PRACTICUM 8

Complexometric Titration
Experiment Summary:
Objectives
1. To determine the concentration of a substance by titrimetric through the formation of coplex
compunds
Materials
Chemicals
Sewage sample
Lab water sample
EBT 20%
EDTA 0,1 M
Buffer solutions pH 10
Aquadest
Filter paper 1 sheet

Equipment
Burette
250 mL erlenmeyer
Beaker glass
10 mL measuring cylinder
50 mL measuring cylinder
Clamps and the stand
Hotplate
Drop pipette
Funnel
Volumetric flask

Introduction
Complexometric titration is a titrimetric, based on the ability of metal ions to form complex
compounds that are stable and water soluble. By this principal, some ways of titration has been
developed to determine the levels of metal ion in a sample. Complexometric titration is a formation of
neutral molecule dissociated in solution. To form complex substances, we need a high level of solubility.
The most common used of complexing agent (reagent) is ethylenediaminetetraacidic acid (EDTA).
Complexometric titration once is used to determine water hardness which caused by the presence of Ca2+
and Mg2+ ions. This titration can be measured directly with EDTA at pH 10 using EBT indicator, the end
point of titration is marked by a color change from red to blue. Equilibrium reaction of complex-forming
is widely used in titrimetric. This titrimetric is based on the ability of metal ions to form stable and water
soluble complex compounds. Therefore this method is often called complexometric titration.

HOOC - CH2

CH2 - COOH
N CH2 CH2 - N

HOOC - CH2

CH2 - COOH

Figure 1. The structure of EDTA

The structure of EDTA above shows that EDTA molecule contains both an electron donor of
oxygen atoms and nitrogen atoms, so it can produce a ringed chelate up to six ring simultaneously. EDTA
is soluble in water, it can be obtained in a pure state, but due to the uncertain amount of it, it should be
standardized. EDTA is potential as a seksidentat ligands that can coordinate with a metal ion through a
cluster of two nitrogen and four carboxyl. In other cases, EDTA can act as kuinkedentat ligands or
kuadridentat ligands with one or two free carboxyl group of the strong interaction with the metal. EDTA
is often abbreviated by H4y.
Because EDTA containing of six base sites-four two carboxylic oxygen and nitrogen, then six acid
species may be present: H6y2+, H5y+, H4y, H3y-, H2y2-, dan H3y3-. H6y2+ and H5y+ are strong acid and they
usually are not important in equilibrium calculations. Of the many organic ligands, acids Paraminocarboxylate (komplekson) is a ligand that is essential in the chemical examination. The most important
characteristic and typical of complex compounds is their ability to form a complex chelate with many
branches, because EDTA complex is very stable, so it is obvious that in the point area of metal ion equality
concentration will be decline very sharply.
EDTA is a tetraprotic with 4 kind of acid dissociation, namely:

K1 = 1.10-2

K3 = 6,9. 10-7

K2 = 2,1.10-3

K4 = 7. 10-11

The dissociation constant above shows that there are only two strong acid-protons. In that pH,
the reaction on the formation of a complex of EDTA with polyvalent metal ions: MNN +, stated as follows:
Mn2+ + H2Y2-

MY(n-4) + 2H+

The reaction is reversible and its direction go to the formation of metal complexes, followed by
H+ release. When the acidity of solution is high (low pH), the metal complex will be dissociates and the
equilibrium will shift to the left. While the alkaline solution (high pH) is likely to form the hydroxide of
metal. To keep this balance, the addition of certain pH should be done. The lower metal EDTA complex
stability, then the titration should be done in high pH.

OOC - CH2 H+

H+

H+

H+ - CH2 - COOH

N CH2 CH2 - N
-

H2 - COO-

OOC - CH2

Figure 2. EDTA has "zwitterionic" duplex formula

These compounds are commonly used in sodium salt form that often called EDTA or occasionally
Na2EDTA. The release of four protons from the EDTA molecule caused these ligands have six pairs of
electrons. To prevent any changes happened, buffer solutions is used in this complexometric titration.
Complexometric titration is used to determine the water hardness which is caused by the presence of
Ca2+ and Mg2+ ions. This titration is occurred directly with EDTA at pH 10 using Erchom Black T (H 3In)
indicators, end point of titration is marked by discoloration from red to blue. At pH 10, EBT (Hin = blue)
this form is reacting with Mg and form red complex.
Mg2+ + Hln2-

Mgln- + H+

Metal chelate is formed with EBT by the losing of hydrogen ions from the phenolic-OH group and
the formation of the bond between metal ions and oxygen atoms. EBT molecules are usually presented in
abbreviated form as triprotic acid, H3In. Sulfonic acid species is seen in the image as ionized, it is a strong
acid which is decomposed in an aqueous solution that doesnt rely on pH, so the structure shown is H2In.
Complex formed 1:1 stable colored red wine, with a number of cations e.g. Mg2+, Ca2+, Zn2+, and
Ni2+. Many EDTA titration occurs in the buffer pH 8 to pH 10. A range where the dominant form of EDTA
is a new form of Hin2-.
Complex formed 1: 1 stable colored red wine, with a number of cations such as Mg2+, Ca2+, Zn2+ and Ni2+.
Many EDTA titration occurs in the buffer pH 8 to 10. A range where the dominant form of renewable
energy is a form of new Hin2-. The complex which is formed by the indicators are weaker than the metal
ion complexes between the metal ions with EDTA (complex Mgln is weaker than MgY2-) thus the excess
of EDTA will bind Mg of MgIn to form Mg2+ complexes.
Mgl- + H2Y2Red

MgY2- + Hln2- + H+
Colorless

Blue

EBT indicator structure:

Na+SO3-

Experimental Methode
Determination of Water Hardness
1. Total Water Hardness
a. Fill 100 mL water sampleto erlenmeyer.
b. Add 5 mL buffer solutions ph 10 and 2 drops of EBT indocator.
c. Titrate the mixture with EDTA until the solutions change the color from red to blue.
d. Calculate the total hardness in ppm CaCO3.
2. Fixed Water Hardness
a. Measure 250 mL of sample water and boil it in the 40 mL beaker glass for 3 menit without
closing the beaker.
b. Let it chill dan filter, then put it into 500 mL volumetric flask.
c. Without abstersion of filter paper, dilute the solutions with aquadest up to mark, then shake
it.
d. Pipette 50 mL solution no. 4 and add it in to erlenmeyer then titrate it to EDTA until the
solutions change the color from red to blue.
e. Calculate the fixed hardness in ppm CaCO3.
3. Temporary Water Hardness
Temporary water hardness = Total Hardness Fixed Hardness.

PRELAB
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