FACULTY OF SCIENCE

Bachelor of Science (Hons) Chemistry

Year 1 Trimester 3
UDEC 1134 – CHEMISTRY LABORATORY I

Name: OH ZI YI 1802711
Experiment: Experiment 9
Title: Preparation and Studies of Potassium Diaquabis (Oxalato)
Chromate (III) Dihydrate {K[Cr(C2O4)2.2H2O]
Date of experiment: 100.02.2020
Date of submission: 24.02.2020
Practical Group: P3
Lecturer: Dr. Ooi Zhong Xian
Lab Partner: Chan Yong Li
1.0 Title: Preparation and Studies of Potassium Diaquabis (Oxalato)
Chromate (III) Dihydrate {K[Cr(C2O4)2.2H2O]
2.0 Objective:
 To prepare potassium diaquabis(oxalato)chromate(III)dihydrate
complexes and study its reactions.
 To determine the potassium diaquabis(oxalato)chromate(III)dihydrate
complexes by condutind qualitative analysis.
3.0 Introduction:
In 1780, chromium was discovered by Nicolas Louis Vauquelin and is
classed as a transition metal. Chromium is a hard and lustrous metal that can
take high mirror polish. Chromium also has very high boiling point and widely
used as a catalyst. (Stewart, 2012) Chromium (Cr) is found in group 6 (VIB) of
the Periodic Table along with molybdenum (Mo) and tungsten (W). These
metals, therefore, have 6 valence electrons.
In the chromium atom, the 3d-orbital is half-filled with 5 electrons and 6
th electron is present in 3s orbital. The most common ore of chromium is
chromite [chrome ironstone/iron (II) chromite, FeCr2O4] which can be used
directly for the manufacture of steel and other chromium compounds. An alloy
of chromium and nickel, nichrome is used for electrical heating elements.
Chromium also used in stainless steel and other alloys. For example, chromium
plating on cars and bicycles, gives a smooth, silver finish that is highly resistant
to corrosion. (Stewart, 2012)
Chromium (III), the most stable oxidation state of chromium, forms a
number of complexes, in which six monodentate ligands surround the cation
octahedrally. In the above compound, two oxalate anions (bidentate ligands)
and two water molecules coordinate the chromium cation to provide oxygen
atoms at the corners of the octahedron. Two geometrical isomers exist for the
complex ion, [Cr(C2O4 )2 (H2O)2 ] - , two (C2O4 ) 2- ions [or two H2O molecules]
can be on the same side of octahedron structure of the complex ion giving the
cis isomer or on the opposite sides giving trans isomer.

4.0 Apparatus:
  Pestle
 Mortar
 100ml beaker
 Watch glass
 Hot plate
 Glass rod
 Sintered glass crucible
 Analytical balance
 Filter paper
5.0 Materials:
 0.055mole oxalic acid
 0.0068mole K2Cr2O4
 Absolute ethanol
 Dilute ammonia solution
 Dilute hydrochloric acid
6.0 Procedure:
A. Preparation
Firstly, 0.055mole oxalic acid and 0.0068mole K2Cr2O4 were powdered
separately using a pestle and mortar. The powder was mixed thoroughly and
gently regrind. The mixture transferred into a 100ml beaker and covered with
a watch glass and the beaker was heated on the hot plate. Next, the beaker
was removed from the hot plate and 15ml of absolute ethanol was added
immediately. The mixture was stirred with a glass rod for 5 minutes. 15ml of
fresh absolute ethanol was added. The product was grinded using a beaker and
glass rod until crystalline violet powder was obtained. Then, the crystal was
filtered by vacuum suction using sintered glass crucible. The crystal was
washed with 5ml ethanol two times and I was dried in the air by vacuum
suction. The product was weight on the top loading balance, and transferred
into a properly labelled vial. The test was carried out to determine the product.
B. Qualitative Analysis
1. Test for Potassium
The flame-test for potassium was performed in the fume cupboard using
a platinum wire. The colour of the flame was noted.
2. Test for cis and trans isomers
 A few crystals of the product was placed on a small filter paper rested on
a watch glass. It moistened with a few drops of dilute ammonia solution first
and then with dilute hydrochloric acid. The observation was recorded.
7.0 Result:
A. Preparation
Theoretical mass of 0.0555 mole of oxalic acid
¿ 0.0555 mole ×126.03 g/mol
¿ 7.00 g

Theoretical mass of 0.0068 mole K2Cr2O7

¿ 0.0068 mole × 294.19 g /mol
¿ 2.00 g

Mass of oxalic acid used = 7.0005g

Mass of K2Cr2O7 used = 2.0012g
Mass of empty sintered glass = 85.16g
Mass of sintered glass + product = 89.49g
Mass of product = 4.33g
B. Qualitative Analysis
Tests Observation
Flame test for A flame in violet colour is formed.
potassium
Test for cis and The solid dissolved and dark green solution is formed.
trans isomer

8.0 Discussion:
 In this experiment, potassium diaquabis (oxalato) chromate (III)
dihydrate complex was prepared and qualitative analysis such as test for
potassium and test for cis or trans isomer were carried out. 7.0005g oxalic acid
dihydrate and 2.0012g potassium dichromate were used as reactants to
produce potassium diaquabis (oxalato) chromate (III) dihydrate complex.
Oxalic acid dihydrate is an odourless white crystalline solid which has
molecular weight 126.03g/mol, is classified as simplest dicarboxylic acid and
act as reducing agent. (National Center for Biotechnology Information, 2020)
Potassium dichromate is an oxidising agent which appears in crystalline solid
state with reddish orange colour. The molecular weight of potassium
dichromate is 294.19g/mol. (National Center for Biotechnology Information,
2020) At the end of the reaction between oxalic acid dihydrate and potassium
dichromate, a black crystalline solid of product which is potassium diaquabis
(oxalato) chromate (III) dihydrate complex formed.
To prepare the potassium diaquabis (oxalato) chromate (III) dihydrate
complex, the oxalic acid dihydrate and potassium dichromate were mixed and
heated. A semi-solid compound that appeared in black colour formed proved
that the reactants undergo the reaction with each other. Next, the semi-solid
compound was grinded until crystalline solid in dark purple colour under light
was obtained. After the product was filtered by vacuum suction and the final
product was potassium diaquabis (oxalato) chromate (III) dihydrate, a solid in
black colour. In this reaction, there were oxidation and reduction occurred. For
oxidation:
3H2C2O4 (aq)  6CO2 (aq) + 6H+ (aq) + 6ē
The equation that represent reduction was
Cr2O72- (aq) + 14H+ (aq) + 6ē  2Cr3+ (aq) + 7H2O (l)
From the equation above, it shown that the oxidation state Of Cr changes from
+6 to +3 and the oxalic acid is oxidised. Hence, the overall equation for
reaction is
Cr2O72- (aq) + 8H+ (aq) + 3H2C2O4 (aq)  2Cr3+ (aq) + 7H2O (l) + 6CO2 (g)
(Chegg Study, n.d)
 In the process of vacuum filtration to collect the product, absolute
ethanol was used to rinse the crystal solid. Absolute ethanol refers to pure
ethanol with no water content. (Barnes, n.d) Compare to distilled water,
absolute ethanol is more volatile and the product was less soluble in absolute
ethanol. The crystal solid able to dry faster by vacuum suction and easier to
obtained by using absolute ethanol. Hence, absolute ethanol was used to rinse
the crystal solid.
After preparing the potassium diaquabis (oxalato) chromate (III)
dihydrate complex, qualitative analysis was carried out to test for potassium
and for cis and trans isomers. Flame test was conducted to test the presence of
potassium by using platinum wire. The purpose of conducting flame test was to
identify the presence of relatively small number of metal ions in a compound.
(Clark, 2018) From the observation, the product gave a violet or lilac flame
when it placed on Bunsen burner. This indicates that the potassium ions were
present in the compound. Next, dilute ammonia solution and dilute
hydrochloric acid were used to test for is cis or trans isomers. Cis form shows
that a deep green solution formed spread over and no solid remains. With the
trans form, there is no green colour but a light brown solid formed and
remains undissolved. After few drops of dilute ammonia solution and
hydrochloric acid were added, the crystal solid product was dissolved and a
dark green solution was formed spread over the filter paper. This indicates that
the product was in cis form. The ammonia acts as both a base and a ligand.
When dilute ammonia is added to the solid complex, one molecule of the
ligand H2O is replaced by OH- ion. The equation of both isomers are shown
below:
K[Cr(C204)2 (H20)2].2H20 + NH3  K[ Cr(C204)2 (H20)(OH)].2H2O + NH4+
K[Cr(C204)2 (H20)(OH)].2H20 + HCl  K[Cr(C204)2 (H20)2].2H20 + Cl-
 After collecting and weighing the product, the percentage yield can be
calculated.
K2[Cr2O7] + 7H2C2O4.2H2O 2K[Cr(H2O)2(C2O4)2].2H2O + 6CO2 + 13H2O
From the equation: 1 mole of K2Cr2O7 produce 2 moles of
K[Cr(H2O)2(C2O4)2].2H2O
Mass( g)
Number of moles of K2[Cr2O7] = Molar Mass g
( mol )
2.0012 g
= 294.19 g
( )
mol

= 6.802 ×10-3 mol

Number of moles of K[Cr(H2O)2(C2O4)2].2H2O = 6.802 ×10-3 mol × 2
= 0.01360 mol
Theoretical mass of K[Cr(H2O)2(C2O4)2].2H2O = no. of moles× molar mass
= 0.01360 × 339.1935
= 4.613 g
Actual mass of K[Cr(H2O)2(C2O4)2].2H2O = 4.15 g
Actual mass
Percentage yield (%) = Theoretical mass ×100%

4.33 g
= 4.613 g ×100 %

= 93.87 %
Besides, there were some precaution steps are taken in this experiment.
Firstly, the crystalline solid product was spread in order to add in absolute
ethanol before the crystalline violet powder was being filtered by vacuum
suction. This is to ensure that the product can dry up faster and the unreacted
impurities are able to wash away. Next, the crystalline solid product was rinsed
with absolute ethanol few times when was being filtered by vacuum suction.
This is to ensure that all product were completely filtered and did not left any
product in beaker in order to prevent any inaccuracy in percentage yield.
Lastly, gloves and safety googles were worn throughout the experiment to
prevent any injuries and to avoid any direct contact with chemicals.
9.0 Conclusion:
In conclusion, potassium diaquabis(oxalato) chromate (III) dehydrate
complexes was prepare in this experiment. This product was prepared form
potassium dichromate and oxalic acid dihydrate. The percentage yield of the
product is 93.87%. Violet or lilac flame can be seen when the product was
tested for flame test showing the presence of potassium ion. Besides, a dark
green solution was formed and no solid remains showing the product with cis
isomers.
10.0 References:
Barnes, K., n.d. What is Absolute Alcohol? Preparation & Uses. [online]
Available at :< https://study.com/academy/lesson/what-is-absolute-alcohol-
preparation-uses.html> [Accessed at 16 February 2020]
Chegg Study, n.d. General Chemistry. [online] Available at :<
https://www.chegg.com/homework-help/acidic-solution-dichromate-ion-
oxidizes-oxalic-acid-h2c204-a-chapter-20-problem-4pea-solution-
9780135042922-exc> [Accessed at 16 February 2020]
Clark, J., 2018. Flame Tests. [online] Available at :<
https://www.chemguide.co.uk/inorganic/group1/flametests.html> [Accessed
at 16 February 2020]
National Center for Biotechnology Information, 2020. Oxalic acid. [online]
Available at :<https://pubchem.ncbi.nlm.nih.gov/compound/Oxalic-acid>
[Accessed at 15 February 2020]
National Center for Biotechnology Information, 2020. Potassium dichromate.
[online] Available at
:<https://pubchem.ncbi.nlm.nih.gov/compound/Potassium-dichromate>
[Accessed at 15 February 2020]
Stewart, D., 2012. Chromium Element Facts. [online] Available at :<
https://www.chemicool.com/elements/chromium.html> [Accessed at 12
February 2020]