Download (PDF) - Metrohm
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Metrosep A Supp 10In focus: the new Metrosep A Supp 10 IC anion columnWith the Metrosep A Supp 10, Metrohm presents a favorably-priced anion columnthat is not only suitable for the determination of the standard anions, but also forcomplex applications. The straightforward separation of sulfite and sulfate is just oneexample of the wide range of uses of this new IC column. An additional advantage ofthe Metrosep A Supp 10 is the position and small size of the system peak (carbonate),which appears clearly before the chloride peak and therefore does not interferewith the determination (see the following two chromatograms).The separation of sulfite and sulfate can be achieved evenwith the 50 mm version of the Metrosep A Supp 10.Separation column: Metrosep A Supp 10 – 50(6.1020.050)Eluent: 5.0 mmol/L Na 2CO 3,5.0 mmol/L NaHCO 3Flow rate:1.0 mL/minTemperature: 45 °CPosition of the system peak using a carbonate/hydrogencarbonate eluent.Separation column: Metrosep A Supp 10 – 100(6.1020.010)Eluent: 5.0 mmol/L Na 2CO 3,5.0 mmol/L NaHCO 3Flow rate:1.0 mL/minTemperature: 45 °CThe new Metrosep A Supp 10 is based on a high-capacity styrene/divinylbenzenecopolymer with a particle size of only 4.6 µm. Metrohm has developed and optimizedthis well-proven column design even further. The result is an extremely robustanion column with excellent separation performance and adjustable selectivity.In chromatographic work the selectivity of the column with respect to the substancesto be determined is of great importance, particularly when separating componentswith very similar properties. In contrast to HPLC, for example, in ion chroma-14 Metrohm Information Issue 2/2005
Metrosep A Supp 10tography the elution sequence is normally determined by the charge and radius ofthe ions. Only a few IC separation columns offer the possibility of altering the selectivitytowards individual ions by changing external parameters such as temperature,pH value of the eluent or the eluent composition in general.The new Metrosep anion column has this characteristic. Its separation propertiescan be altered by varying the above-mentioned parameters and thus be perfectlymatched to the particular application. The Metrosep A Supp 10 is extremely flexibleregarding alterations in selectivity. It is, for example, possible to shift the bromideand nitrate peaks widely within the chromatogram by just varying the column temperature.As shown in the following diagram, the retention times of these anionsbecome shorter as the temperature increases.Shifting of the bromide and nitrate peaks within the chromatogramby varying the column temperature.Separation column: Metrosep A Supp 10 – 100(6.1020.010)Eluent: 5.0 mmol/L Na 2CO 3,5.0 mmol/L NaHCO 3Flow rate:1.0 mL/minTemperature: 25...70 °CIf the standard eluent (5.0 mmol/L Na 2CO 3, 5.0 mmol/L NaHCO 3) is used then thephosphate peak appears unusually early in the chromatogram: Phosphate alreadyelutes between nitrite and bromide. However, by varying the eluent composition,the phosphate peak can also be shifted within the chromatogram, which allows anadaptation to the given separation problem.The tailing of bromide and nitrate caused by the column’s basic material is minimizedby increasing the temperature or by adding small amounts of perchlorate tothe eluent. Metrohm recommends either using the standard eluent and a columntemperature of 45 °C or, if no column oven is available, adding 5 µmol/L perchlorateto the eluent (see diagram below).Comparison of the standard chromatograms obtainedunder the recommended conditions.Separation column: Metrosep A Supp 10 – 100(6.1020.010)Eluent: (a) 5.0 mmol/L Na 2CO 3,5.0 mmol/L NaHCO 3(b) 5.0 mmol/L Na 2CO 3,5.0 mmol/L NaHCO 3,–5 µmol/L ClO 4Flow rate:1.0 mL/minSample:Standard containing 2 ppm chloride;5 ppm nitrite; 10 ppm phosphate,bromide, nitrate, sulfateTemperature: (a) 45 °C(b) 30 °CMetrohm Information Issue 2/2005 15
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Metrosep A Supp 10tography the elution sequence is normally determined by the charge and radius ofthe ions. Only a few IC separation columns offer the possibility of altering the selectivitytowards individual ions by changing external parameters such as temperature,pH value of the eluent or the eluent composition in general.The new Metrosep anion column has this characteristic. Its separation propertiescan be altered by varying the above-mentioned parameters and thus be perfectlymatched to the particular application. The Metrosep A Supp 10 is extremely flexibleregarding alterations in selectivity. It is, for example, possible to shift the bromideand nitrate peaks widely within the chromatogram by just varying the column temperature.As shown in the following diagram, the retention times of these anionsbecome shorter as the temperature increases.Shifting of the bromide and nitrate peaks within the chromatogramby varying the column temperature.Separation column: Metrosep A Supp 10 – 100(6.1020.010)Eluent: 5.0 mmol/L Na 2CO 3,5.0 mmol/L NaHCO 3Flow rate:1.0 mL/minTemperature: 25...70 °CIf the standard eluent (5.0 mmol/L Na 2CO 3, 5.0 mmol/L NaHCO 3) is used then thephosphate peak appears unusually early in the chromatogram: Phosphate alreadyelutes between nitrite and bromide. However, by varying the eluent composition,the phosphate peak can also be shifted within the chromatogram, which allows anadaptation to the given separation problem.The tailing of bromide and nitrate caused by the column’s basic material is minimizedby increasing the temperature or by adding small amounts of perchlorate tothe eluent. <strong>Metrohm</strong> recommends either using the standard eluent and a columntemperature of 45 °C or, if no column oven is available, adding 5 µmol/L perchlorateto the eluent (see diagram below).Comparison of the standard chromatograms obtainedunder the recommended conditions.Separation column: Metrosep A Supp 10 – 100(6.1020.010)Eluent: (a) 5.0 mmol/L Na 2CO 3,5.0 mmol/L NaHCO 3(b) 5.0 mmol/L Na 2CO 3,5.0 mmol/L NaHCO 3,–5 µmol/L ClO 4Flow rate:1.0 mL/minSample:Standard containing 2 ppm chloride;5 ppm nitrite; 10 ppm phosphate,bromide, nitrate, sulfateTemperature: (a) 45 °C(b) 30 °C<strong>Metrohm</strong> Information Issue 2/2005 15
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