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Avoiding Matrix Interferences
in Ion Chromatography
Using Solid Phase Extraction
Alltech Associates, Inc.
Brandstraat 12, 9160 Lokeren
Phone: 09 340 65 65 • Web Site: www.alltechweb.com
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Types of Sample Matrix Interferences in
Ion Chromatography
• Samples with components that will damage the column.
• Samples that are too acidic for cation analysis.
• Samples that are too basic for anion analysis.
• Samples that contain high concentrations of interfering ions.
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Problems with Common Sample
Preparation Techniques
Dilution and Filtration are not suitable when:
• The analytes are present at trace levels.
• The analytes differ greatly in concentration.
• Interfering compounds and analytes are both soluble.
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Solid Phase Extraction (SPE) Cartridges for
Ion Chromatography
• Stable from pH 2 to 13.
• Low IC interference levels.
• Requires only 2 - 3mL of samples.
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The Alltech Maxi-Cleanв„ў IC Cartridge
Construction
Polypropylene Housing
Packing Material
Female Luer
Inlet
Male Luer
Outlet
Polyethylene Frits
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Types of Maxi-Cleanв„ў IC SPE Cartridges:
• Maxi-Clean™ IC-RP
• Maxi-Clean™ IC-Ag
• Maxi-Clean™ IC-Ba
• Maxi-Clean™ IC-OH
• Maxi-Clean™ IC-H
• Maxi-Clean™ IC-Na
• Maxi-Clean™ IC-Chelate
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General Procedure for Using Maxi-Cleanв„ў
IC Cartridges
1. Precondition the cartridge by passing 5-10mL of IC grade
water (use 5mL of methanol followed by 5mL of Water for
Maxi-Cleanв„ў IC-RP).
2. Load the sample at a rate of 1mL/min or less. (Adjust the
sample size to use 50% or less of the device’s capacity).
3. Discard the first 1mL eluate.
4. Collect and analyze the remaining eluate.
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Maxi-Cleanв„ў IC-RP
Product Specifications
Packing:
Particle Size:
Retains:
Applications:
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Polystyrene
300Вµm
Hydrophobic components by a
reversed-phase mechanism
Removal of hydrophobic organic
components
Maxi-Cleanв„ў IC-RP Removes Organic
Contaminants
5351
Trace Anions in Aniline
1. Chloride
2. Nitrate
3. Sulfate
Column:
Mobile Phase:
Flowrate:
Detector:
Original Sample
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After Cleanup with
Maxi-Cleanв„ў IC-RP
Anion/S, 250 x 4.1mm
4mM KHP pH 4.5
2.0mL/min
Alltech Conductivity
Average % Recovery of Ions with
Maxi-Cleanв„ў IC-RP Cartridge
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Sample Preparation by Precipitation
Maxi-CleanTM IC-Ba
• For removal of sulfate and phosphate prior to analysis
Resin-2-Ba+2 + M+2SO4-2
Resin-2-M+2 + Ba+2SO4-2
Maxi-CleanTM IC-Ag
• For removal of halides prior to analysis
Resin--Ag+ + M+X-
M=Sample cations
X= Cl-, Br-, I-
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Resin--M+ + Ag+X-
The Solubility of Barium and Silver Salts in
Aqueous Solutions
Compound
Solubility (g/100mL)
Temperature (В°C)
0.12
37.5
67.5
8.7
0.01 - 0.02
2.2 x 10-4
182
2.8 x 10-7
8.9 x 10-5
0.155
3.7 x 10-4
122
0.57
25
26
20
20
N/A
25
15.5
25
10
0
100
0
100
BaF2
BaCl2
Ba(NO2)2
Ba(NO3)2
BaHPO4
Ba2SO4
AgF
AgI
AgCl
AgNO2
AgBr
AgNO3
Ag2SO4
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Maxi-Cleanв„ў IC-Ba
Product Specifications
Packing:
Particle Size:
Capacity:
Retains:
Applications:
Strong cation exchanger in the Ba2+ form
106Вµm
0.8/2.4 meq.
Sulfate by precipitation
Removal of sulfate before the analysis of
other anions
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Maxi-Cleanв„ў IC-Ba Removes Sulfate
5348
Anions in Battery Acid
1.
2.
3.
4.
5.
6.
7.
Fluoride
Chloride
Nitrite
Bromide
Nitrate
Phosphate
Sulfate
Column:
Mobile Phase:
Flow rate:
Detector:
Original Sample
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After Cleanup with
Maxi-Cleanв„ў IC-BA
Anion/R, 250 x 4.1mm
5mM p HBA, pH 8.5
1.5mL/min.
Alltech Conductivity
Average % Recovery of Ions with
Maxi-Cleanв„ў IC-Ba Cartridge
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Maxi-Cleanв„ў IC-Ag
Product Specifications
Packing:
Particle Size:
Capacity:
Strong cation exchanger in Ag+ form
Retains:
Halides by precipitation
Removal of halides before analysis of
other anions
Applications:
106Вµm
0.8/2.4 meq.
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Maxi-Cleanв„ў IC-Ag Removes Chloride
5347
1
Nitrite in Brine
1. Chloride
2. Nitrite
2
Column:
Packing:
Mobile Phase:
Flow rate:
Detector:
Original Sample
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After Cleanup with
Maxi-Cleanв„ў
250 x 4.1mm
Anion/R
5mM p HBA, pH 8.5
1.5mL/min.
Alltech Conductivity
Average % Recovery of Ions with
Maxi-Cleanв„ў IC-Ag Cartridge
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Maxi-Cleanв„ў Cartridges to Adjust Sample pH
• Baseline disturbances and/or system peaks result when sample
pH differs from eluant pH.
• Strong anion exchange resin in the hydroxide form removes
anions and neutralizes an acidic sample.
• Cation exchange resin in the hydrogen form removes cations
and neutralizes an alkaline sample.
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Maxi-Cleanв„ў IC-OH
Product Specifications
Packing:
Particle Size:
Capacity:
Retains:
Applications:
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Strong anion exchanger in OH- form
75Вµm
0.6/1.8 meq
Anions
Adjusting sample pH before
cation analysis
Maxi-Cleanв„ў IC-OH Neutralizes Acid
5352
Monovalent Cations
in 1M Nitric Acid
1. Sodium
2. Potassium
Column:
Mobile Phase:
Flowrate:
Detector:
Original Sample
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After pH
Neutralization with
Maxi-Cleanв„ў IC-OH
Cation/R, 100 x 43.1mm
3.2mM nitric acid
1.0mL/min
Alltech Conductivity
Recovery of Ions with Maxi-Cleanв„ў IC-OH
Cartridges
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Maxi-Cleanв„ў IC-H
Product Specifications
Packing:
Particle Size:
Capacity:
Retains:
Applications:
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Strong cation exchanger in H+ form
106Вµm
0.8/2.4 meq.
Cations
Adjusting sample pH before
anion analysis
Maxi-Cleanв„ў IC-H Neutralizes Hydroxide
Trace Anions
In Caustic Solution
1.
2.
3.
4.
5.
6.
7.
8.
Original Sample
After pH
Neutralization with
Maxi-Cleanв„ў IC-H
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5349
Fluoride
Bicarbonate
Chloride
Nitrite
Bromide
Nitrate
Phosphate
Sulfate
Column:
Mobile Phase:
Flowrate:
Detector:
Anion/R, 150 x 4.1mm
5mM pHBA, pH 8.5
1.5mL/min.
Alltech Conductivity
Recovery of Ions with Maxi-Cleanв„ў IC-H
Cartridges
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Maxi-Cleanв„ў IC-Na
Product Specifications
Packing:
Particle Size:
Capacity:
Retains:
Applications:
Strong cation exchanger in Na+ form
106Вµm
0.8/2.4 meq.
Cations (exchanges cations for
sodium)
Removal of cations from sample
without changing sample pH
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Maxi-Cleanв„ў IC-Na+ Isolates Iron (III)
5813
Analysis of Iron (III)
Procedures:
1. Precondition IC-Na+ cartridge with 5mL water.
2. Load the sample to preconcentrate iron (III) present.
3. Wash with 10mL water.
4. Elute the iron (III) with 5mL of 25mM EDTA, disodium salt.
5. Analyze the eluant for iron (III).
1. Iron (III)
Column:
Alltech Universal Anion, 150 x 4.6mm
Mobile Phase: 2mM EDTA, disodium salt
Flowrate:
1.0mL/min.
Detector:
UV at 330nm
*Problem with IC-H+--> the precipitation of H4EDTA
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Maxi-Cleanв„ў IC-Chelate
Product Specifications
Packing:
Particle Size:
Capacity:
Retains:
Applications:
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Styrene-divinylbenzene copolymer
containing iminodiacetate ion
225Вµm
0.2/0.6 meq.
Polyvalent metal ions
(exchanges cations for sodium)
Removal of polyvalent metal ions
from sample
Benefits of Alltech Maxi-Cleanв„ў IC
Cartridges
• Remove interfering components from the sample matrix.
• Little or no loss of sample.
• Easy, quick, and convenient.
• Disposable.
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