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Reporter: Cesarah Justine M.

Cabungcal Instructor: Sir Basil James Santos


Section: 2 ChE B Date Performed: April 5, 2017
Group No: 2 Date Submitted: May 2, 2017

Experiment No. 8: Determination of Water Hardness


INTRODUCTION
Water is one of the essential needs of any living thing to sustain life. It accumulates
majority of the Earths surface. A factor to consider in establishing the quality of water is its
degree of hardness. Water hardness is defined as the presence of its calcium and magnesium ion.
Since most analyses do not distinguish between Ca2+ and Mg2+, and most hardness in water is
caused by carbonate mineral deposits (see figure 1). It is ususally written as parts per million
(ppm) of calcium carbonate (by weight). All natural waters have salts dissolved in them. It is
these salts that give water a unique taste. When a water contains an abundant amount of these
salts, it can cause health risks. These problems are caused by the presence of magnesium and
calcium ions in water.
The goal of this experiment is to conduct a quantitative analysis on the total hardness of
water as calcium carbonate (CaCO3) on a commercial water sample. An EDTA solution will be
standardized by titration against a standard solution from calcium carbonate (CaCO3). The
EDTA solution can then be used to determine the hardness of an unknown water sample. Since
both EDTA and Ca2+ are colorless, Eriochrome Black T is used as the indicator and produces a
wine-red complex (Frey, 2011). A clear blue color will be the indication of the endpoint of the
titration and from the data collected, the hardness of the water sample can be determined.

Figure 1. Total Hardness Scale (As CaCO3)

METHODOLOGY
The goal of this experiment is to conduct a quantitative analysis on the total hardness of
water as calcium carbonate (CaCO3). A 0.200 g of calcium carbonate (CaCO3) was prepared and
weighed accurately using an analytical balance then dissolved in 50 mL of distilled water.
Addition of drop-wise 0.1 M HCl was made to stop the presence of effervensence. The mixture
was then transferred into a 250 mL volumetric flask and a reasonable amount of distilled water to
reach the 250 mL mark was added. A 50 mL aliquot was collected from the mixture and 4 mL of
ammonia-ammonium chloride (NH4/NH3Cl) and 5 drops of Eriochrome Black T (EBT) was
added. The solution must manifest a wine-red complex (as shown in figure 2). It was then titrated
using a standardized EDTA solution and was put into a stop when the solution has turned into a
clear blue color (as shown in figure 3). The process was repeated to produce two (2) more trials.
Afterwards, a blank titration using the standardized EDTA solution was performed with
25 mL of distilled water dropped with 2 mL of ammonia-ammonium chloride (NH4/NH3Cl) and
5 drops of EBT. 25 mL of Evian water was then prepared for titration and was dropped the same
amount of ammonia-ammonium chloride (NH4/NH3Cl) and EBT on the blank titration process.
The solution must produce a wine-red color and the endpoint has been reached once the solution
has turned into a clear blue color. Data were recorded for the calculations needed for the
determination of the total hardness as ppm calcium carbonate (CaCO3).

Figure 2. Wine-red complex Figure 3. Clear blue color


DATA SHEET

Table 1. Standardization of EDTA Solution


Trial 1 Trial 2 Trial 3

V of CaCO3 soln

50 mL 0.5 mL

-3 -7
M
of CaCO
3 soln
7.995x10
M 1x10 M
-4
Moles
of CaCO
3 soln
3.998x10
0.0003 mol
Moles of EDTA soln 3.998x10-4 0.0003 mol
Vfinal of EDTA soln 5.6 0.1 mL 3.4 0.1 mL 5.7 0.1 mL
Vinitial of EDTA soln 50.0 0.1 mL 50. 0 0.1 mL 50.0 0.1 mL
Vused of EDTA soln 44.4 0.1 mL 46.6 0.1 mL 44.3 0.1 mL
M of EDTA soln 0.00900 0.006 M 0.00862 0.006 M 0.009020.006 M
Average molarity 0.00888 M 0.0103 M
Standard deviation 2.254x10-4
Relative standard deviation 0.02538

Table 2. Determination of Water Hardness


Blank Trial 1 Trial 2 Trial 3
V of water sample 25.0 mL 0.5 mL
Vfinal of EDTA soln 44.9 0.1 mL 10.5 0.1 25.1 0.1 mL 17.9 0.1 mL
mL
Vinitial of EDTA soln 45.0 0.1 mL 17.7 0.1 32.0 0.1 mL 25.1 0.1 mL
mL
Vused of EDTA soln 0.1 0.1 mL 7.2 0.1 mL 6.9 0.1 mL 7.2 0.1 mL
M of EDTA soln 0.00888 M 0.0103 M
Moles EDTA 8.8x10-7 mol 6.336x10-5 6.022x10-5 mol 6.336x10-5 mol
mol
Moles CaCO3 8.8x10-7 mol 6.336x10-5 6.022x10-5 mol 6.336x10-5 mol
mol
Moles CaCO3 per L 3.52x10-5 2.5344x10-3 2.4288x10-3 2.5344x10-3
mol/L mol/L mol/L mol/L
Grams CaCO3 per L 3.541x10-3 g/L 0.2536 0.2430 0.2536
ppm CaCO3 253.6 ppm 243.0 ppm 253.6 ppm
Average ppm CaCO3 250.1 ppm
Standard deviation 6.120
Relative standard 0.02447
deviation
Theoretical ppm 307 ppm
CaCO3
% Error 18.5 %

TREATMENT OF DATA AND RESULTS


For Trial 1:
a) Moles of CaCO3 soln = Moles of EDTA soln
!!
moles CaCO3 = 7.994x10-4 x 50 mL x !""" !" = 3.998 x 10-4 mol CaCO3 soln

1 mol CaCO3 = 1 mol EDTA


3.998 x 10-4 mol CaCO3 soln = 3.998 x 10-4 mol EDTA soln

b) M of CaCO3
! !"# !"!#! !
M of CaCO3 = 0.2000g CaCO3 x !"".!"! !"!#! x !! = 7.995 x 10-4 M CaCO3
!"# !" !
!"""!"

c) Average molarity
!!!!!!!!
=
!.!!"!! !.!!" !! !.!!"#$ !.!!" !! !.!!"!#!.!!" ! = 0.00888 M 0.0103 M
! !

d) M of EDTA solution
!"#$% !" !"#$ !"#$%&"'
=
!.!!"#$%!! !.!!!" !"# = 0.00900 0.006 M
!"#$% !" !"#$ !"#$%&"' !!.! !.! !"
e) Standard deviation

.! . ^! .!. ^!(.!.)^
=

= 2.254x10-4

f) Relative Standard deviation

!
RSD = -4
! = 2.254x10 / 0.00888 M 0.0103 M = 0.2538

g) ppm CaCO3
7.2 0.1 mL
=
25.0 mL 0.5 mL

= 253.6 ppm

h) Average ppm CaCO3


!!"!!!!"!!!!"! !"#.! !!"!!"#.! !!"!!"#.! !!" = 250.1 ppm
!
= !

i) Standard deviation

. . ^+ .. ^+(..)^
=

= 6.120

j) Relative Standard deviation

! = 6.120 / 250.1
RSD = = 0.02447
!
k) % Error

%Error = (theoretical experimental)/ theoretical


%Error =(307 ppm 250.1 ppm) / 307 ppm

= 18. 5 %

DISCUSSION OF RESULTS
An addition of a small amount of MgCl22 6H2O in preparing a standardized EDTA
solution is done because EDTA binds with calcium ions very slowly, therefore another metal is
needed so that it could bond quicker to form a metal-EDTA complex, which are usually
magnesium in form of salts. The metal-EDTA complex formed is less stable than the calcium-
EDTA complex. The magnesium forming calcium-EDTA complex and resulting in free Mg2+
ions, which can be titrated easily, will then replace the free Ca2+ (Cassiday, 1998). The amount
of liberated Mg2+ is equivalent to the original concentration of Ca2+. The color of the EDTA
solution and Ca2+ are colorless, therefore an indicator was used to easily determine the endpoint
of the solution to be titrated. Eriochrome Black T (EBT) is a metal ion indicator is a compound
whose color changes when it binds to a metal ion. For such an indicator to be useful in the
titration of a metal with EDTA, the indicator must give up its metal ion to the EDTA. The
indicator in its free form, i.e. not bound to any metal, is blue (as shown in figure 5). A small
amount of indicator is added to the solution containing the Ca2+ forming a wine red complex (as
shown in figure 4) (Pennsylvania State University, 2014). Furthermore, titration using
Eriochrome Black T as indicator determines total hardness due to Ca2+ and Mg2+ ions.

Figure 4. Formation of a wine-red complex

Figure 5. Formation of a clear blue color


To obtain the ppm CaCO3, the commercial water sample Evian was titrated and the
volume used of EDTA solution was recorded. These data collected was used to compute for the
ppm of the total hardness of the water sample as CaCO3. The results calculated showed that the
average ppm of CaCO3 present in the water sample is 250.1 ppm. From the scale below (see
table 3), the water sample used in the experiment exhibits a hard hardness as ppm CaCO3. Hard
hardness means it is highly dissolved in high amounts of Ca2+ and Mg2+. The theoretical CaCO3
computed from the Ca2+ and Mg2+ on the product description of the Evian water sample was 307
ppm, however, from the experiment it only produced 250.1 ppm, which indicates, there is 18.5%
error.

Table 3. Water Hardness Scale


CaCO3 (ppm) Hardness
<43 Soft
43 - 150 Slightly hard
150 - 300 Moderately Hard
300 - 450 Hard
450 Very hard

CONCLUSIONS AND RECOMMENDATIONS


The determination of the total hardness is essential to know if the water being consumed
is a risk to the health of the users. The amount of Ca2+ and Mg2+ ions present in the water must
be known to verify the total hardness of the water. Calcium ions determination via EDTA is one
of the processes to know the amount of Ca2+ and Mg2+ ions. The experiment produced an 18.5%
error because only 250.1 ppm was calculated against the 307 ppm from the Evian water sample.
To produce error-prone results, the standardization must be done well to eradicate impurities
present in the solution, the preparation of the solvents to be used must also be, as much as
possible, free from impurities, and the titration method should be executed in a way the analyte
will not be overtitrated.

REFERENCES
[1] Austin Community College. (n.d.). Experiment 47: Determination of water
hardness. Retrieved from
http://www.austincc.edu/dsackett/CHEM1412/lab/1412exp47.pdf.
[2] Casiday R. (1998). Water hardness: Inorganic reactions experiment. Retrieved
from http://www.chemistry.wustl.edu/~edudev/LabTutorials
/Water/FreshWater/hardness.html.

[3] Experiment on determination of total hardness. (n.d.). Retrieved from


http://nitttrc.ac.in/Four%20quadrant/eel/Quadrant%20-
%201/exp5_pdf.pdf.

[4] Frey, R. (2011). Determination of the hardness of water. Retrieved from


http://chemistry.bd.psu.edu/jircitano/Water05.pdf.

[5] Hardness of water by EDTA titration. (2011). Retrieved from


http://cd1.edb.hkedcity.net/cd/science/chemistry/s67chem/pdf/sOL_6_
Water_hardness.pdf.

[6] Nuffield Foundation. (2016). Testing the hardness of water. Retrieved from
http://www.rsc.org/learn-chemistry/resource/res00000426/testing-the-
hardness-of-water?cmpid=CMP00005922.

[7] Pennsylvania State University. (2014). Testing the hardness of water. Retrieved
from http://chemistry.bd.psu.edu/halmi/chem3waterhardnessS%2705.pdf.
APPENDIX
For Trial 2:
a) Moles of CaCO3 soln = Moles of EDTA soln
!!
moles CaCO3 = 7.994x10-4 x 50 mL x !""" !" = 3.998 x 10-4 mol CaCO3 soln

1 mol CaCO3 = 1 mol EDTA


3.998 x 10-4 mol CaCO3 soln = 3.998 x 10-4 mol EDTA soln

b) M of CaCO3
! !"# !"!#! !
M of CaCO3 = 0.2000g CaCO3 x !"".!"! !"!#! x !! = 7.995 x 10-4 M CaCO3
!"# !" !
!"""!"

c) Average molarity
!!!!!!!!
=
!.!!"!! !.!!" !! !.!!"#$ !.!!" !! !.!!"!#!.!!" ! = 0.00888 M 0.0103 M
! !

d) M of EDTA solution
!"#$% !" !"#$ !"#$%&"'
=
!.!!"#$%!! !.!!!" !"# = 0.00862 0.006 M
!"#$% !" !"#$ !"#$%&"' !".! !.! !"

e) Standard deviation

.! . ^! .!. ^!(.!.)^
=

= 2.254x10-4
f) Relative Standard deviation

!
RSD = -4
! = 2.254x10 / 0.00888 M 0.0103 M = 0.2538

g) ppm CaCO3
6.9 0.1 mL
=
25.0 mL 0.5 mL

= 243.0 ppm

h) Average ppm CaCO3


!!"!!!!"!!!!"! !"#.! !!"!!"#.! !!"!!"#.! !!" = 250.1 ppm
!
= !

i) Standard deviation

. . ^+ .. ^+(..)^
=

= 6.120

j) Relative Standard deviation

! = 6.120 / 250.1
RSD = = 0.02447
!

k) % Error

%Error = (theoretical experimental)/ theoretical


%Error =(307 ppm 250.1 ppm) / 307 ppm

= 18. 5 %
For Trial 3:
a) Moles of CaCO3 soln = Moles of EDTA soln
!!
moles CaCO3 = 7.994x10-4 x 50 mL x !""" !" = 3.998 x 10-4 mol CaCO3 soln

1 mol CaCO3 = 1 mol EDTA


3.998 x 10-4 mol CaCO3 soln = 3.998 x 10-4 mol EDTA soln

b) M of CaCO3
! !"# !"!#! !
M of CaCO3 = 0.2000g CaCO3 x !"".!"! !"!#! x !! = 7.995 x 10-4 M CaCO3
!"# !" !
!"""!"

c) Average molarity
!!!!!!!!
=
!.!!"!! !.!!" !! !.!!"#$ !.!!" !! !.!!"!#!.!!" ! = 0.00888 M 0.0103 M
! !

d) M of EDTA solution
!"#$% !" !"#$ !"#$%&"'
=
!.!!"#$%!! !.!!!" !"# = 0.00902 0.006 M
!"#$% !" !"#$ !"#$%&"' !!.! !.! !"

e) Standard deviation

.! . ^! .!. ^!(.!.)^
=

= 2.254x10-4

f) Relative Standard deviation

!
RSD = -4
! = 2.254x10 / 0.00888 M 0.0103 M = 0.2538
g) ppm CaCO3
7.2 0.1 mL
=
25.0 mL 0.5 mL

= 253.6 ppm

h) Average ppm CaCO3


!!"!!!!"!!!!"! !"#.! !!"!!"#.! !!"!!"#.! !!" = 250.1 ppm
!
= !

i) Standard deviation

. . ^+ .. ^+(..)^
=

= 6.120

j) Relative Standard deviation

! = 6.120 / 250.1
RSD = = 0.02447
!

k) % Error

%Error = (theoretical experimental)/ theoretical


%Error =(307 ppm 250.1 ppm) / 307 ppm

= 18. 5 %
Figure 6. Titration set-up Figure 7. Presence of effervescence

Figure 8. Evian water sample


Figure 7. Successful titrations of the 3 trials
Figure 9. Copy of the data sheet from the log book