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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).
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
!
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
i) Standard deviation
. . ^+ .. ^+(..)^
=
= 6.120
! = 6.120 / 250.1
RSD = = 0.02447
!
k) % Error
= 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.
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.
[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
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
!"#$% !" !"#$ !"#$%&"' !".! !.! !"
e) Standard deviation
.! . ^! .!. ^!(.!.)^
=
= 2.254x10-4
f) Relative Standard deviation
!
RSD = -4
! = 2.254x10 / 0.00888 M 0.0103 M = 0.2538
g) ppm CaCO3
6.9 0.1 mL
=
25.0 mL 0.5 mL
= 243.0 ppm
i) Standard deviation
. . ^+ .. ^+(..)^
=
= 6.120
! = 6.120 / 250.1
RSD = = 0.02447
!
k) % Error
= 18. 5 %
For Trial 3:
a) Moles of CaCO3 soln = Moles of EDTA soln
!!
moles CaCO3 = 7.994x10-4 x 50 mL x !""" !" = 3.998 x 10-4 mol CaCO3 soln
b) M of CaCO3
! !"# !"!#! !
M of CaCO3 = 0.2000g CaCO3 x !"".!"! !"!#! x !! = 7.995 x 10-4 M CaCO3
!"# !" !
!"""!"
c) Average molarity
!!!!!!!!
=
!.!!"!! !.!!" !! !.!!"#$ !.!!" !! !.!!"!#!.!!" ! = 0.00888 M 0.0103 M
! !
d) M of EDTA solution
!"#$% !" !"#$ !"#$%&"'
=
!.!!"#$%!! !.!!!" !"# = 0.00902 0.006 M
!"#$% !" !"#$ !"#$%&"' !!.! !.! !"
e) Standard deviation
.! . ^! .!. ^!(.!.)^
=
= 2.254x10-4
!
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
i) Standard deviation
. . ^+ .. ^+(..)^
=
= 6.120
! = 6.120 / 250.1
RSD = = 0.02447
!
k) % Error
= 18. 5 %
Figure 6. Titration set-up Figure 7. Presence of effervescence