This action might not be possible to undo. Are you sure you want to continue?
Synthesis and Analysis of a Coordination Compound
Department of Chemical Engineering and Chemistry, Mapua Institute of Technology February 8, 2006
In this experiment, the compound was prepared to contain cobalt ion, ammonia, and chloride ions. Our objective was to determine the umber of atoms using different methods for each ions. Our unknown compound analyzed was Co1(NH3)5Cl3.
Introduction One of the many interesting areas of chemistry is the study of a class of substances called coordination compounds or complexes. These compounds are typically salts. One or both of the ions in the salt can be composed of a central metal atom, which is bonded to Lewis bases. In this discipline of chemistry, the Lewis bases are called ligands. In this experiment, a compound was made that can have ion isomers. In many reactions involving complex ion formation the rate of reaction is very fast, so that the thermodynamically stable form of the complex is the one produced. By changing ligand concentrations, one can quickly convert from one complex to another. Those complexes undergo rapid exchange with other Lewis bases are referred to as labile; conversely, those complexes that only exchange slowly with other Lewis bases are referred to as inert. Methodology Preparation of Cox(NH3)yClz Using a piece of weighing paper and a top-loading balance, 10 g of ammonium chloride was weighed. NH4Cl was poured into a 250-mL beaker and 40 mL of distilled water was added. To this, 8 g of cobalt (II) chloride hexahydrate, CoCl2 · 6H20 and 0.8 g activated charcoal was added. The mixture was heated to boiling point with stirring to dissolve the soluble components. The beaker was cooled in water, then in an ice bath. Slowly, in a hood, 40 mL of 15 M NH3 was added. After stirring, 50 mL of 10% H2O2, hydrogen peroxide was added slowly, a few mL at a time, while continuing to stir. When the
bubbling had stopped, the 250-mL beaker was placed in a 600-mL beaker containing 100 mL of water at about 60ºC. The beaker was left in the water bath for 30 minutes, holding the temperature of the bath at about 60ºC as long as the liquid has a pink color. It was stirred occasionally. When the 40 minutes were up, the 250-mL beaker was removed from the water bath and cooled, first in a water bath and then in an ice bath, until the liquid in the beaker had a temperature below 5ºC for 5 minutes. The Buchner funnel was setup and, with suction, the mixture was filtered through the filter paper in the funnel. The solid was scrapped from the filter paper in the 250-mL beaker. 100 mL distilled water was then added, and in a hood, 4 mL 12 M HCl was also added. The mixture was heated to boiling, with stirring, to dissolve the crystals. The suction flask was rinsed with distilled water, and the Buchner funnel was reassembled. The hot mixture was then filtered through the paper in the funnel, under suction. In this operation, the charcoal was removed and placed on the filter paper. The filtrate was transferred to the 250-mL beaker and, in the hood, 15 mL 12 M HCl was added. The beaker was placed in an ice bath and was stirred for 5 minutes to promote formation of the golden crystals of the product Cox(NH3)yClz, 50 mL of nice-cold distilled water was poured on to a piece of filter paper in the Buchner funnel. The flask was then emptied and the cold mixture was filtered containing the product through the funnel, using suction. The suction was turned off, and 20 mL 95% ethanol was poured on to the crystals. The crystals was transferred from the filter paper to the beaker and stored.
Note: The methodology of the gravimetric determination of chloride content and the colorimetric determination of cobalt content will not be discussed in this report since it was performed by the other groups. Volumetric Determination of Ammonia Content In this part of the experiment the complex was decomposed, releasing NH3 to the solution. The NH3 was then distilled off into another container, and was titrated against an acid. The procedure is called a Kjeldahl analysis, and is used for determining nitrogen content of many organic and inorganic substances. The distillation apparatus was assembled as shown in the figure.
(inert). For such species, the preparation reaction takes time, but once formed, the complex ion in solution may resist change rather dramatically. In the complex ion NH3 and Cl- may be ligands. Some of the Cl- ions may be in the complex and some may simply be anions in the crystal. Cox(NH3)zCly(s) + OH-(aq) Co3O4(s) + O2(g) + NH3(aq) + H2O2 + ClCo3O4(s) + SO32-(aq) + 6 H+(aq) 3 Co2+(aq) + SO42(aq) + 3 H2O(l) When the compound is dissolved in water, the free anions will go into solution, but the ones in the complex will remain firmly attached to cobalt. They neither will nor react with a precipitating agent such as Ag+ ion, which will tend to form AgCl with any free Clions. All of the NH3 molecules will be in the complex ion, and will not react with added H+ ion, as they would if they were free. NH3 and Cl- that is present in the compound was destroyed attempting any analysis. The complete analysis involves a gravimetric procedure for chloride ion. A volumetric procedure for ammonia was followed. The chemical reaction for cobalt analysis which is a calorimetric method is as follows: Cox(NH3)zCly(s) + heat CoCl2(s) + N2(g) + NH4Cl(s) + NH3(g) CoCl2(s) + water 3 Co2+(aq) (λ = 510 nm) + Clfollows: Cobalt Content: Molarity of Co ion = 0.0445 M Molarity of Co in sample = (0.0445 M)(0.05L) =2.225x10-3 mol Mass of sample = (2.225x10-3 mol) / (0.5053 g) = 4.4033x10-3 mol/g Molarity of Co per 100 g sample = (4.4033 x10-3 mol/g)(100) = 0.4403 mol Chloride Content: Mass of AgCl = 1.5055 g Mass of Cl- in AgCl = 1.5055 g (1 mol / 143.32 g AgCl)(1 Cl- / 1 AgCl)(35 g / 1 Cl-) = 0.1210 g 2
50 mL saturated boric acid solution was inserted in the 125-mL receiving flask; with five drops bromcresol green indicator, the level of the flask was adjusted so that the latex tubing is well under the liquid surface. 1 g of the compound was weighted into a beaker and transferred in the distilling flask using a funnel. The beaker was rinsed several times with small portions of distilled water. Distilled water was added to give a final volume of about 50 mL. The flask was stirred to dissolve the sample. A few boiling chips and several pieces of granulated zinc was added. 40 mL 6 M NaOH was poured with 50 mL distilled water into the flask and reconnected to the distilling head. The plated was turn on. Ammonia was recovered in the receiving flask.
The calculations for the ions were as
Interpretation of Results
The synthesis of the unknown inorganic compound followed this (unbalanced) equation: CoCl2 · 6 H2O(s) + H2O + NH4Cl(s) + NH3 Cox(NH3)zCly(s) + H2O(l) Many, but by no means all, complexes are labile. It exchanges ligands only very slowly
Mass of Cl- per 100 g sample = (0.1210 g / 0.2307 g) x 100 = 52.4491 g Moles of Cl- per 100 g sample = 52.4491 g / 35 g/mol = 1.4794 mol Ammonia Content: Moles of NH3 in 40 mL = (32.4 mL)(0.09533 M) = 3.085x10-3 mol Moles of NH3 in 250 mL = (3.085x10-3 mol)(250 / 40) = 19.3x10-3 Molarity of NH3 per 100 g sample = (19.3x10-3) (100) = 1.928 mol From the calculations we can determine the number of moles for each species present in a mole of compound. Moles cobalt / 100 g sample = 0.4403 mol Moles chloride / 100 g sample = 1.4794 mol Moles ammonia / 100 g sample = 1.928 mol Because the mole ratio must equal the atom or molecule ratio, we can determine the formula of the compound. x=1 y=3 z=5 Hence our unknown compound is Co1(NH3)5Cl3(s) Conclusion Coordination compounds can be prepared that have the same molecular formula but different in the composition of ions. The complete analysis involves a gravimetric procedure for chloride ion, a calorimetric method fro cobalt ion, and a volumetric procedure for ammonia. Using these methods of analysis the authors derive the unknown inorganic compound which is Co1(NH3)5Cl3. References www.accd.edu/nvc/areas/chem/ComDALab/Synt handAnalofCoordinate.pdf cod.edu/people/.../CHEM153/SyntheisiAnalysisCoordinationCompExp30.pdf
employees.oneonta.edu/kotzjc/LAB/Complex_E xpt.pdf http://www.dit.ie/DIT/science/chemistry/rsccom p/competition00/distillation/labdistillation.JPG
This action might not be possible to undo. Are you sure you want to continue?
We've moved you to where you read on your other device.
Get the full title to continue reading from where you left off, or restart the preview.