Procedures
4.1 Preparation of Cis–diaquabis(glycinato)copper(II)monohydrate
Dissolve about 1.0 g of copper sulphate, CuSO4.5H2O, in 8.5 ml of 1 M HCl and add 700 mg of glycine (H2NCH2CO2H). Cautiously warm the mixture in the water bath or on hot plate for 30 minutes, and during this period, slowly add solid NaHCO3 to the warm solution until a crystalline precipitate is completely formed (Do not overheat). Filter the solid by suction (filtrate discard at waste container No. 4). Allow the crystal to dry in the oven at 100 0 C. Record the product. Divided the product for the solution 8 (4.3), and for IR, NMR studies (4.4).
4.2 Preparation of Bis(acetylacetonato)copper(II).
Dissolve 0.31 g of acetylacetone (CH3COCH2COCH3) in 10 ml of 0.25 M NaOH. Add a solution of 0.37 g of CuSO4.5H2O in 15 ml of H2O. The sparingly insoluble Bis(acetylacetonato)copper(II) is immediately formed as a crystalline precipitate. Filter the product by suction (filtrate discard at waste container No. 5). Allow the crystal to dry at room temperature. Record the product.
**Divided the product for the solution 9 (4.3), and for IR, NMR studies (4.4).
4.3 Absorbance Measurement of Complex Solutions
The following stock solutions will be prepared:
0.01 M Cu(NO3)2 in H2O using ultrasonic apparatus (Use for preparation of solution 1-7)
0.10 M NH3 (Use for preparation of solution 2-5)
0.10 M ethylenediamine (Use for preparation of solution 6 and 7)
Then, the Copper(II) complexes solution will be prepared with total volume about 10-15 ml in the different ratios as shown below. For solution 2-5, the solutions should immediately homogeneous mix and then measure the absorbance as soon as possible.
Measure the absorbance of these solutions in the range of 500–850 nm. Compare the max values obtained when different ligands are used and suggest the spectrochemical series. Solid products discard at waste container No. 8. Solutions of products discard at waste container No. 4. Filter papers discard at waste container No. 7.
4.4 IR and NMR spectra of copper complexes
IR spectra of free glycine, acetylacetone and copper complexes (4.1 and 4.2) are recorded and assigned in mid IR.
1H and 13C-{1H}, 13C DEPT-135 NMR spectra of free glycine, acetylacetone and copper complexes are examined and assigned.
Discuss and conclude the structure of complexes using the data from spectroscopic techniques.
record the weight obtained
Procedures4.1 Preparation of Cis–diaquabis(glycinato)copper(II)monohydrateDissolve about 1.0 g of copper sulphate, CuSO4.5H2O, in 8.5 ml of 1 M HCl and add 700 mg of glycine (H2NCH2CO2H). Cautiously warm the mixture in the water bath or on hot plate for 30 minutes, and during this period, slowly add solid NaHCO3 to the warm solution until a crystalline precipitate is completely formed (Do not overheat). Filter the solid by suction (filtrate discard at waste container No. 4). Allow the crystal to dry in the oven at 100 0 C. Record the product. Divided the product for the solution 8 (4.3), and for IR, NMR studies (4.4).4.2 Preparation of Bis(acetylacetonato)copper(II).Dissolve 0.31 g of acetylacetone (CH3COCH2COCH3) in 10 ml of 0.25 M NaOH. Add a solution of 0.37 g of CuSO4.5H2O in 15 ml of H2O. The sparingly insoluble Bis(acetylacetonato)copper(II) is immediately formed as a crystalline precipitate. Filter the product by suction (filtrate discard at waste container No. 5). Allow the crystal to dry at room temperature. Record the product.**Divided the product for the solution 9 (4.3), and for IR, NMR studies (4.4).4.3 Absorbance Measurement of Complex SolutionsThe following stock solutions will be prepared:0.01 M Cu(NO3)2 in H2O using ultrasonic apparatus (Use for preparation of solution 1-7)0.10 M NH3 (Use for preparation of solution 2-5)0.10 M ethylenediamine (Use for preparation of solution 6 and 7)Then, the Copper(II) complexes solution will be prepared with total volume about 10-15 ml in the different ratios as shown below. For solution 2-5, the solutions should immediately homogeneous mix and then measure the absorbance as soon as possible.Measure the absorbance of these solutions in the range of 500–850 nm. Compare the max values obtained when different ligands are used and suggest the spectrochemical series. Solid products discard at waste container No. 8. Solutions of products discard at waste container No. 4. Filter papers discard at waste container No. 7.4.4 IR and NMR spectra of copper complexesIR spectra of free glycine, acetylacetone and copper complexes (4.1 and 4.2) are recorded and assigned in mid IR.1H and 13C-{1H}, 13C DEPT-135 NMR spectra of free glycine, acetylacetone and copper complexes are examined and assigned.Discuss and conclude the structure of complexes using the data from spectroscopic techniques.record the weight obtained
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