Gaus Nadela BioSci1-A

Angelou Puyo BS BioMed

Shaira Cogollodo
Submitted to: Dr. Nathan Ray Alim, PhD.
Analytical Chemistry Lab Report
Complex Formation Titrimetry: Determination of Hardness in Water

Objectives:

The objectives of this experiment are:

1. To learn how to standardize a solution of ethylenediaminetetraacetic acid (EDTA).

2. To determine the hardness of a water sample by measuring the amount of Calcium
present; and
3. To identify the hardness of the unknown solution as ppm CaCO3 and calculate the
average ppm CaCO3, SD and RSD.

Outline of Experiment (Steps)

A. Preparation of EDTA solution

Quantitatively transfer the salt to When the entire solid has

Weigh about 1.860
grams of the salt in
the analytical balance.
a 500 mL beaker. Add about 300
mL distilled water and stir.
Dissolution may take 15 minutes
or longer.
dissolved, quantitatively transfer
the EDTA solution to a 500 mL
volumetric flask. Wash the beaker
with a stream of distilled water and
dilute the solution to the mark.

B. Standardization of EDTA solution

Weigh accurately Quantitatively transfer the salt to a 250

Let the solution cool
0.1500 grams of mL beaker, add 50 mL distilled water
and a few drops of concentrated HCl
down into room
CaCO3 in the
to dissolve the salt. Do not add more temperature.
analytical balance
than 1 mL of the acid. Boil the solution
gently to near boiling to remove CO2.

Titrate the solution with Pipet out 20 mL of the Quantitatively transfer

0.01 M EDTA solution
until the color changes
from red to pure blue.
Ca2+ solution to a 250 mL
the solution to a 100
erlenmeyer flask. Add 1 mL
of pH 10 buffer, 1 mL of mL volumetric flask
MgEDTA solution and 3 to and dilute to the mark.
4 drops of Erio T indicator.
 Perform at least 5
trials.
C. Analysis of unknown solution
You will be assigned to a
particular volume of
unknown solution to be
used throughout the
experiment.
Titrate the unknown
solution with 0.01 M EDTA
until the color changes from
red to pure blue.
Perform at least three
trials.
D. Analysis of hardness in water
Collect about 1 liter of
water sample.
Calculate the hardness of
the water sample as ppm
CaCO3. Calculate the
average ppm CaCO3, SD
and RSD.
Calculate the Molarity of the
EDTA solution. Calculate
the M EDTA, SD and RSD.
Pipet out the assigned Dilute the solution to the
volume of the unknown mark and homogenize the
solution into a 250 mL mixture. This solution
volumetric flask. would serve as your
unknown.
Add 1 mL of pH 10 Transfer 50.00 mL
buffer, 1 mL of MgEDTA aliquots of the unknown
solution and 3 to 4 drops solution into 250-mL
of Erio T indicator. Erlenmeyer flasks.
Calculate the hardness of
the unknown solution as
ppm CaCO3. Calculate the
average ppm CaCO3, SD
and RSD.
Pipet 20 mL of the water Titrate the unknown
sample into a 250 mL
solution with 0.01 M EDTA
erlenmeyer flask, add 1 mL of
pH 10 buffer, 1 mL of MgEDTA
until the color changes from
red to pure blue.
solution and 3 to 4 drops of Erio
T indicator.
If the volume of EDTA
Perform at least three solution exceeds 40 mL,
trials. reduce the volume of water
sample for the titration.
Data and Results
A. Standardization of EDTA

Mean of EDTA = 0.010466

Sd = 6.44x10-5
%RSD = 0.6153 or 62%

B. Unknown Sample

Mean of ppm CaCO3 = 1653.673

Sd of CaCO3= 10.55
%RSD = 0.64 or 64%

C. Analysis of Hardness of Water

Water Sample: River water

Mean of ppm CaCO3 = 239.96

Sd of CaCO3= 19.89
%RSD = 8.29%
Results and Discussion
In this experiment, complexometric titration is involved. Complexiometric titration is a form
of volumetric analysis in which the formation of a colored complex is used to indicate the end
point of a titration. It is another example of classical titrimetry analysis which are usually capable
of very high precision and accuracy, however, the problem is that classical methods are much
slower and less sensitive compared to the modern instrumental methods of analysis.

The experiment was divided into four procedures. The first procedure involves the
preparation of EDTA wherein the students were tasked to first weigh about 1.860 grams of the
salt in the analytical balance. After that, they quantitatively transfer the salt to a 500 mL beaker
and added about 300 mL of distilled water and stirred it for more than 15 minutes. After the entire
solid was dissolved, they transferred the EDTA to a 500 mL volumetric flask where it is diluted.

The second procedure involves the standardization of EDTA solution wherein the students
weighed 0.1509 grams of CaCO3 and then transferred it to a 250 mL beaker and added about 50
mL distilled water together with a few drops of concentrated HCl to dissolve the salt. After that,
they transfer the solution to a 100 mL volumetric flask and dilute to the mark. Then 20 mL of the
Ca2+ solution is added to a 250 mL erlenmeyer flask together with 1 mL of pH 10 buffer, 1 mL of
MgEDTA solution and 3 drops of Erio T indicator. The students titrated the solution with 0.01 M
EDTA solution and performed it for 5 trials. This gives them the result of 0.010466 M as mean of
EDTA, 6.44e-5 as the standard deviation of the experiment, and 0.62 as %RSD.

After the standardization of EDTA is the analysis of unknown sample. Here, the students
were given an unknown solution to be used throughout the experiment and pipetted it into a 250
mL volumetric flask then diluted it to homogenize the mixture. They then transfered 50.00 mL
aliquots of the unknown solution into 250-mL Erlenmeyer flasks and then added 1 mL of pH 10
buffer, 1 mL of MgEDTA solution and 3 drops of Erio T indicator. After which they titrated the
solution with 0.01 M EDTA and performed it for 3 trials. This yielded a mean of ppm CaCO3 of
1653.673, 10.55 standard deviation, and 0.64 %RSD.

The final procedure was the analysis of hard water. Water hardness is particularly due to
the large amounts of minerals that are found in the ground and surface water, namely, calcium
and magnesium. In high concentration, the water will be considered as “hard” if either or both
minerals are present in the water sample. With the presence of calcium and magnesium in the
hard water, it will form a colorless complex with EDTA. Calcium carbonate, which are expressed
in parts per million (ppm), are usually the criteria in which to determine if a water sample is “hard”.
According to the USGS Water Science Scool (2016), the general guidelines for classification of
waters are: if CaCO3 concentration is at 0 to 60 mg/ L, the water sample is soft. If, however, it as
61 to 120 mg/ L, then it is moderately hard, and hard if the CaCO3 concentration is at 121 to 180
mg/ L. The water sample will only be considered as very hard if the concentration of CaCO 3
exceeds 180 mg/ L. Using river water as the water sample of the experiment, the students pipetted
20 mL of the water sample into a 250 mL erlenmeyer flask and then added yet again 1 mL of pH
10 buffer, 1 mL of MgEDTA solution and 3 to 4 drops of Erio T indicator. After which, they titrated
the unknown solution with 0.01 M EDTA and performed it for 3 trials, giving them the results of
their calculations of 239.96 having a mean of ppm CaCO3, which indicates that the river water
sample is very hard in terms of water hardness standards.

Conclusion
1. Complexiometric titration is a form of volumetric analysis in which the formation of a colored
complex is used to indicate the end point of a titration.

2. Water hardness is particularly due to the large amounts of minerals that are found in the ground
and surface water, namely, calcium and magnesium. In high concentration, the water will be
considered as “hard” if either or both minerals are present in the water sample. With the presence
of calcium and magnesium in the hard water, it will form a colorless complex with EDTA. Calcium
carbonate, which are expressed in parts per million (ppm), are usually the criteria in which to
determine if a water sample is “hard”.

3. EDTA react with almost all metal cation. For this experiment, it shows that EDTA react with
calcium.

4. From the calculation, the mean concentration of the EDTA used is 0.010 M and the mean ppm
of the unknown calcium solution is 1653.673 M. Furthwrmorw, thw standard deviation of the
unknown sample of CaCO3 is 10.55 and the %RSD is 64%.
5. 239.96 is the mean ppm of CaCO3, which indicates that the river water sample is very hard in
terms of water hardness standards.
References:

Kiruthiga, B. (n.d.). Complexiometrix Titration. Retrieved March 5, 2019, from www.srmuniv.ac.in:

http://www.srmuniv.ac.in/sites/default/files/downloads/Complexometric_Titration.pdf

Perlman, H. (2015, December 15). Water Hardness. Retrieved March 5, 2019, from USGS Water Science
School: https://water.usgs.gov/edu/hardness.html

What is water hardness? (n.d.). Retrieved March 5, 2019, from www.thirteen.org:

https://www.thirteen.org/edonline/studentstake/water/schoolwater/Hardness/whatiswaterhar
dness.htm