The University of the South Pacific

School of Biological and Chemical Sciences

CH204 – Inorganic Chemistry

Preparative
Inorganic Chemistry
Experiment 1

Author(s): Shradha Chandra (S11196781)

Lab Session: Wednesday (8am – 12pm)
Lab Partner: Kartik Nath (S11196794)
Date: 24th August 2022
1.0 Introduction
Chemistry tends to be a broad subject which can be challenging to grasp it all, thus it
has been branched into various areas such inorganic chemistry, physical chemistry,
quantum chemistry and many more to name. Inorganic chemistry tends to be our area
of focus which deals with non-carbon compounds. However, it has some overlap with
Organic chemistry regarding organometal compounds and their bonding to carbons
(Inorganic Chemistry - American Chemical Society, 2022).

Moving on, the experiment was sectioned into two parts. The first one deals with the
production of sodium perborate. Under standard conditions such as standard
temperature and pressure, sodium perborate tends to be an odorless solid which is
white in colour (Robinson, 2022). The second part deals with manufacturing of
potassium aluminium, this tends to be a double salt which comes from the reactants
aluminium sulfate and potassium sulfate (University of the South Pacific,2022). All in
all, this experiment aims to form the products of sodium perborate and potassium
aluminium together with understanding the various procedures of achieving the
products.

2.0 Experimental
2.1 Materials and Chemicals Utilized
- Measuring cylinders - Borax
- Beakers - Sodium hydroxide
- Test tubes and Test tube rack - Hydrogen peroxide (30%)
- Watch glass - Potassium sulfate crystals
- Ice cubes - Aluminium sulfate crystals
- Glass rode - 𝐻2 𝑆𝑂4 (Dilute)
- pH paper - 𝐾𝑀𝑛𝑂4 (Dilute)
- Distilled water - Kl solution
- Filter paper
2.2 Methodology
2.2.1 Procedure One: Preparation of Sodium Perborate
Borax and sodium hydroxide were dissolved in cold water in the minimal quantity,
about 5.0 g borax and 1.09 g NaOH. The dissolved combination was then gradually
added to a 6ml solution of 30% H2O2 in 10ml of water. After cooling, the solution
was dissolved in ice water. Small sodium perborate crystals started to separate after
15 minutes of stirring. The crystals were subsequently cleaned using cold water and a
little amount of ethanol while undergoing vacuum filtration. The crystals were
allowed to air dry. The salt was steady before it stopped, then it slowly began to break
down. The yield % was then calculated once the crystals had been weighed.
Furthermore, to crystals were mixed with water and several tests were conducted. To
begin with, a pH test was done by placement of small amount of solution on a pH
paper. Secondly, 2-3 drops were added to a dilute solution of H2SO4 and KI solution
then tested on a starch iodide solution. Moreover, some drops were applied to H2SO4
and KMnO4 mixture. Lastly, these tests were repeated with H2O2.
 2.2.2 Procedure Two: Preparation of Potassium Aluminium
Addition of 0.63 g of crystallized potassium sulfate, a 50 ml beaker was utilized.
Followed by a 6.60ml of distilled water using a measuring cylinder. The crystals'
dissolution had been agitated. 2.51 g of aluminium sulfate crystals were taken to a
second 50 ml beaker. To stop the hydrolysis of aluminium sulfate, 6.5ml of distilled
water was added to 1ml of sulfuric acid to form a mixture. Furthermore, blending of
the two solutions proceeded in a china bowl, which was then submerged in cold
water. A glass rod had been used to stir the fluid. The solution was concentrated until
a firm crust had formed on top of the solution. This demonstrated that crystallization
had progressed to its final stage. The dish was then put in a tiny bowl of cold water.
The octahedral crystals started to split quickly. Ice-cold distilled water was utilized
for cleansing the crystals after the main liquid had been decanted. By sandwiching the
crystals between filter pads, they have been dried. The obtained double salt's melting
point was discovered by measuring it in a melting point equipment, and its value was
compared to that of the literature.

3.0 Data and Calculation

3.1 Procedure One Results

Test Observation With H2O2
A small drop of solution pH level = 10 pH level = 5
on pH paper
Starch Iodide Paper Colour change to bluish Colour change to bluish
black black
H2SO4 and KMNO4 Colour change to Colour change from
solution with sodium colourless purple to clear
perborate

Equation of Sodium Perborate

Na2[B4O5(OH)4].6H2O + 2NaOH +4H2O2 → 2Na2[B2(O2)2(OH)4].6H2O + 3H2O

Borax: Sodium Hydroxide:

n = m/Mr n = m/Mr
= 5.00 g/381.38 g/mol = 0.98 g/ 39.997 g/mol
= 0.0131 moles = 0.0245 moles

➢ By the mole calculation, it is found

that the mole of Borax is less
compared to the Sodium Hydroxide
moles. Thus, Borax is the limiting
reagent.
 Mole Ratio: Theoretical Value Experimental Value
(Sodium Perborate) (Sodium Perborate)
Borax : Sodium Perborate
1: 2 m = n × Mr Watchglass = 24.82g
0.0131 : x = 0.013 × 153.86 Watchglass with
= 4.03grams product=28.5g
x(Sodium Perborate) =
0.00655 moles Yield = 3.68grams

Percentage Yield:

% Yield = Experimental Value/Theoretical Value × 100

= 3.68g / 4.03 g × 100
= 91.32%

3.2 Procedure Two Results

Expected yield = 2.5 grams
Actual yield of potassium aluminium = 1.69 grams
Literature melting point of potassium aluminium = 92.5°𝐶
(Potassium Aluminum Sulfate, 2022)
Experimental melting point of potassium aluminium = 86.5°𝐶

4.0 Discussion

➢ When viewing the yield achieved of sodium perborate in procedure one, being
91.32%, it can be safely assumed that the experimental yield is very close to the
expected yield (4.03grams). These values display the success of the carried
procedures and also indicates that there had been utmost minimum amount of
experimental errors occurring during the procedures.

➢ Some experimental errors may have occurred which resulted in the achieved yield,
such as the measure of reactants and the product and failure to completely remove
water from the final product achieved.

➢ Moreover, in procedure two, experimental errors may have occurred resulting in

failure of accuracy within the experiment. Some errors that occurred was the
fluctuation of heat on the heating plate which resulted in less crystal formation.
Secondly, at the decanting stage, not all crystals were entirely removed resulting in a
1.68grams of yield rather than the expected yield of 2.5grams.
 ➢ Furthermore, the literature melting point of potassium aluminium varies from the
experimental melting point, this may have resulted due to the impurities collected
within the experiment.

5.0 Post – Lab Question Solutions

(1). Borax → Chemical Formula = Na2B4O5(OH)4•6H2O
Molecular Formula = H20B4Na2O17

(2). Perborate Anion Structure

O O
HO OH
- -
B B
HO OH
O O

(3). Only one Boron tends to have an orthoborate and metaborate, in perborate
anion alignment. Atoms tend to be less visible towards Oxygen, thus making
their bond with Boron a negative bond.

(4). Na2B407. 10H2O + 2NaOH + 4H2O2 → 4 NaBO3. 4H2O + 11H2O

(5). The product obtained cannot kept as sodium perorate always goes into
decomposition with the free oxygen and water. This can be displayed in the
equation; 2Na2[B2(O2)2(OH)4]. 6H2O → 2𝑁𝑎𝐵𝑂2 + 6𝐻2 0 + 2𝐻2 𝑂2

(7). To remove contaminants and water molecules, there was an addition of

alcohol and ethanol. This also helped avoid the decomposition of the product
obtained.

6.0 Conclusion
Upon the completion of the experiment, it can be concluded that both the procedures
were carried out successfully and the results obtained were carefully. Although, there
were experimental errors due to not having the exact standard conditions as required
by the products, very close results to literature values for both the experiments were
achieved. All in all, the aim of the experiment was achieved together with refreshing
and learning the basics laboratory materials.

7.0 References
American Chemical Society. 2022. Inorganic Chemistry - American Chemical
Society. [online]. [Accessed 2 September 2022].
https://www.acs.org/content/acs/en/careers/chemical-sciences/areas/inorganic-
chemistry.html

Robinson, A., 2022. How to Use Sodium Perborate. [online] Sciencing. [Accessed 2
September 2022].
https://sciencing.com/use-sodium-perborate-5215007.html
 Science.jrank.org. 2022. Potassium Aluminum Sulfate. [online] [Accessed 2
September 2022]
https://science.jrank.org/pages/5422/Potassium-Aluminum-Sulfate.html

University of the South Pacific (2022) CH201 Laboratory Handout, Suva: University
of the South Pacific

8.0 Appendix