Complex Chemistry of Nickel
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1 AC practicum complex chemistry of nickel Complex Chemistry of Nickel Synthesis of Different Nickel(II)-Complexes with Ligand Change Reactions Marcel Ottiger, D-CHAB, 1. Semester, Assistents: Tew, Rahul Fortedar Abstract: The goal to synthesise different nickel(ii)-complexes with ligand change reactions was reached. The colour changed into that one which was said out of the theory. The spectrochemic serie of ligands was experienced and approved. The proposed recycling method to regain nickel in the form of NiCl 2 didn't work. Zurich, Marcel Ottiger
2 Introduction [1][2] : Nickel appears in the coordination numbers 4, 5 and 6. In that range, almost every steric constitution of the ligands is possible: octaedric, trigonal-bipyramidal, quadraticpyramidal, tetraedric and quadratic. This steric constitution can be explained with the ligand field theory (LFT). This theory says that the ligands should treated like point charges which influence the five steric arranged d-orbitals. Every steric constitution has its specific split up of the five degenerated orbitals, e.g. tetraedric constitution: d x2-y2, d z2 are energeticly lower better arranged than d xy, d yz, d xz orbitals. This developed difference in energy Δ is called field force parameter. This makes a change of the electron from the lower energiced orbital to a higher possible. The absorbed energy of the field force parameter is equal to the absorbed wavelength of light, so the complex appears in the complementary colour. But this split up of the d-orbitals also depends of the ligand which is bonded. Consequential there is a list with increasing Δ-values called spectrochemical serie: I - < Br - < S 2- < Cl - < SCN - < F - < OH - < H 2 O < NH 3 < en < NO 2 - < CN - < CO Which means that a central atom prefers OH - as ligand instead of Br - but it would prefere more a CN - molecule as ligand. If the Δ-value is too small, the split up in different energy levels is not high enough and the orbitals are treated like degenerated orbitals. Experimental: Informations about the used chemicals can be found in appendix A1. Experimental set-up: Procedure: NiCl 2 *6H 2 O was solved in water: NiCl 2 6H 2 O [ Ni OH 2 6 ] 2+ 2Cl - bright green solution Into the solution was added concentradet ammonia. A fallout was observed. By adding more ammonia a clear, blue solution was generated: [ Ni OH 2 6 ] 2+ 2NH 3 Ni OH 2 2NH + 4 4H 2 O fallout Ni OH 2 4NH 3 2NH + 4 [ Ni NH 3 6 ] 2 + 6H 2 O clear blue solution
3 This solution was boiled and K 2 C 2 O 4 *H 2 O was added and put for 2 hours into a ice-water-bath: [ Ni NH 3 6 ] 2+ 2C 2 O 4 2- [ Ni C 2 O 4 2 ] 2-6NH 3 turquoise coloured After the solution was on room temperature a solution of glycine and some drops of ammonia was added: [ Ni C 2 O 4 2 ] 2-2Gly - [ Ni Gly 2 ] 2C 2 O 4 2- bright blue/turquoise solution Acetylaceton was added and the solution was stired for 10 minutes: [ Ni Gly 2 ] 2Hacac - [ Ni Hacac 2 ] 2Gly - bright blue fallout A solution of diacetyldioxim (DMG) in diluted sodium hydroxide was added: [ Ni Hacac 2 ] 2Hdmg - [ Ni Hdmg 2 ] 2Hacac - dark-red fallout The ph was raised up to 12 with concentrated NaOH and a solution of Na 2 EDTA was added. This solution was boiled until a clear blue solution occured: [ Ni Hdmg 2 ] edta 4- [ Ni edta ] 2-2Hdmg - clear solution Results: Up to the second last complex ( [ Ni Hdmg 2 ] ) everything worked fine. But the very last complex was not clear blue it was more greenish after 4 houres of boiling. But the recycling to regain NiCl 2 was started anyway. For the recycling of the nickel the solution was brought to ph 1 with sulfuric acid until a green colour appears and something falls out. The solution was filtered and 5g active carbon was added and boiled and then the hot solution was filtered. The cooled down solution was added again active carbon and also H 2 O 2 and was stired for about 1 hour, then boiled and filtrated. The solution was brought to a ph of 12 with concentrated NaOH but instead of a bright green solution as the manual says the solution was dark-green and the more base was added the solution slowly turned to pink. And there was a pink dust over the beaker. The recycling was cancelled by the assistant and the solution was disposed in the basic metal solution box. Structure of the nickel-complexes: Hexaaquonickel(II) [Ni(OH 2 ) 6 ] octaedric
4 Hexaamminnickel [Ni(NH 3 ) 6 ] 2+ octaedric Oxalatonickel-complex [Ni(C 2 O 4 ) 2 ] 2- quadratic planar Nickelglycinat [Ni(Gly) 2 ] quadratic planar Nickelacetylacetonat [Ni(Hacac) 2 ] tetraedric Bis(dimethylglyoximato)nickel(II)-complex [Ni(Hdmg) 2 ] quadratic planar
5 NiEDTA-complex [Ni(edta)] 2- octaedric Why are quadratic planar nickel complexes diamagnetical? The solution is already given by the introduction. The split up of the d-orbitals in a quadratic planar field is not that easy as it is in a octaedric or in a tetraedric field. In a tetraedric or in a octaedric field are unpaired electrons. That means that they are paramagnetical. In a quadratic planar nickel complex the orbitals are all with paired electrons so these complexes are diamagnetical. Discussion: The synthesis of this nickel-complexes does work with the used manual [1]. But the recycling method had a failure-quote of 100% when 10 different people made this experiment. Sometimes the problems began with the dark-red fallout, sometimes the solution was green and not blue. And even if everything went alright, when the ph has to be brought to 11 with concentrated NaOH the problem with the pink solution and the pink dust appeared. The behaviour of the complex with different ligands of the spectrochemical serie was proofed. The weaker ligand was displaced by the stronger one.
6 Literature: [1] H.Schönberg. Praktikum in allgemeiner Chemie, Laboratorium für anorganische Chemie ETH Zürich. Zürich [2] Charles E. Mortimer, Ulrich Müller. Chemie. 9.Auflage. Georg Thieme Verlag. Stuttgart Appendix A1: chemicals Sodium Hydroxide NaOH corrosive C R35: Causes severe burns (S1/2): Keep locked up and out of the reach of children S26: In case of contact with eyes, rinse immediately with plenty of water and seek medical advice S37/39: Wear suitable gloves and eye/face protection S45: In case of accident or if you feel unwell seek medical advice immediately (show the label where possible) Ammonia NH 3 toxic T damaging environement N R10: Flammable R23: Toxic by inhalation R34: Causes burns R50: Very toxic to aquatic organisms (S1/2): Keep locked up and out of the reach of children S9: Keep container in a well-ventilated place S16: Keep away from sources of ignition - No smoking S26: In case of contact with eyes, rinse immediately with plenty of water and seek medical advice S36/37/39: Wear suitable protective clothing, gloves and eye/face protection S45: In case of accident or if you feel unwell seek medical advice immediately (show the label where possible) S61: Avoid release to the environment. Refer to special instructions/safety data sheet Sulfuric Acid H 2 SO 4 corrosive C R35: Causes severe burns (S1/2): Keep locked up and out of the reach of children S26: In case of contact with eyes, rinse immediately with plenty of water and seek medical advice S30: Never add water to this product S45: In case of accident or if you feel unwell seek medical advice immediately (show the label where possible
7 Nickel(II)-chlorid-hexahydrat NiCl 2 *6H 2 O toxic T damaging environement N R25: Toxic if swallowed R43: May cause sensitisation by skin contact R50/53: Very toxic to aquatic organisms, may cause long-term adverse effects in the aquatic environment S24: Avoid contact with skin S37: Wear suitable gloves S45: In case of accident or if you feel unwell seek medical advice immediately (show the label where possible) S61: Avoid release to the environment. Refer to special instructions/safety data sheet Kaliumoxalat K 2 C 2 O 4 damaging health Xn R20/21/22: Harmful by inhalation, in contact with skin and if swallowed (S2): Keep out of the reach of children S24/25: Avoid contact with skin and eyes Glycine NH 2 -CH 2 -COOH nothing special Acetylaceton CH 3 -CO-CH 2 -CO-CH 3 damaging health Xn R10: Flammable R22: Harmful if swallowed (S2): Keep out of the reach of children S21: When using do not smoke S22: Do not breathe dust S23: Do not breathe gas/fumes/vapour/spray (appropriate wording to be specified by the manufacturer) S24/25: Avoid contact with skin and eyes Diacetyldioxim nothing special EDTA Ethylendiamintetraacetat
8 irritating Xi R36: Irritating to eyes R52/53: Harmful to aquatic organisms, may cause long-term adverse effects in the aquatic environment S61: Avoid release to the environment. Refer to special instructions/safety data sheet very good complex builder; not dispose in the sink, dispose in a metal solution box! A2: copy of the lab journal
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