a Grace company Avoiding Matrix Interferences in Ion Chromatography Using Solid Phase Extraction Alltech Associates, Inc. Brandstraat 12, 9160 Lokeren Phone: Web Site:

a Grace company 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.

a Grace company 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.

a Grace company Solid Phase Extraction (SPE) Cartridges for Ion Chromatography Stable from pH 2 to 13. Low IC interference levels. Requires only 2 - 3mL of samples.

a Grace company The Alltech Maxi-Clean IC Cartridge Construction Polypropylene Housing Female Luer Inlet Polyethylene Frits Packing Material Male Luer Outlet

a Grace company Types of Maxi-Clean 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

a Grace company General Procedure for Using Maxi-Clean 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-Clean 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 devices capacity). 3.Discard the first 1mL eluate. 4.Collect and analyze the remaining eluate.

a Grace company Product Specifications Maxi-Clean IC-RP Packing:Polystyrene Particle Size:300µm Retains:Hydrophobic components by a reversed-phase mechanism Applications:Removal of hydrophobic organic components

a Grace company Maxi-Clean IC-RP Removes Organic Contaminants Trace Anions in Aniline Original Sample After Cleanup with Maxi-Clean IC-RP Column: Anion/S, 250 x 4.1mm Mobile Phase: 4mM KHP pH 4.5 Flowrate: 2.0mL/min Detector: Alltech Conductivity 1. Chloride 2. Nitrate 3. Sulfate 5351

a Grace company Average % Recovery of Ions with Maxi-Clean IC-RP Cartridge

a Grace company Sample Preparation by Precipitation Maxi-Clean TM IC-Ba For removal of sulfate and phosphate prior to analysis Resin -2 -Ba +2 + M +2 SO 4 -2 Resin -2 -M +2 + Ba +2 SO 4 -2 Maxi-Clean TM IC-Ag For removal of halides prior to analysis Resin - -Ag + + M + X - Resin - -M + + Ag + X - M=Sample cations X= Cl -, Br -, I -

a Grace company The Solubility of Barium and Silver Salts in Aqueous Solutions CompoundSolubility (g/100mL)Temperature (°C) BaF BaCl Ba(NO 2 ) Ba(NO 3 ) BaHPO N/A Ba 2 SO x AgF AgI2.8 x AgCl8.9 x AgNO AgBr3.7 x AgNO Ag 2 SO

a Grace company Maxi-Clean IC-Ba Product Specifications Packing:Strong cation exchanger in the Ba 2+ form Particle Size:106µm Capacity:0.8/2.4 meq. Retains:Sulfate by precipitation Applications:Removal of sulfate before the analysis of other anions

a Grace company Maxi-Clean IC-Ba Removes Sulfate Original Sample After Cleanup with Maxi-Clean IC-BA Column:Anion/R, 250 x 4.1mm Mobile Phase:5mM p HBA, pH 8.5 Flow rate:1.5mL/min. Detector:Alltech Conductivity 5348 Anions in Battery Acid 1. Fluoride 2. Chloride 3. Nitrite 4. Bromide 5. Nitrate 6. Phosphate 7. Sulfate

a Grace company Average % Recovery of Ions with Maxi-Clean IC-Ba Cartridge

a Grace company Maxi-Clean IC-Ag Product Specifications Packing: Strong cation exchanger in Ag + form Particle Size:106µm Capacity:0.8/2.4 meq. Retains: Halides by precipitation Applications: Removal of halides before analysis of other anions

a Grace company 5347 Maxi-Clean IC-Ag Removes Chloride Column:250 x 4.1mm Packing:Anion/R Mobile Phase:5mM p HBA, pH 8.5 Flow rate:1.5mL/min. Detector:Alltech Conductivity Original Sample After Cleanup with Maxi-Clean Nitrite in Brine 1. Chloride 2. Nitrite 1 2

a Grace company Average % Recovery of Ions with Maxi-Clean IC-Ag Cartridge

a Grace company Maxi-Clean 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.

a Grace company Maxi-Clean IC-OH Product Specifications Packing: Strong anion exchanger in OH - form Particle Size: 75µm Capacity: 0.6/1.8 meq Retains: Anions Applications: Adjusting sample pH before cation analysis

a Grace company 5352 Maxi-Clean IC-OH Neutralizes Acid Column:Cation/R, 100 x 43.1mm Mobile Phase:3.2mM nitric acid Flowrate:1.0mL/min Detector:Alltech Conductivity Original Sample After pH Neutralization with Maxi-Clean IC-OH Monovalent Cations in 1M Nitric Acid 1. Sodium 2. Potassium

a Grace company Recovery of Ions with Maxi-Clean IC-OH Cartridges

a Grace company Maxi-Clean IC-H Product Specifications Packing: Strong cation exchanger in H + form Particle Size: 106µm Capacity: 0.8/2.4 meq. Retains: Cations Applications: Adjusting sample pH before anion analysis

a Grace company 5349 Maxi-Clean IC-H Neutralizes Hydroxide Column:Anion/R, 150 x 4.1mm Mobile Phase:5mM pHBA, pH 8.5 Flowrate:1.5mL/min. Detector:Alltech Conductivity Original Sample After pH Neutralization with Maxi-Clean IC-H Trace Anions In Caustic Solution 1. Fluoride 2. Bicarbonate 3. Chloride 4. Nitrite 5. Bromide 6. Nitrate 7. Phosphate 8. Sulfate

a Grace company Recovery of Ions with Maxi-Clean IC-H Cartridges

a Grace company Maxi-Clean IC-Na Product Specifications Packing: Strong cation exchanger in Na + form Particle Size: 106µm Capacity: 0.8/2.4 meq. Retains: Cations (exchanges cations for sodium) Applications: Removal of cations from sample without changing sample pH

a Grace company 5813 Maxi-Clean IC-Na + Isolates 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 H 4 EDTA 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)

a Grace company Maxi-Clean IC-Chelate Product Specifications Packing: Styrene-divinylbenzene copolymer containing iminodiacetate ion Particle Size: 225µm Capacity: 0.2/0.6 meq. Retains: Polyvalent metal ions (exchanges cations for sodium) Applications: Removal of polyvalent metal ions from sample

a Grace company Benefits of Alltech Maxi-Clean IC Cartridges Remove interfering components from the sample matrix. Little or no loss of sample. Easy, quick, and convenient. Disposable.