Solvents Mobile Phase

Electrochemical detectors sense electroreducible and electrooxidizable compounds at low concentrations. Eor these detectors to work efficiently, the mobile phase (solvent) must be conductive and not subject to electrochemical decomposition. 

The injection device is also an important component in the LC system and has been discussed elsewhere (2,18). One type of injector is analogous to sample delivery in gas chromatography, namely syringe injection through a self-sealing septum. While this injection procedure can lead to good column efficiency, it generally is pressure limited, and the septum material can be attacked by the mobile phase solvent. 

Snyder and Soczewinski created and published, at the same time, another model called the S-S model describing the adsorption chromatographic process [19,61]. This model takes into account the role of the mobile phase in the chromatographic separation of the mixture. It assumes that in the chromatographic system the whole surface of the adsorbent is covered by a monolayer of adsorbed molecules of the mobile phase and of the solute and that the molecules of the mobile phase components occupy sites of identical size. It is supposed that under chromatographic process conditions the solute concentrations are very low, and the adsorption layer consists mainly of molecules of the mobile phase solvents. According to the S-S model, intermolecular interactions are reduced in the mobile phase but only for the... 

Coupling HPLC to a mass spectrometer is far more complicated than in a GC system because of the large amount of mobile phase solvent expanding into the system (see Table 1 for expansion volumes). Typical mobile phase flow rates for HPLC are 0.5-2 mL min which translates into gas flow rates of 100-3000 mL min . ... 

The popularity of reversed-phase liquid chromatography (RPC) is easily explained by its unmatched simplicity, versatility and scope [15,22,50,52,71,149,288-290]. Neutral and ionic solutes can be separated simultaneously and the rapid equilibration of the stationary phase with changes in mobile phase composition allows gradient elution techniques to be used routinely. Secondary chemical equilibria, such as ion suppression, ion-pair formation, metal complexatlon, and micelle formation are easily exploited in RPC to optimize separation selectivity and to augment changes availaple from varying the mobile phase solvent composition. Retention in RPC, at least in the accepted ideal sense, occurs by non-specific hydrophobic interactions of the solute with the... 

Solvent strength refers to the ability of a particular mobile phase (solvent) to elute mixture components. For example, if use of a particular solvent results in short retention times for mixture components, the solvent is strong. If use of a solvent increases retention times, it is a weak solvent. 

The general flow scheme of a production liquid chromatograph is similar to that of the corresponding GC unit, shown in Figure 19.5, with four main differences. First, thermostatting requirements for the column are less strict, and may sometimes even be dispensed with. Secondly, the feed is injected as a liquid, and not vaporised. Thirdly, if the product is to be separated from the mobile-phase solvent, distillation or evaporation and solvent recycle are incorporated in the loop(28,41,42). Finally, the liquid streams are filtered to ensure column longevity, and de-aerated to prevent air bubbles forming. 

The mass spectrometer is a very sensitive and selective instrument. However, the introduction of the eluent into the vacuum chamber and the resulting significant pressure drop reduces the sensitivity. The gas exhaust power of a normal vacuum pump is some 10 ml min-1 so high capacity or turbo vacuum pumps are usually needed. The gas-phase volume corresponding to 1 ml of liquid is 176 ml for -hexane, 384 ml for ethanol, 429 ml for acetonitrile, 554 ml for methanol, and 1245 ml for water under standard conditions (0°C, 1 atmosphere). The elimination of the mobile phase solvent is therefore important, otherwise the expanding eluent will destroy the vacuum in the detector. Several methods to accomplish this have been developed. The commercialized interfaces are thermo-spray, moving-belt, electrospray ionization, ion-spray, and atmospheric pressure ionization. The influence of the eluent is very complex, and the modification of eluent components and the selection of an interface are therefore important. Micro-liquid chromatography is suitable for this detector, due to its very small flow rate (usually only 10 p min - ). 

After a plate has been exposed to the mobile-phase solvent for the required time, the compounds present can be viewed by several methods. Polynuclear aromatic hydrocarbons, other compounds with conjugated systems, and compounds containing heteroatoms (nitrogen, oxygen, or sulfur) can be viewed with long-and short-wave ultraviolet light. The unaided eye can see other material, or the plates can be developed in iodine. Iodine has an affinity for most petroleum compounds, including the saturated hydrocarbons, and stains the compounds a reddish-brown color. 

Ducey, M.W., Jr., Orendorff, C.J., Pemberton, J.E., and Sander, L.C., Structure-function relationships in high density octadecylsilane stationary phases by Raman spectroscopy 2. Effect of common mobile phase solvents, Anal. Chem., 5585, 2002... 

A method that can decrease the viscosity of the mobile phase without impacting the mobile phase solvent strength (i.e., maintaining k) would therefore decrease the analysis time linearly. The next section illustrates the diffusion coefficients and viscosities, the unique relationship between them for EEL mixtures, their solvent-strength and other important properties. 

Note After Experiment 4, one should switch the 1000 psi back-pressure device with a validated Cl8 column and adequately equilibrate the column with the appropriate mobile phase required for the subsequent experiment. The mobile phase solvents are usually percentages of methanol and water, depending on the chromatographic requirements for eluting the standard components that are used. 

The particle-beam interface is an analyte-enrichment interface in which the column effluent is pneumatically nebulized into a near atmospheric-pressure desolvation chamber connected to a momentum separator, where the high-mass analytes are preferentially directed to the MS ion source while the low-mass solvent molecules are efficiently pumped away (71, 72). With this interface, mobile phase flow rates within the range O.l-l.O ml/min can be applied (73). Since the mobile phase solvent is removed prior to introduction of the analyte molecules into the ion source, both EI and CI techniques can be used with this interface. 

HPLC mobile phase solvent (e.g., ethyl acetate, methanol, water, and/or acetone for continuous-flow FAB/LSIMS LC/MS)... 

---