1. I-Ion Exchange Separations: Complexometric Titrations Dr. Prem D. Sattsangi Copyright © 2009

2. Exp.#5Ion-Exchange Separations of CuCl 4 -2, CoCl 4 -2 complexes AMBERLITE: IRA-400 with Copper and Cobalt complexes Chloro- Complexes Dark Purple

3. #2-Chloro-Complexes, U.K.#9, Volumetric Flasks 1-3 Chloro- Complexes U.K.Mixture Labeled

4. #3-Pipetting U.K. mixture in Vol. Flask #1 Use micropipet for the last few mL, avoid over shooting. 1. Pipet 1 mL U.K. 2. Add it to flask 1 3. Make it up to the mark No need to rinse 1 mL pipet here.

5. #4-Get Ready with Resin Column 1.Resin column is prepared in 3 M HCl. 2.Clamp it securely to a Buret stand. 3.Place a 50 mL Beaker underneath. 4.Take 50 mL, 3 M HCl in a 50 mL Graduated Cylinder and a micropipet.

6. #5-Applying 1 mL sample to the column (1)(2) Drain (3) Apply (4) sides (5)(6) Drain (7) Rinse Use M.P. 3M HCl Apply 1 mL pipet (1” above) Along sides of buret Drain HCl Flush Drain Flush Resin in 3 M HCl

7. #6-Insert a small wad of cotton on the top. Elute with 3 M HCl. Notice the Faint Greenish band 11-14 mL region Add 3 M HCl. Do NOT Over-fill. Keep watch on the Migrating Band. It grows fainter as it migrates. Chloro-complexes are changing to aquo- complexes.

8. #7- Cobalt elutes first. After ~10 mL of 3 M HCl, switch to small test tubes in a rack. Collect ~ 5 mL in each test tube. Watch the white glass wool area turn slight pink. Slight pink Cobalt is coming out. Tubes 1 and 7 seem to contain NO Cobalt. All these are taken.

9. #8-Elution of Copper with distilled water Copper elutes fast. 1.Collect in test tubes to begin with. 2.Color on the white glass wool, at the bottom will turn to a faint Blue. 3.DW converts Copper(II) to positively charged aquo-complex. 4.It is repelled by the + charge on the resin. Tubes 1 and 11 seem to contain NO Copper. All these are taken CuCl 4 -2 + H 2 O  [Cu(H 2 O) 4 ] 2+ (Repelled)

10. #9-Transferring the fractions in the test tube to Volumetric 3. Cu +2 1.Place a funnel on the top. 2.First pour tubes #2-9 3.Put tubes back in their place. 4. Use Tube #1 to rinse tubes 2-9 5. Pour tubes 9 and 10 to the flask

11. #10-Rinse Funnel with DW (1) Use Squeeze bottle to wash the funnel with DW. (2) Use 50 mL beaker to add more DW. Do not fill up to the neck. (3) Use Micropipet to make it up to the mark. Stopper securely. Shake and store for the next turn. (1) (3) (2)

12. General Advice: Economize, time, resources. Record everything directly in your note book. DO NOT WAIT FOR pH meter. APPROXIMATE readings will do. Washing glass ware: Use cold Tap water. Flush generously. Rinse with DW, using squeeze bottle. Squirt about 5 mL DW along sides of the flask. Drain excess on a paper towel. Weighing Murexide: Use the same weighing paper for all the weighings. Approximate 2.2-2.4 g is accurate enough. After finishing, do not forget to wash generously with ordinary water the buret and the pipet, before storing.

13. #11-Titration of Mixture in Vol. Flask -1 Experiment Mixture #_____ Cu 2+ (H 2 O) 4 and Co 2+ (H 2 O) 4 a. Pour ~20 mL of mixture in a Beaker. Rinse the 25.00 mL pipet. b. Pipette 25mL of Mixture into 2 Erlenmeyer flasks A, and B c. Adjust pH and make each flask ready for titration. Observations:

14. #12-Titration of Mixture in Vol. Flask -1 INSTRUCTIONS: 1.Use pH meter, add 3M NH 3 to adjust pH to 9. Repeat the procedure for flask (B). 2. Add 0.2-0.25g of Murexide, to flask “A” swirl. Color (Green - Yellow - Orange). Titrate flask A. Color, at end point, will be ~red. 3. Add Murexide and titrate “B” 4.Calculate molarity (M) for Co +2 + Cu +2.

15. Lab-Notes for Mixture Titrations OBSERVATIONS: Color ____________ Color with Murexide ________ Experiment: Added 3M NH 3 ____drs to pH 9. Used pH meter (3M NH 3 /3MHCl). Added ______g of Murexide, swirled to mix. TITRATION OF MIXTURE :Concentration of EDTA_____. Buret readings Set – A Set – B Final______mL _____mL Initial ______mL _____mL EDTA used ______mL _____mL Color at end point ___________

16. #13-Calculations One mole of EDTA reacts with 1 mol of M 2+ to form a Chelate complex. EDTA+M 2+  M(EDTA) 2+ complex EDTA is ~0.01 M. Copy exact concentration of EDTA from the reagent bottle. EDTA _____M Molar concentration of Co +2 (mL cancels) Molar concentration of Cu +2 (Show calculations same way) Molar concentration of Mixture of Co +2 and Cu +2 (Show calculations same way)

17. #14-Titration of Cobalt(II) INSTRUCTIONS: (Co 2+ (H 2 O) 4 ) 1. Rinse pipet. Take 25 mL of Co +2 in each flask A and B. 2. Use pH meter. Add 15M NH 3 to pH 8-9 light blue/Turquoise color. 3. Add 3M NH 3 until pH is 9. Repeat the procedure for flask (B). 4.Add 0.2-0.25g of Murexide to flask A, swirl. Color will be orange. Titrate flasks A to a pinkish red end point. 5.Add Murexide and titrate “B” 6. Calculate molarity (M) for Co 2+.

18. Lab-Notes for Co +2 Titrations OBSERVATIONS: Color ____________ Color with Murexide ________ Experiment: Added 3M NH 3 ____drs to pH 9. Used pH meter. Added ______g of Murexide, swirled to mix. TITRATION OF MIXTURE :Concentration of EDTA_____. Buret readings Set – A Set – B Final______mL _____mL Initial ______mL _____mL EDTA used ______mL _____mL Color at end point ___________

19. INSTRUCTIONS: (Cu 2+ (H 2 O) 4 ) 1. Rinse pipet. Take 25 mL of Cu +2 in each flask A and B. 2. Use pH meter. Add 3M NaOH to get a distinct blue/turquoise color (pH10-12). 3. Add few drops of 6M HCl to make the color disappear. 4.Add 3M NH 3 until pH is 9-10. Add 10 drops of pH 10 buffer If needed, adjust pH to 10 (3M NaOH) Do the same for Flask “B”. 5. Add 0.2-0.25g of Murexide and swirl. Color will be Yellow/ green. 6.Titrate to pinkish red. 7.Add Murexide and titrate “B” 8.Calculate molarity of Cu 2+ #15-Titration of Copper(II) 2. 3. 4. 5. 6.

20. Lab-Notes for Cu +2 Titrations OBSERVATIONS: Color ____________ Color with Murexide ________ Experiment: Added 3M NH 3 ____drs to pH 9. Used pH meter. Added ______g of Murexide, swirled to mix. TITRATION OF MIXTURE DATA:Concentration of EDTA_____. Buret readings Set – A Set – B Final______mL _____mL Initial ______mL _____mL EDTA used ______mL _____mL Color at end point ___________