Analytical Chemistry Laboratory 2

Determination of Magnesium by Ion-Exchange Chromatography

Mr. *****

Department of Chemical Engineering and Chemistry, Mapua Institute of Technology

November 22, 2005

A charged substance, Magnesium, was separated via column materials (resins and glass
wool) that carry a negative charge. The ionic groups of exchanger columns are covalently bound
to the gel matrix and are compensated by small concentrations of counter ions, which are present
in the buffer. When the unknown sample was added to the column, an ion exchange with the
weakly bound counter ions takes place. The percentage of Magnesium oxide in the sample was
computed to be 66.27% for sample #4.

Objective
ions such as Cl- or OH- accompany the
The purpose of this experiment is to positive sites. If the polymer structure is not
understand the principles of given in detail the anion exchange bead can
chromatographic separations particularly on be shown diagrammatically below:
ion exchange. The main objective is to
determine the concentration of Magnesium
in the sample.

Discussion

Overview

In ion-exchange column
chromatography the stationary phase is
composed of beads of a high molecular
weight organic polymer which are closely
related to the polystyrene from which coffee
cups are made. In the beads the long
polymer chains have a small percentage of
crosslinking via divinyl benzene, and
contain a large number of either anionic or
cationic groups which are covalently bound
to the polymer structure. Each of these
charged sites in the polymer must be
accompanied by a small ion of the opposite
charge in order to insure total electrical
neutrality. An anion exchange must contain
positive charges. These are usually
quaternary ammonium groups where counter
In either cation or anion-exchange
chromatography, the attraction for the
stationary phase is simple electrostatic
attraction of positive charges for negative
charges, but each different type of cation or
anion has its own affinity for the
corresponding resin.
Cations in an aqueous solution are
never monoatomic species but are bonded to
water molecules to form Lewis acid-base
adducts called "complex ions". In many
instances it is possible to replace these water
molecules with other electron donating
species, e.g. Cl- or NH3. Collectively these
electron donating species are referred to as
ligands. If negatively charged ligands are
used, the positive ions can become neutral or
even negative species.
In the experiment, the titrant 0.05 M
NaOH was standardized with primary-
standard potassium hydrogen phthalate
(KHP). Magnesium is the element to be
analyzed in the sample.
Magnesium is a very important
essential macromineral, even though there
are only several ounces in the body (0.05
percent of body weight). It is involved in
several hundred enzymatic reactions, many
of which contribute to production of energy
and cardiovascular function. As time goes
on, magnesium is recommended and used in
more and more treatments. Prevention or
treatment of myocardial infarctions (MIs),
prevention of kidney stones, and in
treatment of premenstrual syndrome are
some important recent uses. Magnesium has
been used with some success in relieving
certain kinds of angina and reducing the
risks of coronary artery spasms, which can
lead to angina or, more severely, heart
attack. Deficient magnesium levels have
been found in the blood and hearts of
cardiac victims. Besides preventing heart
attacks, magnesium has a mild effect on
lowering blood pressure and so is used to
treat and prevent hypertension and its
effects. Magnesium supplementation can
reduce many of the symptoms of mitral
valve prolapse, such as palpitations or
arrhythmias, and it may help in other cardiac
arrythmias such as atrial tachycardia or
fibrillation, or those caused by taking excess
digitalis, a cardiac drug. It may also reduce
the bronchoconstriction in asthma by
relaxing the muscle around the bronchial
tubes. Intravenous solutions containing
magnesium and other nutrients have been
used successfully to break acute asthma
attacks.
Toxicity due to magnesium overload
is almost unknown in a nutritional context,
as excesses are usually eliminated in the
urine and feces. However, symptoms of
magnesium toxicity can occur more likely if
calcium intake is low. These symptoms may
include depression of the central nervous
system, causing muscle weakness, fatigue,
sleepiness, or even hyperexcitability. In
extreme states, magnesium overload can
cause death.
Methodology
Preparation of ion-exchange columns
A plug of glass wool was inserted to
retain the resin particles. A sufficient strong-
base anion-exchange resin was then
introduced to give a 10- to 15-cm column.
The column was washed with about 50 mL
of 6 M NH3, followed by 100 mL of water
and 100 mL of 2 M HCl. At the end of this
cycle, the flow was stopped so that the
liquid level remains about 1 cm above the
resin column.
Chromatographic Analysis
The number of tablets in the sample
was recorded. The tablet was then
transferred to a clean 500 mL volumetric
flask. They were dissolved in a minimum
volume of 3 M HCl. Then it was diluted to
the mark with distilled water. The free acid
was titrated in several 15-mL aliquots of the
dissolved sample; phenolphthalein was used
as an indicator. The column was conditioned
with about 15 mL of 3 M HCl, followed by
three 15-mL portions of distilled water.
Each column was charged with a 15-mL
aliquot of the sample. It was eluted of about
2 to 3 mL/min. The column was washed
with three 15-mL portions of water. The
elute and washings were collected in a
conical flask. The eluted samples (and
washings) were titrated with standard base.
The total volume that needed to titrate the
free acid was corrected.
Instrumentation
 2. Skoog, D. A., and Leary, J. J., Principles
of Instrumental Analysis, 4th edition,
Saunders, New York 1992.

3. Harris, D.C., Quantitative Chemical

Analysis, 3rd edition, Freeman, New York,
1991.

The column contains resins which is 4. © 1993-2003 Microsoft Corporation. All

a quaternary ammonium ion. Beneath the rights reserved.
resins contains a glass wool to retain the
resin particles.

Interpretation

This experiment requires the weight

of a certain mass of the unknown salt, which
is 1.0019 g dissolved in a solvent, and
passed over a column of ion-exchange resin.
As mentioned previously, this process
serves the purpose of converting the salt into
its corresponding acid, MgCl., would all be
transformed to HCl. Once the salt has been
converted, the acid solution which is a result
of this procedure is titrated using a
standardized solution (KHP) of sodium
hydroxide. With the information obtained
from the titration, you can MgOH in the
unknown sample
mmol H+ = 2x mmol Mg2+
The percentage of concentration computed
was approximately 66.72%.

Conclusion

Ion exchange chromatography uses

an ion exchange resin as the stationary phase
and the sample as the mobile phase. The
mechanism of separation is based on ion
exchange equilibria. The Magnesium cation
in the sample was exchanged with the anion
resin. Due to this process MgO content in
the unknown can be computed.

References

1. Christian, G.D., Analytical Chemistry, 6th

edition, New Jersey, John Wiley, 2004.