Multielement

Almost any type of analyzer could be used to separate isotopes, so their ratios of abundances can be measured. In practice, the type of analyzer employed will depend on the resolution needed to differentiate among a range of isotopes. When the isotopes are locked into multielement ions, it becomes difficult to separate all of the possible isotopes. For example, an ion of composition CgHijOj will actually consist of many compositions if all of the isotopes ( C, C, H, H, 0, O, and 0) are considered. To resolve all of these isotopic compositions before measurement of their abundances is difficult. For low-molecular-mass ions (HjO, COj) or for atomic ions (Ca, Cl), the problems are not so severe. Therefore, most accurate isotope ratio measurements are made on low-molecular-mass species, and resolution of these even with simple analyzers is not difficult. The most widely used analyzers are based on magnets, quadrupoles, ion traps, and time-of-flight instruments. 

An energy dispersive spectrometer is cheaper and faster for multielement analytical purposes but has poorer detection limits and resolution. 

Fig. 4. Diaphragm pressure elements (a) cormgated diaphragm (b) flat diaphragm (c) multielement diaphragm capsules (d) convex capsule and (e)...

Advantages and drawbacks are iadicated by + and —, respectively. Thus, + implies iuexpensive, multielement capability, wide dynamic range, relative freedom from iaterferences, and the abiUty to analyze refractory elements. 

THE ENVIRONMENTAL MULTIELEMENT REFERENCE MATERIAL COLLECTION OF THE INSTITUTE OF GEOCHEMISTRY, SIBERIAN BRANCH,... 

Inductively coupled plasma-mass spectrometry (ICP-MS) is a multielement analytical method with detection limits which are, for many trace elements, including the rare earth elements, better than those of most conventional techniques. With increasing availability of ICP-MS instalments in geological laboratories this method has been established as the most prominent technique for the determination of a large number of minor and trace elements in geological samples. 

Multielement analysis, excellent detection limits for heavy metals quantitative measurement of heavy-metal trace contamination on silicon wafers... 

In Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES), a gaseous, solid (as fine particles), or liquid (as an aerosol) sample is directed into the center of a gaseous plasma. The sample is vaporized, atomized, and partially ionized in the plasma. Atoms and ions are excited and emit light at characteristic wavelengths in the ultraviolet or visible region of the spectrum. The emission line intensities are proportional to the concentration of each element in the sample. A grating spectrometer is used for either simultaneous or sequential multielement analysis. The concentration of each element is determined from measured intensities via calibration with standards. 

EDS and WDS spectra of a multielement glass, shown in Figure 4, illustrate some major strengths and weaknesses ... 

Figure 4 Comparison of EDS and WDS spectra from a complex, multielement glass.

Experience gained in the ZAF analysis of major and minor constituents in multielement standards analyzed against pure element standards has produced detailed error distribution histograms for quantitative EPMA. The error distribution is a normal distribution centered about 0%, with a standard deviation of approximately 2% relative. Errors as high as 10% relative are rarely encountered. There are several important caveats that must be observed to achieve errors that can be expected to lie within this distribution ... 

Atomic absorption spectroscopy of VPD solutions (VPD-AAS) and instrumental neutron activation analysis (INAA) offer similar detection limits for metallic impurities with silicon substrates. The main advantage of TXRF, compared to VPD-AAS, is its multielement capability AAS is a sequential technique that requires a specific lamp to detect each element. Furthermore, the problem of blank values is of little importance with TXRF because no handling of the analytical solution is involved. On the other hand, adequately sensitive detection of sodium is possible only by using VPD-AAS. INAA is basically a bulk analysis technique, while TXRF is sensitive only to the surface. In addition, TXRF is fast, with an typical analysis time of 1000 s turn-around times for INAA are on the order of weeks. Gallium arsenide surfaces can be analyzed neither by AAS nor by INAA. 

The dependence on target mass makes ion scattering techniques ideal for the study of multielement systems. By increasing the incident ion mass, the energy separation between different elements becomes larger. On the other hand, radiation-induced damage becomes a more important consideration. 

The Inductively Coupled Plasma (ICP) has become the most popular source for multielement analysis via optical spectroscopy since the introduction of the first commercial instruments in 1974. About 6000 ICP-Optical Emission Spectrometry (ICP-OES) instruments are in operation throughout the world. 

ICP-OES is one of the most successful multielement analysis techniques for materials characterization. While precision and interference effects are generally best when solutions are analyzed, a number of techniques allow the direct analysis of solids. The strengths of ICP-OES include speed, relatively small interference effects, low detection limits, and applicability to a wide variety of materials. Improvements are expected in sample-introduction techniques, spectrometers that detect simultaneously the entire ultraviolet—visible spectrum with high resolution, and in the development of intelligent instruments to further improve analysis reliability. ICPMS vigorously competes with ICP-OES, particularly when low detection limits are required. 

G. M. Levy, A. Quaglia, R, E. Lazure, and S. W. McGeorge. Spect. Acta. 42B, 341, 1987. Describes the diode array-based spectrally segmented spectrometer for simultaneous multielement analysis. 

The discrete line sources described above for XPS are perfectly adequate for most applications, but some types of analysis require that the source be tunable (i.e. that the exciting energy be variable). The reason is to enable the photoionization cross-section of the core levels of a particular element or group of elements to be varied, which is particularly useful when dealing with multielement semiconductors. Tunable radiation can be obtained from a synchrotron. 

Ix is the background-corrected net intensity of the principal peak of analyte X, Kx a proportionality factor for the absolute sensitivity of the standard reference, e. g. an Ni plate, and c the concentration of X. Multielement analyses are based on known relative sensitivities S ... 

Monochromator 663, 791 Monodentate ligand 51 Morphine (and codeine) D. of (fu) 740 Mortar agate, 155 mullite, 155 percussion, 155 synthetic sapphire, 155 Muffle furnace 97 Multielement analysis 174, 184, 775 Multiple range indicators 268 Murexide 316... 

Lukco, R.G., Kosman, J.J., "The Use of GC-AES Multielement Simulated Distillation for Petroleum Product Fingerprinting , J. Chrom. Set. 1993, March... 

The efficiency of the condenser is reduced by poor air removal (and the presence of other noncondensable gases), so surface condensers usually are equipped with vacuum pumps but also may incorporate older style, single or multistage multielement, steam-jet air ejectors. Under most normal operations, the residual oxygen level is below 20 to 40 ppb 02. 

Minganti V, Capelli R, Depellegrini R (1995) Evaluation of different derivatization methods for the multielement detection of Hg, Pb and Sn compounds by gas chromatography-microwave induced plasma-atomic emission spectrometry in environmental samples. Fresenius Journal of Analytical Chemistry, 351 (4-5) 471 77. 

TOF-SIMS can be applied to identify a variety of molecular fragments, originating from various molecular surface contaminations. It also can be used to determine metal trace concentrations at the surface. The use of an additional high current sputter ion source allows the fast erosion of the sample. By continuously probing the surface composition at the actual crater bottom by the analytical primary ion beam, multi element depth profiles in well defined surface areas can be determined. TOF-SIMS has become an indispensable analytical technique in modem microelectronics, in particular for elemental and molecular surface mapping and for multielement shallow depth profiling. 

Vol. 107. Multielement Detection Systems for Spectrochemical Analysis. By Kenneth W. Busch and Marianna A. Busch... 

Flame and spark emission spectroscopy Not very accurate. Gives multielement analyses 10 = to 10 M... 

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