Wednesday, April 3, 2019

Synthesis of nickel complexes

Synthesis of nickel complexesAbstractThe excogitation of this experiment was to investigate the Ligand exchange that occurs when different Nickel complexes and reacted with Triphenylphosphine.IntroductionTriphenylphosphine was initiative prepared by Pfeiffer and Sauvage in 1904ExperimentalTriphenylphosphine (1.408g) was dissolve at a lower place reflux with Propan-2-ol (15cm3) forming a colourless upshot to which 5 boiling chips were added. Nickel chloride hexahydrate (0.603g) was turn in absolute Ethanol (10cm3) and heated until a green/ sensationalistic issue formed. This solution was poured into the reaction mixture through the condenser. Immediately the solution turned grisly green, the solution was refluxed for a elevate 6mins. The reaction was remove from the heat and all(a)ow to cool for 4mins, a dark precipitate was perceptible in the flask. The warm solution was filtered under suction to collect the dark blue/green crystals which were washed with ice cooled absolu te ethanol (1x10cm3 + 1x3cm3). one time dry the boiling chips were removed with a spatula and the crystals were transferred to a n render sample vial and dried in the desiccator for a week.A further solution of Triphenylphosphine (1.410g) and Propan-2-ol (15cm3) was made and set to reflux as before. Sodium thiocyanate (0.601g) was dissolved in Ethanol (11cm3), to this nickel nitrate hexahydrate (0.773g) was added. The flask was warmed until all the green solid has dissolved and a white solid has formed. formerly cooled the solution was filtered under suction and the Filtrate (aqua blue liquid in Buchner flask) was added to the refluxing Triphenylphosphine through the condenser. Immediately the solution turned blood red/brown. The solution was refluxed for a further 7mins and then cooled for 5 mins. The warm solution was filtered under suction and the orange/ red crystals washed with ice cooled Ethanol ( 1x10cm3 + 1x8cm3). erst dry the boiling chips were removed as before and the crystals were transferred to the desiccator for a week.Results and discussionTriphenylphosphine + Propan-2-ol+ Nickle Chloride hexahydrate + Ethanol Bis(triphenylphosphine)nickel(II)chlorideP(C6H5)3 + C3H7OH + NICl2.6H2O + C2H5OH C36H30Cl2NiP2Triphenylphosphine + Propan-2-ol+ Nickle Chloride hexahydrate + Ethanol Bis(triphenylphosphine)nickel(II)chlorideP(C6H5)3 + C3H7OH + NaSCN + C2H5OH + Ni(H2O)6(NO3)2 Ni(PPh3)2(NCS)2EquationsXM = Molar magnetic susceptibility (cgs units)C= normalization constant = 1.044L= Length of sample (cm units)R= Balance practice session with FULL samples underpassRo= Balance reading with EMPTY sample tubeM= Relative molecular weight of samplem= potentiometer of samples (units grams)XM = XM- (diamagnetic correction)XM = Corrected Molar susceptibilityXM = Molar magnetic susceptibility (cgs units)diamagnetic correction = Calculated from literature table of diamagnetic corrections (Xd) have inter physique= Magnetic moment (units Bohr Magneton (BM))XM = Corrected Molar susceptibilityT= Temperature (units thousand (K))CalculationsXM = 294.0798111 x10-6Diamagnetic correction (data obtained from Inorganic Chemistry CMB004 d-block Chemistry Laboratory course 2009-10 page 14)Compound Ni(PPh3)2Cl2Diamagnetic correction = (-13 x10-6) + (-46 x10-6) + (-400 x10-6) = -459 x10-6XM = XM- (diamagnetic correction)XM = 294.07981110-6 -(- 459) x10-6 = 753.07981110-6eff =1.33 BM composite plant B showed a magnetic moment decrease of -055 to -073 on the foremost measurement so I re ran the measurement.

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