Experiment 1 - Chem 114'

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Purpose

The purpose of this lab was to determine the concentration of sodium, calcium, and magnesium
ions in a small, undiluted sample of sea water. This was done by performing a cation exchange and a
complex metric titration using the chelating agent ethylenediamine-tetraacetic acid.
The cation-exchange resin, which is an organic polymer that has an acidic group located at
regular intervals along a carbon chain, is a very porous molecule. These pores are filled with positive
ions, such as H+ which help keep it neutrally charged against its normal negative charge. In this
experiment the resin is used to stoichiometrically exchange H+ ions for the cations present in the sample.
The sample solution is diluted to ⅕ of its original concentration with deionized water, going from 25mL of
the sample to 250mL. It is then eluted through the cation exchange column using deionized water and the
exchanged H+ ions are flushed out into an Erlenmeyer flask. This solution is used to find the
stoichiometric amount of H+ ions that were displaced by the cations that are in the sample. This is done
by titrating it with NaOH. From there the combined concentrations of Ca 2+ and Mg 2+ ions will be
found by performing a complexometric titration with the diluted sample and Ethylenediamine-tetraacetic
acid anion (EDTA). One mole of EDTA is stoichiometrically equivalent to one mole of metallic cation.
The endpoint of this titration is discovered using the indicator Eriochrome Black T. This indicator is a
chelating agent. When the pH is between 7-12 the The Eriochrome Black T forms a red complex with the
metal ions but with the addition of EDTA the metal cations are complexed preferentially and it changes to
blue.
After completing the cation exchange and both the titrations, we will know the moles of H+ ions
that reacted in the first equation, therefore the total moles of Na+, Ca2+, and Mg2+, and the total moles of
Ca2+ and Mg2+ from the second titration. Using those values we can then figure out the individual moles
of Na+, Ca2+, and Mg2+ that were found in the diluted sea water sample. In order to find the moles in the
original sample we simply multiply the moles of the ions in the diluted sample with the dilution factor to
give us the moles of the ions in the undiluted sample.

Data
Observations

Cation Exchange
Before the cation exchange column was able to be used in the experiment it first had to be regenerated to
the acidic form. In order to do this it was rinsed with 3mL of HCl and then six 30mL portions of
deionized water. The sixth rinse was collected in a beaker and tested with methyl orange indicator to see if
the solution turned yellow and the column was sufficiently rinsed. When it was first tested with methyl
orange the solution turned orange and indicated that there was still free acid in the solution. After the
column was rinsed a seventh time and the collect solution was tested again it turned a translucent yellow,
meaning the column was sufficiently rinsed.

NaOH Titration
Before the titration was performed the diluted seawater was eluted through the resin column. The solution
stayed clear and colorless as it went through the column. 5 additional 30mL portions of deionized water
was eluted through and collected at the bottom along with the sea water. This solution was then titrated
using phenolphthalein as the indicator. Once the end point of the titration was reached the phenolphthalein
caused the solution to go from colorless to a light pink color. This indicated that the moles of NaOH were
stoichiometrically equal to the moles of H+ ions the were displaced from the ions in the seawater when it
was eluted through the resin column.

EDTA Titration
For this titration the diluted seawater was titrated with EDTA in a complexometric titration. Eriochrome
Black T. was used as the indicator and indicated when the moles of EDTA were stoichiometrically equal
to the moles of Ca2+ and Mg2+ ions in the diluted sea water. This endpoint was clear when the sea water
solution turned fully from a red color to a blue color during the titration. This was because the metal ions
formed a red complex but once fully titrated the ions were complexed by the EDTA, turning the solution
blue.

Calculations
Results

Conclusion

By performing a cation exchange using a cation column, and two separate titrations, the ion
concentration in undiluted sample of seawater Salween was found. First the seawater was diluted by a
dilution factor of 10 as 25mL of sample was mixed with 225mL of deionized water. The cation exchange
help allowed H+ ions to displace the Na+, Ca2+ and Mg2+ ions within the diluted sample. This collected
solution with the displaced H+ ions was titrated with 0.09683M NaOH to determine the moles of H+,
0.001098 moles, and therefore the total moles of Na+, Ca2+ and Mg2+ ions in the diluted solution. In
order to find the moles of each individual ion a second titration was performed with the diluted sample
and EDTA. The EDTA reacted with the Ca2+ and Mg2+ ions, giving us the total moles of those two ions
in the sample which was 1.452 x 10^-4 moles. Using the fact that the ratio of Mg2+ to Ca2+ in the sample
was 5:1, the individual moles of Mg2+ were found to be1.210 x 10^-4 moles and the moles of Ca2+ were
2.420 x 10^-5 moles. By subtracting the moles of Ca2+ and Mg2+ form the moles of H+, the number of
moles of Na+ was found to be 8.076 x 10^-4 moles. From there the concentrations of all the ions in the
diluted sample were found and by multiplying them by the dilution factor of 10 we found the
concentration of Na+ in the undiluted sample Salween was 3.230 x 10^-2, the concentration of Ca2+ was
9.680 x 10^-4 and the concentration of Mg2+ was 4.840 x 10^-4.

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