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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.
Preparation
(1)
A pestle and mortar were used to powder 0.0555 mole oxalic acid dihydrate and
separately 0.0068 mole K2Cr2O7. The powders were mixed thoroughly, regrinding
them gently.
(2)
The mixture was transferred into a 100 ml beaker. The beaker was covered with a
small watch glass and heated gently the beaker on the hot-plate. A vigorous reaction
commenced with the evolution of steam and carbon dioxide and with the formation
of a dark semi-solid compound.
(3)
The beaker was removed from the hot-plate and immediately added 15 ml absolute
ethanol. The mixture was stirred with a glass rod and the mixture was transferred into
a small mortar (or stir with a beaker and glass rod). Stirring was continued for further
5 minutes breaking up the product and decant the ethanol. A fresh 15 ml absolute
ethanol was added. The product was grinded using a beaker and glass rod until a
crystalline violet powder is obtained.
(4)
The crystals were filtered by vacuum suction using a sintered glass crucible. The
crystals were washed two times with 5 ml ethanol and dried in the air by vacuum
suction. The product was weighed on a top loading balance and transferred into a
properly labelled vial.
(5)
The following tests were carried out on the product. Qualitative Analysis
(i)
The flame-test for potassium was performed in a fume cupboard using a platinum
wire. The colour of the flame was noted.
(ii)
The following test was carried out to determine the nature of the isomer prepared in
this experiment:
A few crystals of the product was moisten and placed on a small filter paper resting
on a watch glass, first with a few drops of dilute ammonia solution and then with
dilute hydrochloric acid. Observations were recorded. With the cis- form, a deepgreen solution rapidly forms and spreads over the filter paper, no solid remains. With
the trans- form there is no green colour, but light-brown solid forms and remains
undissolved. In each case, reaction with dilute HCl restores the original colour of the
isomeric form.
Results:
Mass of oxalic acid dehydrate
6.9879g
Mass of K2Cr2O7
2.0058g
19.8201g
23.9701g
Mass of product
23.9701g-19.8201g
= 4.15g
Observations:
i)
ii)
Discussion:
further. Furthermore, by drying the product in the air by vacuum suction as in the experiment,
the product formed was far easier to dry with absolute ethanol in it than with water as ethanol
is volatile. That is why absolute ethanol was used to wash the product for few times.
After had collected the product, following test were carried out on the product. Flame
test was used to test for the presence of potassium using a platinum wire. Colour of the
product formed was determined under the flame of Bunsen burner. A flame test is to detect
the presence of certain element, basically metal ions which based on each elements
characteristic emission spectrum. From the difference in colour for each of the element, we
can differentiate between one element to another element. In this experiment, the colour of
flame changes from orange to pinkish purple. This observation that obtained had indicates
that potassium ion was present in this compound. Next, test for cis and trans isomer by
adding ammonia solution and dilute hydrochloric acid. Both isomers are in equilibrium when
solid complex is dissolved in water. Cis form is more soluble and exists in high proportion
solution but it is slowly converted into trans from when the solution is evaporated slowly. In
solid state only one isomer can exits depending on the method of preparation of the complex.
Firstly, few drops of dilute ammonia solution and then dilute hydrochloric acid were added.
Based on observations obtained, a deep green solution was rapidly formed and spread over
the filter paper but there were no solid remains. This had showed for the cis-form on the
product. Furthermore, as the solution evaporated slowly, light brown solid was formed and
remains undissolved and there is no longer green colour solution.
In this experiment, percentage yield was calculated. By taking the theoretical mass
and actual mass of the product, percentage yield can be obtained. Thus, the formula is
Actual mass
Theoretical mass
There were some precautionary steps taken in this experiment. Firstly, before started
the experiment, all the apparatus must washed with acetone then put into the oven to remove
acetone. We have to use acetone instead of using water because the product formed later will
dissolved in water and this will affect the percentage yield of the product. Besides, before the
crystalline violet powder was being filtered by vacuum suction, the powder must be spread in
order to add in absolute ethanol. This is to ensure that the product can dry up faster and the
unreacted impurities are able to wash away. Moreover, absolute ethanol was chosen to be
used in this experiment because it has a high proportion of ethanol than water and thus,
product formed would not easily dissolved. Furthermore, gloves and safety googles must be
worn throughout the experiment to prevent any injuries and to avoid any direct contact with
chemicals.
Questions and Answers:
(1)
What is the oxidation state of chromium in K2Cr2O7 and in the product? Write two
half-equations for each reaction involved in the preparation of the complex using
oxalic acid dihydrate (H2C2O4.2H2O) and potassium dichromate (K2Cr2O7) and a
balanced equation for the overall reaction.
Oxidation state of chromium in K2Cr2O7 : +1(2) + 2x -2(7) =0
2x =12
X= +6
Oxidation state of chromium in product: x + 0(2) + 0(2) = -1
x= -1
Two half equations:
Oxalic acid dehydrate: H2C2O4 2CO2 + 2H+ + 2e- ( Oxidation reaction)
Potassium dichromate: Cr2O72(aq) + 14H+ + 6e 2Cr3+(aq) + 7H2O
(Reduction reaction)
Balanced
equation
for
overall
equation:
K2[Cr207]
7H2C204*2H20
(2)
Molar Mass
( molg )
2.0058 g
g
294.185
mol
( )
Actual mass
Theoretical mass
4.15 g
100
4.63 g
= 89.63 %
100%
(3)
Write the chemical equations for the reactions involved in the tests for the detection of
chromium (III) and oxalate ions. Indicate in each case whether it is an acid-base or
oxidation-reduction reaction.
The test for chromium (III) is an acid- base reaction. Product was dissolved in water
and form hexaaquachromium(III) ions [Cr(H2O)6]3+. When a base was added into
the solution, neutral complex and precipitate were formed. For example, reactions
with ammonia solution. The ammonia acts as base and a ligand. By adding small
amount of ammonia solution, hydroxide ions (OH-) are pulled off the hexaaqua ionto
give the neutral complex.
Equation: [Cr(H2O)6]3+ + 3NH3 [Cr(H2O)3(OH)3] + 3NH4+
By adding excess ammonia solution, ammonia will replace water as a ligand to give
hexaamminechromium(III) ions.
Equation: [Cr(H2O)6]3+ +6NH3 [Cr(NH3)6]3+ +6H2O
Next, the test for oxalate ion is oxidation-reduction reaction.
Purple colour of
potassium permanganate will decolourise immediately if react with acid like dilute
sulphuric acid while purple colour of potassium permanganate decolourise slowly
without dilute H2SO4. In this case, acid acts as a catalyst in this redox reaction. The
oxalate ion is oxidised by the permanganate ion in the acid solution. Potassium
permanganate (KMnO4) is acts as oxidising agent. In this oxidation-reduction
reaction, the C2O42- is oxidised to CO2.
Equation: C2O42- 2CO2 + 2eThe permanganate ion (MnO4-) will be reduced to Mn2+.
Equation: MnO4- + 5e- Mn2+
(4)
Draw the structures of the two possible geometrical isomers of the complex. What is
your conclusion regarding the nature of the isomer in the test (iv)? When dilute
ammonia is added to the solid complex, one molecule of the ligand H 2O is replaced
by OH- ion. Write equations for both the isomers to represent this reaction as well as
for the reaction of the hydroxo product and HCl to restore the original complex