Expt7 Determination of Chloride Ions Concentration by Precipitation Titration Method

Experiment No.
Determination of Chloride Ions Concentration by Precipitation Titration Method
Group No. 4 Date Due: February 12, 2015
Group Members: Date Performed: January 29, 2015
Seagal Asjali
Lucen Jane Paden
Sheena Mae A. Resando
Name:
Sheena Mae A. Resando
BS Chemistry II
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Abstract
This experiment aims to determine the percent weight by volume of chloride ions
in water samples and also to determine the percent by weight of chloride ions in cheese
sample.
By knowing the stoichiometry and moles consumed at the end point, the amount of
chloride in an unknown sample can be determined. This report describes experiments aimed
at determining the concentration of chloride in different water samples and in cheese sample.
From the experiment, the percent chloride present in different water samples
(ZCWD, Mineral water, Sea water) and in EDEN cheese sample was obtained. ZCWD has
0.00141% chloride, mineral water sample has 0.00106%, which has the lowest percent
chloride among the three samples and sea water has 2.14333% chloride, which has the
highest percent. Replicate 1 in EDEN cheese sample has the average percent chloride of
2.53670 ± 0.00577% and replicate 2 has 2.51330 ± 0.00577% chloride.
Chapter I
Introduction
Titration is a process by which the concentration of an unknown substance in

solution is determined by adding measured amounts of a standard solution that reacts with the
unknown. Then the concentration of the unknown can be calculated using the stochiometry of
the reaction and the number of moles of standard solution needed to reach the so called end
point.
Precipitation titrations are based upon reactions that yield ionic compounds of
limited solubility. The most important precipitating reagent is silver nitrate. Titrimetric
methods based upon silver nitrate are sometimes termed argentometric methods. Potassium
chromate can serve as an end point indicator for the argentometric determination of chloride,
bromide and cyanide ions by reacting with silver ions to from a brick-red silver chromate
precipitate in the equivalence point region.
The Mohr method uses chromate ions as an indicator in the titration of chloride
ions with a silver nitrate standard solution. After all the chloride has been precipitated as
white silver chloride, the first excess of titrant results in the formation of a silver chromate
precipitate, which signals the end point. The reactions are:
Ag+ + Cl- AgCl (s)
2Ag+ + CrO42- Ag2CrO4 (s)
at determining the concentration of chloride in a solid sample.
Volhard method uses a back titration with potassium thiocyanate to determine the
concentration of chloride ions in a sample. Before the titration an excess volume of a silver
nitrate solution is added to the solution containing chloride ions, forming a precipitate of
silver chloride. The indicator Fe(III), ferric ion, is then added and the solution is titrated with
the potassium thiocyanate solution. The titrate remains pale yellow as the excess (unreacted)
silver ions react with the thiocyanate ions to form a silver thiocyanate precipitate.
This experiment aims to determine the percent weight by volume of chloride ions
in water samples and also to determine the percent by weight of chloride ions in cheese
sample.
Chapter II
Methodology
MOHR METHOD
1. Preparation of 5% K2CO4 and 0.10 M AgNO3 Solution
a. Preparation of 5% K2CrO4 Solution
About 1.0 grams of K2CrO4 was weighed and dissolved in 20 ml distilled water.
b. Preparation of 0.01 M AgNO3 Solution
About 9.0 grams of AgNO3 was weighed in a 50 ml beaker and small amount of
distilled water was added to dissolve. The solution was transferred into a 500 ml volumetric
flask. More distilled water was added into the beaker and then transferred into the flask.
Distilled water was added to the flask up to mark.
2. Standardization of 0.01 M AgNO3 against Primary Standard NaCl
About 0.2500 grams of dried NaCl which was heated at 110°C for two hours was
weighed into an Erlenmeyer flask and 100 ml distilled water was added to dissolve the
sample. Small amount of NaHCO3 was also added to adjust the pH of the solutions until
effervescence ceased. Another 2 ml of 5% K2CrO4 was added and then titrated with the first
appearance of red Ag2CrO4.
3. Analysis of Chloride Ion Concentration in Water Sample
Three 250-ml Erlenmeyer flasks were filled with 25 ml water. Small quantity of
NaHCO3 was added to adjust pH of the solution. Two (2) ml K2CrO4 solution was also
added into it and then titrated with standard 0.01 M AgNO3 to the first appearance of red
Ag2CrO4. The other two flasks were also tested repeatedly.
Chapter III
Results and Discussion
The tables below show the obtained data on the determination of percent chloride in
different water samples using Mohr method and percent chloride present in cheese using the
Volhard method.
Table 7.1 Standardization of 0.100 M Silver nitrate against Primary standard NaCl
First trial Second trial

Wt. NaCl (g) 0.2500 ± 0.0001 0.2498 ± 0.0001
Calculated no. moles silver 0.004277 0.004274
nitrate (mol)
Titrations
Final volume (mL) 47.60 ± 0.01 44.20 ± 0.01
Initial reading (mL) 4.70 ±0.01 0.90 ± 0.01
Volume of titrant (mL) 42.90 ± 0.01 43.30 ± 0.01
Standardized conc. Of silver 0.0997 0.0987
nitrate (M)
Mean and standard deviation 0.0992 ± 0.0007
The first table above shows the weight of NaCl, volume of titrant used, calculated
moles of silver nitrate, concentration of the standardized silver nitrate in molarity and its
mean and standard deviation.
Table 7.2 Analysis of Cl- ions in water samples using Mohr method
Group No. Type of Trials Volume of Volume of Amount of Cl %Cl in sample

water sample titrant (mL) ions present (w/v)
sample (mL) (grams)
1 0.40 ± 0.01 0.0014067 0.0014067
Group 1 ZCWD 2 100.00 ± 0.40 ± 0.01 0.0014067 0.0014067

water 0.01
3 0.40 ± 0.01 0.0014067 0.0014067
1 0.30 ± 0.01 0.0010603 0.0010603
Group 4 Mineral 2 100.00 ± 0.30 ± 0.01 0.0010603 0.0010603

water 0.01
3 0.30 ± 0.01 0.0010603 0.0010603
1 15.30 ± 0.01 0.05380 2.15
Group 5 Sea water 100.00 ±
2 15.29 ± 0.01 0.05377 2.15
0.01
3 15.15 ± 0.01 0.05328 2.13
The second table shows the obtained amount of chloride ions in different water
samples for three trials and its percent in weight by volume. The percent weight by volume of
chloride was obtained through multiplying the volume and molarity of Ag+ and relates it to
the moles of chloride ions present by stoichiometry, divided by the volume of water sample
times 100. This is merely associated with the Mohr method. The working formula:
%Cl in water sample = MAg+ VAg+ × ×
×100
VH2O sample
Based from the calculated data, sea water has the highest amount of chloride present
among the three samples tested with 2.14% chloride and the lowest is the mineral water
sample with 0.00106% chloride.
Table 7.3 Analysis of Cl- ions in EDEN cheese using Volhard method
Group no. Cheese Trials Mass of cheese Volume of Amount of % Cl in

sample sample (g) titrant (mL) Cl- in cheese
sample sample
(grams)
1 6.60 ± 0.01 0.1524 2.54
Group 2 2 6.003 ± 00.001 6.60 ± 0.01 0.1524 2.54
EDEN 3 6.70 ± 0.01 0.1521 2.53

Cheese
1 7.13 ± 0.01 0.1506 2.51
Group 3 2 6.004 ± 00.001 7.00 ± 0.01 0.1510 2.52
3 7.09 ± 0.01 0.1507 2.51
This table shows the obtained amount of chloride (moles) in EDEN cheese sample in
separate replicates for three trials and the percent chloride in cheese sample. Volhard method
was used in this part. The working formula:
%Cl in cheese = (MAg+ VAg+added – MKSCNVtitrant) ×
grams cheese sample ×100
Chapter IV
Summary and Conclusion
at determining the concentration of chloride in different water samples and in cheese sample.
From the experiment, the percent chloride present in different water samples
(ZCWD, Mineral water, Sea water) and in EDEN cheese sample was obtained. ZCWD has
0.00141% chloride, mineral water sample has 0.00106%, which has the lowest percent
chloride among the three samples and sea water has 2.14333% chloride, which has the
highest percent. Replicate 1 in EDEN cheese sample has the average percent chloride of
2.53670 ± 0.00577% and replicate 2 has 2.51330 ± 0.00577% chloride.
Appendix
Sample calculations:
MOHR METHOD
%Cl = ×100
= 0.0014067% Cl- in water sample (ZCWD water)
VOLHARD METHOD
%Cl = ×100
= 2.54% Cl- in EDEN cheese sample
Reference
 http://academic.brooklyn.cuny.edu/esl/gonsalves/tutorials/Writing_a_Lab_Report/xPr
ecipitation%20Titration%20edited%203.pdf
 www.wikipedia.org
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Experiment No.

Determination of Chloride Ions Concentration by Precipitation Titration Method

Group No. 4 Date Due: February 12, 2015

Group Members: Date Performed: January 29, 2015

Lucen Jane Paden

Sheena Mae A. Resando

Sheena Mae A. Resando

Titration is a process by which the concentration of an unknown substance in

Ag+ + Cl- AgCl (s)

2Ag+ + CrO42- Ag2CrO4 (s)

1. Preparation of 5% K2CO4 and 0.10 M AgNO3 Solution

a. Preparation of 5% K2CrO4 Solution

b. Preparation of 0.01 M AgNO3 Solution

2. Standardization of 0.01 M AgNO3 against Primary Standard NaCl

3. Analysis of Chloride Ion Concentration in Water Sample

Results and Discussion

First trial Second trial

Group No. Type of Trials Volume of Volume of Amount of Cl %Cl in sample

1 0.40 ± 0.01 0.0014067 0.0014067

Group 1 ZCWD 2 100.00 ± 0.40 ± 0.01 0.0014067 0.0014067

1 0.30 ± 0.01 0.0010603 0.0010603

Group 4 Mineral 2 100.00 ± 0.30 ± 0.01 0.0010603 0.0010603

1 15.30 ± 0.01 0.05380 2.15

%Cl in water sample = MAg+ VAg+ × ×

Group no. Cheese Trials Mass of cheese Volume of Amount of % Cl in

1 6.60 ± 0.01 0.1524 2.54

Group 2 2 6.003 ± 00.001 6.60 ± 0.01 0.1524 2.54

EDEN 3 6.70 ± 0.01 0.1521 2.53

Group 3 2 6.004 ± 00.001 7.00 ± 0.01 0.1510 2.52

3 7.09 ± 0.01 0.1507 2.51

%Cl in cheese = (MAg+ VAg+added – MKSCNVtitrant) ×

grams cheese sample ×100

Summary and Conclusion

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