Analytical Capabilities

Does the facility have a QC laboratory with analytical capabilities for the tolling contract Level of staffing ... 

Round robin A process involving an exchange of samples intended to transfer analytical capabilities from the client to the toller to support the toll project. 

The discovery of the phenomenon that is now known as extended X-ray absorption fine structure (EXAFS) was made in the 1920s, however, it wasn t until the 1970s that two developments set the foundation for the theory and practice of EXAFS measurements. The first was the demonstration of mathematical algorithms for the analysis of EXAFS data. The second was the advent of intense synchrotron radiation of X-ray wavelengths that immensely facilitated the acquisition of these data. During the past two decades, the use of EXAFS has become firmly established as a practical and powerfiil analytical capability for structure determination. ... 

Besides the conventional Grimm-type dc source, which has dominated the GD-OES scene for approximately 30 years, other discharge sources are well known. Among those are various boosted sources which use either an additional electrode to achieve a secondary discharge, or a magnetic field or microwave power to enhance the efficiency of excitation, and thus analytical capability none of these sources has, however, yet been applied to surface or depth-profile analysis. 

In conclusion, GD-OE S is a very versatile analytical technique which is still in a state of rapid technical development. In particular, the introduction of rf sources for non-conductive materials has opened up new areas of application. Further development of more advanced techniques, e. g. pulsed glow discharge operation combined with time-gated detection [4.217], is likely to improve the analytical capabilities of GD-OE S in the near future. 

The analytical capabilities of LIBS and LA-MIP-OES were recently noticeably improved by use of an advanced detection scheme based on an Echelle spectrometer combined with a high-sensitivity ICCD (intensified charge-coupled device) detector. 

The analytical capability of a SEC column is sometimes judged by the peak capacity, which is the number of unique species that can be resolved on any given SEC column. This number will increase with decreased particle size, increased column length, and increased pore volume. Because small particlesized medium generally has a lower pore volume and a shorter column length, peak capacities of ca. 13 for fully resolved peaks can be expected for high-resolution modern media as well as traditional media, (see Eig. 2.5). It was found that SEC columns differ widely in pore volume, which affects the effective peak capacity (Hagel, 1992). 

The analytical capability of these matrices has been demonstrated for chiral amines [12, 13]. The procedure is illustrated in Fig. 8-4 for the separation of NapEtNH " CIO . Concentrated methanol/dichloromethane solutions of the racemic mixture were placed on a column containing the chiral macrocycle host. The enantiomers of the ammonium salts were resolved chromatographically with mixtures of methanol and dichloromethane as the mobile phase. The amounts of R and S salts in each fraction were determined by polarimetry. Because the chiral supported macrocycle interacts more strongly with S salts, the R salt passes through the column first and the S salt last, as seen in Fig. 8-4. 

The combination of chromatography and mass spectrometry (MS) is a subject that has attracted much interest over the last forty years or so. The combination of gas chromatography (GC) with mass spectrometry (GC-MS) was first reported in 1958 and made available commercially in 1967. Since then, it has become increasingly utilized and is probably the most widely used hyphenated or tandem technique, as such combinations are often known. The acceptance of GC-MS as a routine technique has in no small part been due to the fact that interfaces have been available for both packed and capillary columns which allow the vast majority of compounds amenable to separation by gas chromatography to be transferred efficiently to the mass spectrometer. Compounds amenable to analysis by GC need to be both volatile, at the temperatures used to achieve separation, and thermally stable, i.e. the same requirements needed to produce mass spectra from an analyte using either electron (El) or chemical ionization (Cl) (see Chapter 3). In simple terms, therefore, virtually all compounds that pass through a GC column can be ionized and the full analytical capabilities of the mass spectrometer utilized. 

This will be discussed in greater detail in Chapter 5, but at this point it is worthwhile to consider a brief example of the analytical capabilities of MS-MS. 

The lack of a definitive explanation, however, does not affect our ability to appreciate the analytical capabilities of the technique, the HPLC characteristics that will affect the production of ions by the electrospray process and the mass spectra that may be obtained. 

Atmospheric-pressure chemical ionization (APCI) is another of the techniques in which the stream of liquid emerging from an HPLC column is dispersed into small droplets, in this case by the combination of heat and a nebulizing gas, as shown in Figure 4.21. As such, APCI shares many common features with ESI and thermospray which have been discussed previously. The differences between the techniques are the methods used for droplet generation and the mechanism of subsequent ion formation. These differences affect the analytical capabilities, in particular the range of polarity of analyte which may be ionized and the liquid flow rates that may be accommodated. 

Commercially produced amines contain Impurities from synthesis, thus rigid specifications are necessary to avoid unwanted Impurities In final products. Modern-day analytical capability permits detection of minute quantities of Impurities In almost any compound. Detection In parts per million Is routine, parts per billion Is commonplace, and parts per trillion Is attainable. The significance of Impurities In products demands careful and realistic Interpretation. Nltrosatlng species, as well as natural amines, are ubiquitous In the environment. For example, Bassow (1976) cites that about 50 ppb of nitrous oxide and nitrogen dioxide are present In the atmosphere of the cities. Microorganisms In soil and natural water convert ammonia to nitrite. With the potential for nitrosamine formation almost ever-present In the envlronmeit, other approaches to prevention should Include the use of appropriate scavengers as additives In raw materials and finished products. 

Supported platinum-palladium. This aspect of the study focused on the characterization of platinum and palladium on alumina. The analytical capability of STEM Is fully demonstrated In a problem of this type, because of the rapid manner In which crystallite composition can be analyzed. This study Is especially Interesting because of Che use of platinum and palladium combinations In automotive catalysis. 

In petrochemical and bulk commodity chemical manufacture, real-time process control has been a fact of life for many years. There is considerable understanding of processes and control of process parameters is usually maintained within tight specifications to ensure statistical process control to within six sigma, or the occurrence of one defect in a million. This has been enabled through the use of real-time analytical capability that works with programmable logic circuits to make small changes to various process inputs and physical parameters as required. 

Chemistry really should be at the heart of this revolution in materials. Chemistry is the discipline that has been associated with the study of matter that is the science of chemistry. Moreover, chemistry is also the discipline associated with the purposeful manipulation of matter at the atomic and molecular level. But, in terms of materials chemistry, the time is right because of the ability to do analysis at an unprecedented level of resolution. However, our academic system has not yet responded for our students because our laboratory and lecture subjects have not yet included the dramatic advances in analytical capability. This is an important charge to the academic community. 

Some of the challenges facing the industrial laboratory are limited resources, cost containment, productivity, timeliness of test results, chemical safety, spent chemicals disposal, technician capability, analytical capability, disappearing skills, and reliability of test results. The present R D climate in the chemical industry is one of downsizing at corporate level (lean and mean), erosion of boundaries between basic and applied science, and polymer science and analytical chemistry as Cinderella subjects. Difficult chemical analyses are often run by insufficiently skilled workers (a managerial issue). 

Laser desorption methods (such as LD-ITMS) are indicated as cost-saving real-time techniques for the near future. In a single laser shot, the LDI technique coupled with Fourier-transform mass spectrometry (FTMS) can provide detailed chemical information on the polymeric molecular structure, and is a tool for direct determination of additives and contaminants in polymers. This offers new analytical capabilities to solve problems in research, development, engineering, production, technical support, competitor product analysis, and defect analysis. Laser desorption techniques are limited to surface analysis and do not allow quantitation, but exhibit superior analyte selectivity. 

Coordinating with analytical laboratories, including sample scheduling, sample bottle acquisition reporting, chain-of-custody records, and procurement of close support laboratories or other in-field analytical capabilities... 

In recent years the interest of environmental analytical chemistry was turned to the so-called emerging contaminants or new unregulated contaminants including pharmaceuticals, endocrine disruptors, detergents, personal care products, plasticizers, flame retardants, gasoline additives, etc. These compounds are released continuously to the environment and can be found in water, sediments, soils, etc. In most of the cases they are found at trace level concentration (ng/L) therefore, powerful analytical capabilities are required for their determination. 

Sometimes for some very potent pollutants analytical methodologies provide limits of detection (LODs) higher than the concentrations that cause effects, as derived from ecotoxicological studies. Therefore efforts in the field of analytical chemistry (see Sect. 2) are focused on making available the necessary analytical capabilities to detect pollutants at the required low levels found in the environment. This was the case of pharmaceuticals, illicit drugs, perfluorinated compounds (PFCs), sunscreens/UV filters, etc. few years ago. However, this list is likely to increase with new family candidates. 

The extension of analytical mass spectrometry from electron ionization (El) to chemical ionization (Cl) and then to the ion desorption (probably more correctly ion desolvation ) techniques terminating with ES, represents not only an increase of analytical capabilities, but also a broadening of the chemical horizon for the analytical mass spectrometrist. While Cl introduced the necessity for understanding ion—molecule reactions, such as proton transfer and acidities and basicities, the desolvation techniques bring the mass spectrometrist in touch with ions in solution, ion-ligand complexes, and intermediate states of ion solvation in the gas phase. Gas-phase ion chemistry can play a key role in this new interdisciplinary integration. 

E.P. Medyantseva, E.V. Khaldeeva, and G.K. Budnikov, Immunosensors in biology and medicine analytical capabilities, problems, and prospects. J. Anal. Chem. 56, 886-900 (2001). 

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