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Immobilised chiral polymers with chemically bonded metal - useful in chromatographic separations and analyses or in nuclear resonance analysis

机译:固定的具有化学键合金属的手性聚合物-适用于色谱分离和分析或核共振分析

摘要

Metal-contg. polymers (e.g., polysiloxanes, block polymers or smectic phases) are claimed which have a chiral coordination cpd. chemically bonded to the polymer chain and which are immobilised on glass, fused silica or silica gel (silica bead) surfaces. The metal coordination cpd. is pref. (a) a transition metal cpd., esp. an Mn(II)-, Co(II)- Ni(II)-, Cu(II)- or Zn(II)-bischelate of a chiral ketone; or (b) a lanthanide metal cpd., esp. an Ey(III)-, Gd(III)- or Yb(III)-tris-chelate of a chiral diketone. USE/ADVANTAGE - The immobilised polymers can be used: (i) in the sepn. of isomers, isotopes, enantiomers or complex mixts. by chromatography using liqs. or gases in normal or supercritical state as mobile phase (e.g., SCF) or by electrokinetic methods and ultra- or hyper-filtration; and (ii) in the analysis of isotopes, isomers and esp. enantiomers by high resolution nuclear resonance (both (i) and (ii) are claimed). The chemically bonded metal-contg. polymers show better heat stability and wash-out resistance when used as stationary phases on the inside of chromatographic columns than do prior art physical mixts. They can be synthesised from silane monomers and show up to 80% immobilisation after conditioning at 180 deg.C for 24 hrs. under an iner
机译:金属接触的。要求具有手性配位cpd的聚合物(例如聚硅氧烷,嵌段聚合物或近晶相)。化学键合到聚合物链上,并固定在玻璃,熔融石英或硅胶(硅胶珠)表面上。金属配位cpd。是首选。 (a)过渡金属cpd。,尤其是手性酮的Mn(II)-,Co(II)-Ni(II)-,Cu(II)-或Zn(II)-双螯合物;或(b)镧系金属cpd。,尤其是手性二酮的Ey(III)-,Gd(III)-或Yb(III)-三螯合物。用途/优点-固定的聚合物可用于:(i)隔膜中。异构体,同位素,对映异构体或复杂混合物。通过使用liq的色谱法。或处于正常或超临界状态的气体作为流动相(例如SCF)或通过电动方法和超滤或超滤; (ii)在同位素,异构体和特别是分析中。通过高分辨率核共振的对映异构体(要求保护(i)和(ii))。化学键合金属。当用作色谱柱内部的固定相时,聚合物比现有技术的物理混合物具有更好的热稳定性和耐洗出性。它们可以由硅烷单体合成,并在180℃下老化24小时后,固定化率高达80%。在下

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