Sample, preparation elemental composition

Accuracy and precision - in respect to LASMA s implementation in environmental screening and monitoring of heavy metal contamination, the requirement for measurement precision is not decisive. The accuracy depends on the quality of the reference material. Two approaches are possible - to use commercial reference samples (Atomic standard solutions of metals and powder standards) or to prepare sets of reference samples with elemental compositions, not available on the market. Another possibility is to use the chemical matrix of clearly defined soil types [Zimmermann, 1989],... 

The complex of the following destmctive and nondestmctive analytical methods was used for studying the composition of sponges inductively coupled plasma mass-spectrometry (ICP-MS), X-ray fluorescence (XRF), electron probe microanalysis (EPMA), and atomic absorption spectrometry (AAS). Techniques of sample preparation were developed for each method and their metrological characteristics were defined. Relative standard deviations for all the elements did not exceed 0.25 within detection limit. The accuracy of techniques elaborated was checked with the method of additions and control methods of analysis. 

M.15 In addition to determining elemental composition of pure unknown compounds, combustion analysis can be used to determine the purity of known compounds. A sample of 2-naphthol, C)0H7OH, which is used to prepare antioxidants to incorporate into synthetic rubber, was found to be contaminated with a small amount of LiBr. The combustion analysis of this sample gave the following results 77.48% C and 5.20% H. Assuming that the only species present are 2-naphthol and I.iBr, calculate the percentage purity by mass of the sample. 

In most alpha and mass spectrometric methods for which sample preparation is extensive and chemical recoveries can vary considerably from sample to sample, precise elemental concentrations are determined by isotope dilution methods (e.g., Faure 1977). This method is based on the determination of the isotopic composition of an element in a mixture of a known quantity of a tracer with an unknown quantity of the normal element. The tracer is a solution containing a known concentration of a particular element or elements for which isotopic composition has been changed by enrichment of one or more of its isotopes. 

Analyte dilution sacrifices sensitivity. Matrix matching can only be applied for simple matrices, but is clearly not applicable for complex matrices of varying composition. Accurate correction for matrix effect is possible only if the IS is chosen with a mass number as close as possible to that of the analyte elements). Standard addition of a known amount of the element(s) of interest is a safe method for samples of unknown composition and thus unknown matrix effect. Chemical separations avoid spectral interference and allow preconcentration of the analyte elements. Sampling and sample preparation have recently been reviewed [4]. 

An understanding of the chemical behaviour of the element can aid in the choice of appropriate techniques and methods, the application of which would not disrupt the interaction of the element with associated constituents. For example, in the study of aluminium some relevant information may include its amphoteric nature, its ability to form predominantly ionic complexes, its tendency to form hydroxides, and the stability of aluminium complexes formed with biological ligands. It is clear that in order to maintain the ionic interactions the pH, ionic strength and, of lesser importance, the ionic composition of the medium used for sample preparation should be similar to that found in vivo. In addition, highly charged surfaces should not come into contact with the sample. 

PIXE is a technique that uses a MeV proton beam to induce inner-shell electrons to be ejected from atoms in the sample. As outer-shell electrons fill the vacancies, characteristic X-rays are emitted and can be used to determine the elemental composition of a sample. Only elements heavier than fluorine can be detected due to absorption of lower-energy X-rays in the window between the sample chamber and the X-ray detector. An advantage of PIXE over electron beam techniques is that there is less charging of the sample from the incoming beam and less emission of secondary and auger electrons from the sample. Another is the speed of analysis and the fact that samples can be analyzed without special preparation. A disadvantage for cosmochemistry is that the technique is not as well quantified as electron beam techniques. PIXE has not been widely used in cosmochemistry. 

X-ray fluorescence is a spectroscopic technique of analysis, based on the fluorescence of atoms in the X-ray domain, to provide qualitative or quantitative information on the elemental composition of a sample. Excitation of the atoms is achieved by an X-ray beam or by bombardment with particles such as electrons. The universality of this phenomenon, the speed with which the measurements can be obtained and the potential to examine most materials without preparation all contribute to the success of this analytical method, which does not destroy the sample. However, the calibration procedure for X-ray fluorescence is a delicate operation. 

Typical detection limits for various elements in a biological sample are shown in Figure 13.5. Typically, PIXE has sensitivity at the parts per million level for many elements. About 25% of the applications of PIXE are in biology and medicine. The light-element matrices lead to smaller continuous backgrounds, and many trace and toxic elements are easily detected by PIXE. (There are no holes in detection limits as there are in activation analysis as all the elements emit some X-rays.) Considerable attention has been and must be devoted to the preparation of thin, representative samples. Note that PIXE is only sensitive to the elemental composition of the sample and not to the isotopic composition. 

IR data. Spectroscopic techniques were then employed to determine more about the composition of the fracture surfaces. ATR of the adhesive side of the fracture surfaces showed only slight differences in the composition of the organic phase near the interface as a result of applying primer to the adherend surface before applying the adhesive. The spectrum shown in Fig. 7C (obtained with the 45° KRS-5 reflection element) is the difference between a sample prepared from an unprimed adherend (Fig. 7B) and one prepared from a primed... 

In recent decades we have seen an explosion of various spectroscopic techniques for analyzing the elemental composition and chemical states of solid surfaces and films. This explosion has stemmed in part from the large number of surface- or interface-related problems seen in integrated-circuit performance, composite reliability, corrosion, nanostructured components, and so on. Instruments themselves can range from stand-alone units to attachments in national synchrotron facilities or multitechnique systems built around special fabrication sites. However, the basic principle of the technique, and therefore the basic concerns with sample preparation, stay the same. 

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