Degassing instruments

The solvent reservoir is a storage container made of a saterial resistant to chemical attack by the mobile diase. In its simplest fora a glass jug, solvent bottle or Erlenmeyer flask with a cap and a flexible hose connection to the pump is adequate. The PTFE connecting hose is terminated on the solvent side with a 2 micrometer pore size filter to prevent suspended particle matter from reaching the pump. In more sophisticated instruments the solvent reservoir may also be Cjquipped for solvent degassing, as... 

Physical properties of calcined catalysts were investigated by N2 adsorption at 77 K with an AUTOSORB-l-C analyzer (Quantachrome Instruments). Before the measurements, the samples were degassed at 523 K for 5 h. Specific surface areas (,S BEX) of the samples were calculated by multiplot BET method. Total pore volume (Vtot) was calculated by the Barrett-Joyner-Halenda (BJH) method from the desorption isotherm. The average pore diameter (Dave) was then calculated by assuming cylindrical pore structure. Nonlocal density functional theory (NL-DFT) analysis was also carried out to evaluate the distribution of micro- and mesopores. 

The dilatometer is generally made of glass and is the vessel where the mercury is intruded into the sample pores. The design is dependent on the pressure source and monitoring system of the instrument. The dilatometer consists of a sample holder and a calibrated stem, which is used to measure the amount of mercury intruded into the sample. The sample in the dilatometer must be cleaned from adsorbed species by degassing the material in a vacuum [42], Most commercial instruments degas the sample in the instrument before mercury intrusion. Once the sample is degassed, the dilatometer (sample holder and stem) are filled with mercury. 

A simple system is comprised of an isocratic pump, a manual injector, a UV detector, and a strip-chart recorder. A schematic diagram of an HPLC instrument is shown in Fig. 15.4. This simple configuration is rarely used in most modern laboratories. A typical HPLC system is likely to consist of a multi-solvent pump, an autosampler, an on-line degasser, a column oven, and a UV/Vis or photodiode array detector all connected to and controlled by a data-handling workstation. Examples of modular and integrated systems are shown in Fig. 15.5. Some of the important instrumental requirements are summarized in Table 15.2. 

High Performance Liquid Chromatography (HPLC) (Chapter 30) gives an elaborate discussion of theoretical aspects. Instrumentation encompasses the various important components e.g., solvent reservoir and degassing system pressure, flow and temperature pumps and sample injection system ... 

The traditional HPLC instrument is composed of two different parts the first part separates the components of the sample and the other part accomplishes the detection of the components separated. The part of the HPLC carrying out the separation contains a column, an injection device and the eluent delivery system (pump with filters, degasser and transfer tubing, eventually a mixer for gradient elution). One or more detectors, a signal output device coupled with appropriate software, are responsible for detection and primary data evaluation. Pumps deliver the eluent or the different components of the eluent into the column with a precise, constant and reproducible flow rate. 

Figure 8.3—Schematic of a standard capillary electrophoresis instrument. The electrolyte is an aqueous ionic solution that has been filtered and degassed. It can contain several additives. There are several processes that can be used to introduce the sample into the capillary (cf. 8.4). The use of voltages above 30 kV is rare because they require special insulation. The length of the capillary (L) and the effective distance of migration (/) must not be confused since the latter is shorter by 10 or 20 cm.

Continuous analytical methods (amperometric and UV-absorption methods) are advantageous. However, sometimes only discontinuous methods (titrimetric and some photometric methods) are available due to expense. In such cases it is important to measure immediately after sampling to avoid the decay of ozone and in the case of liquid ozone to avoid degassing. Discontinuous photometric methods requiring the addition of chemicals to the sample can be converted to a continuous method by combination with flow injection analysis (FIA). This analytical technique requires instrumentation and is not easy to handle. 

Nitrogen sorption measurements were performed on a Quantachrome Autosorb 6B (Quantachrome Corporation, Boynton Beach, FL, USA). All samples were degassed at 423 K before measurement for at least 12 hours at 1 O 5 Pa. Mercury-porosimetrie has been measured on a Porosimeter 2000 (Carlo Erba Instruments) Scanning electron micrographs were recorded using a Zeiss DSM 962 (Zeiss, Oberkochen, Germany). The samples were deposited on a sample holder with an adhesive carbon foil and sputtered with gold. 

A low temperature nitrogen sorption was carried out on an automated physisorption instrument (ASAP 2000, Micromeritics Instrument Corporation). Before the measurement, the sample was degassed at 350 C for 4-5 h until the vacuum of system was better than 0.67 Pa. The data for micropore were obtained from t-plot, and those for mesopore and distribution of mesopore were calculated by BJH method (using desorption curve). The single point total pore volume at high relative pressure was taken as the total volume. 

The specific surface area of the fibers was determined using inert gas adsorption in a commercial volumetric adsorption system (Micromeritics Instrument Corp.). Krypton gas was used because of its sensitivity to the small specific surface areas of the glass fibers ( 0.2 mz/g). The fibers were degassed at 100°C to a pressure of 80mTorr before introducing the adsorbate gas into the sample chamber. Several samples were also outgassed at 80 and 200°C (to 80 mTorr) to confirm that outgassing was sufficiently complete under the standard test conditions. A standard five-point surface area determination was made for each inert gas adsorption experiment. 

All syntheses discussed below used commonly available commercial materials without further purification. Manually sampled reactions were analyzed for their density at temperatures between 20-30°C. Continuously sampled reactions were analyzed at the polymerization temperature. Temperature control in the density cell was better than 0.1°C for static samples. Temperature fluctuated more for continuously sampled reactions, sometimes rising. 1-.3°C because of the exothermic reaction continuing in the density cell. Calibration of the density cell below 95°C was accomplished using values for densities for moist air(10) and degassed, distilled water(11). For measurements above 95°C a certified viscosity standard oil (Number S-200 oil from Cannon Instrument Co.) was used. 

The analysis of aliphatic acids was performed using a P/ACE MDQ capillary electrophoresis instrument equipped with a 60 cm x 50 pm id fused silica capillary (Beckman Coulter, Fullerton, CA). The samples were filtered through a 0.45-gm cellulose acetate filter (Whatman, Maidstone, UK) prior to hydrodynamic injection at 15 psi for 4 s. The voltage was set to 20 kV at reversed polarity. The electrolyte, composed of 5.0 mM trimellitic acid, 50 mM tris(hydroxymethyl)-aminomethane, 1.0 mM tetradecyl-trimethylammoniumbromide, and 0.5 mM calcium chloride, had a pH of 9.8. Before use, it was filtered through a 0.2-gm cellulose nitrate filter and degassed withhelium. Detection was performedby indirect UV absorption at 220 nm. Succinic acid was used as internal standard. 

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