Reaction detector with three dimensional coiled open tubes in HPLC

Summary A reaction detector with non-segmented flow in open tubes as reaction track is described. To minimize peak broadening the open tubes are arranged in a three dimensional coiled structure by knitting. At low volume flow rates the h-values in these open tubes are independent of flow rate and are significantly lower than predicted by theory. The applicability of this reactor for classical colorimetric detection with corrosive reagents is shown.Part of Ph. D. Thesis, Saarbrücken 1976     

Differences in preparative loadability between the charged and uncharged forms of ionizable compounds

Ionizable compounds experience a drastic difference in preparative loadability as a function of pH. It can be shown that the preparative loadability of a compound in the ionic form is by a factor of 20 or more inferior to the loadability of the same compound in the unionized form. In this paper, we demonstrate the reason for this behavior, and show practical applications of the principle.     

Selectivity in reversed-phase separations Influence of the stationary phase

The selectivity difference between 15 different stationary phases was measured using a large number of analytes at 2 or 3 different pH values (3, 7 and 10) with acetonitrile and methanol as the mobile phase modifiers. The packings discussed include standard C(8) and C(18) packings, packings with embedded polar groups, a phenyl packing, a pentafluoro-phenyl packing, an adamantylethyl packing and others. The major selectivity differences observed are discussed in detail. Specific effects such as pi-pi interactions on phenyl packings or hydrogen-bond interactions on phases with embedded polar groups are confirmed.     

A detailed discussion of the influence of the amount of deposited polymer on the retention properties of polymer-coated silicas

Problems of the modification of the surface of micro-spherical silica gel with layers of polymer and the influence of the quantity of the coated polymer on the chromatographic properties of the resulting sorbents have been considered. The polymer modification of the surface of wide-pore micro-spherical silica gel obtained by means of hydrothermal treatment of the meso-porous silica gel under autoclave conditions is described. The polymer layer itself is formed by an octadecylmethacrylate-methylmethacrylate co-polymer. As a result, packings for RP-HPLC were obtained. An increase of the capacity factor (k) has been observed with an increase of the quantity of the polymer deposited during the polymer modification process. The indicated phenomenon depends on the increase of the number of C18 groups in the packing.     

Determining temperature in a magic-angle spinning probe using the temperature dependence of the isotropic chemical shift of lead nitrate

The calibration of temperature in a magic-angle spinning probe with lead nitrate is discussed. The effects of rotation frequency on temperature are demonstrated.     

Peak capacity in gradient reversed-phase liquid chromatography of biopolymers. Theoretical and practical implications for the separation of oligonucleotides

Reversed-phase ultra-performance liquid chromatography was used for biopolymer separations in isocratic and gradient mode. The gradient elution mode was employed to estimate the optimal mobile phase flow rate to obtain the best column efficiency and the peak capacity for three classes of analytes: peptides, oligonucleotides and proteins. The results indicate that the flow rate of the Van Deemter optimum for 2.1 mm I.D. columns packed with a porous 1.7 microm C18 sorbent is below 0.2 mL/min for our analytes. However, the maximum peak capacity is achieved at flow rates between 0.15 and 1.0 mL/min, depending on the molecular weight of the analyte. The isocratic separation mode was utilized to measure the dependence of the retention factor on the mobile phase composition. Constants derived from isocratic experiments were utilized in a mathematical model based on gradient theory. Column peak capacity was predicted as a function of flow rate, gradient slope and column length. Predicted peak capacity trends were compared to experimental results.