Exercise 4

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EXERCISE 4: PREPARATION, COMPARISON AND STANDARDIZATION

OF SODIUM HYDROXIDE AND HYDROCHLORIC ACID SOLUTIONS


I.

OBJECTIVES

At the end of this exercise, the student should be able to:


1. Prepare 0.5 N NaOH and 0.05 HCl solutions;
2. Compare the relative strengths of the prepared acid and base solutions;
3. Standardize the acid and base solutions; and
4. Apply the techniques involved in the preparation, comparison and standardization of
solutions to be used in the acid-base titrations.
II.

PRINCIPLES

Volumetric Analysis is a quantitative method of determining the reagent needed to react


with analyte and there are different kinds of titration conducted like oxidation-reduction,
complex formation, precipitation reactions and acid-base titration (Harris, 2007). Acid-base
titration is the process of using a standard solution to determine the concentration of a solution. It
is used by measuring the delivered volume of the standard solution (titrant) required to react
stoichiometrically with the sample of a base or acid (analyte). It is usually conducted using a
buret that will deliver the titrant into a receiving container containing the analyte.
Prior to titration, standard solutions (titrant) are prepared and later standardized because it
should be of known concentration.
Standard solutions are prepared from strong acids (ex. HCl and H 2SO4) or bases (NaOH
and KOH). Their concentrations are expressed as either molarity, the number of moles solute per
liter of solution, or normality, the number of equivalents solute per liter of solution.
Acids are usually used as standard solutions because bases react with the glass when they
absorb atmospheric carbon dioxide; hence, better stored in plastic containers. In preparing solid
standard solutions, the accurately weighed solid is dissolved in a small amount of distilled water,
quantitatively transferred in a volumetric flask, added with distilled water up to the mark, and
mixing the contents thoroughly using a stopper. In preparing liquid standard solutions on the
other hand, the accurately measured liquid is transferred to a volumetric flask, distilled water is
added up to the mark and mixed (except for acidic solutions where the flask is half filled with
distilled water before adding the concentrated acid).
After the preparation from strong acids or bases, they are standardized to be officially
called standard solutions. Standardization is the process of determining the concentration of a
solution by calibration, directly or indirectly, with a primary standard, a solid pure substance.
A primary standard is a reference reagent of high purity for titration or other quantitative
methods. The accuracy of determining the concentration of a solution needed to react with a
primary standard depends on the characteristics of a primary standard. Some of the good
characteristics of a primary standard are: high purity, atmospherically stable compound, has no

water hydration, and of high molar mass so error is minimized when weighing. Since a few
compounds meet these criteria for a good primary standard, secondary standards are sometimes
used. A secondary standard is a compound whose purity has been determined by chemical
analysis.
There are different examples of primary standards used for titration of acids and bases.
For standardization of acids, the most commonly used primary standards are Sodium Carbonate
(Na2CO3) and Tris-(hydroxymethyl)aminomethane, ((HOCH2)3CNH2), while for the
standardization of bases, Potassium hydrogen iodate, KH(IO 3)2 and Potassium acid phthalate
(KHC8H4O4 or KHP) are used (Skoog, West, Holler & Crouch, 2014).
The concentration of the standard solution will now be determined using the volume of it
required to react with an accurately weighed amount of primary standard. KHP is the commonly
used primary standard for the standardization of sodium hydroxide (NaOH) solutions because it
has only one acidic proton per molecule of the potassium salt. The salt dissociates completely
into its ions K+ and biphthalate (HP-) when dissolved in water and the acidic hydrogen reacts
with the hydroxide of NaOH shown in the equation:
--------- Equation in book -----------

The steep rise in pH at the equivalence point is centered at about 8.8 and phenolphthalein
is used as an indicator.
In this exercise, HCl will not be standardized against a primary standard since the relative
strengths of NaOH and HCl has been determined. The normality of HCl can be calculated from
the normality of the NaOH solution (a secondary standard) and the ratio determined previously.
After the standardization of the standard solution which will be used as the titrant,
titration can now be conducted. When the exact amount of the titrant is added, necessary for the
stoichiometric reaction of the analyte, the equivalence point is reached; however, what we
actually measure is the end point where a sudden change in the physical or chemical property of
the analyte is observed e.g. indicator color change. The equivalence point and the end point are
rarely the same. However, in a good method the end point falls close to the equivalence point
that the two can be considered equal within experimental error, or, if there is a significant
difference between the two points, the difference is reproducible and may be corrected for.
For acid-base titrations, there are two most common methods for determining the end points of
titrations: use of colored indicators and use of a pH meter to monitor the solution pH as a
function of the volume of the added titrant. According to a book of Harris (2007), An indicator
is a compound with a physical property (usually color) that changes abruptly near the

equivalence point and the change is caused by the disappearance of analyte or the appearance of
excess titrant.
There are two types of titration conducted, the direct and back titration. In direct titration,
the titrant is added to the analyte until the reaction is complete, whereas in back titration, a
known excess of a standard solution is added to the analyte then the excess is titrated with a
second standard solution (Harris). Back titration is primarily used when the rate of reaction
between the analyte and reagent is slow or when the standard solution lacks stability (Skoog,
West, Holler & Crouch, 2014).
III.

PRE LAB CALCULATIONS AND FORMULAS

IV.

DATA AND RESULTS

Table 4.1 Determination of the weight of the primary standard (KHP)


Trial I

Trial II

Weight of vial + KHP, g


Weight of vial KHP, g
Weight of KHP, g
Trial I

Trial II

NaOH
Final buret reading, mL
Initial buret reading, mL
Volume of NaOH used, mL
HCl (in case of back titration)
Final buret reading, mL
Initial buret reading, mL
Volume of HCl used, mL
Normality of NaOH, N
Average Normality d, N
Table 4.2 Standardization of Sodium Hydroxide (NaOH) solution

Table 4.3. Determination of the volume needed to titrate the Hydrochloric acid (HCl) solution

Trial I

Trial II

HCl
Final buret reading, mL
Initial buret reading, mL
Volume of HCl used, mL
NaOH
Final buret reading, mL
Initial buret reading, mL
Volume of NaOH used, mL
Table 4.4 Comparison of sodium hydroxide (NaOH) and hydrochloric acid (HCl) solutions
Ratio
Trial I
Trial II
Vol. of NaOH/Vol. of HCl
Average: 1 mL HCl =
mL NaOH
Vol. of HCl/Vol. of NaOH
Average: 1 mL NaOH =
mL HCl
Table 4.5 Determination of the normality of Hydrochloric Acid (HCl) solution
Trial I

Trial II

Normality of HCl, N
Average Normality d, N
Signature: __________
Date: __________

V.

ANSWERS TO PRE LAB QUESTIONS

1. What are the characteristics of a good primary standard?


It should be stable, of high purity, and of large molar weight to minimize errors on the
balance.
2. What is the purpose of drying the primary standard prior to usage?
The purpose of drying is removing the traces of water adsorbed from the environment.
VI.

ANSWERS TO POST LAB QUESTIONS

REFERENCES:

Analytical and Environmental Chemistry Division. (2008). Instruction Manual for CHEM 32.1:
Quantitative Inorganic Analysis Laboratory: Institute of Chemistry, Laguna.
Harris, D.C. (2007). Quantitative Chemical Analysis 7th Ed.: W.H Freeman and Company, USA.
Skoog, D.A., West, D.M., Holler, F.J. & Crouch, S.R. (2014). Fundamentals of Analytical
Chemistry 9th Ed.: Mary Finch, USA.

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