Blan Jericho Caloyloy Date Submitted: September 6, 2016

Justine Rose Escultero Date Finished: August 30, 2016

Therese Javellana

Experiment 4
Precipitation Titration: Determination of the Chloride in the Sample

I. Introduction
Titration is the analytical procedure in which the titrant from the buret is added to another
substance. Stochiometric reaction happens as the titrant is added until it will reach to the end
point. The purpose of titration is to determine concentration of the unknown substance (Fromm,
1997). One type of titration is precipitation titration which started in the early 18th century and
was considered as the oldest analytical techniques. Precipitation titrations are based on reactions
that yield ionic compounds of limited solubility. Only limited precipitating agents are used
because of the slow rate of appearance of precipitate (Skoog, et al., 2014). In this reaction, the
analayte and titrant form an insoluble precipitate that can serve as a basis for a titration
(LibreTexts.org, 2016).
Silver nitrate is an important precipitating reagent which can also be used for the
determination of the halogens, halogenlike anions, mercaptans, fatty acids, and several divalent
inorganic anions. When silver nitrate is used in titrations, it can be called as argentometric
titrations. Potassium chromate can serve as indicator in titrating chloride, bromide and cyanide
ions by reacting with silver ions to form a brick-red silver chromate precipitate in the
equivalence point region. As the silver nitrate solution is slowly added, a precipitate of silver
chloride forms
Ag+(aq) + Cl-(aq) --> AgCl(s)

According to the University of Canterbury, the indicator used is dilute potassium chromate
solution. When all the chloride ions have reacted, any excess silver nitrate added will react with
chromate ions to form a red-brown precipitate of silver chromate. This procedure is known as
Mohr’s method.
2Ag+(aq) + CrO42-(aq) --> Ag2CrO4(s)
II. Results and Discussion

Results

Table 1.1 Standardization of Silver Nitrate Solution

Primary Standard used: AgNO3
Formula mass of 1O standard:
% Purity of 1O standard: 99.8%

Trials 1 2 3
Weight of NaCl (g) 0.0594 0.0487 0.0589

Final Reading AgNO3 (ml) 12.5 21.4 31.6

Initial Reading AgNO3 (ml) 2.1 12.5 21.4
Volume AgNO3 used (ml) 10.4 8.9 10.2

Corrected Volume of AgNO3, ml 10.4 8.9 10.2

Molarity of AgNO3, M 0.1004 0.0967 0.1026

Average Molarity of AgNO3, M 0.0999

Titer NaCl (mg/mL) 3.56 3.43 3.64

Average Titer NaCl (mg/ml) 3.54

Table 1.2 Indicator Blank

Trials 1 2 3
Final volume AgNO3 (ml) 0.6 0.9 1.3
Initial volume AgNO3 (ml) 0.3 0.6 0.9
Net Volume AgNO3 (ml) 0.3 0.3 0.4
Average volume of AgNO3, (ml) 0.3

Table 1.3 Analysis of Unknown

Trials 1 2 3
Weight of the sample (g) 0.501 0.538 0.619
Final volume AgNO3 (ml) 5.7 10.4 16.7
Initial volume AgNO3 (ml) 1.3 5.8 10.4
Net Volume AgNO3 (ml) 4.4 4.6 6.3
Corrected volume of AgNO3, ml 4.4 4.6 6.3
mg Cl- of unknown 303.32 325.73 374.77
% Cl- of unknown 60.5 60.5 60.5
Average % Cl- of unknown 60.5
Discussion

The Mohr’s Method is a direct way of determining the chloride content of a sample. In
Mohr’s method, alkaline or alkaline earth chlorides react with silver nitrate in the presence of the
indicator potassium chromate (K2CrO4) for chloride determination. In this experiment, Mohr
titration was used to determine the amount of chloride in the unknown sample. It follows the
equation:

2Ag+ + CrO42- Ag2CrO4

The chromate indicator added to the concentration developed the red precipitate as it
reached the equivalence point. The end point takes place when the chloride ions react and forms
a precipitate. Lower concentrations of chromate are generally used because high concentrations
of chromate ion could cause misdetection of red silver chromate. Blank determination was also
used. Blank determination corrects the positive systematic errors in the Mohr method. These
errors become significant when concentrations are lower than 0.1 M. All steps of the chemical
analysis are performed without the presence of the analyte in blank determination. A solution of
chloride-free Calcium Carbonate (CaCO3) and the indicator potassium chromate was titrated
with standard silver nitrate solution. Calcium carbonate imitates the white precipitate of silver
chloride.

To indicate the concentration of standardized silver nitrate solution, the following

formula was used:

( )

( )

As indicated in the results, the resulting average molarity of the standardized silver nitrate
solution was 0.0999 M.

For the titer which refers to the strength of the solution determined through titration, a
different formula was used.

( )

For the determination of Cl in the sample, which is the objective of this experiment, the
following formula was used:

( ) ( )

As stated in the results, the masses of chloride in the sample were 303.32mg, 325.73 mg and
374.77 mg for trials one, two and three respectively. The calculations were done according to the
formula presented. The silver nitrate reacts with chloride ion in a 1:1 ratio. This reaction forms
silver chloride and the precipitate forms in the bottom of the flask. As the end point takes place,
the extra silver ions react with chromate ions to form the brownish red precipitate of silver
chromate.

III. Calculations

Standardization of AgNO3

Sample 1

( )

= 0.1004M

Sample 2

( )

Sample 3
( )

Titer

Sample 1

Sample 2

Sample 3
Chloride Determination

Sample 1

( ) ( )

Sample 2

( ) ( )

Sample 3

( ) ( )
IV. Conclusion
All titration processes are done in three trials. The average concentration of the
standardized silver nitrate needed to titrate sodium chloride solution (purity of the solid sodium
chloride is 99.8%)is 0.0999 M. The average titer (strength of the solution) of the sodium chloride
solution is 3.54 mg/mL. To minimize errors, blank determination was conducted and the average
volume of silver nitrate used in titrating the blank sample is 0.3 mL. The average percentage of
chloride found in the sample is 60.5%.

V. References
Determination of Chloride in Water by Mohr Method. (2015). Retrieved September 3, 2016 from
Hard and Soft Water website, http://hardsoftwater.com/determination-of-chloride-in-
water-mohr-method/
Fromm, James Richard (1997). Precipitation Titrations. Retrieved online:
http://www.3rd1000.com/chem101/chem104d.html

LibreTexts.org (2016). Precipitation Titrations. University of California. Retrieved online:

http://chem.libretexts.org/

Skoog D. A.; West D. M.; Holler F. J. Fundamentals of Analytical Chemistry, 9th Edition,
Thomson Learning, Inc, USA, 2012.

University of Canterbury. Determination of Chloride by Precipitation Titration with Silver

Nitrate - Mohr's Method. Retrieved online:
http://www.outreach.canterbury.ac.nz/chemistry/chloride_mohr.shtml