EXERCISE 4

PREPARATION, COMPARISON AND STANDARDIZATION OF SODIUM HYDROXIDE AND

HYDROCHLORIC ACID SOLUTIONS

Volumetric analysis is a method of determining the concentration of an analyte by measuring

the volume of a solution that it occupies or relates to. A form of volumetric analysis is titration
where a known substance or solution, called the titrant, is made to react with the analyte until
it is consumed for a complete reaction (Harris, 2010). This method is used to identify the
amount of the analyte. This method is usually done using a buret, which is a long, narrow glass
tube with calibration marks fitted with a stopcock at one end to control the flow of the titrant
(Harvey, 2000).
When the needed quantity of the titrant for a reaction was added to the analyte, equivalence
point is reached. But in titration, what we can actually identify is the end point which is marked
by a sudden physical change in the solution. The end point is not equal to the equivalence point
and usually occurs after the equivalence point since an extra amount of the titrant is needed to
react with the analyte for a physical change to occur (Harris, 2010). The difference between the
two is called the titration error which cannot be avoided. To estimate this error, a method
called blank titration is done where in the procedure was done without the analyte.
There are different methods used as an end point determination or determining when an
analyte has been consumed. One common method involves observing a change in color in the
solution and this method involves the use of an indicator. What actually changes color is the
indicator as it changes abruptly near the equivalence point which is caused by the
disappearance of an analyte or the appearance of excess titrant. One method uses electrodes
to detect changes in the voltage and current in the solution. Another method uses
spectrophotometry to measure the absorption of light brought by the reaction.
There are different methods of titration depending on how the end point of a reaction is
determined. One method is called direct titration where the titrant is added to the analyte until
the end point is observed. This requires a fast-enough reaction for an observable end point. For
slow reactions, where the end point is hard to be determined, an indirect analysis can be used.
Back titration is an indirect method where an excess titrant is added to the analyte for an
observable end point. This can be used when the endpoint in a titration was overrun. This
method gives a more accurate result as it utilizes more than one reaction and titration
procedure. Another indirect method is the displacement method wherein the analyte displaces
a reagent which is then used to determine the concentration of the analyte.
In titration, one reactant must be known as it would determine the validity of the method.
From this, pure and known substances that which can be weighed directly, or primary
standards, are used in titration. Chemicals have grades of purity or purity standards set by the
manufacturer. Reagents used as standards are usually from the primary and secondary grade.
Primary reagents are classified as chemicals that have a known purity, known stoichiometry,
and have a high stability and low hygroscopicity. Chemicals which does not satisfy the last two
conditions falls under secondary reagents. The purity and the stoichiometry of the secondary
reagents depends on the primary reagents. Other reagents other than these two are added to
prepare a primary standard and these reagents must be reagent grade chemicals.
Characteristics of a primary standard includes known high purity, known stoichiometry, high
molar mass, high stability and low hygroscopicity for storage.
But not all titrants are available as primary standards which brings us the process of
standardization. Standardization is the determination of the exact concentration of a solution.
This uses titration in determining the exact concentration of an analyte by titrating a primary
standard using a titrant with an approximation of the desired concentration to determine the
concentration of the titrant, giving us a standard solution.
The concentration of standard solutions may be expressed either as molarity or normality.
Molarity is the concentration of a particular chemical species in a solution and is expressed as
the number of moles solute per liter of a solution. Normality, on the other hand, makes use of
chemical equivalent or the amount of a part of a chemical species involved in the reaction, and
is dependent on how this species reacts with another chemical species.

Formulas

FW / n
EW =

NnM

N=(0.05M)(1)

C1V1=C2V2

V2=(0.5L)(0.05M)/(12.4M)

(0.15g KHP) (1 mol KHP)/MM g KHP) (1 mol NaOH)/(1 mol KHP) (1 mol NaOH)/(volume req. L NaOH)

(0.05mol)/(1L) (MM g NaOH)/(1 mol NaOH) (0.5L)

EXERCISE 5
DETERMINATION OF THE EQUIVALENT WEIGHT
OF AN UNKNOWN ACID
The concentration of standard solutions may be expressed either as molarity or normality.
Molarity is the concentration of a particular chemical species in a solution and is expressed as
the number of moles solute per liter of a solution. However, this unit is used only as the basis of
strength of a solution and not to compare two or more solutions. In the comparison of the
strengths of two or more solutions, normality is preferred. Normality makes use of the reaction
occurring between two species. This unit utilizes chemical equivalents which is based on a
reaction unit. A reaction unit can be described as that part of a chemical species that explains
how the species in the given reaction reacts with each other. In precipitation reaction, what
relates the two chemical species are the charges of each ions, and thus are considered its
reaction unit. In complexation reaction, the reaction unit are the number of electron pairs that
is being given by the metal and received by the ligand in the reaction. In oxidation-reduction
reaction, the reaction unit is the number of electrons accepted by the oxidizing agent and given
by the reducing agent. In this exercise, we will be dealing with acid-base reaction, and the
reaction unit in this case are the number of hydrogen atoms donated by an acid and received
by a base.
Mass, as a basis of measurement, is widely used in quantitative analysis. It is, then, convenient
to have a unit of mass that is related to the number of equivalents in a given reaction, and this
unit is called equivalent weight. Equivalent weight is the mass of a species containing one
equivalent. It relates the formula mass of a species to the number of its equivalents in a
reaction. With this, comparison of the strengths of two or more solutions would be possible.

Data/results

Table 1.1 Data on the determination of the initial and final mass of the unknown iron sample to
be used for the calculation of the percentage of Fe and Fe2O3 in the sample
Parameter Data/Observation
Trial 1 Trial 2
Initial mass of the
unknown sample, g
Final mass of the
unknown sample, g
Mass of Fe2O3 in the
sample, g
Formula mass for Fe,
g/mol
Formula mass for Fe2O3,
g/mol
Mass of Fe in the
sample, g
Percentage Fe in
sample, %
Percentage Fe2O3 in
sample, %

Prelab

1. The primary characteristic of a good primary standard is its high purity. Primary
standards are used to show the validity of an analytical result and having a high purity
makes it more accurate. A primary standard must also have a high molar mass. This is to
reduce the error in the mass measurement. Also, a primary standard must have high
stability especially with heat, and low hygroscopicity, or its ability to attract and absorb
 moisture from the air, for storage. Ideally, a primary standard must be cheap, readily
available, and non-toxic, as it is commonly used in experiments.
2. Drying increases accuracy in an analytical result as it removes any trace of water it
adsorbed from the atmosphere.