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1
ION CHROMATOGRAPHY
Introduction
Ion chromatography is an example of liquid solid chromatography
(adsorption chromatography). It is simply a high performance
version of ion exchange chromatography. First developed in 1940s,
this technique is used to identify the molecular make up of
materials. Thus, ion chromatography is separation and
quantification of anions and cations using HPLC (High
Performance Liquid Chromatography) technique and ion exchange
resins.
Instrumentation and Technique
Ion chromatography can be performed on standard HPLC
instrument. The instrumental set up is as follows:-
1. Solvent delivery system: It consists of solvent reservoir,
pump, pressure control and filter.
2. Sample injection system: Sample is fed into the flowing
stream of solvent with an injector.
3. Separating column: Ionic separation of components take
place here. Ion exchange resins based on styrene divinyl
benzene copolymers are used. The column is stainless steel
column of length 10- 30 cm and internal diameter 4- 10 mm.
The resin material is either bound to the surface of moderately
large (30 – 50 μm) glass beads to form a pellicular packing, or
by coating surface of a rigid microparticle to give special type
of packing.
4. Stripping column: Also called suppressor column, it is the
second ion exchange column which is used to selectively
remove only the mobile phase ions from eluate of separating
column.
5. Detector: Conductivity detector is
detector. Apart from this,
6. Recorder: The recorder records the signa
Two types of ion chromatography are currently in use:
based and single-column.
the conductivity of the eluting electrolyte from interfering with the
measurement of analyte conductivit
A. Ion Chromatography based on Suppressor
It is also popularly called Double
Chromatography. In this, the
the injector where sample is added and into the separating
column. Here, the sample component ions separate. The eluate
flows in stripping column, where mobile phase ions are
removed and remaining sample ions are detected
conductivity detector.
Working of stripping column:
 If the electrolyte in the mobile phase is HCl (often used
during the separation of cations), an anion exchange resin in
the hydroxide form is used in the stripping column. The
chloride from the dilut
Conductivity detector is the most commonly used
tector. Apart from this, UV detector is also used sometimes.
The recorder records the signal in form of graph.
Two types of ion chromatography are currently in use: suppressor
column. They differ in the method used to prevent
the conductivity of the eluting electrolyte from interfering with the
measurement of analyte conductivities.
Ion Chromatography based on Suppressor
is also popularly called Double – Column
hromatography. In this, the mobile phase is pumped through
the injector where sample is added and into the separating
column. Here, the sample component ions separate. The eluate
flows in stripping column, where mobile phase ions are
removed and remaining sample ions are detected
conductivity detector.
Working of stripping column:
If the electrolyte in the mobile phase is HCl (often used
during the separation of cations), an anion exchange resin in
the hydroxide form is used in the stripping column. The
chloride from the dilute HCl in the mobile phase exchanges
2
the most commonly used
is also used sometimes.
l in form of graph.
suppressor-
They differ in the method used to prevent
the conductivity of the eluting electrolyte from interfering with the
olumn Ion
mobile phase is pumped through
the injector where sample is added and into the separating
column. Here, the sample component ions separate. The eluate
flows in stripping column, where mobile phase ions are
removed and remaining sample ions are detected in the
If the electrolyte in the mobile phase is HCl (often used
during the separation of cations), an anion exchange resin in
the hydroxide form is used in the stripping column. The
e HCl in the mobile phase exchanges
3
with hydroxide on the column and then reacts with
hydronium ions (from the HCl) to form water. The net result
is the removal of mobile phase ions from solution. Because
the stripping column is an anion exchange column, it does
not affect the separated cations in the sample.
 If anions are to be separated and the mobile phase contains
dilute NaOH, the anion exchange separating column is
followed by a cation exchange stripping column in the
hydrogen form. On the resin of stripping column, the
sodium ion exchange with hydronium ion which
subsequently react with hydroxide to form water and
effectively remove mobile phase ions from the solution.
The stripping columns get exhausted, and must be replaced or
regenerated.
 Recently, stripping columns have been designed which
continuously refurbish the reactant ion and which
consequently eliminate the need to remove the column to
regenerate the reactant. Typical stripping column consist of
2 concentric compartments. The effluent from the separating
column flows downward through the inner compartment
where the mobile phase ions are exchanged.
Simultaneously, a solution of the ions that were consumed
from the resin of stripping column flows upward through
the outer compartment. As the ions are used in inner
compartment, they are replaced by ions from outer
compartment. This device is termed as Hollow Fibre
Suppressor.
B. Single Column Ion Chromatography
This relies upon electronic suppression of background signals
from conductivity detector. The apparatus uses a pump to
force the mobile phase through the separating column; no
4
stripping column is used. Effluent from separating column
flows directly into the conductivity detector.
The problem of large background signal owing to high
concentration of electrolyte in the mobile phase is overcome
by use of a relatively low concentration electrolyte solution
with a low capacity column, and a detector with capability to
suppress large signals.
 Use of a single column eliminates the relatively large
dead volumes often associated with use of stripping
columns. It also eliminates the additional expense
associated with stripping column and its regeneration.
Applications
Ion Chromatography analysis can be used to determine either or
both qualitative and quantitative conclusions about a material's
composition. Material identification is accomplished by comparing
a sample's results against those of known reference materials.
Quantitation, or quantification of concentrations, is achieved by
comparing each anion's or cation's peak height in the chromatogram
to a standard curve of known concentration.
Ion Chromatography is often used as a material analytical technique
in the environmental, industrial, biological, pharmaceutical,
chemical and food sectors.
It is commonly used in:-
1. Separation and detection of trace ionic species – Ion
chromatography is the only technique that can provide
quantitative analysis of anions at the ppb level and is used to
detect ions in liquids. Trace analysis of common anions like
F‾, Cl‾, Br‾, I‾, NO2‾, NO3‾, SO4
2--
, PO4
3--
and that of cations
like Li+
, Na+
, K+
, Mg+2
, Ca+2
, Sr+2
, Ba+2
can be easily
performed.
2. Food product analysis – Ionic contamination on the surfaces
of wafers, chips, and packages can be detected easily. Thus, it
5
can be an essential tool for guaranteeing quality control. IC
analysis is also a great way to test the cleanliness of a product
following the manufacturing process.
3. Environmental analysis - It is used to analyse soil extracts,
pond water, industrial process waste.
4. Biological application – Organic acids, amino acids and
peptides can be determined by selecting proper polymeric
column, mobile phase and detector.
5. Polyvalent anion such as pyrophosphate, tripolyphosphate and
trimetaphosphate can be differentiated.
6. It is used to analyse multi element transition metals, at levels
lower than those possible with AAS.
IC analysis is a simple, fast and accurate materials analysis
technique. Setting up and analyzing a single sample typically takes
1 hour with each additional sample taking 15-30 minutes to analyze.
References:-
1. Introduction to Instrumental Analysis; Robert D. Braun
2. Principles of Instrumental Analysis (6th
edition); Douglas A.
Skoog, F James Holler, Stanley R. Crouch
3. Vogel’s textbook of Chemical Analysis (6th
edition); J.
Mendham, R.C. Denney, J.D. Barnes, M. Thomas, B.
Sivasankas.
4. Instrumental Methods of Chemical Analysis; H. Kaur
THANK YOU

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Ion chromatography copy

  • 1. 1 ION CHROMATOGRAPHY Introduction Ion chromatography is an example of liquid solid chromatography (adsorption chromatography). It is simply a high performance version of ion exchange chromatography. First developed in 1940s, this technique is used to identify the molecular make up of materials. Thus, ion chromatography is separation and quantification of anions and cations using HPLC (High Performance Liquid Chromatography) technique and ion exchange resins. Instrumentation and Technique Ion chromatography can be performed on standard HPLC instrument. The instrumental set up is as follows:- 1. Solvent delivery system: It consists of solvent reservoir, pump, pressure control and filter. 2. Sample injection system: Sample is fed into the flowing stream of solvent with an injector. 3. Separating column: Ionic separation of components take place here. Ion exchange resins based on styrene divinyl benzene copolymers are used. The column is stainless steel column of length 10- 30 cm and internal diameter 4- 10 mm. The resin material is either bound to the surface of moderately large (30 – 50 μm) glass beads to form a pellicular packing, or by coating surface of a rigid microparticle to give special type of packing. 4. Stripping column: Also called suppressor column, it is the second ion exchange column which is used to selectively remove only the mobile phase ions from eluate of separating column.
  • 2. 5. Detector: Conductivity detector is detector. Apart from this, 6. Recorder: The recorder records the signa Two types of ion chromatography are currently in use: based and single-column. the conductivity of the eluting electrolyte from interfering with the measurement of analyte conductivit A. Ion Chromatography based on Suppressor It is also popularly called Double Chromatography. In this, the the injector where sample is added and into the separating column. Here, the sample component ions separate. The eluate flows in stripping column, where mobile phase ions are removed and remaining sample ions are detected conductivity detector. Working of stripping column:  If the electrolyte in the mobile phase is HCl (often used during the separation of cations), an anion exchange resin in the hydroxide form is used in the stripping column. The chloride from the dilut Conductivity detector is the most commonly used tector. Apart from this, UV detector is also used sometimes. The recorder records the signal in form of graph. Two types of ion chromatography are currently in use: suppressor column. They differ in the method used to prevent the conductivity of the eluting electrolyte from interfering with the measurement of analyte conductivities. Ion Chromatography based on Suppressor is also popularly called Double – Column hromatography. In this, the mobile phase is pumped through the injector where sample is added and into the separating column. Here, the sample component ions separate. The eluate flows in stripping column, where mobile phase ions are removed and remaining sample ions are detected conductivity detector. Working of stripping column: If the electrolyte in the mobile phase is HCl (often used during the separation of cations), an anion exchange resin in the hydroxide form is used in the stripping column. The chloride from the dilute HCl in the mobile phase exchanges 2 the most commonly used is also used sometimes. l in form of graph. suppressor- They differ in the method used to prevent the conductivity of the eluting electrolyte from interfering with the olumn Ion mobile phase is pumped through the injector where sample is added and into the separating column. Here, the sample component ions separate. The eluate flows in stripping column, where mobile phase ions are removed and remaining sample ions are detected in the If the electrolyte in the mobile phase is HCl (often used during the separation of cations), an anion exchange resin in the hydroxide form is used in the stripping column. The e HCl in the mobile phase exchanges
  • 3. 3 with hydroxide on the column and then reacts with hydronium ions (from the HCl) to form water. The net result is the removal of mobile phase ions from solution. Because the stripping column is an anion exchange column, it does not affect the separated cations in the sample.  If anions are to be separated and the mobile phase contains dilute NaOH, the anion exchange separating column is followed by a cation exchange stripping column in the hydrogen form. On the resin of stripping column, the sodium ion exchange with hydronium ion which subsequently react with hydroxide to form water and effectively remove mobile phase ions from the solution. The stripping columns get exhausted, and must be replaced or regenerated.  Recently, stripping columns have been designed which continuously refurbish the reactant ion and which consequently eliminate the need to remove the column to regenerate the reactant. Typical stripping column consist of 2 concentric compartments. The effluent from the separating column flows downward through the inner compartment where the mobile phase ions are exchanged. Simultaneously, a solution of the ions that were consumed from the resin of stripping column flows upward through the outer compartment. As the ions are used in inner compartment, they are replaced by ions from outer compartment. This device is termed as Hollow Fibre Suppressor. B. Single Column Ion Chromatography This relies upon electronic suppression of background signals from conductivity detector. The apparatus uses a pump to force the mobile phase through the separating column; no
  • 4. 4 stripping column is used. Effluent from separating column flows directly into the conductivity detector. The problem of large background signal owing to high concentration of electrolyte in the mobile phase is overcome by use of a relatively low concentration electrolyte solution with a low capacity column, and a detector with capability to suppress large signals.  Use of a single column eliminates the relatively large dead volumes often associated with use of stripping columns. It also eliminates the additional expense associated with stripping column and its regeneration. Applications Ion Chromatography analysis can be used to determine either or both qualitative and quantitative conclusions about a material's composition. Material identification is accomplished by comparing a sample's results against those of known reference materials. Quantitation, or quantification of concentrations, is achieved by comparing each anion's or cation's peak height in the chromatogram to a standard curve of known concentration. Ion Chromatography is often used as a material analytical technique in the environmental, industrial, biological, pharmaceutical, chemical and food sectors. It is commonly used in:- 1. Separation and detection of trace ionic species – Ion chromatography is the only technique that can provide quantitative analysis of anions at the ppb level and is used to detect ions in liquids. Trace analysis of common anions like F‾, Cl‾, Br‾, I‾, NO2‾, NO3‾, SO4 2-- , PO4 3-- and that of cations like Li+ , Na+ , K+ , Mg+2 , Ca+2 , Sr+2 , Ba+2 can be easily performed. 2. Food product analysis – Ionic contamination on the surfaces of wafers, chips, and packages can be detected easily. Thus, it
  • 5. 5 can be an essential tool for guaranteeing quality control. IC analysis is also a great way to test the cleanliness of a product following the manufacturing process. 3. Environmental analysis - It is used to analyse soil extracts, pond water, industrial process waste. 4. Biological application – Organic acids, amino acids and peptides can be determined by selecting proper polymeric column, mobile phase and detector. 5. Polyvalent anion such as pyrophosphate, tripolyphosphate and trimetaphosphate can be differentiated. 6. It is used to analyse multi element transition metals, at levels lower than those possible with AAS. IC analysis is a simple, fast and accurate materials analysis technique. Setting up and analyzing a single sample typically takes 1 hour with each additional sample taking 15-30 minutes to analyze. References:- 1. Introduction to Instrumental Analysis; Robert D. Braun 2. Principles of Instrumental Analysis (6th edition); Douglas A. Skoog, F James Holler, Stanley R. Crouch 3. Vogel’s textbook of Chemical Analysis (6th edition); J. Mendham, R.C. Denney, J.D. Barnes, M. Thomas, B. Sivasankas. 4. Instrumental Methods of Chemical Analysis; H. Kaur THANK YOU