ICP optical emission spectrometry

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. 

Solid Sampling Atomic Absorption Spectrometry ICP Optical Emission Spectrometry ICP Mass Spectrometry... 

The certification procedure for seven trace metals (Ba, Ca, Li, Mg, Mn, Na and Sr) in the certified reference material FEBS-1 (National Research Council Canada, Institute for National Measurement Standards, Ottawa, Canada) based on fish otolith matrix by isotope dilution - ICP-MS in comparison to ICP optical emission spectrometry and X-ray fluorescence analysis, is described by Sturgeon et al4X The isotope dilution technique is also employed for species analysis in biological systems,46 e.g., for the determination of mercury species in tuna material,54 or in aquatic systems using cold vapour ICP-MS.55... 

Spray Chambers. Spray chambers [14] were designed mostly empirically for use with conventional pneumatic nebulizers during the development of ICP optical emission spectrometry. The main purpose of the spray chamber was thought to be to remove large droplets that would not have sufficient time to be completely vaporized during their 1- to 2-msec travel in the plasma, although what... 

Two different kinds of direct injection nebulizers are available commercially. The total consumption nebulizer was developed by Greenfield et al. [36] for ICP optical emission spectrometry. The concept for the Cetac direct injection nebulizer (DIN) was developed by Fassel, Houk, and coworkers [35,37]. It has a narrow sample-carrying capillary [30-50 xm inner diameter (i.d.), 0.5 to 1 m long] that extends slightly past the nebulizer gas tube. A second, auxiliary or makeup, nebulizer gas is introduced through another concentric tube outside the nebulizer gas tube. A gas displacement pump (up to 1500 psi) or HPLC pump is used to deliver the sample to the nebulizer through the long, narrow capillary. 

When compared with optical spectrometric techniques of elemental analysis, the techniques based on mass spectrometry provide an increase in sensitivity and in analytical working range of some orders of magnitude. For instance, the detection limits with ICP-MS are three orders of magnitude better than ICP-optical emission spectrometry (ICP-OES). Figure 1.45 shows the maximum sensitivity obtained for the different elements, using an ICP-MS coupling with a quadrupole. 

To study the influence of chemical impurities on labelhng yields of DOTATATE, a solution of °Y or Lu was added to 50 mL of 0.4M sodium acetate containing 10 gg of DOTATATE and 50 mg/mL of ascorbic acid (pH4.5) to obtain a DOTATATE to radionuclide molar ratio of about 20. These solutions were spiked with varying quantities of metallic contaminants (e.g. Ca, Cu, Cd, Fe, Zn). The quantities of metal cations were adjusted to obtain metal to radiometal molar ratios ranging from 1 to 100. The concentration of each analyte was verified by ICP optical emission spectrometry. The reaction mixture was incubated at 95°C for 25 min. Each point was tested in duplicate. 

Today, analyses of bulk fossil chemistry are largely conducted by inductively coupled plasma (ICP) atomic emission spectrometry (AES), ICP mass spectrometry (MS) or ICP optical emission spectrometry (OES) techniques (e.g. Rosenthal et al. 1999 DeVilliers et al. 2002 Green et al. 2003). These techniques permit rapid and precise (c. 1% for many elements) measurement of a number of chemical constituents simultaneously. ICP-MS offers higher sensitivities than AES and OES, enabling measurement of more elements and smaller sample sizes. 

Yttrium was found to be effective for signal compensation in the detection of boron and titanium in human blood using axial-view ICP optical emission spectrometry (Garavaglia et al. 2002). 

ICP optical emission spectrometry (ICP-OES) is also well established, and numerous procedures exist for a host of complex sample types. It is not uncommon to employ internal standards for ICP-OES. This is particularly useful to compensate partially for variations in sample delivery rate and, to a lesser extent, for small fluctuations in the plasma. The technique is relatively free of chemical interferences, and most spectral interferences can be corrected for. In addition to providing parts per billion to parts per million limits of detection for most of the periodic table with precisions of a few per cent or less, ICP-OES can also provide five to six orders of magnitude in analytical dynamic range. 

Although originally FIA was conceived as a special technique for delivery of a sample segment into the instrument, the combination of flow injection as a sample pretreatment tool with atomic spectrometry has been shown to be of great potential for enhancing the selectivity and sensitivity of the measurements. Moreover, contamination problems are reduced due to the closed system used, making this interface suitable for ultratrace determination of metal species. Hyphenated techniques such as FIA/ SIA with flame atomic absorption spectrometry, inductively coupled plasma (ICP)-optical emission spectrometry, and ICP-mass spectrometry (MS) have been exploited extensively in recent years. The major attraction of FIA-ICP-MS is its exceptional multi-elemental sensitivity combined with high speed of analysis. In addition, the possibility of... 

Many methods used for qualitative analysis are destructive either the sample is consumed during the analysis or must be chemically altered in order to be analyzed. The most sensitive and comprehensive elemental analysis methods for inorganic analysis are ICP atomic emission spectrometry (ICP-AES or ICP optical emission spectrometry [ICP-OES]), discussed in Chapter 7, and ICP-MS, discussed in Chapters 9 and 10. These techniques can identify almost all the elanents in the periodic table, even when only trace amounts are present, but often require that the sample be in the form of a solution. If the sample is a rock or a piece of glass or a piece of biological tissue, the sample usually must be dissolved in some way to provide a solution for analysis. We will see how this is done later in this chapter. The analyst can determine accurately what elements are present, but information about the molecules in the sample is often lost in the sample preparation process. The advantage of ICP-OES and ICP-MS is that they are very sensitive concentrations at or below 1 ppb of most elements can be detected using these methods. 

Although ICP-MS is not the only technique that can be used for this type of investigation and results obtained with ICP-optical emission spectrometry (multi-elemental analysis only) [9] or secondary ion mass spectrometry (SIMS) [10] have been reported, it is clear that ICP-MS is becoming more and more popular for this type of application. Table 14.1 shows the main applications published on this topic based on the use of ICP-MS. 

FD/FI field desorption/field ionization ICP-OES ICP optical emission spectrometry... 

Preconcentration by cloud point extraction of the complex determination by ICP optic emission spectrometry. Simultaneous spectrophotometric determination of cadmium and mercury... 

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