Spectrometry spark emission

Spark Emission Spectrometry. Spark emission spectrometry is a standard method for direct analysis of metallic samples and is of great use for production as well as for product control in the metals industry [215], [216]. 

BeryUium aUoys ate usuaUy analyzed by optical emission or atomic absorption spectrophotometry. Low voltage spark emission spectrometry is used for the analysis of most copper-beryUium aUoys. Spectral interferences, other inter-element effects, metaUurgical effects, and sample inhomogeneity can degrade accuracy and precision and must be considered when constmcting a method (17). 

Inductively coupled argon plasma (icp) and direct current argon plasma (dcp) atomic emission spectrometry are solution techniques that have been appHed to copper-beryUium, nickel—beryUium, and aluminum—beryUium aUoys, beryUium compounds, and process solutions. The internal reference method, essential in spark source emission spectrometry, is also useful in minimizing drift in plasma emission spectrometry (17). Electrothermal (graphite... 

Neutron Activation Analysis X-Ray Fluorescence Particle-Induced X-Ray Emission Particle-Induced Nuclear Reaction Analysis Rutherford Backscattering Spectrometry Spark Source Mass Spectrometry Glow Discharge Mass Spectrometry Electron Microprobe Analysis Laser Microprobe Analysis Secondary Ion Mass Analysis Micro-PIXE... 

Applications Atomic emission spectrometry has been used for polymer/additive analysis in various forms, such as flame emission spectrometry (Section 8.3.2.1), spark source spectrometry (Section 8.3.2.2), GD-AES (Section 8.3.2.3), ICP-AES (Section 8.3.2.4), MIP-AES (Section 8.3.2.6) and LIBS. Only ICP-AES applications are significant. In hyphenated form, the use of element-specific detectors in GC-AED (Section 4.2) and PyGC-AED deserves mentioning. 

Principles and Characteristics Arc and spark discharges have widely been used as excitation sources for qualitative and quantitative emission spectrometry since the 1920s commercial instruments became available during the 1940s. 

Spark sources are especially important for metal analysis. To date, medium-voltage sparks (0.5-1 kV) often at high frequencies (1 kHz and more), are used under an argon atmosphere. Spark analyses can be performed in less than 30 s. For accurate analyses, extensive sets of calibration samples must be used, and mathematical procedures may be helpful so as to perform corrections for matrix interferences. In arc and spark emission spectrometry, the spectral lines used are situated in the UV (180-380nm), VIS (380-550nm) and VUV (<180 nm) regions. Atomic emission spectrometry with spark excitation is a standard method for production and product control in the metal industry. 

SS-AES Sliding spark-source atomic emission spectrometry... 

Heavy Metals, Isotope Dilution, Spark Source Mass Spectrometry, and Inductively Coupled Plasma Atomic Emission Spectrometry... 

Instrumentation. Sample Preparation. Qualitative and Quantitative Analysis. Interferences and Errors Associated with the Excitation Process. Applications of Arc/Spark Emission Spectrometry. 

The basic instrumentation used for spectrometric measurements has already been described in the previous chapter (p. 277). Methods of excitation, monochromators and detectors used in atomic emission and absorption techniques are included in Table 8.1. Sources of radiation physically separated from the sample are required for atomic absorption, atomic fluorescence and X-ray fluorescence spectrometry (cf. molecular absorption spectrometry), whereas in flame photometry, arc/spark and plasma emission techniques, the sample is excited directly by thermal means. Diffraction gratings or prism monochromators are used for dispersion in all the techniques including X-ray fluorescence where a single crystal of appropriate lattice dimensions acts as a grating. Atomic fluorescence spectra are sufficiently simple to allow the use of an interference filter in many instances. Photomultiplier detectors are used in every technique except X-ray fluorescence where proportional counting or scintillation devices are employed. Photographic recording of a complete spectrum facilitates qualitative analysis by optical emission spectrometry, but is now rarely used. 

Only arc/spark, plasma emission, plasma mass spectrometry and X-ray emission spectrometry are suitable techniques for qualitative analysis as in each case the relevant spectral ranges can be scanned and studied simply and quickly. Quantitative methods based on the emission of electromagnetic radiation rely on the direct proportionality between emitted intensity and the concentration of the analyte. The exact nature of the relation is complex and varies with the technique it will be discussed more fully in the appropriate sections. Quantitative measurements by atomic absorption spectrometry depend upon a relation which closely resembles the Beer-Lambert law relating to molecular absorption in solution (p. 357 etal.). 

During the many years that atomic emission spectrometry has been employed for chemical analysis a variety of types of excitation sources have been used. In earlier times electric discharges, dc-arcs and ac-sparks, found considerable favour. The inherent instability of the discharges has meant that as more stable alternatives have been developed they have been progressively replaced by them. Where electrical excitation is still employed it is achieved by an electrically controlled spark with far greater stability and much improved precision for the analysis. 

Table 8.9 shows an analysis of a silicate rock and compares the precision of X-ray fluorescence analysis with wet chemical methods and arc/spark emission spectrometry. 

Emission spectrometry (ES). Emission spectrometry is based on the excitation of an element to an upper electronically excited state, from which it returns to the ground state by the emission of radiation. As discussed in Chapter 3, the wavelength emitted is characteristic of the emitted species, and, under the approximate conditions, the emission intensity is proportional to its concentration. Means of excitation include arcs and sparks, plasma jets (see ICP), and lasers. 

Atomic emission spectrometry (AES) is also called optical emission spectrometry (OES). It is the oldest atomic spectrometric multielement method which originally involved the use of flame, electric arc or spark excitation. Recently there has been considerable innovation in new sources plasma sources and discharges under reduced pressure. Littlejohn et al. (1991) have reviewed recent advances in the field of atomic emission spectrometry, including fundamental processes and instrumentation. 

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