Guide to Volumetric Analysis
Volumetric Analysis involves the reaction of a
substance, called a titrant with the analyte. The
volume of the titrant is measured with a glassware
known as buret.
The amount of the titrant required to
react with the analyte is then used to
determine the amount of the analyte
present.
- implies that the reaction stoichiometry
of the titrant and analyte &
concentration of the titrant must be
known.
(refer to p. 25 of manual for equations)
Standardization
(compared to a standard)
(determining the exact conc. of the titrant)
- to know the volume needed to
completely react with 0.2xxx of KHP when
the reaction ratio for NaOH & KHP is 1:1
Compleximetric Determination of Water
Hardness
- direct titration because the titrant reacts
directly with the analyte
Modified Winkler Method for Dissolved Oxygen
- indirect titration because a reagent is
added to the analyte
- reaction results in a product that is
proportional to the amount of the analyte.
Determination of the pKa of a Weak Acid
- chemical property of a weak acid is
determined by titration
3 Distinct Stages (Pre, Sta, Tit or PST)
1. Preparation of the Titrant
2. Standardization of the Titrant
3. Titration of the sample
Usual data in volumetric analysis include initial and
final volume of the buret, weight of the sample
or standard.
Compleximetric Determination of Water Hardness
Water hardness
- concentration of CaCO3 and MgCO3 in
water expressed as ppm CaCO3
A. Preparation of 5x10^-3 M EDTA Titrant
- Dissolve 0.47g of EDTA in 250mL
distilled water
- Add pinch of MgCl2 * 6H20 (ca. 0.05 g)
B. Preparation of Diluted EDTA Titrant
- Take a 10.00mL aliquot of the prepared
titrant
- Place in a 100mL volumetric flask and
dilute to volume
C. Preparation of Standard CaCO3
- Weigh 0.10-0.15g (0.1mg) CaCO3 in a
250mL beaker
- Add concentrated HCl drop by drop until
all the CaCO3 dissolves.
- Cover the beaker with a watch glass
and evaporate the HCl
- Quantitatively transfer the residue to
a 500mL volumetric flask and dilute to
volume
D. Standardization of EDTA
- Place 10mL of the Standard CaCO3 in a
convenient titration vessel
- Add 5mL of Ammonia buffer
- Add 5 drops of the EBT indicator
Wine red coloration
- titrate until light blue
E. Determination of Water Hardness
- Use DILUTED EDTA TITRANT for the
titration
- Follow procedure D but instead of using
10mL of the standard CaCO3 use 10mL of
the sample
Determination of the pKa of a Weak Acid
When a solution of a weak acid is titrated
completely with a strong base, the salt that is
formed is the conjugate base of the weak acid.
If the reaction is only 50% complete, then we have a
situation wherein only half of the weak acid has been
titrated while the other half remains untitrated. In
other words, the concentration of the weak acid is
the same as the concentration of its conjugate
base.
At this point, pH = pKA
A. Preparation of the NAOH Titrant
- Boil 250mL distilled water to remove
the dissolved carbon dioxide
- Add 1g of NaOH
- cool and store
B. Preparation of the pH meter
- Be sure to rinse the electrode tip with
distilled water before and after soaking the
electrode in a solution
C. Standardization of the NaOH Titrant
D. Preparation of the sample
E. Determination of pKa

- Adding NaOH in 0.5mL increments until
there is a sudden rise in pH
- At this point, add the increments of 0.1mL
until the pH shows a gradual rise in pH
F. Treatment of Results
- Volume of NaoH (x-axis)
- pH (y-axis)
- Determine the volume of NaOH at the
inflection point on the curve
- Divide the volume by 2
- Determine the pH coordinate of the
quotient