Packing materials, costs

When low boiling ingredients such as ethylene glycol are used, a special provision in the form of a partial condenser is needed to return them to the reactor. Otherwise, not only is the balance of the reactants upset and the raw material cost of the resin increased, but also they become part of the pollutant in the waste water and incur additional water treatment costs. Usually, a vertical reflux condenser or a packed column is used as the partial condenser, which is installed between the reactor and the overhead total condenser, as shown in Figure 3. The temperature in the partial condenser is monitored and maintained to effect a fractionation between water, which is to pass through, and the glycol or other materials, which are to be condensed and returned to the reactor. If the fractionation is poor, and water vapor is also condensed and returned, the reaction is retarded and there is a loss of productivity. As the reaction proceeds toward completion, water evolution slows down, and most of the glycol has combined into the resin stmcture. The temperature in the partial condenser may then be raised to faciUtate the removal of water vapor. 

Colin2 came to a similar conclusion in a review of this subject area. He emphasizes that it is important to distinguish early on the difference between purification costs (e.g., equipment, solvents, packing material) and production costs (purification and cost of making the crude sample). He noted that a crude sample resulting from a multistep synthesis can itself be very expensive and will enable one to tolerate much higher purification costs. This is indeed the case in purification of synthetic oligonucleotides, where even very steep purification costs are a fraction of the costs of even the raw materials required for synthesis, let alone the total cost of synthesis. 

Monolithic column — The trend to use shorter columns in liquid chromatography means that the resultant lower separation efficiency is of concern. One way to improve HPLC separation efficiency on a shorter column is to reduce the size of the packing material, but at the cost of increased backpressure. Another approach to improve performance is increasing permeability with a monolithic column. Such a column consists of one solid piece with interconnected skeletons and flow paths. The single silica rod has abimodal pore structure with macropores for through-pore flow and mesopores for nanopores within a silica rod8182 (Figure 12.1). 

Fast gradient separations can be achieved, at a cost of decreased peak capacity, by using short packed columns and simultaneously decreasing the particle size, dp, of the packing material to keep a constant ratio of the column length to the mean particle diameter, lidp, e.g., with a 3 cm column packed with a 3 [im material, or even a 1 cm, 1 pm column for very fast separation instead of a conventional 5 cm, 5 pm or a 10 cm, 10 pm column. At constant Vq/V , and Hdp ratios, the... 

Many packing materials are available only in pre-packed columns and, in this respect, packing can be avoided altogether. However, the cost of pre-packed columns is extremely high, and this is one of the most undesirable features of HPLC at present. 

In recent years h.p.l.c. has become a valuable chromatographic tool for analytical and preparative scale work. In this latter area the separation of isomers (structural, diastereoisomeric, and enantiomeric) has been possible by the selection of appropriate column packing material and solvent systems. However, the equipment, operating costs, and column packing materials are more expensive than those in t.l.c., g.l.c. and conventional liquid-solid column chromatography. 

Due to the high sensitivity it is favorably to couple a nanoHPLC to an ESI-source. As mass spectrometers are concentration dependent detectors, the sensitivity of an instrumental setup is mostly determined by the peptide concentration of the eluate but not by the peptide amount. Thus a nanocolumn with a flow rate of 300 nL/min provides an about thousand times higher sensitivity than a microbore column with a flow rate of 300 (xL/min. As an alternative to buying a nanoHPLC system it is also possible to use a relatively inexpensive flow splitter after the pump and before the injection valve and the column. Thereby the flow rate can be reduced to use a capillary column (flow rate 4 (xL/min) on an analytical HPLC system or a nanocolumn on a capillary HPLC system. Instead of a flow-splitter it is preferred to couple a nanoHPLC to an ESI-source. Thereby, the flow rate is split according to the column backpressure, i.e., mostly the column volumes if the same packing materials are used. However, these low-cost setups are less reliable than a nanoHPLC and the reproducibility is worse. 

Tray costs are shown in Fig. 16-26 for conventional installations. The approximate prices for various types and sizes of the most common industrial packings are indicated in Table 7. Costs for other packing materials are listed in Table 8. For rough estimates, the cost for a distributor plate in a packed tower can be assumed to be the same as that for one bubble-cap tray. 

---