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Date Performed: 12 July 2016

MANALO, JEAN LOUISE B. Date Submitted:

Experiment 4


Titrimetry is any method in which volume is the signal. This makes use of a titrant, the reagent added to
a solution containing the analyte and whose volume is the signal. Titrimetric methods are classified into
four groups based on the type of reaction involved. One among these groups is acid–base titrations, in
which an acidic or basic titrant reacts with an analyte that is a base or an acid (Harvey, 2000).

For a titration to be accurate, addition of stoichiometrically equivalent amount of titrant to a solution

containing the analyte should be done. This stoichiometric mixture is called the equivalence point
(Harvey, 2000). The equivalence point in a titration is a point where stoichiometrically equivalent
amounts of analyte and titrant react (Skoog et al, 2014). Unlike precipitation gravimetry where the
precipitant is added in excess, determining the exact volume of titrant needed to reach the equivalence
point is important. Based on Equation 4.1, the product of the equivalence point volume, Veq, and the
titrant’s concentration, CT, gives the moles of titrant reacting with the analyte. Knowing the
stoichiometry of the titration reaction, the moles of analyte can be calculated (Harvey, 2000).

Moles titrant = Veq x CT (Equation 4.1)

However, in most titrations, there is no obvious indication that the equivalence point has been reached.
Instead, addition of titrant is stopped when endpoint is reached. This endpoint is indicated by a change
in the color of a substance added to the solution containing the analyte. Such substances are known as
indicators (Harvey, 2000). Indicators are colored compound whose change in color signals the end point
of a titration (Skoog et al, 2014). In most experiment when access to some laboratory equipment is very
limited, addition of slight excess of the titrant is performed to visualize experimental estimate of the
equivalence point. When pH meter is available, another way to determine the endpoint is by using pH
meter. A titration curve provides with a visual picture of how a property, such as pH, changes as we add
titrant, as shown in Figure 4.1. This titration curve can be measured experimentally by suspending a pH
electrode in the solution containing the analyte, monitoring the pH as titrant is added.

Figure 4.1. Sample of titration curve: Acid–base titration curve for 25.0 mL of 0.100 M HCl with 0.100 M
NaOH (Harvey, 2000)
Acid-base titration is a titration in which the reaction between the analyte and titrant is an acid–base
reaction. Standard solutions have a very big role in all titrations. Therefore, the properties of the
solutions must be desirable, how they are prepared, and how their concentrations are expressed. The
ideal standard solution for a titrimetric method must be stable so that it is necessary to determine its
concentration only once. The standard solution should also react rapidly with the analyte so that the
time required between additions of reagent is minimized. Lastly, standard solutions should react
completely with the analyte so that the endpoints are correctly identified (Skoog et al, 2014).
Concentrations of standard solution are expressed in terms of molarity or normality (equivalence per
liter of solution) (Harvey, 2000).

The accuracy of a titration is affected heavily by the accuracy of the concentration of the standard
solution used. Two basic methods can be used to determine the accurate concentration of such
solutions. First is the direct method wherein a carefully determined mass of a primary standard is
dissolved and diluted to a known volume in a volumetric flask. The second is by standardization in which
the prepared solution to be standardized is used to titrate a known mass of a primary standard, or a
measured volume of another standard solution (Skoog et al, 2014). In this experiment, the former will
be used to standardize NaOH solution, while the latter will be performed on the standardization of HCl
solution. For NaOH solution standardization, the primary standard will be used. A primary standard is
any reagent of known purity that can be used to determine the actual concentration of a prepared
solution (Harvey, 2000). It serves as a reference material in titrations and the accuracy of a method
greatly depends on the properties of the primary standard. A primary standard should be of high purity
wherein established methods can be used to confirm its purity. The primary standard should also have
atmospheric stability and must be dried and free from hydrate water, since the composition of the
primary standard should not change with variations in humidity. The primary standard should also be
soluble to the solvent where the analyte will be dissolved. Lastly, it should have a relatively large molar
mass so that the error obtained from weighing the standard is minimized (Skoog et al, 2014).
Standardization of NaOH solution should be performed so that accurate results from chemical analysis
will be obtained. In this experiment, standard NaOH solution will be used to determine the identity and
equivalent weight of an unknown acid, and the actual concentration of NaOH, when determined
correctly, plays a crucial role in analysis. Standardization will make use of potassium acid phthalate, KHP
(KHC8H4O4; MM = 204.2 g/mol). When dissolved in water, KHP dissociates completely into its ions, K⁺
and phthalate ion, HP¯. The acidic hydrogen in phthalate ion reacts with NaOH in an acid-base type
reaction (Figure 4.2).

Figure 4.2. Reaction between phthalate ion and NaOH

Indicator to be used in this experiment is phenolphthalein, a colorless indicator that turns pink between
pH 8.2 and 10.0. The drastic rise in pH at the equivalence point can be observed between pH 8.7 or 8.8
(Harvey, 2000).

In this experiment, using standard NaOH solution, the equivalent weight of an unknown acid can be
determined. In contrast to the mole, the amount of a substance contained in one equivalent can vary
from reaction to reaction. Also, the weight of one equivalent of a compound can never be calculated
without looking at the chemical reaction in which that compound is, directly or indirectly, included.
Equivalent weight specialized basis for expressing mass in chemical terms similar to, but different from,
molar mass. As a consequence of definition, one equivalent of an analyte reacts with one equivalent of a
reagent, even if the stoichiometry of the reaction is not one to one (Skoog et al, 2014). One equivalent
weight of a substance participating in a neutralization reaction is that amount of substance (molecule,
ion, or paired ion such as NaOH) that either reacts with or supplies one mole of hydrogen ions, H⁺, in
that reaction (Harvey, 2000). For monoprotic acid such as HCl, the equivalent weight is the same as the
formula weight. One mole of the acid provides one mole of H3O⁺.

EW HCl = FW HCl = 1 mol HCl = 1 mol H3O⁺

However, for diprotic acid such as sulfuric acid, one-half mole of the acid provides one mole of H3O⁺.

EW H2SO4= ½ FW H2SO4 = ½ mol H2SO4 = 1 mol H3O⁺

In this experiment, the equivalence of the unknown acid is equal to the equivalence of the NaOH at
equivalence point.

Generally, this experiment aims to discuss the principles and techniques in acid-base titration: the
preparation, comparison and standardization of solutions. Also, this experiment involves identification
of an unknown acid and determining its equivalent weight using acid-base titration principles and data
collected from the experiment.




moles NaOH = (MNaOH)(Vsolution) 40.00 g

mass NaOH = (0.025 mole) •
= (0.05 M)(0.500 L) mole
= 0.025 mole NaOH = 1.00 gram NaOH
to be dissolved in 500-mL dH2O


VHCl =
(0.05 M) (0.500 L)
= = 0.025 mL = 25.00 mL of 1.0 M HCl
1.0 M
to be diluted in 500-mL dH2O



Table 4.1. Preparation of standard NaOH solution

Mass of 50-mL beaker, g
Mass of beaker + NaOH pellets, g
Mass of NaOH pellets, g
Volume of NaOH prepared, mL

Table 4.2. Preparation of standard HCl solution

Volume of 1.0 M HCl used, mL
Volume of HCl prepared, mL

Table 4.3. Standardization of NaOH solution

Trial 1 Trial 2
Weight of E-flask, g
Weight of E-flask + KHP, g
Weight of KHP, g
Final volume of NaOH, mL
Initial volume of NaOH, mL
Volume used, mL
(In case of back titration)
Final volume of HCl, mL
Initial volume of HCl, mL
Volume used, mL
Normality of NaOH solution, N

Table 4.4. Volume ratios of standard solutions

Trial 1 Trial 2
Final volume of HCl, mL
Initial volume of HCl, mL
Volume used, mL
Final volume of NaOH, mL
Initial volume of NaOH, mL
Volume used, mL
1.000 mL HCl = =
1.000 mL NaOH = =
Normality of HCl solution, N

Table 4.5. Determination of equivalent weight of unknown acid

Unknown No.
Trial 1 Trial 2
Weight of E-flask, g
Weight of E-flask + unknown, g
Weight of unknown, g
Final volume of NaOH, mL
Initial volume of NaOH, mL
Volume used, mL
Equivalent weight
Identity of the acid:

Date completed: