trials conducted in the standardization of the
silver nitrate solution. The average molarity of AgNO3 solution is calculated to be 0.01722 M.

In table 2, three trials of titration on the unknown sample is conducted that yields an
average molarity of Cl of 0.0216 M; a standard deviation of 0.004310; a relative standard
deviation of 19.95%; and a percent error of 35%.

These values represent the quality and reliability of the data from the experiment. The
average molarity of the AgNO3 solution and Cl ion determines the central tendency of the
measured values for replicate analysis. The relative standard deviation indicates the random error
that are inevitably present in any experiment. The percent error shows how accurate or precise
the standard deviation is from the theoretical value.

Considering the reaction, Ag+ (aq) + Cl- (aq) → AgCl (s), it shows that when AgNO3 and
NaCl reacts, it forms AgCl which is insoluble in water that can be physically observed as a white
precipitate before it reaches the endpoint. One probable cause of error from the experiment is
personal error that is why it is important to practice good mixing technique when titrating the
analyte with the titrant in order for the ions to touch and react with each other completely. It is
best to be extra cautious when titrating to avoid exceeding the endpoint by controlling the rate of
titrant that is dispensed into the analyte. Method errors are also unavoidable thus, Mohr method
must be executed under conditions of pH 6.5 to 9 due to the fact that silver ions can be
eliminated at higher pH, and eliminate chromate ions at low pH as well, in which it can affect the
accuracy in determining the endpoint and the resulting chloride concentration in the unknown
solution.

CONCLUSION AND RECOMMENDATIONS

It can be concluded that the least amount of volume of AgNO 3, which is 2.1 mL on trial 2,
among the three trials in the standardization of AgNO3 solution yielded a higher molarity
concentration of AgNO3 at 0.0952 M. This implies the endpoint at which titration is stopped
because of the visibility of a brick red precipitate, wherein excess silver ions reacts with the
indicator. Contrarily, the largest volume of AgNO3, which is 0.6 mL from trial 1, among the three
trials on the test for the chloride ion in the unknown sample yields higher Cl- concentration of
0.0259 M. The average molarity concentration of chloride ions obtained, which is 0.0216 M,
from the three trials were precise which is somewhat close to the theoretical true value of 0.016
M so in essence, systematic errors such as personal error and method error were encountered.

Errors can be avoided in conducting the experiment primarily by applying good titration
techniques. This can be done by controlling the rate of titrant that flows into the analyte by
carefully adjusting the stopcock of the burette, and good mixing is also needed so that the two
solutions can react completely react with each other. The slow addition of silver nitrate into the
chloride-containing unknown sample is important because it allows the silver chloride to
precipitate first before it can precipitate with the indicator which is the potassium chromate.

REFERENCES

1. Korkmaz, D. (2001). Precipitation titration:“Determination of Chloride by the Mohr

Method”. Methods, 2(4).

2. Sheen, H. T., & Kahler, H. L. (1938). Effect of ions on Mohr method for chloride
determination. Industrial & Engineering Chemistry Analytical Edition, 10(11), 628-629.

3. Skoog, D. A., West, D. M., Holler, F. J., & Crouch, S. (1996). Fundamentals of
Analytical Chemistry, Thomson Learning. Inc, USA.

4. Stewart, D. (2019, March 02). Precipitation Titration Techniques. Retrieved from

https://sciencing.com/precipitation-titration-techniques-8665193.html

5. Gillespie, C. (2019, March 02). Definition of Endpoint Titration. Retrieved from

https://sciencing.com/definition-endpoint-titration-5172167.html
APPENDIX

C1V1=C2V2

(0.1 M NaCl)(0. 05 L NaCl)

C2=
0.250 L

C2= 0.02 M

Molarity of AgNO3

( VxM ) NaCl
V AgNO 3

Trial 1

(0.02 M )(10 ml)

2.4 mL

= 0.0833 M

Trial 2

(0.0 2)(10 ml)

2.1mL

= 0.0952 M

Trial 3

(0.0 2)(10 ml)

2.5mL

= 0.0800 M
Average Molarity

0.0833+0.0952+0.0800
3
= 0.0862 M

Molarity of Cl- in sample

1mmol Cl 1
V AgNO3 * M Agno * * * df
1mmol Ag V of sample

Trial 1

1mmol Cl 1 250 mL
0.6 ml * 0.0862 M * * *
1mmol Ag 10 m L 5 0 mL

= 0.0259 M Cl-

Trial 2

1mmol Cl 1 250 mL
0.4 mL * 0.0862 M * * *
1mmol Ag 10 m L 5 0 mL

= 0.0172 M Cl-

Trial 3

1mmol Cl 1 250 mL
0.5 ml * 0.0862 M * * *
1mmol Ag 10 m L 5 0 mL

= 0.0216 M Cl-

Average Molarity of Cl-

0.0259+0.0172+0.0216
3
=0.0216 M

Standard Deviation

(0.0259−0.0216)2 +(0.0172−0.0216)2 +( 0.0216−0.0216)2

√ 3−1

=0.004310

Relative Standard Deviation

0.004310
* 100
0.0216

= 19.95%

Percent Error

¿ 0.0216−0.016∨ ¿ ¿
0.016 * 100

= 35%