Surname and initials: Vezi A
Student number: 22029908
Name of Lecture: Dr TH Mokhothu
Date of experiment: 18/05/2021
Group: B
Experiment 4
COMPLEXATION FORMATION.
Aim:
To prepare complexes of chromium (III) and iron (III).
Theory:
Synthesis is a type of chemical reaction in which two or more simple substances combine to
form a more complex product. In this experiment we synthesize the complexes of chromium
(IIII) and iron (III), A coordination compound has at least one complex ion as said by Professor
Toto. A complex ion consists of two parts, a metal ion (usually a transitional metal) and a fixed
number of ligands, such as EDTA. In this experiment oxalate is used as a ligand. In the first
complex, we prepare a chromium oxalate complex this reaction included the formation of
geometrical isomers cis-K[Cr(2H2O)(C2O4)2(H2O)2] and trans –K[Cr(C2O4)2(H2O)2].3H2O.
Chromium (III) is the most stable oxidation state of Chromium it has a green color in
appearance, and it forms paramagnetic species since it has unpaired electrons in the d orbital.
Chromium is an abundant element in the earth’s crust. Chromium is mostly used for plating and
in chrome steels. For the other experiment Ferric chloride is used to produce the oxalate
complex of iron (III). This solution appears as a light brown aqueous solution.
Experimental:
Apparatus: Five test tubes and a hot water bath.
Reagents: 0.1M of Chromium (III) Chloride, Iron (III) chloride, iron (II) sulphate, Solid sodium
oxalate, 2M NaOH, 0.1M NH4SCN, solid sodium fluoride, 0.1M KI, chloroform, iodine solution
(iodine dissolved in potassium iodine solution).
Procedure:
4.1. A 3 ml of chromium (III) chloride solution was placed in a test tube and then a small portion
of solid sodium oxalate was added to the solution with continuous shaking until the oxalate
particles are dissolved. A few drops of NaOH were added to the solution to form a chromium
(III) hydroxide precipitate.
4.2 3 ml of iron (III) chloride solution was placed in a test tube. Two drops of ammonium
thiocyanate was added to the iron (III) chloride solution the color change was observed and
recorded. Then a portion of solid sodium oxalate was added to the solution, the color change
was observed.
4.3. 3 ml of iron (III) chloride solution was placed in a test tube and then a small fraction of solid
sodium fluoride was added to the solution, then color changes were observed. The solution was
then divided into two equal portions. On one portion a little amount of ammonium thiocyanate
solution was added, which confirmed the presence of Fe3+ ions if a deep red color appeared. To
the other portion a bench sodium hydroxide solution was added.
4.4 3 ml of iron (III) chloride solution was placed in a test tube and a little portion of potassium
iodide solution was added. If there’s no iodine liberated a little solution of carbon tetrachloride
was added along with continuous shaking, then the color changes of the top layer of
tetrachloromethane or carbon tetrachloride layer were observed. The experiment was then
repeated but before the addition of potassium iodide solution a small portion of sodium
fluoride was added to the iron (III) chloride solution. 3 ml of a dilute solution of iron (II)
sulphate was placed in another test tube and then a little solution of iodine solution was added
then the mixture was warmed, but not heated strongly until the iodine vapourises. The
experiment was then repeated but before the addition of iodine, a small portion of solid
sodium fluoride is added then the solution is warmed gently.
Results:
Reactions Compound formed Color formed
Oxalate complex of chromium (III) K3[Cr(C2O4)3] Cloudy green
Oxalate complex of iron (III) (with NH4SCN) [Fe(SCN)]2+ Red
Oxalate complex of iron (III) (with Oxalate) [Fe(C2O4)33- Yellow
Fluoride complex of iron (III) (with NaF) [FeF6]3- Yellow
Fluoride complex of iron (III) (with NaOH) Fe(OH)3 Cloudy orange
Iodide complex of iron (III) I2 Brick yellow
Iodide complex of iron (III) (with NaF) [FeF6]3- Light green
Answers to questions:
4.1 The complex is very stable since the metal io which is Cr (III) is the most stable oxidation
state of chromium and therefore forms stable complexes.
K2Cr2O7 +7H2C2O4 + 2K2C2O4 → 2K3[Cr(C2O4)3].3H2O + 6CO2 + H2O
4.2 (a) After the addition of ammonium thiocyanate a red precipitate of [Fe(SCN)]2+ was
formed.
(b) After the addition of sodium oxalate a yellow precipitate of [Fe(C2O4)3]3- was formed.
(c) The addition of more of ammonium thiocyanate will produce a red color because excess
Fe3+will react with SCN- to from a red precipitate.
Fe3+ + SCN- → [Fe(SCN)]2+
Fe3+ + 3C2O42- → [Fe(C2O4)3]3-
4.3 (a) After the addition of sodium fluoride a yellow precipitate of FeF63- is formed.
Fe3+ + 6F- → [FeF6]3-
(b) There were no Fe3+ ions present since the solution formed a cloudy solution after adding
ammonium thiocyanate.
(c) After adding the NaOH the solution turned cloudy orange indicating that there was no
formation of Fe(OH)3.
4.4 (a)There was iodine liberated since the precipitate was yellow.
(b) After the addition of NaF the solution turned light green.
Discussion:
From the results obtained above I can conclude that chromium (III) is able to form very stable
complexes because it has 3 unpaired electrons in the d orbital which are available to form a
coordination compound. For the oxalate complex of iron (III), the iron (III) reacted very
impressively with the thiocyanate because after the formation of the oxalate complex there
was excess amounts of the Fe3+ ions enough to form another reddish thiocyanate complex. For
the reactions the fluoride complex of iron (III), the formation of the fluoride complex was
perfect but when testing for presence of Fe3+ ions we obtained a negative test, maybe there
were some errors during the separation of the resulting solution or there was too much of
sodium fluoride which ended up reacting with all of the Fe3+ ions present.
Conclusion:
Chromium (III) is an excellent metal ion which forms stable complexes due to its stable
oxidation state. Iron (III) can form useful precipitates.
References:
• Thanh Tran and Professor Toto.2019.Synthesis and Analysis of iron (III) oxalate complex.
https://www.coursehero.com/file/57882967/LAB-REORT-6-SYNTHESIS-AND-ANALYSIS -OF-IRON-
III-OXALATE-COMPLEXdocx/.
• Prof. Robert J. Lancashire. The Department of Chemistry, University of the West Indies.
Synthesis of potassium tris(oxalato) chromium.
http://wwwchem.uwimona.edu.jm/lab_manuals/c10expt15.html.
REACTIONS OF ZINC.
Aim:
To determine the ways zinc reacts under different reagents.
Theory:
Zinc is a very useful metal around the world. Its ore is found in the earth’s crust as ZnS which is
oxidized to form ZnO during the extraction. Zinc is found in the transition metals group in the
periodic table, although Zinc is not a true transition metal since it does not have a partially filled
d orbital it is placed with the transition metals due to having similar properties as that of
transition metals.
Experimental:
Apparatus: Six test tubes and a Dropper
Reagents: zinc sulphate, NaOH, HCl, H2S, ZnO.
Procedure: 4.4.2 A 2 ml solution of NaOH was added to 1 ml of Zinc (II) solution.
4.4.3 A 1 ml solution of zinc was treated with aqueous ammonia solution.
4.4.4 A 2 ml solution of NaOH was added to 1 ml of zinc then a dilute HCl was added to the
mixture.
4.4.5 A 2 ml solution of NaOH was added to 1 ml zinc solution followed by an excess solution of
NaOH.
4.4.6 A solution of H2S was added to 1 ml solution of zinc and then dilute HCl was added.
4.4.7 A 2 ml solution of NaOH was added to 1 ml of zinc solution followed by an excess solution
of NaOH then H2S was added.
4.4.8 ZnO was treated with dilute HCl.
4.4.9 ZnO was treated with NaOH.
Results:
Reactions Color formed
4.4.2 Colorless
4.4.3 Colorless
4.4.4 Colorless
4.4.5 Cloudy
4.4.6 Cloudy
4.4.7 Cloudy
4.4.8 Colorless
4.4.9 Cloudy
Answers:
4.4.1 ZnSO4
4.4.2 The solution was colorless, hence there was no reaction.
4.4.3 The solution was colorless, hence there was no reaction.
4.4.4 The solution was colorless, hence there was no reaction.
4.4.5 The resulting solution was cloudy.
Zn + 2NaOH → Na2ZnO2 + H2
4.4.6 The resulting solution was cloudy.
ZnS +2HCl → ZnCl2 + H2S
4.4.7 The resulting solution was cloudy. H2S acts as a precursor to elemental sulfur.
4.4.8 The solution was colorless, hence there was no reaction.
4.4.9 The solution was cloudy due to the formation of Na2ZnO2
