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A new hybrid monolithic column (HMC) was prepared in stainless steel chromatographic column using nitric acid as catalysis and methyltrimethoxysilane as sole precursor. The influences of the precursor ratio, catalyst concentrations, gelation temperatures on properties of HMC were investigated, and the formation mechanism of the HMC was discussed. The obtained monolithic column was characterized by (SEM) and chromatographic evaluation. The results showed that the homogeneous network skeleton structure was formed in the HMC with a controlled microchannel (10.3 μm) and nanopore (13.6 nm) and the lower shrinking ratio of HMC in comparison with silica monolithic column were obtained. Introduction The macroporous monolithic materials have used in various fields for heterogeneous catalysis and separation. The monolithic materials include polymer materials , inorganic materials [3] and organic-inorganic hybrid materials. The hybrid column research is mainly focused on capillary monolithic column. There are few reports on the application of stainless steel monolithic columns. The traditional stainless steel monolithic column has the advantages of high hardness, strong toughness, large internal diameter, uniform structure, and large column capacity. Lvs groups reported an internal surface reversed-phase monolithic column was prepared by in situ modification of hybrid monolithic columns (HMC) in a stainless steel column. The HMC was synthesized via the cocondensation of methyltrimethoxysilane (MTMS) and tetraethoxysilane (TEOS). The synthetic conditions were optimized for obtaining the uniform microchannel and the stable skeleton structure. In this work, organic-silica hybrid monolithic columns were prepared by sol-gel process in the stainless steel column with methyltrimethoxysilane as the sole precursor. The effect of reaction conditions on the properties of the HMC was studied, and the formation mechanism of the HMC was investigated. The morphology, porosity, and stability of the HMC were characterized by scanning electron microscopy and chromatographic analysis. Materials and Methods Instrumental and materials Methyltrimethoxysilane (MTMS) are obtained from Nanjing Lianye Chemical Co. Ltd. (Shanghai, China). All other chemicals are of analytical or HPLC grade and used. Double deionized water (DDW) is used in all the experiment. All sample solutions for HPLC are filtered through a 0.22 m filter to remove large polymers and particles. A Shimadzu LC-20A HPLC system (Kyoto, Japan) was used in this study, and a Venusil XBP C18 column (5 m, 250 mm × 4.6 mm, Agela, China) was used as column pressure contrast experiment. Methods Hybrid monolithic columns were prepared in stainless steel column (150 mm × 4.6 mm). 2 mL of MTMS, 0.75 mL of methanol and 0.5 mL of 1.0 mL L nitric acid were vortexed in an Erlenmeyer flask. The mixture was sonicated for 10 min and then poured into a stainless steel 223 2016 International Conference on Engineering and Advanced Technology (ICEAT-16) Advances in Engineering Research (AER), volume 82

The controllable synthesis of the hybrid silica monolithic materials with the stable skeleton macroporous structure