FACULTY OF SCIENCE

ANALYTICAL CHEMISTRY

Student Surname : MVITA

Student Name : KANDE HENOCH

Student Number : 220130820

Course name : Analytical Chemistry Practical

Lecturers Name : Ms. HANNELI DU PLESSIS-FISCHER

Ms. PHILISWA NOMNGONGO

Title of Assignment : Laboratory report on Standardization of

a solution of H3PO4

Due date for Assignment : Friday, 19th March, 2021

Numbers of Pages :9

Locker Number : B140

Laboratory : Q/K LAB

ANTI-PLAGIARISM DECLARATION

1. Plagiarism is to present someone else’s ideas as my own.

2. I know that plagiarism is wrong.
2.1 I understand what plagiarism is and am aware of the University’s policy in this regard.
A. I declare that I have written my own sentences and paragraphs throughout my report.
B. I declare that this report is my own original work.
C. I have not allowed, and will not allow, anyone to copy my work with the intention of
passing it off as his or her own work.

SIGNATURE:_________________________ DATE:__19 March 2021

 STANDARDIZATION OF PHOSPHORIC ACID AGAINST SODIUM
HYDROXIDE (volume/volume Titration)

1. Aim
The aim of this experiment is to prepare solution of Sodium Hydroxide (NaOH) and
standardize a primary solution Phosphoric Acid using screened methyl orange indicator for
the first end point and Thymolphthalein indicator against a solution of Sodium Hydroxide, first
of all, the concentration of NaOH must be determined by titrating it against a standard
solution of Potassium Hydrogen phthalate (KHC 8H4O4 or KHP) using a mass/volume titration
and phenolphthalein as the indicator.

2. References
• GH Jeffery, J Bassett, J Mendham and RC Denney, Vogel’s Textbook of Quantitative
Chemical Analysis, 5th ed., Longman Scientific and Technical, London, 1989. p.265-
268;276-277; 297
• DA Skoog, DM West, FJ Holler and SR Crouch, Fundamentals of Analytical Chemistry,
9th ed., Brooks/Cole, USA, 2014, p.326; 352; 367-368
• H Oosthuizen, Practical Manual for Analytical Chemistry Students, University of
Johannesburg, 2000. p.48-50

3. Equation
The chemical equations of the reaction that will take place during this experiment are:
a) Standardization of NaOH against KHP
KHC8H4O4 + NaOH → H2O + NaKC8H4O4

b) Standardization of NaOH against H 3PO4

Titration set 1 (Screened Methyl orange indicator):
H3PO4(aq) + NaOH(aq) → NaH2PO4(aq) + H2O(l)

Titration set 2 (Thymolphthalein indicator):

H3PO4(aq) + 2NaOH(aq) → Na2HPO4(aq) + 2H2O(l)

4. Materials
During this experiment, two types of materials were used as listed below:
REAGENTS
Potassium hydrogen phthalate solid AR
Sodium Hydroxide solid
Phenolphthalein indicator
Distilled water
Phosphoric Acid [0.1M]
Screened Methyl orange indicator
Thymolphthalein indicator
 5. Preliminary calculations

a. Concentration of NaOH needed

Is 0.1 M NaOH suitable?
For end point 1, volume of NaOH required to perform this titration will be approximatively
25.00mL if the concentration is 0.1 M NaOH and this volume is suitable for the end point 1
0.1 𝑚𝑜𝑙 𝐻3 𝑃𝑂4 1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1
𝑉𝑜𝑙𝑢𝑚𝑒 𝑁𝑎𝑂𝐻 = ( × 0.025𝐿 ) × × × 1000𝑚𝐿
𝐿 1 𝑚𝑜𝑙 𝐻3 𝑃𝑂4 0.1 𝐿
𝑉𝑜𝑙𝑢𝑚𝑒 𝑁𝑎𝑂𝐻 = 25𝑚𝐿

For end point 2, the mole ratio is 2 moles NaOH : 1 mole H3PO4 and the volume of NaOH will
be 50.00mL if the concentration of NaOH 0.1M which is not suitable because that is the
entire volume of the burette.
0.1 𝑚𝑜𝑙 𝐻3 𝑃𝑂4 2 𝑚𝑜𝑙𝑒𝑠 𝑁𝑎𝑂𝐻 1
𝑉𝑜𝑙𝑢𝑚𝑒 𝑁𝑎𝑂𝐻 = ( × 0.025𝐿 ) × × × 1000𝑚𝐿
𝐿 1 𝑚𝑜𝑙 𝐻3 𝑃𝑂4 0.1 𝐿
𝑉𝑜𝑙𝑢𝑚𝑒 𝑁𝑎𝑂𝐻 = 50.00𝑚𝐿

The concentration of NaOH can’t be 0.1 M because it is not suitable for both titration sets.

Is 0.2 M NaOH suitable?

For end point 1, volume of NaOH required to perform this titration will be approximatively
12.50mL if the concentration is 0.2 M NaOH and this volume is not suitable because it is too
close to the volume of 10.00mL.
0.1 𝑚𝑜𝑙 𝐻3 𝑃𝑂4 1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1
𝑉𝑜𝑙𝑢𝑚𝑒 𝑁𝑎𝑂𝐻 = ( × 0.025𝐿 ) × × × 1000𝑚𝐿
𝐿 1 𝑚𝑜𝑙 𝐻3 𝑃𝑂4 0.2 𝐿
𝑉𝑜𝑙𝑢𝑚𝑒 𝑁𝑎𝑂𝐻 = 12.50𝑚𝐿

For end point 2, the mole ratio is 2 moles NaOH : 1 mole H3PO4 and the volume of NaOH will
be 25.00mL if the concentration of NaOH 0.1M which is suitable for the titration.
0.1 𝑚𝑜𝑙 𝐻3 𝑃𝑂4 2 𝑚𝑜𝑙𝑒𝑠 𝑁𝑎𝑂𝐻 1
𝑉𝑜𝑙𝑢𝑚𝑒 𝑁𝑎𝑂𝐻 = ( × 0.025𝐿 ) × × × 1000𝑚𝐿
𝐿 1 𝑚𝑜𝑙 𝐻3 𝑃𝑂4 0.2 𝐿
𝑉𝑜𝑙𝑢𝑚𝑒 𝑁𝑎𝑂𝐻 = 25.00𝑚𝐿

The concentration of NaOH can’t be 0.2 M because it is not suitable for both titration sets.

For titration set 1

For end point 1, the mole ratio is 1:1 and the volume of NaOH will be 16.67 mL which is
suitable if the concentration of NaOH 0.15M.
0.1 𝑚𝑜𝑙 𝐻3 𝑃𝑂4 1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1
𝑉𝑜𝑙𝑢𝑚𝑒 𝑁𝑎𝑂𝐻 = ( × 0.025𝐿 ) × × × 1000𝑚𝐿
𝐿 1 𝑚𝑜𝑙 𝐻3 𝑃𝑂4 0.15 𝐿
𝑉𝑜𝑙𝑢𝑚𝑒 𝑁𝑎𝑂𝐻 = 16.67 𝑚𝐿
 For titration set 2
For end point 2, the mole ratio is 2 moles NaOH : 1 mole H3PO4 and the volume of NaOH will
be 33.33 mL which is suitable if the concentration of NaOH 0.15M.
0.1 𝑚𝑜𝑙 𝐻3 𝑃𝑂4 2 𝑚𝑜𝑙𝑒𝑠 𝑁𝑎𝑂𝐻 1
𝑉𝑜𝑙𝑢𝑚𝑒 𝑁𝑎𝑂𝐻 = ( × 0.025𝐿 ) × × × 1000𝑚𝐿
𝐿 1 𝑚𝑜𝑙 𝐻3 𝑃𝑂4 0.15 𝐿
𝑉𝑜𝑙𝑢𝑚𝑒 𝑁𝑎𝑂𝐻 = 33.33 𝑚𝐿

All the volumes are suitable for the titration to happen, however the concentration of NaOH
needed to complete this titration will be 0.15 M

b. Mass of NaOH needed to prepare 500mL of ca. 0.15M NaOH solution

I will perform a minimum of 9 titrations with a maximum volume of 50mL for each titration.
I will need an extra 50 mL for cleaning the burette and for precaution. So I will prepare
500mL.
0.15 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 39.997𝑔 𝑁𝑎𝑂𝐻
𝑚𝑎𝑠𝑠 𝑁𝑎𝑂𝐻 = ( × 0.500𝐿) × = 2.999775𝑔 = 3.0𝑔
𝐿 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻
𝑚𝑎𝑠𝑠 𝑁𝑎𝑂𝐻 = 3.0𝑔
Weigh approximately 3.0 g of NaOH solid and dissolve in 500mL distilled water into a
beaker.
c. Masses of KHP needed to standardize 20-30mL of ca. 0.15M NaOH

For 20mL

0.15 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝐾𝐻𝑃 204.23 𝑔 𝐾𝐻𝑃

𝑚𝑎𝑠𝑠 𝐾𝐻𝑃 = ( × 0.020𝐿 ) × × = 0.61269 𝑔 = 0.61𝑔
𝐿 1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 𝑚𝑜𝑙 𝐾𝐻𝑃
𝑚𝑎𝑠𝑠 𝐾𝐻𝑃 = 0.61𝑔

For 30mL
0.15 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1 𝑚𝑜𝑙 𝐾𝐻𝑃 204.23 𝑔 𝐾𝐻𝑃
𝑚𝑎𝑠𝑠 𝐾𝐻𝑃 = ( × 0.030𝐿) × × = 0.9190𝑔 = 0.92𝑔
𝐿 1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 𝑚𝑜𝑙 𝐾𝐻𝑃
𝑚𝑎𝑠𝑠 𝐾𝐻𝑃 = 0.92 𝑔

Weigh approximately between 0.61g and 0.92g of KHP solid and dissolve in ca. 50mL
distilled water into a conical flask.
6. Flow chart
a) Standardization of ca. 0.15M of NaOH with KHP (m/v titration)

Weigh 0.61-0.92g of
KHP accurately into a
conical flask (x3)
Weight accurately 3.0 g of
NaOH and dissolve with
distilled water to the
Dissolve into 50mL of 500mL mark into a beaker
distilled water

Add 1-2 drops of

phenolphthalein indicator Burette : ca. 0.15M
NaOH
Titrate

Titrate until color changes

from colorless to faint pink Determine
concentration of NaOH

b) Standardization of ca. 0.1M of H3PO4 with 0.15M NaOH using screened methyl
orange indicator (v/v titration)

Pipette 25mL of 0.1M of

H3PO4 into a conical flask (x3)

Add 1-2 drops of indicator

screened methyl orange Burette : ca. 0.15M NaOH
indicator
Titrate

Titrate until color changes Determine

from magenta to grey concentration of H3PO4
c) Standardization of ca. 0.1M of with H3PO4 NaOH using thymolphthalein indicator
(v/v titration)

Pipette 25mL of 0.1M of

H3PO4 into a conical flask (x3)

Add 10 drops of
thymolphthalein indicator Burette : ca. 0.15M NaOH

Titrate

Titrate until color changes Determine

from colorless to faint blue concentration of H3PO4
 7. Results
Table 1 : Masses of KHP weighed out
Mass vial+ Salt Mass vial Mass Salt
(g) (g) (g)
1

Table 2 : Standardization of 0.15M NaOH with KHP (m/v titration)

Mass of KHP Initial reading Final reading Volume NaOH [NaOH] δ [NaOH]
burette Burette
X̄ (M)
(g) (mL) (mL) (mL) (M) (M)

CV
(%)

[NaOH] = _________ M
Table 3 : Standardization of H 3PO4 against 0.15M NaOH using screened methyl orange indicator
V(sample) Initial reading Final reading Volume NaOH
burette Burette S
X̄
(mL) (mL)
(mL) (mL) (mL) (mL)
25.00

25.00
CV
25.00 (%)

25.00

[NaOH] = _________ M

[H3PO4]= _________ M
Table 4 : Standardization of H 3PO4 against 0.15M NaOH using thymolphthalein indicator
V(sample) Initial reading Final reading Volume NaOH
burette Burette S
X̄
(mL) (mL)
(mL) (mL) (mL) (mL)
25.00

25.00
CV
25.00 (%)

25.00

[NaOH] = _________ M

[H3PO4]= _________ M
 8. Final Calculations

a) Standardization of ca. 0.15M NaOH with KHP

For replicate 1

1 𝑚𝑜𝑙 𝐾𝐻𝑃 1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1

[NaOH]1 = 𝑚𝑎𝑠𝑠 𝐾𝐻𝑃(𝑔) × × ×
204.23 𝑔 𝐾𝐻𝑃 𝑚𝑜𝑙 𝐾𝐻𝑃 −3
10 𝐿
𝑉(𝑁𝑎𝑂𝐻)𝑡𝑖𝑡𝑟𝑎𝑡𝑒𝑑 (𝑚𝐿) × 𝑚𝐿

1 𝑚𝑜𝑙 𝐾𝐻𝑃 1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 1

[NaOH]1 = _______𝑔 𝐾𝐻𝑃 × × ×
204.23 𝑔 𝐾𝐻𝑃 𝑚𝑜𝑙 𝐾𝐻𝑃 −3
10 𝐿
_______𝑚𝐿 × 𝑚𝐿

[NaOH]1 = _______________ 𝑀

Repeat the same calculations for replicate 2 and 3

[NaOH]2 = _______________ 𝑀

[NaOH]3 = _______________ 𝑀

𝐴𝑣𝑒𝑟𝑎𝑔𝑒 [NaOH] = _______________ 𝑀

b) Standardization of ca. 0.1M of H3PO4 against 0.15M NaOH using screened methyl
orange indicator (v/v titration)
C1×V1=C2×V2
𝐶𝑎𝑣𝑒𝑟𝑎𝑔𝑒 𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑁𝑎𝑂𝐻 × 𝑉𝑎𝑣𝑒𝑟𝑎𝑔𝑒 𝑣𝑜𝑙𝑢𝑚𝑒 𝑁𝑎𝑂𝐻
𝐶2 = ( )=
𝑉2

−3
________𝑀 × _______𝑚𝐿 × 𝑚𝐿 𝐿
10
[𝐻3 𝑃𝑂4] = −3
= ___________𝑀
25 × 10 𝐿
( )

[𝐻3 𝑃𝑂4] = _______________ 𝑀

 c) Standardization of ca. 0.1M of H3PO4 against 0.15M NaOH using thymolphthalein
indicator (v/v titration)

𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑚𝑜𝑙 NaOH 1 𝑚𝑜𝑙 𝐻3 𝑃𝑂4 1

[𝐻3 𝑃𝑂4 ] = ( × 𝑉𝑎𝑣𝑒𝑟𝑎𝑔𝑒 𝑣𝑜𝑙𝑢𝑚𝑒 𝑁𝑎𝑂𝐻 ) × ×
𝐿 2 𝑚𝑜𝑙𝑒𝑠 𝑁𝑎𝑂𝐻 10−3 𝐿
25𝑚𝐿 ×
𝑚𝐿

_________𝑚𝑜𝑙 NaOH 10−3 𝐿 1 𝑚𝑜𝑙 𝐻3 𝑃𝑂4 1

[𝐻3 𝑃𝑂4 ] = ( × _____𝑚𝐿 × )× ×
𝐿 𝑚𝐿 2 𝑚𝑜𝑙𝑒𝑠 𝑁𝑎𝑂𝐻 10−3 𝐿
25𝑚𝐿 ×
𝑚𝐿

[𝐻3 𝑃𝑂4 ] = _______________ 𝑀