Trennung und Bestimmung von Spaltprodukten mittels Hochdruckflüssigkeits-Chromatographie (HPLC)

Starke, Renate; Weuster, W.; Specker, H.

doi:10.1007/bf00469977

Cited by 7 publications

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“…Quantification of Lanthanides. Quantification of lanthanides in the absence of any other transition metal ions may easily be performed by ICPOES (vide supra), HPLC, ,− CE, − or isotachophoresis . Half-quantitative results may even be obtained with TLC .…”

Section: Resultsmentioning

confidence: 99%

Quantification of Lanthanides in Rocks Using Succinic Acid-Derivatized Sorbents for On-Line SPE-RP-Ion-Pair HPLC

2000

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The use of new poly(norbornene-block-7-oxanorborn-2ene-5,6-dicarboxylic acid)-coated silica-based sorbents as well as of beaded polymers based on poly(norborn-2-ene-5,6-dicarboxylic acid-co-1,4,4a,5,8,8a-hexahydro-1,4,5,8-exo-endo-dimethanonaphthalene) for the on-line preconcentration of lanthanides from rock digests and their subsequent RP-ion-pair HPLC separation is described. Block co-polymers of norborn-2-ene and 7-oxanorborn-2-ene-5,6-dicarboxylate used for coating were prepared by ring-opening metathesis polymerization (ROMP) and poly(norborn-2-ene-5,6-dicarboxylic acid-co-1,4,4a,5,8,-8a-hexahydro-1,4,5,8-exo-endo-dimethanonaphthalene)-based polymer beads were prepared by ring-opening metathesis precipitation polymerization. Both types of sorbents exhibit an extraordinarily good pH stability, are hydrophilic and therefore easily wetable by water alone, and show high extraction efficiencies for lanthanides within a pH of 3.5-5.5. The rare earth element (REE) content in the investigated rocks varied over 3 orders of magnitude (0.19-108 microg/g). REE concentrations prior to enrichment were typically in the range of 1-25 ng/mL; the total amount of each REE sorbed onto the precolumn was in the range of 8-270 ng. Extraction selectivities of the sorbent may be enhanced by adding 5-sulfosalicylic acid as a masking agent for iron and aluminum as well as methanol as an inhibitor for the precipitation of o-silicic acid. Gradient elution of the lanthanides from the precolumn and their subsequent separation on a RP-C18 column was achieved using hydroxyisobutyric acid (HIBA) and sodium octanesulfonate. Depending on the actual concentration of the lanthanides in the digests and in order to suppress interfering cations, UV detection was carried out with two different postderivatization reagents, 4-(2-pyridylazo)resorcinol (PAR) and arsenazo III. The high selectivity in enrichment as well as the complementary use of post-derivatization reagents allows the fast, quantitative, and highly reproducible quantification of REEs present in rocks by complete removal or suppression of all other interfering components. Thus, recoveries were found to be within a range of 97-103% for most REEs with relative standard deviations of 2-5%.

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Section: Resultsmentioning

confidence: 99%

Quantification of Lanthanides in Rocks Using Succinic Acid-Derivatized Sorbents for On-Line SPE-RP-Ion-Pair HPLC

2000

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Präparative Trennung von Lanthanoiden durch Hochdruck‐Flüssigkeitschromatographie (HPLC)

Weuster

Specker

1981

Angewandte Chemie

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Preparative Separation of Lanthanoids by High‐Pressure Liquid Chromatography (HPLC)

Weuster

Specker

1981

Angew. Chem. Int. Ed. Engl.

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The separation of the lanthanoids can be carried out on a preparative scale without the use of ion‐exchange, by high pressure liquid chromatography. As an example, the lanthanoids in a monazite sand (5.2 mg in total) were separated in 35 min using this method. From the 8.5 fractions collected, 4 contained pure Er, 2 pure Y, 6 pure Gd, 5 pure Sm, 10 pure Nd, 4 pure Pr, 12 pure Ce, and 18 pure La.

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Trennung und Bestimmung von Spaltprodukten mittels Hochdruckflüssigkeits-Chromatographie (HPLC)

Cited by 7 publications

References 1 publication

Quantification of Lanthanides in Rocks Using Succinic Acid-Derivatized Sorbents for On-Line SPE-RP-Ion-Pair HPLC

Quantification of Lanthanides in Rocks Using Succinic Acid-Derivatized Sorbents for On-Line SPE-RP-Ion-Pair HPLC

Präparative Trennung von Lanthanoiden durch Hochdruck‐Flüssigkeitschromatographie (HPLC)

Preparative Separation of Lanthanoids by High‐Pressure Liquid Chromatography (HPLC)

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