QUADRASORB™ SI; Surface Area and Pore Size Analyzer - QUANTACHROME INSTRUMENTS - #5

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A section of one greatly enlarged particle of a solid. 1 The monolayer of adsorbed molecules; typically 15 - 20% saturation. 2 The multilayer capillary condensation stage approximately 70% saturation. 3 Total pore volume filling; approximately 100% saturation. 4 Dimensions: Weight: Electrical: Environmental: Physical Specifications Height: 29.0 inches (73.6 cm) Height Open: 44.0 inches (111.6 cm) Width: 25.25 inches (63.7 cm) Depth: 21.0 inches (53.3 cm) Depth Open: 26.2 inches (66.5 cm) 60 kg (132 lbs.) 100 - 240 VAC, 50/60 Hz 10 - 38°C operating range at 90% maximum relative humidity Accessories Regulator Assembly Proper Quadrasorb functioning is assured when high-quality gas regulators are used. Quantachrome supplies complete assemblies which include two-stage regulators with dual gauges, cylinder connector, isolation valve and 1/8" gas line connector. The regulators feature stainless steel, non-venting diaphragms and the appropriate CGA fitting for specific gases. Different assemblies are available for nitrogen (and other inerts including helium), hydrogen, carbon monoxide, oxidizing gases etc. Vacuum Pump (standard applications). All vacuum-volumetric gas sorption analyzers require a good vacuum pump and the Quadrasorb- SI is no exception. The pump shall have the capability to pull an ultimate vacuum of 10 millitorr or below. Quantachrome can supply the correctly sized pump complete with oil, hoses and fittings. You are not required to purchase the necessary vacuum pump from Quantachrome, but if you do the entire system will have been qualified in our factory as a set, ensuring consistent performance. Vacuum Pumps (krypton/micropore model). Low pressure applications require a deeper vacuum that can only be achieved by a turbomolecular pump. The turbo pump is included, and the correct backing pump can be supplied by Quantachrome either as a rotary oil pump or as an oil-free, dry diaphragm (membrane) pump. Storage Dewars For the convenience of having larger quantities of liquefied gases on hand, Quantachrome offers storage dewars in sizes ranging from 5 liters to 30 liters, plus a transfer device and trolley for the largest size. The Gas Sorption Process Before performing gas sorption experiments, solid surfaces must be freed from contaminants such as water and oils. Surface cleaning (degassing) is most often carried out by placing a sample of the solid in a glass cell and heating it under vacuum or flowing gas. Figure 1 illustrates how a solid particle containing cracks, orifices and pores of different sizes and shapes might look after pretreatment. Once clean, the sample is brought to a constant temperature by means of an external bath. Then, small amounts of a gas (the adsorbate) are admitted in steps into the evacuated sample chamber. Gas molecules that stick to the surface of the solid (adsorbent) are said to be adsorbed and tend to form a thin layer that covers the entire adsorbent surface. Based on the well-known Brunauer, Emmett and Teller (B.E.T.) theory, one can estimate the number of molecules required to cover the adsorbent surface with a monolayer of adsorbed molecules, Nm (Figure 2). Multiplying Nm by the cross-sectional area of an adsorbate molecule yields the sample’s surface area. Continued addition of gas molecules beyond monolayer formation leads to the gradual stacking of multiple layers (multilayers). The formation occurs in parallel to capillary condensation (Figure 3). The latter process is approximately described by the Kelvin equation, which relates equilibrium gas pressure to the size of capillaries capable of condensing gas within them. As the equilibrium gas pressure approaches saturation, the pores largely completely fill with adsorbate (Figure 4). Knowing the density of the adsorbate, one can calculate the volume it occupies and, consequently, the total pore volume of the sample. If at this stage one reverses the adsorption process by withdrawing known amounts of gas from the system in steps, desorption isotherms are generated. The resulting hysteresis leads to isotherm shapes that can be mechanistically related to those expected from particular poreshapes. Older calculation methods such as the one by Barrett, Joyner and Halenda (B.J.H.) allow the computation of pore sizes from equilibrium gas pressures. One can therefore take experimental curves (isotherms) of adsorbed gas volumes versus relative pressures and convert them to cumulative or differential pore size distributions. Modern pore size models are based on Non-local Density Functional Theory (DFT)- a statistical mechanics approach that allows one to describe the sorption of gas molecules in nanoporous materials at a molecular level. Hence, the application of such microscopic methods produces the most accurate surface area and pore size results. QUADRASORB™ SI

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