Chemical preparation techniques

Historically, the target analytes in clinical mass spectrometric applications were small, volatile compounds that could be analyzed by GC-MS (see Chapter 4). With time, new chemical preparation techniques and derivatization schemes broadened the scope of these metabolites to include fatty acids, amino acids, intermediates of glucose oxidation, phospholipids, steroids, neurogenic amines, nucleic acids, etc. The molecular weights (molar masses) after derivatization were less than 1000 Da, a mass range easily within the limits of most conventional mass spectrometers. 

To convert geologic samples to a suitable form for analysis, many different chemical preparation techniques must be used. These diverse techniques all have one general feature in common any preparation procedure providing a yield of less than 100% may produce a reaction product that is isotopically different from the original specimen because the different isotopic species have different reaction rates. 

Analogously to the previous oxide sytems discussed above a great variety of chemical preparation techniques have been reported for doped and undoped ZnO. Again chemical transport is seldom used for this kind of application. 

There are ill-defined limits on EI/CI usage, based mostly on these issues of volatility and thermal stability. Sometimes these limits can be extended by preparation of a suitable chemical derivative. For example, polar carboxylic acids generally give either no or only a poor yield of molecular ions, but their conversion into methyl esters affords less polar, more volatile materials that can be examined easily by EL In the absence of an alternative method of ionization, EI/CI can still be used with clever manipulation of chemical derivatization techniques. 

Since then, TXRE has become the standard tool for surface and subsurface microanalysis [4.7-4.11]. In 1983 Becker reported the angular dependence of X-ray fluorescence intensities in the range of total reflection [4.12]. Recent demands have set the pace of further development in the field of TXRE - improved detection limits [4.13] in combination with subtle surface preparation techniques [4.14, 4.15], analyte concentrations extended even to ultratraces (pg) of light elements, e. g. A1 [4.16], spe-dation of different chemical states [4.17], and novel optical arrangements [4.18] and X-ray sources [4.19, 4.20]. 

Up to the present, a number of conventional film preparation methods like PVD, CVD, electro-chemical deposition, etc., have been reported to be used in synthesis of CNx films. Muhl et al. [57] reviewed the works performed worldwide, before the year 1998, on the methods and results of preparing carbon nitride hlms. They divided the preparation techniques into several sections including atmospheric-pressure chemical processes, ion-beam deposition, laser techniques, chemical vapor deposition, and reactive sputtering [57]. The methods used in succeeding research work basically did not... 

Lead sulfide films have been prepared by various deposition processes like vacuum evaporation and chemical bath deposition. Electrochemical preparation techniques have been used in a few instances. Pourbaix diagrams for all three aqueous lead-chalcogen Pb-S, Pb-Se, and Pb-Te systems, along with experimental results and cited discussion on the chemical etching and electrolytic polishing of lead chalcogenide crystals and films, have been presented by Robozerov et al. [201]. 

Sample preparation techniques vary depending on the analyte and the matrix. An advantage of immunoassays is that less sample preparation is often needed prior to analysis. Because the ELISA is conducted in an aqueous system, aqueous samples such as groundwater may be analyzed directly in the immunoassay or following dilution in a buffer solution. For soil, plant material or complex water samples (e.g., sewage effluent), the analyte must be extracted from the matrix. The extraction method must meet performance criteria such as recovery, reproducibility and ruggedness, and ultimately the analyte must be in a solution that is aqueous or in a water-miscible solvent. For chemical analytes such as pesticides, a simple extraction with methanol may be suitable. At the other extreme, multiple extractions, column cleanup and finally solvent exchange may be necessary to extract the analyte into a solution that is free of matrix interference. 

None of the above-mentioned ICPMS techniques can rival MC-TIMS and MC-ICPMS in terms of analytical precision, but the advantage of conventional ICPMS lies in the speed and ease with which data can be acquired. Analysis times are typically less than 10 minutes, and results can be obtained on solid, liquid or gas samples directly, without chemical preparation. Direct analysis will, however, give rise to high levels of molecular... 

MAP makes use of physical phenomena that are fundamentally different compared to those applied in current sample preparation techniques. Previously, application of microwave energy as a heat source, as opposed to a resistive source of heating, was based upon the ability to heat selectively an extractant over a matrix. The fundamental principle behind MAP is just the opposite. It is based upon the fact that different chemical substances absorb microwave energy... 

G.J. DeMenna and W.J. Edison, Novel Sample Preparation Techniques for Chemical Analysis - Microwave and Pressure, Dissolution, Chemical Analysis of Metals, ASTM STP 994 (F.T. Coyle, ed.), American Society for Testing and Materials, Philadelphia, PA (1987), p. 45. 

The understanding of phosphors and solid-state luminescence has matured to the point at which relatively rational design and preparation of new light-emitting materials can be achieved. This has resulted from advances in solid-state physics and optical spectroscopy coupled to the development of new chemical synthesis techniques. This has led to the rapid development of phosphors as important industrial/technological materials. Examples of the occurrence of phosphors in everyday use include ... 

Figure 14 shows the Cl data [13] where the events are plotted on a two-parameter display of range vs. energy. When improved chemical separation preparation techniques were used in later experiments on antarctic meteorites [14], the lower limit of Cl detection that was reached was 2 x 10 16 for 36C1/C1, with a quoted accuracy between 5 percent and 10 percent. 

The dynamic range of protein expression represents a main obstacle since abundant proteins are seldom of interest and others such as transcription factors are only present in a few copies. There is no detector that is able to visualize all proteins at the same time so that prefractionation and the investigation of subproteomes is required. In fact, pre-MS sample preparation techniques exploiting electrophoretic, chromatographic, or chemical properties of the analyte are often the bottleneck of proteomics. 

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