Name: DAYAO, Marco Angelo C. Instructor: Engr. Noel S. Sabarillo, M.Sc.

Section: 1-ChE-C Date Experiment Performed: July 4, 2019

Group No.: 4 Date Report Submitted: July 9, 2019

Experiment 5: DETERMINATION OF CHLORIDE BY MOHR METHOD

ABSTRACT: The amount of caffeine in a commercial teabag, Lipton ____was quantitively

determines using Liquid-Liquid Extraction. The Analyte was placed in 100 ml of boiling water and
was then squeezed, collecting the extract. It was later placed in an iced-bath colled and colled to
room temperature. The Extract was placed in a separatory funnel mixed with 1 gram of Na2CO3.
Twenty milliliters (20ml) was added to the funnel for extraction, releasing gas pressure regularly
and collecting the liquid lower layer . This was done three times. Anhydrous Na2SO4 was then
added, eliminating traced H20 from the solution. It was then heated in a weighed beaker and
allowed to evaporate. The crude caffeine with beiker was then weighed resulting to : ____

The concentration of chloride in a commercial drink, Pocari sweat was quantitively determined
using Mohr Method. The analyte was diluted and mixed with 1 ml of chromate indicator. With this
technique, the analyte was then titrated using 0.1M AgNO3 Solution. The appearance of the brick-
red color marked the endpoint of the titration. Three trials were performed. In doing so, it was
found that the analyte’s Chloride concentration resulted in an average of 0.01723 M which was
relatively close to the actual value of 0.0160 M.

Keywords: Titration, Mohr Method, Chloride Concertation, Chromate Indicator, AgNO 3 Titrant

INTRODUCTION

Precipitation titrations are forms of titration used to determine halides concentration of a

specific substance. These type of titrations use a precipitating agent to the analyte to form an
insoluble precipitate.(Stewart,2018) Titrations involving the used of silver nitrate (AgNO3 ) as
titrants are knowns as argentometric titrations.The most well-known methods are Mohr, Fajans,
and Volhard.
The Mohr method is used for determining the Chlorides content of the analyte. The silver
ions (Ag+) reacts with the chloride ions (Cl-) to form AgCl [ Ag+ + Cl- → AgCl(s)]. The Mohr method
 uses chromate ions, potassium chromate (K2CrO4) in this experiment, as an indicator in the
titration of chloride ions with a silver nitrate standard solution. With the chromate added in, the
solution will give a lemon-yellow color. As silver chloride (AgCl) precipitated first, the solution
turns cloudy due to the white color of the precipitate. When all the chloride ions reacted with Ag+
ions, the excess silver ions react with chromate ions(CrO4 2-) to produce silver (II) chromate [2
Ag+ + CrO42- → Ag2CrO4]. Silver (II) chromate gives a brick-red color of precipitate that marks
the endpoint of the titration. With this, the chloride concentration of an unknown sample could
now be determined.

In this experiment, the Mohr method was used to determine the chloride molar concentration
of a commercial drink, namely, Pocari Sweat. Given the true value, the sample was analyzed
whether it contained a higher or lower concentration of chloride. Moreover, it was also used for
determining the molar concentration of the prepared NaCl solution. Waste containing Silver ions
were separated for the recovery of silver metal.

MATERIALS AND METHODOLOGY

Reagents and Equipment

Commercial drink sample (Pocari Sweat) and K2CrO4 were prepared with graduated
cylinders, 250ml volumetric flask, beakers, pipette, dropper, funnel, Erlenmeyer flask, glass rods,
titration set-up and bond paper for a white background. The AgNO3, 0.1 M NaCl solution were
obtained from the laboratory pre-prepared

Procedure

The titration set-up was prepared and 25ml of AgNO3 was transferred to the burette using
a pipette. Approximately 1.000 gram of K2CrO4 was weighed concurrently using an analytical
balance and dissolved with 20ml distilled water in a beaker. Fifty milliliters (50 ml) of 0.1M NaCl
was diluted in a 250ml volumetric flask with distilled water that was then filled to mark. The
analysts pipetted three samples of 10 ml aliquot portion of the diluted NaCl into different
Erlenmeyer flasks and further diluted to 50 ml solutions. A beaker was used as a substitute for an
Erlenmeyer flask. The analyst added 1 ml of the chromate indicator to each of the NaCl samples
and was titrated till endpoint with the AgNO3 one at a time. The initial and final volume of the
titrant was recorded for each titration.
 The commercial drink(pocari sweat) sample was obtained subsequently. The analysts
measured 50 ml of the sample and diluted to a 250 ml Volumetric flash in a similar manner as
the NaCl Solution. Then, 10 ml aliquot portion was transferred and added with 50ml distilled water
and 1ml chromate indicator to an Erlenmeyer flask. The aliquot portion was done 3 times in
separate Erlenmeyer flasks. The samples were titrated with the AgNO3 Solution one at a time and
all the waste that contains AgNO3 was discarded in a separate waste bottle for the extraction od
Silver metal. A bond paper was used as a white background to help the analyst determine the
appearance of brick-red color in the solution.

RESULTS AND DISCUSSION

Figure 1.1. NaCl Sample before Titration Figure 1.2. NaCl Solution after Titration

Figure 1. Pocari sweat samples after titration

Table 1.0 Standardization of AgNO3

Standardization of AgNO3.
Molarity of NaCl Solution 0.1 M
Trial 1 2 3
 Initial Volume of AgNO3 26.8 ml 29.5 31.4
Final Volume of AgNO3 28.8ml 31.4 33.55
Volume used of 2ml 1.9 ml 2.15 ml
AgNO3
Molarity of AgNO3 0.1M 0.1053M .0930 M
Average Molarity of AgNO3 0.0994 M

Table 2.0 Chloride Content of Pocari Sweat

Chloride Content
Trial 1 2 3
Initial Volume of AgNO3 39.5 ml 37.9 ml 38.8 ml
Final Volume of AgNO3 40.5 ml 38.8 ml 39.5 ml
Volume used of 1 ml .09 ml .07 ml
AgNO3
Molarity of Cl- in the .01988 M .017892 M .013916 M
sample
Average Molarity of Cl- in 0.01723 M
the sample
Standard Deviation 3.01 x10-3
Relative Standard 174. 70
Deviation
Theoretical Molarity of Cl- 0.0160 M
in the sample
Percent Error % 7.68%

Figure 1.1 showed the 3 trials of NaCl before titration. The yellow-lemon color was visible.
While Figure 1.2 showed the solutions at the endpoint. The volume used of AgNO3 for
standardization was recorded in table 1.0. Using the results in table 1.0, the molar concentration
of AgNO3 was determined. The volumes of the titrant used in the 3 trials were 2 ml, 1.9 ml, and
2.15ml respectively. Trial 1 contained 0.1M AgNO3, trial 2 contained 0.1053 M AgNO3 and trial
contained 0.0930 M AgNO3 The 3 trials averaged at 0.0994 M, whereas the true value is 0.1 M.
 On the other hand, Table 2.0 showed the data in terms of Molar Concentration of Chloride
ion in the commercial drink sample. The volumes of the titrant used in the 3 trials of pocari sweat
were 1.00 ml, 0.9 ml, and 0.7 ml respectively. The same color of endpoint are shown in figures
1.1 and 2. The analyst failed to dilute the sample into 250 ml volumetric flask. Which corresponds
to the error in the computation for the molarity of Chloride. Instead, it was diluted to 100 ml. To
adjust the error in mathematical terms, the 250ml factor on Eqn. 2 was changed to 100ml factor
in Eqn 3 below. Eqn 3 was used to compute the molarity of the chloride ions.

Standardization of AgNO3
25 𝑚𝑙 1 𝑚𝑜𝑙 𝐴𝑔+ 1
MAgNO3= 0.100𝑀 𝑁𝑎𝐶𝑙 𝑥 𝑥 10 𝑚𝑙 𝑥 𝑥 Eqn.1
250 𝑚𝑙 1 𝑚𝑜𝑙 𝐶𝑙 𝑉 𝐴𝑔𝑁𝑂3

Molar Concentration of Cl-

1 𝑚𝑜𝑙 𝐶𝑙 1 250 𝑚𝑙
MCl= M AgNO3 x V AgNO3 𝑥 1 𝑚𝑜𝑙 𝐴𝑔 𝑥 10𝑚𝑙 𝑥 50 𝑚𝑙
Eqn. 2

Adjusted Formula (Molar Concentration of Cl-)

1 𝑚𝑜𝑙 𝐶𝑙 1 100 𝑚𝑙
MCl= M AgNO3 x V AgNO3 l 𝑥 𝑥 𝑥 Eq. 3
1 𝑚𝑜𝑙 𝐴𝑔 10𝑚𝑙 50 𝑚𝑙

Using Eqn.1 to solve the molarity of the titrant, the molarity of the chloride was solved using
Eqn.3. The values were 0.01988 M, 017892 M and 0.0189156 M for the 3 trials respectively. An
average of 0.01723 M was calculated from the given values of the 3 trials. Given the true value
of the Chloride concentration: 0.016 M, and the average concentration of the 3 trials, the percent
error was obtained with a value of 7.68%

With these findings, the method of titration was proven to give accurate and precise results;
especially when the procedure was strictly followed with minimal to no-error made by the analysts.
The solution needed a good mixing so that a sharp and reproducible endpoint was achieved and
to ensure no silver chromate form before equivalence point. Moreover, silver chromate that
formed before the endpoint could lead to errors in the data and experiment. A white precipitate
was first to form to complete the reaction of all the Chloride ions with Ag+ ions in the sample. The
red color indicated that all the chloride ions were already consumed and reacted with Ag+ ions
and the CrO4 ions were reacting with Ag2CrO4 .

Multiple trials were required so that the analysts were familiarized with the color end point
of the titration. The Mohr titration should be carried out under the conditions of Ph 6.5 to 9
because silver ions could be removed by the precipitation with hydroxide ions (AgOH). At low
pH, the chromate ions may be removed by an acid-base reaction to form hydrogen chromate
(H2CrO4) ion or dichromate ions, affecting the accuracy of the endpoint.

CONCLUSIONS AND RECOMMENDATIONS

The experiment’s objectives were achieved. The concepts of Mohr’s method and stoichiometry
to determine the molar concentration chloride from different solutions in the experiment was
practiced . Precise, and accurate measurement of dilution was highly encouraged in order to have
a favorable result in the activity. Upon obtaining 7.68% error, the source of the error could be
found in the dilution of the sample. It is recommended to obtain a composite sample of the
commercial drink rather than obtaining an increment of a gross sample from a single batch. Using
separate glass wares or cleaning glassware thoroughly especially the burette is advisable. Lastly,
being familiar with the color of the endpoint could prevent any under or over titration of the sample.
In doing so, the error could be lessened, and the value of the error would be smaller.

REFERENCES

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

https://sciencing.com/precipitation-titration-techniques-8665193.html
 College of Science, University of Canterbury. (n.d.). Determination of Chloride Ion
Concentration by Titration (Mohr’s Method). Retrieved July 7, 2019, from
https://www.canterbury.ac.nz/media/documents/science-outreach/chloride_mohr.pdf
APPENDIX AND DATE SHEET

25 𝑚𝑙 1 𝑚𝑜𝑙 𝐴𝑔+ 1
Trial 1 MAgNO3= 0.100𝑀 𝑁𝑎𝐶𝑙 𝑥 250 𝑚𝑙 𝑥 10 𝑚𝑙 𝑥 1 𝑚𝑜𝑙 𝐶𝑙
𝑥 2𝑚𝑙𝐴𝑔𝑁𝑂3 = 0.1M
25 𝑚𝑙 1 𝑚𝑜𝑙 𝐴𝑔+ 1
Trial 2 MAgNO3= 0.100𝑀 𝑁𝑎𝐶𝑙 𝑥 250 𝑚𝑙 𝑥 10 𝑚𝑙 𝑥 1 𝑚𝑜𝑙 𝐶𝑙
𝑥 1.9 𝑚𝑙 𝐴𝑔𝑁𝑂3 = 0.1053 M
25 𝑚𝑙 1 𝑚𝑜𝑙 𝐴𝑔+ 1
Trial 3 MAgNO3= 0.100𝑀 𝑁𝑎𝐶𝑙 𝑥 250 𝑚𝑙 𝑥 10 𝑚𝑙 𝑥 1 𝑚𝑜𝑙 𝐶𝑙
𝑥 2.15 𝑚𝑙 𝐴𝑔𝑁𝑂3 = 0.0930 M
0.1+0.1053+0.0930
Average Molarity= 3
= 0.0994 M AgNO3
1 𝑚𝑜𝑙 𝐶𝑙 1 100 𝑚𝑙
Trial 1 MCl = 0.0994M AgNO3 x 1ml AgNO3 = 𝑥 1 𝑚𝑜𝑙 𝐴𝑔 𝑥 10𝑚𝑙 𝑥 50 𝑚𝑙
= 0.01988M
1 𝑚𝑜𝑙 𝐶𝑙 1 100 𝑚𝑙
Trial 2 MCl = 0.0994M AgNO3 x 0.9 ml AgNO3 𝑥 1 𝑚𝑜𝑙 𝐴𝑔 𝑥 10𝑚𝑙 𝑥 50 𝑚𝑙
= 0.01783 M
1 𝑚𝑜𝑙 𝐶𝑙 1 100 𝑚𝑙
Trial 3 MCl= 0.0994M AgNO3 x 0.7 ml AgNO3 l 𝑥 1 𝑚𝑜𝑙 𝐴𝑔 𝑥 10𝑚𝑙 𝑥 50 𝑚𝑙
=0.013916 M
 0.01988+0.01783+0.013916
Average Molarity= 3
= 0.01783 M Cl-

|0.01783 − 0.0160|
% 𝑬𝒓𝒓𝒐𝒓 = × 100% = 𝟕. 𝟔𝟖%
0.0160