Stationary phases molecular sieves

In gas-solid chromatography (GSC) the stationary phase is a solid adsorbent, such as silica or alumina. The associated virtues associated therewith, namely, cheapness and longevity, are insufficiently appreciated. The disadvantages, surface heterogeneity and irreproducibility, may be overcome by surface modification or coating with small amounts of liquid to reduce heterogeneity and improve reproducibility 4,15). Porous polymers, for example polystyrene and divinyl benzene, are also available. Molecular sieves, discussed in Chapter 17, are used mainly to separate permanent gases. 

This separation method is based on the molecular size of analytes. Analytes pass through porous stationary phase materials having different pore sizes, and molecular interactions between analytes and the stationary phase surface must be eliminated. A very strong solvent is therefore required in this system. This system is also called gel filtration liquid chromatography, gel-permeation liquid chromatography, or molecular sieve chromatography. This system is used to... 

Molecular exclusion chromatography. The stationary phase in molecular exclusion chromatography is a material containing pores, the dimensions of which are chosen to separate the solutes present in the sample based on their molecular size. This can be perceived as a molecular sieve allowing selective permeation. This technique is known as gel filtration or gel permeation, depending on the nature of the mobile phase, which is either aqueous or organic. The distribution coefficient in this technique is called the coefficient of diffusion. 

Conventional high pressure NICI spectra were obtained using a Hewlett-Packard 5985B quadrupole GC/MS, as described previously (1). Methane was used as the Cl reagent gas and was maintained in the source at 0.2-0.4 torr as measured through the direct inlet with a thermocouple gauge. A 200 eV electron beam was used to ionize the Cl gas, and the entire source was maintained at a temperature of 200° C. Samples were introduced into the spectrometer via the gas chromatograph which was equipped with a 25 meter fused silica capillary column directly interfaced with the ion source. For all experiments, a column coated with bonded 5% methyl phenyl silicon stationary phase, (Quadrex, Inc.) was used and helium was employed as the carrier gas at a head pressure of 20 lbs. Molecular sieve/silica gel traps were used to remove water and impurities from the carrier gas. 

The above phases represent the most common phases used in solving nearly all of the frequently encountered application problems. There are many other stationary phases which are produced to tune the phase polarity for specific applications. In addition to these phases, there are liquid crystalline, chiral, cyclodextrin, polymers such as polystyrene, divinylben-zene, molecular sieves, and alumina, which are designed for specific separation problems. The chemistry of fused silica deactivation and stationary-phase application, bonding, and cross-linking has been reviewed in detail [3,4]. 

Competition between liquid mobile phase and solid adsorbent 1 Competition between liquid mobile phase and liquid stationary phase 1 Molecular sieving 1 Lock and Key mechanism 1 Competition between liquid mobile phase and ionic stationary phase... 

Name Gas-liquid (GLC GC) capillary gas (CGC) Stationary phase Solid (absorbent or molecular sieve) Configuration Column Name Gas-solid (GSC)... 

In gas-solid chromatography, the stationary phase is an active solid. These solids may be inorganic materials, e.g. synthetic zeolite molecular sieve, carbon molecular sieve, silica gel, or graphitised carbon, or they may be oiganic polymers. They are generally used for the separation of low molecular weight materials, i.e. gases and liquids. 

The reactor was fed with 1.6 Nl/min of 1000, 2000 and 4000 ppm of methane in air. The mixtures were obtained by mixing N-50 synthetic air and 2.5 % (vol.) CH4 in N-50 synthetic air (Air Products). 40 ppm of SO2 (from a cylinder of 370 ppmV SO2 in N-50 synthetic air. Air Products) were added when the effect of sulphur on the catalysts activity was studied. Flow rates were controlled by calibrated mass flow controllers (Brooks 5850 TR). Exhaust gas was analysed by gas chromatography (Hewlett Packard HP 5890 Series II). Methane in the inlet and outlet streams was analysed using a 30 m fused silica capillary column with apolar stationary phase SE-30, and a FID detector. CO and CO2 were analysed using a HayeSep N 80/100 and a molecular sieve 45/60 columns connected in series, and a TCD detector. Neither CO, nor partial oxidation were detected in any experiment, the carbon mass balance fitting in all the cases within 2%. Methane conversions were calculated both from outlet methane and CO2 concentrations, being both values very close in all the cases. Methane (2000 ppmV) and SO2 (40 ppmV) concentrations have been selected because they are representative of industrial emissions, such as coke oven emissions. 

These polychelates are used as stationary phase in molecular sieve GC to separate gas mixtures of rare gases. 

Even when the stationary phase is of the same composition as the mobile phase, the porous support for the immobilized fluid is customarily referred to as stationary phase. Porath and Flodin " used cross-linked dextrans as a molecular sieve for carrying out separations, and this material has been unusually effective. It... 

Molecular sieve zeolites constitute a class of stationary phase that combines exclusion with specific adsorption properties. These materials, which are crystalline aluminum silicates (commonly sodium or calcium aluminum silicates), have rigid, highly uniform three-dimensional porous structures containing up to 0.5ml/g of free pore volume, resulting when water of crystallization is removed by heating. Although munerous natural zeolites are known, most practical work is done with... 

Commonly used stationary phases in gas-solid chromatography are activated charcoal, silica gel, Fluorosil, and molecular sieves 5A, X, or Y (synthetic zeolites). These are useful to temperatures as high as 500°C. At high temperatures the... 

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