Hardware characterization

In order to operate a process facility in a safe and efficient manner, it is essential to be able to control the process at a desired state or sequence of states. This goal is usually achieved by implementing control strategies on a broad array of hardware and software. The state of a process is characterized by specific values for a relevant set of variables, eg, temperatures, flows, pressures, compositions, etc. Both external and internal conditions, classified as uncontrollable or controllable, affect the state. Controllable conditions may be further classified as controlled, manipulated, or not controlled. Excellent overviews of the basic concepts of process control are available (1 6). 

The simple system of hardware and software described above provides data for orientation characterization of polymer specimens. The system is used to conduct research on a wide variety of materials rather than to provide analytical results for process control. 

Within various pharmaceutical laboratories (industrial and academic), the mul-tinuclear technique of solid state NMR has primarily been applied to the study of polymorphism at the qualitative and quantitative levels. Although the technique ideally lends itself to the structure determination of drug compounds in the solid state, it is anticipated that in the future, solid state NMR will become routinely used for method development and problem solving activities in the analytical/materials science/physical pharmacy area of the pharmaceutical sciences. During the past few years, an increasing number of publications have emerged in which solid state NMR has become an invaluable technique. With the continuing development of solid state NMR pulse sequences and hardware improvements (increased sensitivity), solid state NMR will provide a wealth of information for the physical characterization of pharmaceutical solids. 

Several commercial calorimeters are available to characterize runaway reactions. These include the accelerating rate calorimeter (ARC), the reactive system screening tool (RSST), the automatic pressure-tracking adiabatic calorimeter (APTAC), and the vent sizing package (VSP). Each calorimeter has a different sample size, container design, data acquisition hardware, and data sensitivity. 

Smaller diameter probes reduce sample volumes from 500 to 600 pi typical with a 5 mm probe down to 120-160 pi with a 3 mm tube. By reducing the sample volume, the relative concentration of the sample can be correspondingly increased for non-solubility limited samples. This dramatically reduces data acquisition times when more abundant samples are available or sample quantity requirements when dealing with scarce samples. At present, the smallest commercially available NMR tubes have a diameter of 1.0 mm and allow the acquisition of heteronuclear shift correlation experiments on samples as small as 1 pg of material, for example in the case of the small drug molecule, ibu-profen [5]. In addition to conventional tube-based NMR probes, there are also a number of other types of small volume NMR probes and flow probes commercially available [6]. Here again, the primary application of these probes is the reduction of sample requirements to facilitate the structural characterization of mass limited samples. Overall, many probe options are available to optimize the NMR hardware configuration for the type and amount of sample, its solubility, the nucleus to be detected as well as the type and number of experiments to be run. 

CE has suffered from an assortment of common operator errors, which in turn have characterized the technique as not being robust. Like any analytical piece of equipment, there can be hardware and chemistry/operator issues. CE requires a keen background and user knowledge of the technique so as to avoid common problems that may initially be diagnosed as instrumental issues. For the early user of CE, the table below lists some common problems followed by their root causes and corrective actions. Following the suggested corrective actions should help the beginner get the maximum performance out of the CE instrumentation. 

It is important to note that the same ALIS hardware and software used for combinatorial library screening is applicable to characterizing protein-ligand interactions using the methods described below. 

In response to recent federal and local environmental concerns (e.g., industrial emission controls and lead phase-out) and to the growing interest of refiners in cracking residual fuels, researchers have generated new families of cracking catalysts. There is now a need to review the merits of these newly developed materials. This volume contains contributions from researchers involved in the preparation and characterization of cracking catalysts. Other important aspects of fluid catalytic cracking, such as feedstocks and process hardware effects in refining, have been intentionally omitted because of time limitations and should be treated separately in future volumes. 

In-Plane Shear Properties. The basic lamina in-plane shear stiffness and strength is characterized using a unidirectional hoop-wound (90°) 0.1 -m nominal internal diameter tube that is loaded in torsion. The test method has been standardized under the ASTM D5448 test method for in-plane shear properties of unidirectional fiber-resin composite cylinders. D5448 provides the specimen and hardware geometry necessary to conduct the test. The lamina in-plane shear curve is typically very nonlinear [51]. The test yields the lamina s in-plane shear strength, t12, in-plane shear strain at failure, y12, and in-plane chord shear modulus, G12. 

The explosive was exhaustively characterized for thermal behavior, impact sensitivity and electrostatic discharge sensitivity etc. Based on this data, CP has been described as much less sensitive to accidental initiation than primary explosives such as LA but at the same time, initiation grows rapidly to detonation when properly confined. Its performance evaluation in a test detonator or hardware indicates that CP can replace primary explosives in many hot wire detonator applications especially if safety considerations are of prime importance [239]. 

Table I. Methods and Hardware used in Characterizing the Sensitivity and Radiation Properties of the Polymers...

A large effort has been expended in order to determine accurately the structures of the ylides using a variety of techniques. Single-crystal X-ray structures of over 40 ylides have been reported. Three small ylides have been characterized in the gas phase using electron diffraction techniques. While theoretical chemists had restricted their studies to methyl-enephosphorane, recent advances in computational techniques3 and computer hardware have allowed for the geometry optimization of larger ylides. 

Since investigators continuously strive to extract increasing amounts of data from shrinking sample sizes, much commercial and academic research on NMR hardware focuses on optimizing RF probe sensitivity to allow the analysis of trace materials. Significant advances have been achieved through several distinct modifications of instrumentation. This present chapter provides a review of the characterization of nanoliter volumes via static NMR spectroscopy and emphasizes some of the more relevant developments in probe technology that have enabled such measurements. 

Materials synthesis and characterization hardware technology and methodology... 

Gather the requirements for the systems including functional (e.g. operational checks) requirements, nonfunctional (e.g., coding standards) requirements, users, company-wide regulatory compliance (e.g., Part 11 technical control), safety, process, and other applicable requirements Characterize information, assess its value to the organization, and incorporate information quality as part of the project plan Conduct a system (hardware, software, and process) risk analysis. New requirements may be found as the result of the risk analysis. Any new requirements must be documented in the requirements specification deliverable... 

---