Continuous-flow systems sizing

The requirements for solid-phase synthesis are diverse. The support must be insoluble, in the form of beads of sufficient size to allow quick removal of solvent by filtration, and stable to agitation and inert to all the chemistry and solvents employed. For continuous-flow systems, the beads also must be noncompressible. Reactions with functional groups on beads imply reaction on the inside of the beads as well as on the surface. Thus, it is imperative that there be easy diffusion of reagents inside the swollen beads and that the reaction sites be accessible. Accessibility is facilitated by a polymer matrix that is not dense and not highly functionalized. A matrix of defined constitution allows for better control of the chemistry. Easier reaction is favored by a spacer that separates the matrix from the reaction sites. Coupling requires an environment of intermediate polarity such as that provided by dichloromethane or dimethylformamide benzene is unsuitable as solvent. 

Between the early 1950s, when the dual viscous-flow mass spectrometer was introduced by Nier and the mid 1980s only minor modifications have been made on the hardware of commercial mass spectrometers. Special efforts have been undertaken in the past years to reduce the sample size for isotope measurements. This has led to a modification of the classic dual inlet technique to the continuous-flow isotope ratio monitoring mass spectrometer in which the gas to be analyzed is a trace gas in a stream of carrier gas, which achieves viscous-flow conditions. Today, the majority of gas mass spectrometers are sold with the continuous flow system, instead of the dual inlet system. 

This may be either a continuous process, used when the sample size is relatively large (1 ml or more), or a discrete process, used with samples of less than 20 /il. Continuous-flow systems are simpler to use and more precise, but they are less sensitive. They employ a nebulizer in association with a flame or gas plasma, and either a rotating electrode (Rotrode) or drip-feed to the electrode with the arc or spark. The pneumatic nebulizer has an efficiency of 5-10% and generates an inhomogeneous aerosol. Efiiciency can be improved by proper design of the nebulizer and spray chamber (N4), by use of heated nebulizer gas (R6) or ultrasonic devices (S23). The maximum improvement is a 5- to 10-fold increase in sensitivity. There is also an increase in the complexity and cost of the instrument which usually offsets these benefits. The effect... 

A perfect mixer has an exponential distribution of residence times W t) = exp(—r/7). Can any other continuous flow system have this distribution Perhaps, surprisingly, the answer to this question is a definite yes. To construct an example, suppose the feed to a reactor is encapsulated. The size of the capsules is not critical. They must be large enough to contain many molecules but must remain small compared to the dimensions of the reactor. Imagine them as small ping-pong balls as in Figure 15.1 la. 

Latex particle size is a key parameter for emulsion polymerization, with strong impact on the final properties of the polymers synthesized and, in general, on the polymerization kinetics in heterogeneous systems. An experimental methodology which combines a continuous-flow system and an ESR time sweep experiment was extended by Parker et al. [144] to study the effects of varying latex particle size on polymerization kinetics andradical distribution in the case of MMA emulsion... 

CO oxidation was carried out in a fixed-bed-type apparatus with a continuous flow system at atmospheric pressure. The thermal stability of the supports was determined by the BET method and X-ray diffraction (XRD). The crystallite size of cerium oxide was measured by XRD using the small-angle-scattering method. Lattice parameters were also measured by XRD. The supports were also analyzed by X-ray photoelectrons using VG ESCA Lab MK II. Platinum dispersion was measured with a Quatasorb, which uses the CO adsorption method. 

Because gravity is too weak to be used for removal of cakes in a gravity side filter (2), continuously operated gravity side filters are not practicable but an intermittent flow system is feasible in this arrangement the cake is first formed in a conventional way and the feed is then stopped to allow gravity removal of the cake. A system of pressure filtration of particles from 2.5 to 5 p.m in size, in neutralized acid mine drainage water, has been described (21). The filtration was in vertical permeable hoses, and a pressure shock associated with relaxing the hose pressure was used to aid the cake removal. 

The required orifice continuous flow capacity is determined at steam chest pressure to condensate system pressure at a flow 6 to 8 times design. If designed for normal flow the trap would have to be open 100% of the time. Then, as stated above, a body size is selected that can contain the required orifice (not be above the stated... 

As the flow rate and quantity of liquor are the most important controllable variables in developing design data, a feed pump suitable for accurate and continuous flow is required. Depending on the size of the pilot column system, the use of peristaltic, diaphragm, piston-type or centrifugal pumps are recommended. The feed pump should be used in combination with a volumetric or gravimetric flow control... 

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