Experiment 9: Ion-Exchange Chromatography dela Cruz, Marie Giecel V. Pabilane, Alma L. Group 6, Chem 27.1, SEJ1, Ms.

Noime Walican March 19, 2011 I. Abstract Ion-exchange chromatography is an important method of analysis for alkali metal cations and anions and for determining the distribution of complex species. In this experiment, the equivalent weight of the salt sodium chloride with molecular weight 58.44 g/mol is determined by ion-exchange chromatography, particularly anion exchange, using sodium hydroxide as eluting agent. The NaCl solution being the mobile phase was passed through a column of tightly packed anionexchanger resin, which is the stationary phase. The anion of the resin, which is HO- is exchanged with the anion of the salt which is Cl-. The liberated HO- was titrated to methyl red end point using 3.1 mL of standard 0.1162 M hydrochloric acid. The experimentally determined equivalent weight of the salt was 56.015 g/eq, having a negative percent error of 4.15%. II. Keywords: ion-exchange chromatography, equivalent weight, resin, eluting agent liberated OH- present in the eluent can now be titrated with III. Introduction and Principles a strong acid. A lot of common chemical species such as alkali metal cations and halide anions are difficult to measure in large amounts because they do not readily form insoluble precipitates or colored complexes which would help in the analysis of these species. Moreover, some metal ions may be present in a solution as stable complex species such as the case of Fe(CN)63- and CoCl42- or in different oxidation states such as U4+ or UO22. Ion exchange may be used to concentrate and separate solution species based on their charges. It may also be used to determine quantitatively the concentration of a solution species based on the stoichiometry of the charged species displaced from the solid phase when the analyte binds to the ion exchanger. Ion-exchange chromatography involves the interaction of a solid, insoluble phase that contains positively or negatively charged sites (the resin) with a mobile phase (eluent solution) that contains the counter ion. The ion-exchange equilibrium can be written as, Cation exchange: B+(aq) + A+Res-(s) A+(aq) + B+Res-(s) Anion exchange: X-(aq) + Res+Y-(s) Y- (aq) + Res+X-(s) One of the most common ion-exchange resin used is copolymer of styrene and 4-12%divinylbenzene which has been sulfonated (acidified) to produce a strong-acid cation exchanger or aminated (basified) to give a strongbase anion exchanger. This experiment aims to determine the equivalent weight of the salt. In the experiment, the resin would be basified with a strong base, 4 M sodium hydroxide. The resin would become a strong anion exchanger. Once the salt solution, which is the mobile phase, is passed through the column, it would exchange anion with resin, which is the stationary phase. The salt is converted to a base. The V. Methodology and Materials In a beaker, 0.50-0.51 g of the salt was dissolved with enough distilled water. It was transferred in a 250-mL volumetric flask and diluted to mark. A buret was used as glass column. The bottom of the buret was plugged with cotton. The column was packed with enough resin to fill 10 in of the column. The resin was regenerated using 50 mL of 4 M sodium hydroxide at a flow rate of 3 mL/min. Afterwards, all the traces of OH- was washed off the resin with distilled water added in 10 mL portions at a flow rate of 6 mL/min. To test the completeness of washing, the last 10 mL of washing was added with 1 drop of standard HCl and 3 drops phenolphthalein. The color of the resulting mixture must be identical with the color of 10 mL distilled water with 1 drop standard HCl and 3 drops phenolphthalein. The standard HCl was prepared by diluting 8.62 mL of concentrated HCl to 1 L. It was titrated against primary standard grade sodium carbonate. Ten milliliters (10 mL) of the salt solution was pipetted and passed through the column. Immediately, this was followed bwith 100 mL distilled water. The last 10 mL of washing was tested as described above. The eluent and washing was titrated with standard HCl using methyl red indicator. This was done thrice. From the data gathered, the equivalent weight of the salt was calculated. VI. Results VII. Discussion

Chem 27.1. Spectrophotometric Determination of Stoichiometry of a Complex

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VIII. Conclusion and Reccomendations

IX. References

1. Hargis L.(1988).Analytical Chemistry. Prentice2. Skoog, D.,West, D, Holler, F., Crouch, S.

(2004).Fundamentals of Analytical Chemistry 8th ed.Thomson Learning Brooks/Cole.Singapore. 3. Determination of Equivalent Weight of an Inorganic Salt by Cation Exchange. Retrieved from http://kinardf.people.cofc.edu/221LabCHEM/CHE M221L%20Ion-Exchange%20Equivalent %20Weight.htm on March 14, 2011 Hall Inc.New Jersey.

I hereby certify that I have given substantial contribution to this report. DELA CRUZ, MARIE GIECEL V. PABILANE, ALMA L.

Chem 27.1. Spectrophotometric Determination of Stoichiometry of a Complex

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