Step-growth polymerization of formaldehyde and paraformaldehyde with amine monomers for preparing monolithic capillary columns

Monolith structures are a big research area of material science with different forms and usages. Monoliths are kind a controlled structure to select some analytes which wants to separate. Monoliths are maden from different materials like silica or polymers. Polymer materials have a wide range applications. Polymers had place of metals and some other materials because of their production methods and chemical properties. Polymeric monoliths are mostly in membrane or column form. Membrane types monoliths produce for enviromental industry or health industry. Seperation could be possible for membrane types monoliths by molecularly imprinting technology. Imprinting technology is like a molding of deserved chemical with a structure of polymer. This provide lots of chemial structure can be separate with monolith structures. Just the important part is matching suitable polymer structure with a suitable mold molecule. Column type monoliths are main research area of seperation technology. After chemical processes developed amount of chemicals inside the mixtures were wanted to analyse with different ways and for analyse seperation is necessary. Chromatographic analysis are main driver of that purpose. Chromatographic analysis are combination of seperation technology with a dedector to calculate amount of analytes. Seperation should be perfect for amount analysis of chemical structures Columns are the most important part of that analysis with different structures. Polymer columns are mostly prepared with in-situ polymerization which means synthesis of polymer inseide of column. And polymer should stay inside of column with high pressures. Monomers and template molecule for imprinting are sending inside of column at same time as a homogenious solution to obtain uniform column. Template molecules can be deserved analyte for analysis or a different analyte with similar structure. For health analysis it is not possible always to find same structure with deserved molecule so similar strucure are used for molecular imprinting. Analysis for cancer diagnostics aim is a new study topic now. For that analysis phospopeptide structures are the most used template molecules. That study is a prestudy of preparing a new type phospopeptide imprinted monolithic cappilary column by polycondensation. For this purpose different amine monomers have used for copolymerization. The amine monomers which have used; biguanide, guanide, biuret and biurea. There was not any new study about this monomers forcopolymerization of formaldehyde so firstly suitable polymerization conditions should be found .Investigation of that condtions is a complicated process.Polymerizayion at high temperature is not possible for molecular imprinting because of structure of template molecules. Bulk format polymerization inside the glass vials have investigated before in-situ polymerization to find best conditions for polymerization. FT-IR analysis have maden to investigaste functional bonds. Spectra showed absorbances of expected bonds. Different temperatures, different amount of monomers and different polymerization times have tried for each monomer. BET surface area analysis have maden for some polymers. Higher amounts formaldehyde and polymerization time above 1 hour caused higher surface area. Before in-situ polymerization, wall of columns have prepared by silanization to making active for keeping polymer inside under high pressures. Mostly APTMS is used for silanization of columns. Different amount of APTMS have tried for that study. Columns have tried with HPLC pump and methanol have used as mobile phase to see silanizasyon results. And the most effective pretreatment ways found. SEM images of that columns have taken to see interaction of column and polymer. That discovered; % 50 amount of APTMS with 80 oC silanization temperature was the best one. And also solvent concentration which are used before APTMS for washing column is also has a little effect for result of silanization. Columns are suitable for high pressure liquid chromatography but molecular imprinting results should investigate more. From all that results it was clear that Phenyl-biguanide and paraformaldehyde polymer monoliths could be useful for preparing phospopeptide imprinted columns by polycondensation. But still there is a lot to do for finding useful columns.