Polymer automation

Woodruff and co-workers introduced the expert system PAIRS [67], a program that is able to analyze IR spectra in the same manner as a spectroscopist would. Chalmers and co-workers [68] used an approach for automated interpretation of Fourier Transform Raman spectra of complex polymers. Andreev and Argirov developed the expert system EXPIRS [69] for the interpretation of IR spectra. EXPIRS provides a hierarchical organization of the characteristic groups that are recognized by peak detection in discrete ames. Penchev et al. [70] recently introduced a computer system that performs searches in spectral libraries and systematic analysis of mixture spectra. It is able to classify IR spectra with the aid of linear discriminant analysis, artificial neural networks, and the method of fe-nearest neighbors. 

CHEOPS (we tested Version 3.0.1) is a program for predicting polymer properties. It consists of two programs The analysis program allows the user to draw the repeat unit structure and will then compute a whole list of properties the synthesis program allows the user to specify a class of polymers and desired properties and will then try the various permutations of the functional groups to find ones that fit the requirements. On a Pentium Pro 200 system, the analysis computations were essentially instantaneous and the synthesis computations could take up to a few minutes. There was no automated way to transfer information between the two programs. 

Thermal analysis iavolves techniques ia which a physical property of a material is measured agaiast temperature at the same time the material is exposed to a coatroUed temperature program. A wide range of thermal analysis techniques have been developed siace the commercial development of automated thermal equipment as Hsted ia Table 1. Of these the best known and most often used for polymers are thermogravimetry (tg), differential thermal analysis (dta), differential scanning calorimetry (dsc), and dynamic mechanical analysis (dma). 

One widely used method of formation of protected compounds involves polymer-supported reagents, with the advantage of simple workup by filtration and automated syntheses, especially of polypeptides. Polymer-supported reagents are used to protect a terminal — COOH group as a polymer-bound ester (RCOOR —( ) during peptide syntheses, to protect primary alcohols as... 

Membrane processes also offer other advantages over conventional treatments. They reduce the number of unit processes in treatment systems for clarification and disinfection and increase the potential for process automation and plant compactness. Designers also thought membrane plants could be much smaller than conventional plants of the same capacity and, given their modular configuration, could be easily expanded. Additionally, these plants would produce less sludge than conventional plants because they wouldn t use such chemicals as coagulants or polymers. 

However, for quantities substantially less than this level, 7- to 10-mm i.d. analytical columns can often be used in a semipreparative mode. By repeatedly injecting 300 to 500 ju,l of up to 1% polymer, reasonable quantities of polymer can be isolated. An autosampler and automated fraction collector can be setup to perform such injections around the clock. Although the larger injections and higher concentrations will lead to a loss of resolution, in some situations the result is quite acceptable, with a considerable savings in time being realized over other means of trying to make the same fractionation. 

One widely used method involving protected compounds is solid-phase synthesis (polymer-supponed reagents). This method has the advantage of requiring only a simple workup by filtration such as in automated syntheses, especially of polypeptides, oligonucleotides, and oligosaccharides. 

Substituted 4-aryl-1 -oxo-1,2-dihydropyrazino[l, 2-i]isoquinolinium salts 402 were obtained when 3-substituted isoquinolines 401 were cleaved from a polymer by treatment 25% TFA (00MIP5). c/i-3,lla-H-3-Phenyl-1,2,3,4,11,11 fl-hexahydropyrazino[l, 2-i]isoquinoline-1,4-dione (404) formed when isoquinoline derivative 403 was cleaved from a resin with 25% TFA during an automated solid-phase synthesis (98BMCL2369). 

These conceptual goals are attained by several combinatorial methods and tools. Characteristic for combinatorial chemistry is the synthesis on solid support or by polymer-supported synthesis, allowing for much higher efficiency in library production. Synthesis can be conducted either in automated parallel synthesis or by split-and-recombine synthesis. Centerpieces of combinatorial methods further include specific analytical methods for combinatorial... 

If small or medium libraries for lead optimization are demanded and all synthetic products are to be screened individually, most often parallel synthesis is the method of choice. Parallel syntheses can be conducted in solution, on solid phase, with polymer-assisted solution phase syntheses or with a combination of several of these methods. Preferably, parallel syntheses are automated, either employing integrated synthesis robots or by automation of single steps such as washing, isolation, or identification. The latter concept often allows a more flexible and less expensive automation of parallel synthesis. 

Dynamic shear moduli are conveniently determined with automated equipment, for instance, with the torsion pendulum. However, moduli derived from dynamic tests are often higher than the results from static tests for lack of relaxation. Examples are shown in Table 3.3. Young s moduli of the polymers A, B, C, D, derived from tensile tests (frequency 0.01 Hz) are compared with shear moduli S determined with the torsion pendulum (frequency > 1 Hz). For rubberlike materials is 3S/E = 1, according to Eq. 

In addition to the insoluble polymers described above, soluble polymers, such as non-cross-linked PS and PEG have proven useful for synthetic applications. However, since synthesis on soluble supports is more difficult to automate, these polymers are not used as extensively as insoluble beads. Soluble polymers offer most of the advantages of both homogeneous-phase chemistry (lack of diffusion phenomena and easy monitoring) and solid-phase techniques (use of excess reagents and ease of isolation and purification of products). Separation of the functionalized matrix is achieved by either precipitation (solvent or heat), membrane filtration, or size-exclusion chromatography [98,99]. 

The concept of task automation for the R D worker, discussed in Chapter 1 of Computer Applications in the Polymer Laboratory, ACS Symposium Series No. 313, is well on the way to being realized through the proliferation of powerful, low-cost universal work stations coupled to... 

The computer has become an accepted part of our daily lives. Computer applications in applied polymer science now are focussing on modelling, simulation, robotics, and expert systems rather than on the traditional subject of laboratory instrument automation and data reduction. The availability of inexpensive computing power and of package software for many applications has allowed the scientist to develop sophisticated applications in many areas without the need for extensive program development. 

Koehler, M. E., "Laboratory Automation A New Perspective", In Computer Applications in Applied Polymer Science, Provder, T., Ed. ACS Symposium Series No. 313, American Chemical Society Washington, DC, 1986 pp 2-5. 

An Automated Ferranti-Shirley Viscometer," A.F. Kah, M.E. Koehler, T.F. Niemann, T. Provder, and R.R. Eley, in Computer Applications in Applied Polymer Science. ACS Symposium Series 197, 1982. 

The labor-intensive nature of polymer tensile and flexure tests makes them logical candidates for automation. We have developed a fully automated instrument for performing these tests on rigid materials. The instrument is comprised of an Instron universal tester, a Zymark laboratory robot, a Digital Equipment Corporation minicomputer, and custom-made accessories to manipulate the specimens and measure their dimensions automatically. Our system allows us to determine the tensile or flexural properties of over one hundred specimens without human intervention, and it has significantly improved the productivity of our laboratory. This paper describes the structure and performance of our system, and it compares the relative costs of manual versus automated testing. 

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