Laboratory 1 METAL COMPLEXES OF DIMETHYL SULFOXIDE Adapted from Pike et. al, "Microscale Inorganic Chemistry", Exp. 20, p. 218‐222. Two weeks lab 1) Prepare three complexes 2) Characterize the complexes
Experimental Preparation of Cu(DMSO)2Cl2 150 mg of copper(II) chloride was placed into a 25 mL Erlenmeyer flask equipped with a magnetic stirring bar. 1.0 mL of absolute ethanol was added to the flask by using a Pasteur pipet. The mixture was stirred until all of the copper(II) chloride has dissolved. 0.25 mL of DMSO was then added slowly by using a Pasteur pipet. An immediate exothermic reaction occurred, yielding a light green precipitate. The mixture was stirred for five minutes. The product was collected by suction filtration using a Hirsch funnel. The product was washed with 1 mL cold ethanol (two 0.5 mL portions) and dried by pulling air through the filter paper for 10 minutes. The product was weighed for a percent yield calculation. Melting point of the product was determined by packing the product in a capillary tube. The melting point measurement was done by using a (add model of the apparatus here). Infrared spectrum of the product was collected by using a (add model of the apparatus here). The air background absorption was collect prior to collecting the absorption of the sample. The solid sample was placed on a sample holder and the sample was pressed to scale 12 on the spectrometer while collecting the absorption. Preparation of Pd(DMSO)2Cl2 Preparation of Ru(DMSO)4Cl2
Report Summary: 1. In Introduction part, add short principal of techniques used in preparation, and characterization of the complexes as well as the hard‐soft acid‐base theory. 2. In Experimental section, write in paragraph, no numbered step, use passive form and past tense, specify the exact mass (and moles) used in the experiment (no estimation mass or moles – you have finished the experiment, you know how much you weighed and used). 3. In Results and Discussion part, show data and explain. If no explanation, you will not get any credit for this part. Show IR spectra in the report and assign all of the major peaks, especially those in the vicinity of 1000 cm‐1. Determine the absorption frequency of the S‐O band for both the complex and DMSO solvent. Try to find the literature results, compare to your results and explain the differences. 4. Show calculations for percent yields. 5. Answer Questions in page 222.