Ionic liquid mediated sol-gel sorbents
Ionic liquid (IL)-mediated sol-gel hybrid organic-inorganic materials present enormous potential for effective use in analytical microextraction. One obstacle to materializing this prospect arises from high viscosity of ILs significantly slowing down sol-gel reactions. A method was developed which provides phosphonium-based, pyridinium-based, and imidazolium-based IL-mediated advanced sol-gel organic-inorganic hybrid materials for capillary microextraction. Scanning electron microscopy results demonstrate that ILs can serve as porogenic agents in sol-gel reactions. IL-mediated sol-gel coatings prepared with silanol-terminated polymers provided up to 28 times higher extractions compared to analogous sol-gel coatings prepared without any IL in the sol solution. This study shows that IL-generated porous morphology alone is not enough to provide effective extraction media: careful choice of the organic polymer and the precursor with close sol-gel reactivity must be made to ensure effective chemical bonding of the organic polymer to the created sol-gel material to be able to provide the desired sorbent characteristics.
1. An extraction column, comprising
a column having a wall, wherein the wall has a substantially circular perimeter;
a continuous porous coating disposed on the inner face of the wall, wherein the coating is made from the steps:
obtaining a first sol-gel precursor, wherein the first precursor is hydroxy-terminated poly(dimethylsiloxane), bis[(3-methyldimethoxysilyl)-propyl]polypropylene oxide, poly(tetrahydrofuran) 250, poly(ethylene glycol) MW 600, poly(dimethylsiloxane-co-diphenylsiloxane), dihydroxyterminated, or a derivative thereof;
adding an ionic liquid to the first sol-gel precursor to form a precursor-ionic liquid mixture, wherein the ionic liquid is a phosphonium-based ionic liquid, imidazolium-based ionic liquid, pyridinium-based ionic liquid, or a combination thereof;
mixing a second sol-gel precursor into the precursor-ionic liquid mixture, wherein the second sol-gel precursor is an alkoxy compound of an element M, where M is silicon, titanium, zirconium, germanium, vanadium, zinc, tantalum, niobium, tungsten; and
mixing a catalyst into the precursor-ionic liquid mixture to form a sol-gel mixture, wherein the catalyst is an acid, base, or fluoride compound.
2. The extraction column of claim 1 , wherein the alkoxy compound is tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, tetraisopropoxysilane, or tetrabutoxysilane.
3. The extraction column of claim 1 , wherein the ionic liquid is trihexyltetradecylphosphonium tetrafluoroborate, 1-methyl-3-octylimidazolium chloride, or 4-methyl-N-butylpyridinium tetrafluoroborate.
4. The extraction column of claim 1 , wherein the catalyst is an organic acid or inorganic acid.
5. The extraction column of claim 4 , wherein the catalyst has a pKa of less than 4.
6. The extraction column of claim 5 , wherein the coating is made from the additional step of adding a solvent prior to the addition of the second sol-gel precursor, wherein the solvent is methylene chloride, methanol, ethanol, tetrahydrofuran, or a combination thereof.
7. The extraction column of claim 1 , wherein the catalyst is trifluoroacetic acid.
8. The extraction column of claim 1 , wherein the coating is made from the additional step of conditioning the extraction column, comprising the steps of
placing the extraction column in a gas chromatograph oven;
passing helium gas along the exterior surface of the coating;
elevating the temperature of the gas chromatograph oven at until the oven reaches a conditioning temperature;
where the conditioning temperature is 400° C. or below.