DEPARTMENT OF CHEMISTRY

FACULTY OF SCIENCE OF MATHEMATICS

PRACTICAL ASSIGNMENT 1

STANDARDISATION OF SODIUM HYDROXIDE AND

DETERMINATION OF UNKNOWN ACID
CONCENTRATION

NAME OF GROUP MEMBERS : ID NO. :

THUSHIDRASRI A/P ARMUGAM E20191024039

MUSFIRAH NAFISAH BINTI MUSYIRI E20191024043

H’NG BEI EN E20191024045

DAY/TIME
LABORATORY
DEMONSTRATOR DR. WAN HASLINDA BINTI WAN AHMAD
PRACTICAL ASSIGNMENT 1
STANDARDISATION OF SODIUM HYDROXIDE AND DETERMINATION OF
UNKNOWN ACID CONCENTRATION

Objectives:

Upon completion of this experiment, students should be able to:

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

An acid-base titration is a neutralization reaction that is performed in the lab in order to

determine an unknown concentration of acid or base. Titration, also known as volumetric
analysis, is a quantitative laboratory method used to determine the concentration of a
reactant. During titration, a titrant (a reagent of known concentration) is used to react with the
analyte (a measured volume of the reactant). Within this lab, a titration will be performed
between an acid and a base, using an acid-base reaction. Such a reaction is also known as a
neutralization, for it involves the neutralization of one reactant by another. When a basic
solution is added to an acidic solution of unknown concentration, hydroxide atoms from the
basic solution will react with the hydronium ions from the acidic solution, and thus form
water. As the hydronium ions react with the added hydroxide ions, the pH will change,
because pH measures the molarity of hydronium ions. The solution will reach its equivalence
point, when the number of moles of hydroxide ions added is equal to the number of moles of
hydronium ions. This change will easily be seen on a graph, for pH tends to jump sharply
when the equivalence point has been reached.

Chemical reactions between acids and bases are important processes. These reactions can be
used to synthesize new substances or to analyze the quantity of a pure substance or of a
compound in a mixture. In this experiment, you will first determine the concentration of a
base, NaOH, and then use this standardized base to determine the molar mass of an unknown
weak acid. Based on the molar mass you will determine the identity of the unknown acid.
In water strong acids produce hydronium ions and strong bases produce hydroxide ions. The
reaction of a strong acid with a strong base is represented with the chemical reaction shown
in Equation 1. Chemists regard this as a reaction that goes to completion; that is all of the
reactants are converted to products.

H3O+ + OH- →2H2O (Equation 1)

This equation states that one mole of hydrogen ions (acid) will neutralize one mole of
hydroxide ions (base). Since we can exactly measure the moles of the standard solution, we
can assume that the moles of the solution of unknown concentration will be the same at the
neutral point. This is called the end-point of the titration. Using the equation MaVa = MbVb,
we can use the experimental data from the titration to find the unknown concentration.

In where the number of moles = molarity (M) x volume ( in liter @dm3 )

𝑀𝑎𝑉𝑎 1
=
𝑀𝑏𝑉𝑏 1

where ,

Ma and Mb = Molarity of acid and base

Va and Vb = Molarity of acid and base

For the neutralization between oxalic acid and sodium hydroxide is expressed by
the balanced chemical equation:
H2C2O4 (aq) + 2NaOH (aq)  Na2C2O4 (aq) + 2H2O (l)

The 1:2 ratio of the acid to the base in the balanced equation indicates that twice as
many moles of base are needed than of acid:
𝑀𝑎𝑉𝑎 1
=
𝑀𝑏𝑉𝑏 2

CHEMICALS

Acid solution (HX and H2X)

Distilled water
Oxalic acid dehydrate
Phenolphthalein indicator
Sodium hydroxide pellets
APPARATUS

Analytical balance
Beaker (100 mL and 250 mL)
Burette (50 mL)
Erlenmeyer flask (250 mL)
Glass rod
Pipette (25 mL)
Volumetric flask (100 mL and 250 mL)

PROCEDURE

Part A : Preparation of standard oxalic acid

1. 1.2 g of pure oxalic acid dehydrate crystals weighed accurately in a 100 mL beaker.
2. The crystals were dissolved in the beaker by adding small volume of distilled water.
3. The solution was transferred quantitatively into a 100 mL volumetric flask.
4. The molarity of the oxalic acid solution was calculated.

Part B : Prepration of 250 mL, 0.2 M NaOH solution

1. A quantity of NaOH pellets was weighed by using analytical balance.

2. The pellets were transferred to the 250 mL clean beaker.
3. The pellets were dissolved using small volume of distilled water.
4. The distilled water was added until 250 mL and the solution homogenized using
glass rod.

Part C : Standardization of NaOH solution

1. A burette was set up and NaOH was used as a titrant.

2. The initial burette reading was recorded.
3. 25.00 mL of oxalic acid solution pipette from part A into 250 mL Erlenmeyer
flask. Triplicate samples were prepared.
4. Three drops of phenolphthalein indicator were added into each flask.
5. The acid solution titrated with NaOH solution.
6. The procedures repeated with 2 more samples.
7. The exactly molarity of NaOH solution was calculated.
Part D : Determination of Unknown Acid Concentration

1. 25 mL HX acid solution pipette into 250 mL volumetric flask.

2. The solution was diluted with distilled water until reach the mark.
3. 25 mL of this solution was transferred to 250 mL Erlenmeyer flask.
4. 3 drops of phenolphthalein indicator was added to the solution in the flask.
Triplicate samples were prepared.
5. The unknown acid concentration was titrated using standardized NaOH solution
prepared in part B.
6. The volume of of NaOH solution required to completely react with acid was recorded.
7. The titration was repeated at least 3 times.
8. Steps 1 – 4 above repeated for H2X.
9. The concentration of HX and H2X was calculated.
10. The stock solution of HX and H2X before dilution was calculated.

FLOWCHART

Experiment 1
RESULTS

A. Preparation of standard oxalic acid solution

Mass of H2C2O4.2H2O (g) 1.3068

2(1.0079)+2(12.011)+4(15.999)+4(1.0079)
Molar mass of H2C2O4.2H2O (g/mol)
+2(15.999) = 126.06

B. Preparation of 250 mL, 0.2 M NaOH Solution

Mass of NaOH (g) 1.9998

Molar mass of NaOH (g/mol) (22.990)+(15.999)+(1.0079) = 39.997

C. Standardization of NaOH Solution

2NaOH + H2C2O4.2H2O Na2C204 + 4H2O

𝑀,𝑉, 1
=
𝑀,𝑉, 2

2 𝑀,𝑉, = 𝑀,𝑉,

𝑔𝑟𝑎𝑚 (𝑔)
𝑀𝑜𝑙 𝑜ƒ 𝑂𝑥𝑎𝑙i𝑐 𝐴𝑐i𝑑 𝑆𝑜𝑙𝑢𝑡i𝑜𝑛 𝑔
= 𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 ( )
𝑚𝑜𝑙
1.3068 𝑔
𝑔
= 126.06
𝑚𝑜𝑙

10³ 𝑚𝑚𝑜𝑙
= 0.0104 𝑚𝑜𝑙 x
1 𝑚𝑜𝑙
= 10.400 𝑚𝑚𝑜𝑙

𝑚𝑚𝑜𝑙
𝑀𝑜𝑙𝑎𝑟i𝑡𝑦 (𝑀)𝑜ƒ 𝑂𝑥𝑎𝑙i𝑐 𝐴𝑐i𝑑 𝑆𝑜𝑙𝑢𝑡i𝑜𝑛 =
𝑚𝐿
10.400 𝑚𝑚𝑜𝑙
=
100.0 𝑚𝐿
= 0.104 𝑀
 Volume of NaOH
Concentration of NaOH (M)
Titration (mL)
Final Initial Volume used
2 𝑀,𝑉, = 𝑀,𝑉,
1 26.20 0.00 2(0.104𝑀 x 25.00𝑚𝐿) = (𝑀)(26.20𝑚𝐿)
= 26.20 – 0.00 5.20𝑀. 𝑚𝐿
= 26.20 =𝑀
26.20𝑚𝐿
𝑀 = 0. 198
2 𝑀,𝑉, = 𝑀,𝑉,
2 28.15 1.00 2(0.104𝑀 x 25.00𝑚𝐿) = (𝑀)(27.15𝑚𝐿)
= 8.15 – 1.00 5.20𝑀. 𝑚𝐿
= 27.15 =𝑀
27.15𝑚𝐿
𝑀 = 0. 192

2 𝑀,𝑉, = 𝑀,𝑉,
3 29.10 3.00 2(0.104𝑀 x 25.00𝑚𝐿) = (𝑀)(26.10𝑚𝐿)
= 29.10 – 3.00 5.20𝑀. 𝑚𝐿
= 26.10 =𝑀
26.10𝑚𝐿
𝑀 = 0. 199

0.198 + 0.192 + 0.199

Average = 0. 196
3

D. Determination of unknown acid concentration

i) Determination of HX acid solution

NaOH + HX NaX + H2O

𝑀,𝑉, 1
=
𝑀,𝑉, 1

𝑀,𝑉, = 𝑀,𝑉,
 Volume of NaOH
Concentration of HX (M)
Titration (mL)
Final Initial Volume used
𝑀,𝑉, = 𝑀,𝑉,
1 38.00 0.00 = 38.00 – 0.00 (𝑀)(25.00𝑚𝐿) = (0.2𝑀 x 38.00𝑚𝐿)
= 38.00 7.60𝑀. 𝑚𝐿
𝑀=
25.00𝑚𝐿
𝑀 = 0. 304

𝑀,𝑉, = 𝑀,𝑉,
2 42.00 2.00 (𝑀)(25.00𝑚𝐿) = (0.2𝑀 x 40.00𝑚𝐿)
= 42.00 – 2.00
= 40.00 8.00𝑀. 𝑚𝐿
𝑀=
25.00𝑚𝐿
𝑀 = 0. 320
𝑀,𝑉, = 𝑀,𝑉,
3 41.00 2.00 (𝑀)(25.00𝑚𝐿) = (0.2𝑀 x 39.00𝑚𝐿)
= 41.00 – 2.00
7.80𝑀. 𝑚𝐿
= 39.00 𝑀=
25.00𝑚𝐿
𝑀 = 0. 312

0.304 + 0.320 + 0.312

Average = 0. 312
3

ii) Determination of H2X acid solution

2 NaOH + H2X Na2X + 2 H2O

𝑀,𝑉, 1
=
𝑀,𝑉, 2

2 𝑀,𝑉, = 𝑀,𝑉,
 Volume of NaOH
Concentration of H2X (M)
Titration (mL)
Final Initial Volume used
2 𝑀,𝑉, = 𝑀,𝑉,
1 26.00 0.00 = 26.00 – 0.00 2(𝑀)(25.00𝑚𝐿) = (0.2𝑀)(26.00𝑚𝐿)
= 26.00 5.20𝑀. 𝑚𝐿
𝑀=
50.00𝑚𝐿
𝑀 = 0. 104
2 𝑀,𝑉, = 𝑀,𝑉,
2 29.50 2.00 = 29.50 – 2.00 2(𝑀)(25.00𝑚𝐿) = (0.2𝑀)(27.50𝑚𝐿)
= 27.50 5.50𝑀. 𝑚𝐿
𝑀=
50.00𝑚𝐿
𝑀 = 0. 110

2 𝑀,𝑉, = 𝑀,𝑉,
3 32.00 3.00 = 32.00 – 3.00 2(𝑀)(25.00𝑚𝐿) = (0.2𝑀)(29.00𝑚𝐿)
= 29.00 5.80𝑀. 𝑚𝐿
𝑀=
50.00𝑚𝐿
𝑀 = 0. 116

0.104 + 0.110 + 0.116

Average = 0. 110
3

CALCULATION

i) Stock Solution of HX Before Dilution

HX + NaOH NaX + H2O

𝑀,𝑉, 1
=
𝑀,𝑉, 1

𝑀,𝑉, = 𝑀,𝑉,

(𝑀)(25.00 𝑚𝐿) = (0.2 𝑀)(250 𝑚𝐿)

50.0 𝑀. 𝑚𝐿
𝑀=
25.00 𝑚𝐿

𝑀 = 2.00 𝑀
 i) Stock Solution of H2X Before Dilution

2 NaOH + H2X Na2X + 2 H2O

𝑀,𝑉, 1
=
𝑀,𝑉, 2

2 𝑀,𝑉, = 𝑀,𝑉,

2(𝑀)(25.00 𝑚𝐿) = (0.2 𝑀)(250 𝑚𝐿)

50.0 𝑀. 𝑚𝐿
𝑀=
50.0 𝑚𝐿

𝑀 = 1.00 𝑀

DISCUSSION

The purpose of this lab was to prepare the standard oxalic acid solution which is in part A.
Second, to prepare and standardise the concentration of NaOH solution. Lastly, to determine
the concentration of an unknown , HX solution by titrating measured volumes with a strong
base of known concentration. During this lab, the molarity of H2C2O4 , oxalic acid solution
was calculated in part A. Using the equation for concentration (M= n/V), the molarity of the
oxalic acid solution was 0.104 M. The standard oxalic acid solution was prepared for
titration. In the part B, 0.19998g of NaOH used to prepare 0.2M NaOH solution in 250ml
volumetric flask. Then, the NaOH solution from part B, was used as titrant while as analyte
25mL of oxalic acid solution was pipetted from part A into Erlenmeyer flask for prepare
triplicate samples. During part C, a proper titration technique was applied where the end point
is reached when one drop of NaOH solution turns the entire solution in the Erlenmeyer flask
from colourless to faint pink. The end point colour should be pale pink not dark pink,
otherwise, the reading will overshoot than the actual value. After observed the physical
changed, the initial and final volume of NaOH (mL) is recorded. The concentration of NaOH
(M) was calculated. Using the balanced equation and the equation for concentration which
is, Dissolution of oxalic acid dihydrate in water:

H2C2O4 • 2H2O (s)  H2C2O4 (aq) + 2H2O (l)

Titration of the oxalic acid with NaOH:

H2C2O4 (aq) + 2NaOH (aq)  Na2C2O4 (aq) + 2H2O (l)

 𝑀𝑎𝑉𝑎 1
=
𝑀𝑏𝑉𝑏 2

The average concentration of the NaOH (M) solution was found to be 0.196 M. The results
of this lab were rather inaccurate, as the calculated average concentration of the NaOH
solution almost reached the expected concentration of 0.2M. Part D was determination of
an unknown monoprotic (i) and diprotic acid (ii) solution concentration using the
standardized NaOH solution from part C. The first step is briefly described below which is
neutralization reaction proceeds as follows:

i) Determination of HX acid solution (monoprotic acid)

HX + NaOH  Na+ + X- + H2O

HX + NaOH  NaX + H2O

The 1: 1 ratio of the acid to the base in the balanced equation indicated that 1 mole of NaOH
is equal to the 1 mole of unknown acid. To calculate the concentration of the HX solution has
1
been used this equation: 𝑀𝑎𝑉𝑎 = . From the result we obtained the average concentration of
𝑀𝑏𝑉𝑏 1
HX (M) was 0.312 M by used the equation above.

ii) Determination of H2X acid solution (diprotic acid)

H2X + NaOH  Na+ + X2- + H2O

H2X + 2NaOH  Na2X + 2H2O

The 1: 2 ratio of the acid to the base in the balanced equation indicated that 2 moles of
NaOH is equal to the 1 mole of unknown acid. To calculate the concentration of the H2X
1
solution has been used this equation: 𝑀𝑎𝑉𝑎 = . From the result we obtained the average
𝑀𝑏𝑉𝑏 2
concentration of H2X (M) was 0.110 M by used the equation above.

Once this reaction is complete, an excess of NaOH starts building up, triggering the response
from the indicator:

NaOH + HIn(colorless)  Na+ + In-(pink) + H2O.

At the analyte, the physical change occurred which was from colourless to faint pink.
Safety Precautions

Every laboratory experiment, we must always wear safety goggles and a lab apron to protect
your eyes and clothing. If you get a chemical in your eyes, immediately flush the chemical
out at the eyewash station while informing the lab assistant. We should know the location of
the emergency lab shower and the eyewash station and the procedure for using them.
Do not touch any chemicals. If you get a chemical on your skin or clothing, wash the
chemical off at the sink. Besides that, never return leftovers to their original containers; take
only small amounts to avoid wasting supplies.

CONCLUSION

In this lab, we used titration to explore the concepts of stoichiometry and equivalence
points. The study demonstrates that the titration method relying on visual detection of
the end point allows for fairly precise determination of the unknown concentration.
Both bases and acids can be analysed in this manner , as illustrated in this report
:average CNaOH : 0.196M , average CHX : 0.312M and average CH2X : 0.110M . The precision
and accuracy of the method can be improved by a). fitting the buret with an electronic
device to control the flow of the fluid, b) using a spectrophotometer to detect the color
change at the end point of the titration and c)using a special small-volume chamber
where two solutions – basic and acidic – can be rapidly mixed in order to prevent a time
lag from slow diffusion. Indeed, one could envisage a simpler measurement scheme where
the solution of NaOH is prepared with known concentration and used to titrate an unknown
acid. Bear in mind, however, that NaOH is a poor primary standard: it is highly hygroscopic,
chemically unstable (reacts with CO2 of air), typically low-purity (if purchased cheap), and
has low molecular weight (which leads to higher relative error when the compound is
weighed out). Conversely, H2C2O4 has many desirable characteristics which make it a good
primary standard. This dictates a choice of the two-step scheme, with H2C2O4 as a primary
standard and NaOH as a secondary standard.

REFERENCES
1. https://www.chem.purdue.edu/courses/chm224/Miscellaneous/Model_report_Expt2-
revised_2009.pdf
2. http://www.chem.latech.edu/~deddy/chem104/104Standard.htm
3. https://www.lacitycollege.edu/Departments/Chemistry/documents/Chemistry-101-
Experiments-Documents/E12A_titration12_2017
4. http://ww2.chemistry.gatech.edu/class/3281/janata/3281-3.pdf