Experiment 3

Standardization of 0.1 M NaOH

Objectives
At the end of the experiment, the students should be able to:
 Accurately determine the concentration of an NaOH solution;
 Learn and understand how to standardize a 0.1 M NaOH solution; and 
Conduct titration to perform the standardization procedure.

Introduction
A very useful and widely employed technique in the analytical laboratory is the titrimetric (volumetric)
method of analysis. Titrimetric analysis is the process of measuring a substance of unknown concentration
in a solution of interest via reaction with a standard that is made to contain a known substance
concentration. Taking a known weight or volume of a solid or solution of interest, one can calculate the
concentration of the unknown from the measured use of our known concentration solution. Chemists call
the standard solution the titrant solution.

When performing titrations, it is most optimal if the reaction between the titrant and the analyte basically
goes to completion in a very short amount of time. Then, one needs to determine if the reaction between
the two compounds, the titrant and the sample, is complete and a stoichiometric amount of the titrant
has been added. The point at which the stoichiometry of the reaction has been reached or when equal
amount of titrant has reacted to an equal amount of analyte is known as the equivalence point. This can
be accomplished with an indicator or with some type of potentiometric measurement (often a pH meter).
The determination of this point is called the endpoint of the titration and ideally is equal to the equivalence
point. However, due to various reasons,
this sometimes is not the case (one can
assume for these purposes that the
endpoint is equal to the equivalence
point). A typical titration setup is seen in
Figure 1. The buret is used to contain the
titrant and delivers it in controlled
manner. It is supported by a buret holder
and an iron stand. The sample or analyte is
contained in a conical flask which is added
with an indicator.

Sodium hydroxide (NaOH) is a very

common titrant to use in the analytical
laboratory as a strong base. It is a strong
monoprotic base; thus, its molarity and
normality are equal. Sodium hydroxide in
the solid pellet form often contains a small
Figure 1. Titration Setup amount of both water and sodium
carbonate, approximately 97%–98% pure. The sodium carbonate comes from the reaction of the sodium
hydroxide with carbon dioxide in the ambient atmosphere. For the titration of weak acids, the
preparation of sodium hydroxide solution free of sodium carbonate is essential as the carbonate ion
present can act as a buffer and distort the titration endpoint.
For the titration of strong acids, this is less of a problem.
A convenient and often used primary acid standard for standardizing sodium hydroxide titrants is
potassium hydrogen orthophthalate (KHP, molar mass of 204.14 g/mol). KHP is a moderately weak organic
(structure shown in Figure 2) acid (Ka = 3.9 × 10-6, pKa = 5.4) that gives a good endpoint using
phenolphthalein as indicator. Sodium hydroxide and KHP follows the following reaction:

Equation 1 NaOH + + H2O

Using an accurately weighed KHP to react in a 1:1 stoichiometric ratio with NaOH, one can successfully
determine a standardized concentration of an NaOH solution.

Materials
The following materials are used in the experiment:
Potassium hydrogen o-phthalate (KHP) Buret
Sodium hydroxide pellets Buret holder
Phenolphthalein indicator Iron stand
Distilled water 250-mL Erlenmeyer flask
Weighing balance 1-L beaker
Weighing paper Crucible with cover
Hot plate 500-mL volumetric flask
Wash bottle Dropper

Procedure
Preparation of CO2-free water
Boil 1 liter distilled water in a hot plate for 15 minutes. Secure in a closed container and cool to room
temperature, contents unexposed to open air.

Preparation of KHP sample

Weigh 0.5 g KHP in three clean and dry crucibles. Dry in oven at 115 °C for 2 hours. Transfer in
250mL Erlenmeyer flask and dissolve in 25-mL CO2-free water. Add three drops of phenolphthalein
indicator.

Preparation of 0.1 M NaOH

Weigh 2 g NaOH pellets and dissolve in 500-mL CO2-free water. Secure in a closed container.

Titration proper
Fill-in buret with 0.1 M NaOH solution. Dispense enough titrant to KHP sample prepared in 250-mL
Erlenmeyer flask until light pink coloration of the solution occurs. Record the volume dispensed. Add few
drops of the titrant and confirm end point by formation of a strong pink coloration known as the titration
overrun. Repeat titration for the remaining KHP samples and record all the data.
 Experiment 3 Standardization of 0.1 M NaOH
Data Sheet

Name: Precious Mae C. Barbosa Section: BSFT 2

Observations:
Observations after dispensing titrant during early stages of titration:
There’s a localized color change. A color pink appears and when swirling the flask, the color
fades quickly at first. The color fades more slowly along the process.

Observations during end point of titration:

The pink color stays for more seconds. The pink color is lighter.

Observations during overrun stage:

The pink color is darker.

Data
Trial 1 Trial 2 Trial 3
Weight of KHP 0.4957 g 0.5011 g 0.4982 g
Volume of Titrant 25.45 mL 26.01 mL 25.31 mL
Concentration of NaOH 0.09537 M 0.09434 M 0.09639 M
Average Concentration of NaOH 0.09537
Standard deviation 0.37822
% RSD 25.22%

Calculations of Concentration of NaOH

for three Trial 1:
𝑔 𝐾𝐻𝑃 0.4957 𝑔
𝑀= = = 0.09537 M
204.22 𝑥 𝑉𝑜𝑙𝑢𝑚𝑒 (𝐿) 204.22 𝑥 0.02545 𝐿

of Concentration of NaOH for three Trial 2:

𝑔 𝐾𝐻𝑃 0.5011 𝑔
𝑀= = = 0.09434 M
204.22 𝑥 𝑉𝑜𝑙𝑢𝑚𝑒 (𝐿) 204.22 𝑥 0.02601 𝐿

of Concentration of NaOH for three Trial 3:

𝑔 𝐾𝐻𝑃 0.4982 𝑔
𝑀= = = 0.09639 M
204.22 𝑥 𝑉𝑜𝑙𝑢𝑚𝑒 (𝐿) 204.22 𝑥 0.02531 𝐿
of the Average Concentration of NaOH:
𝑡𝑟𝑖𝑎𝑙 1+𝑡𝑟𝑖𝑎𝑙 2+𝑡𝑟𝑖𝑎𝑙 3 0.09537+0.09434+0.09639
= = 0.09537
𝑛 3

of the % RSD:
Standard Deviation:
∑ 𝑐𝑜𝑛𝑐𝑒𝑡𝑟𝑎𝑡𝑖𝑜𝑛𝑠 𝑜𝑓 𝑁𝑎𝑂𝐻 0.2861 0.2861
s=√ =√ =√ = √0.14305 = 0.37822
𝑛−1 3−1 2

%RSD:
𝑎𝑣𝑒𝑟𝑎𝑔𝑒 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑁𝑎𝑂𝐻
%RSD = x 100
𝑠
0.09537
%𝑅𝑆𝐷 = 𝑥 100 = 25.21548305219 = 25.22%
0.37822

--- END ---