Development and evaluation of gold-centered monolayer protected nanoparticle stationary phases for gas chromatography

• Published in: Journal of Chromatography A 2004-12, Vol.1060 (1), p.225-236
• Main Authors: Gross, Gwen M., Grate, Jay W., Synovec, Robert E.
• Format: Article
• Language: English
• Subjects: Chromatography, Gas - methods; Gold - chemistry; Microscopy, Electron, Scanning; Microscopy, Electron, Transmission; Nanoparticles; Nanotechnology; Particle Size; Selectivity; Stationary phases, GC
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2004.07.077

The current status for the development of novel open-tubular gas chromatography (GC) stationary phases consisting of thin films of gold-centered monolayer protected nanoparticles (MPNs) is reported. Dodecanethiol MPNs, in which the monolayer is dodecanethiol linked to the gold nanoparticle, have shown great promise as a GC stationary phase with efficient columns having been produced in a variety of capillary i.d.'s with stationary phase film depths ranging from 10 to 60 nm, ±2 nm at a given film depth. Stationary phase operational parameters are discussed including maximum operating temperature, sample capacity, and stationary phase lifetime and robustness. An overview of the general method employed for column production is also included. The sample capacity was determined for a 2.5 m, 250 μm i.d. column with a stationary phase film thickness of 40 nm, at 50 °C using anisole ( k′ = 1.86) as the probe analyte. The sample capacity was experimentally found to be 2.3 ng under these conditions, similar to values reported for thicker, polymer stationary phases. The efficiency of the dodecanethiol MPN stationary phase was determined with a 100 μm i.d. capillary and found to have a reduced plate height h min value of 0.95 for octane ( k′ = 0.68). Areas of application illustrated and discussed utilizing the dodecanethiol MPN stationary phase include complementary separations such as two-dimensional GC (GC × GC), potential utilization within a model system for a micro-fabricated GC (μGC), as well as efficient single dimension high-speed separations. Initial development of polar stationary phases utilizing 4-chlorobenzenethiol MPNs and 4-(trifluoromethyl)benzenethiol MPNs is discussed. Included is a selectivity comparison of the retention behavior of the 4-chlorobenzenethiol MPN stationary phase and the dodecanethiol MPN stationary phase.