Experiment 7 Title : Investigation of preparation of some transition metal compounds Introduction : A transition metal is one which forms one

or more stable ions which have incompletely filled d orbitals. Based on the basis of the definition outlined above, scandium and zinc do not count as transition metals, even though they are members of the d block. Scandium has the electronic structure [Ar]3d14s2. When it forms ions, it always loses the 3 outer electrons and ends up with an argon structure. The Sc3+ ion has no d electrons and so does not meet the definition. Zinc has the electronic structure [Ar] 3d104s2. When it forms ions, it always loses the two 4s electrons to give a 2+ ion with the electronic structure [Ar] 3d10. The zinc ion has full d levels and does not meet the definition either. Transition elements are very hard, with high melting points and boiling points. Moving from left to right across the periodic table, the five d orbitals become more filled. The electrons are loosely bound, which contributes to the high electrical conductivity and malleability of the transition elements. The transition elements have low ionization energies. They exhibit a wide range of oxidation states or positively charged forms. The positive oxidation states allow transition elements to form many different ionic and partially ionic compounds. The formation of complexes causes the d orbitals to split into two energy sublevels, which enables many of the complexes to absorb specific frequencies of light. Thus, the complexes form characteristic colored solutions and compounds. Complexation reactions sometimes enhance the relatively low solubility of some compounds. Objective : To investigate the preparation of some transition metal compounds . Apparatus : test tubes, droppers, measuring cylinder, bunsen burner and test tube holder.

Materials : 0.1 mol L-1 CrCl3, 2 mol L-1 NaOH, 0.1 mol L-1 K2CrO4, 2 mol L-1 H2SO4, 0.1 mol L-1 MnSO4, 0.01 mol L-1 KMnO4, 6 mol L-1 NaOH , FeSO4 crystal, distilled water, glucose grain, 0.1 mol L-1 FeCl3, 0.1 mol L-1 NaSCN, 0.1 mol L-1 CuSO4, 5% glucose solution, 2 mol L-1 NH3, concentrated HCl and 0.1 mol L-1 Zn(NO3)2 Procedures : A. Chromium 1. About 3ml of 0.1 mol L-1 CrCl3 solution is placed into a test tube and its color is recorded. 2 mol L-1 NaOH is added to this solution dropwise. A precipitate of Cr(OH)3 is firstly produced and then the complex Cr(OH)4- ion. 2. About 3ml of 0.1 mol L-1 K2CrO4 solution is placed in a test tube and the color is noted. 2 mol L-1 H2SO4 is added dropwise to the solution until a colour change which indicates the formation of Cr2O72-. B. Manganese 1. 3ml of 0.1 mol L-1 MnSO4 is placed into a test tube and its color is recorded 2. The color of the 0.01 mol L-1 KMnO4 solution is noted. 3. About 3ml of 6 mol L-1 NaOH is placed into a test tube and 3 drops of 0.01 mol L-1 KMnO4 is added. A few grains of glucose is added. The green ion which formed is the MnO42- ion. 4. A rice grain size quantity of Fe2SO4 crystals is placed into a test tube and dissolved in 3ml of distilled water. About 1ml of 0.01 mol L-1 KMnO4 is added dropwise to the solution, allowed to stand for a few minutes and its color is noted. The compound formed is manganese (IV) oxide (MnO2).

C) Iron 1. A rice grain size quantity of FeSO4 crystals is dissolved in abput 3ml of distilled water and the color is noted. About 1ml of 2 mol L-1 NaOH is added and the observations are noted. 2. 3ml of 0.1 mol L-1 FeCl3 is placed in a test tube and the color is noted. About 1ml of 2 mol L-1 NaOH is added and the observations are noted. 3. A rice grain size quantity of FeSO4 crystals is dissolved in about 1ml of distilled water and the color is noted. 0.1 mol L-1 NaSCN is added to this solution until about 1ml is added. The observations are recorded. 4. 1ml of 0.1 mol L-1 FeCl3 is placed in a test tube and its color is noted. 2 or 3 drops of 0.1 mol L-1 NaSCN is added to this solution. The observations are recorded. D) Copper 1. 3ml of 0.1 mol L-1 CuSO4 solution is placed into a test tube and its color is noted. 1ml of 2 mol L-1 NaOH and 2ml of 5% glucose solution is added into the solution and the solution is heated. The precipitate which formed is copper (I) oxide (Cu2O). 2. 3ml of 0.1 mol L-1 CuSO4 is placed into a second test tube and 1ml of 2 mol L-1 NaOH is added. The contents of the test tube is carefully heated until a pronounced color change occurred. The black precipitate is copper (II) oxide ( CuO). 3. 1ml of 0.1 mol L-1 CuSO4 solution is added to another test tube and 2 mol L-1 NH3 solution is added dropwise until the Cu(OH)2 precipitate is formed which initially dissolved to formed the Cu(NH3)42+ ion. 4. A further 1ml of 0.1 mol L-1 CuSO4 is placed into another test tube and the color is noted. Concentrated HCl is added dropwise until there is a pronounced color change

due to the formation of the CuCl42- ion. E) Zinc 1. 1ml of 0.1 mol L-1 Zn(NO3)2 solution is placed into a test tube and the color is noted. 2 mol L-1 NaOH is added dropwise until the precipitate of Zn(OH)2 which formed initially has dissolved to form the Zn(OH)42- ion. 2. The procedure above is repeated by using 2 mol L-1 NH3 solution instead of the NaOH. Results : A) Chromium Type of solution 0.1 mol L-1 CrCl3 + 2 mol L-1 NaOH Observations The CrCl3 solution is light blue. When NaOH is added , a little blue-ish white precipitate is formed. The K2CrO4 solution is yellow. When H2SO4 is added, an orange solution formed.

0.1 mol L-1 K2CrO4 + 2 mol L-1 H2SO4

B) Manganese Type of solution 0.1 mol L-1 MnSO4 0.01 mol L-1 KMnO4 The solution is purple. Observations

6 mol L-1 NaOH + 0.01 mol L-1 KMnO4 + The solution do not mix but after glucose is glucose added, the solution turns green. FeSO4 + distilled water + 0.01 mol L-1 KMnO4 Precipitate is formed , solution turned brown after the addition of distilled water.

C) Iron Type of solution FeSO4 + distilled water + 2 mol L-1 NaOH Observations The solution is brown when distilled water is added. The solution changes to green precipitate when NaOH is added into it. The solution is light in yellow. A brown precipitate formed when NaOH is added. A light brown precipitate is formed when distilled water is added. It turned to be a darker brown precipitate when NaSCN is added. The solution is light in yellow. A blood red solution formed when NaSCN is added to it.

0.1 mol L-1 FeCl3 + 2 mol L-1 NaOH FeSO4 + distilled water + 0.1 mol L-1 NaSCN

0.1 mol L-1 FeCl3 + 0.1 mol L-1 NaSCN

D) Copper Type of solution Observations

0.1 mol L-1 CuSO4 + 5% glucose solution + The CuSO4 solution is light blue. When 5% heat glucose solution is added, a dark blue precipitate formed. When it is heated, a dark green precipitate formed. 0.1 mol L-1 CuSO4 + 2 mol L-1 NaOH + heat The CuSO4 solution is light blue. A dark blue solution is formed when NaOH is added. A black precipitate is formed when it is heated. The CuSO4 solution is light blue. When NH3 is added , a dark blue solution is formed and then later it becomes deep purple. The CuSO4 solution is light blue. When HCl is added, a green solution is formed.

0.1 mol L-1 CuSO4 + 2 mol L-1 NH3

0.1 mol L-1 CuSO4 + HCl

E ) Zinc Type of solution 0.1 mol L-1 Zn(NO3)2 + 2 mol L-1 NaOH Observations The solution is colorless. A white precipitate formed when NaOH added into it. It becomes milky. The solution becomes cloudy and colorless.

0.1 mol L-1 Zn(NO3)2 + 2 mol L-1 NH3

Discussion : 1. For chromium , when CrCl3 reacts with NaOH, a blue-ish white precipitate is formed because hydroxide ions from sodium hydroxide solution will remove hydrogen ions from the water ligands attached to the chromium ion. Once a hydrogen ion has been removed from three of the water molecules, you are left with a complex with no charge - a neutral complex. This is insoluble in water and a precipitate is formed. When K2CrO4 reacts with H2SO4, an orange solution is formed due to the equilibrium shift. The equation is shown below :

Cr2O72- + OH-

2CrO42- + H+

2. For manganese , when NaOH reacts with KMnO4 and glucose, the solution turns green. This is because managante (vii) ions is reduced to manganate (vi) ions. It breaks down the c=c double bond of glucose. When FeSO4 reacts with distilled water and KMnO4. The solution turned to be brown because the manganate MnO4- is reduced to MnO2.

3.