EXPERIMENT 3: STANDARDIZATION OF SODIUM HYDROXIDE AND

DETERMINATION OF UNKNOWN ACID CONCENTRATION

OBJECTIVES:
1. To prepare the standard oxalic acid solution
2. To prepare and standardize the concentration of NaOH solution
3. To determine the concentration of an unknown, HX solution

INTRODUCTION:

A titration is an analytical procedure used to determine the concentration of a sample by reacting

it with a standard solution. One type of titration uses a neutralization reaction, in which an acid
and a base react to produce a salt and water. In a titration, the standard solution goes in a burette,
which is a piece of glassware used to measure the volume of solvent to approximately 0.1 mL of
accuracy. The solution that you are titrating goes in an Erlenmeyer flask, which should be large
enough to accommodate both your sample and the standard solution you are adding.
An indicator is any substance in solution that changes its color as it reacts with either an acid or a
base. Selecting the proper indicator is important because each indicator changes its color over a
particular range of pH values. An equilibrium occurs when the amounts of reactants and the
amounts of products are constant. When a system is in equilibrium, it will stay there until
something changes the conditions. In basic solution, there is an excess of OH- ions that react with
the HO- ions to form water. This shifts the equilibrium to the right because water is being formed
and H3O+ ions are being removed and we observe a pink solution. We can use this color change
to determine when the end of the titration has been achieved.

Standardizing a Sodium Hydroxide (NaOH) Solution

In a titration, it is critical to know the exact concentration of the titrant (the solution in the burette
which will be added to the unknown) in order to determine the concentration of the solution being
tested. We will standardize the ~0.1 M NaOH solution (the titrant) with oxalic acid (H2C2O4.2H2O)
and using phenolphthalein as the indicator.
RESULT:

A. Preparation of standard oxalic acid solution

Mass of C2H2O4.2H2O (g) 1.2

Molar mass of C2H2O4.2H2O (g/mol) 90.03

B. Preparation of 250 mL, 0.2 M NaOH solution

Mass of NaOH (g) 2.1

Molar mass of NaOH (g/mol) 39.98

C. Standardize of NaOH solution

Titration Volume of NaOH (mL)

Concentration
of NaOH (M)
Final Initial Volume used

1 28.90 0.00 28.90 0.11

2 29.20 0.00 29.20 0.11

3 29.40 0.00 29.40 0.11

Average 29.20 0.11

 D. Determination of unknown acid concentration

a. Determination of HX acid solution

Titration Volume of HX (mL)

Concentration
of HX (M)
Final Initial Volume used
‘
1 28.30 0.00 28.30 0.12

2 28.40 0.00 28.50 0.13

Average 28.4 0.12

b. Determination of H2X acid solution

Titration Volume of H2X (mL)

Concentration
of H2X (M)
Final Initial Volume used

1 43.00 9.90 33.10 0.15

2 48.50 15.00 33.50 0.15

Average 31.05 0.15

DISCUSSION:
Standardization refers to finding the exact concentration of a prepared solution using a standard
solution as the reference. Standard solutions are solutions of accurately known concentrations,
prepared using standard substances. There are two types of standard solutions known as primary
solution and secondary solution. A primary standard solution is a solution with a high purity and
less reactivity. A secondary standard is not that pure and is chemically reactive than primary
standards. This is the main difference between primary and secondary standard solution.

Primary standard solutions are solutions made out of primary standard substances. A primary
standard is a substance of known high purity (99.9% pure) which may be dissolved in a known
volume of solvent to give a primary standard solution. Primary standards are reagents that can
involve in chemical reactions. These compounds are often used to determine the unknown
concentration of a solution that can undergo a chemical reaction with the primary standard.

Primary standards comprise special chemical and physical properties. These compounds are
extremely pure and highly stable. Therefore, we can obtain pure solutions using these compounds.
For example, if we want to prepare a standard solution of 0.1 molL-1 concentration, we can
calculate the weight of the primary standard required for this and then dissolve that amount in a
suitable solvent. This gives exactly the 0.1 molL-1 solution with a high purity.

Standardization of solutions is a concept of analytical chemistry that is required for the accuracy
of a titration. Before we use any solution in a titration process, all the solutions should be
standardized with a primary standard solution. This is because, even though we weigh the exact
amount of a compound that is required to prepare a 0.1 molL-1 solution, it will not give the exact
concentration (due to the presence of impurities). However, since the concentration of the primary
standard solution is 99.9% accurate, we can titrate the prepared solution with a suitable primary
standard solution to find the exact concentration of the prepared solution.

Primary standards are highly pure due to their low reactivity. If these compounds were highly
reactive, they could get contaminated with many other chemicals, forming impurities. Primary
standards are less hygroscopic. Therefore, they do not absorb moisture from the air in considerable
amounts. This also makes the primary standards highly pure compounds.
A secondary standard solution is a solution that is made specifically for a certain analysis. A
secondary standard is a substance whose active agent contents have been found by comparison
against a primary standard. This means it is usually standardized against a primary standard.

Secondary standard solutions are used to calibrate analytical equipment and analytical techniques.
These solutions do not fulfill the requirements of a primary standard. A secondary standard has a
less purity than a primary standard. These are less stable and chemically reactive than primary
standards. Therefore, these compounds can get contaminated.

Anhydrous sodium hydroxide is a secondary standard. It is highly hygroscopic. Potassium

permanganate is another compound that is often used as a secondary standard. It is less stable and
is reactive. Therefore, in this experiment we used sodium hydroxide solution as the secondary
solution.

By using standard sodium hydroxide solution, NaOH we able to determined HX and H2X acid
concentration based on the result gained from both of the experiment. After the NaOH solution is
titrated with oxalic acid solution, concentration of NaOH solution can be determined. From the
equation below, 1 mol of NaOH is equivalence to 1 mol HX acid. After the standardization of
NaOH with oxalic acid and calculation is made, found that mole for NaOH is 0.11 M. Titration is
made between NaOH solution with HX acid solution to determine the concentration of HX acid
solution.

NaOH + HX NaX + H2O

Step 1: Concentration of oxalic acid

Mole of oxalic acid = mass of oxalic acid/ molar mass of oxalic acid

= 1.2 g/ 90.03g/mol

= 0.013 mol

Concentration of oxalic acid = mole of oxalic acid/ volume of distilled water

= 0.013 mol/ 0.1L

= 0.13 M
Step 2: Determine the concentration of sodium hydroxide from titration

By using this formula, a = refers to acid and b = refers to base

Ma x Va = Mb x Vb

Concentration of acid x volume of acid solution = Concentration of base x volume of base solution

0.13 M x 25mL = Mb x 29.2mL

3.25 MmL = Mb x 29.2 mL

Mb = 3.25 M mL/ 29.2 mL

= 0.11 M

Step 3: Determine the concentration of HX acid solution

Ma x 25mL = 0.11 M x 28.4 mL

Ma x 25 mL = 3.12 MmL

Ma = 3.12 MmL/ 25 mL

= 0.12 M

Step 4: Determine the mole for NaOH and mole HX acid

Mole of NaOH = 0.11 M x (28.4/1000) L

= 3.12x 10-3 mol

Mole of HX acid = 0.12 M x (25/1000) L

= 3.0 x 10-3 mol

So, we can say that mole of NaOH is equivalence to mole of HX acid solution.
From the equation below, 2 mol of NaOH is equivalence to 1 mol HX acid. After the
standardization of NaOH with oxalic acid and calculation is made, found that mole for NaOH is
0.15 M. Titration is made between NaOH solution with HX acid solution to determine the
concentration of H2X solution. Based on the chemical equation below clearly state that it needs
two moles of NaOH to neutralize one mole of H2X.

2NaOH + H2X Na2X + 2H2O

Step 3: Determine the concentration of H2X acid solution

Ma x 25mL = 0.11 M x 31.05 mL

Ma x 25 mL = 3.12 MmL

Ma = 3.12 MmL/ 25 mL

= 0.15 M

Step 4: Determine the mole for NaOH and mole H2X acid

Mole of NaOH = 0.11 M x (31.05/1000) L

= 3.42 x 10-3 mol

1 Mole of HX acid = 2 mole of NaOH

= 3.42 x 10-3 mol/2

= 1.71 x 10-3 mol

So, we can say that 1 mole of NaOH is equivalence to ½ mole of HX acid solution.

From these reactions we can observe that this reaction will produce two equivalence
points or stoichiometric points. The equivalence point, by definition, is the point during an acid-
base titration in which there has been equal amounts of acid and base reacted.
CONCLUSION:
Standard solutions can be divided into two groups as primary standard solutions and secondary
standard solutions. Primary standard solutions are solutions made out of primary standard
substances. Secondary standard solutions are not as pure as primary standard solutions. Purity is
the main difference between primary and secondary standard solution.

A neutralization reaction is when an acid and a base react to form water and a salt and involves
the combination of H+ ions and OH- ions to generate water. The neutralization of a strong acid
and strong base has a pH equal to 7. The neutralization of a strong acid and weak base will have a
pH of less than 7, and conversely, the resulting pH when a strong base neutralizes a weak acid will
be greater than 7.

When a solution is neutralized, it means that salts are formed from equal weights of acid and base.
The amount of acid needed is the amount that would give one mole of protons (H+) and the amount
of base needed is the amount that would give one mole of (OH-). Because salts are formed from
neutralization reactions with equivalent concentrations of weights of acids and bases: N parts of
acid will always neutralize N parts of base.

REFERENCES:

1. Dick, J. (1978). Analytical chemistry. Huntington, N.Y.: R.E. Krieger Pub. Co.

2. Difference Between Primary and Secondary Standard Solution | Definition, Properties,

Examples. (2019). Retrieved from https://pediaa.com/difference-between-primary-and-
secondary-standard-solution/

3. Harvey, D. (2019). Analytical Standards. Retrieved from

http://.libretexts.org/Bookshelves/Analytical_Chemistry/Book%3A_Analytical_Chemistr
y_2.0_(Harvey)/05_