Inductively coupled plasma optical emission spectroscopy instrumentation

Multielement analysis will become more important in industrial hygiene analysis as the number of elements per sample and the numbers of samples increases. Additional requirements that will push development of atomic absorption techniques and may encourage the use of new techniques are lower detction and sample speciation. Sample speciation will probably require the use of a chromatographic technique coupled to the spectroscopic instrumentation as an elemental detector. This type of instrumental marriage will not be seen in routine analysis. The use of Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) (17), Zeeman-effect atomic absorption spectroscopy (ZAA) (18), and X-ray fluorescence (XRF) (19) will increase in industrial hygiene laboratories because they each offer advantages or detection that AAS does not. 

The analyst uses ICP-OES (inductively coupled plasma, optical emission spectroscopy) to measure twenty different metal ions in solution. To fully calibrate the instrument requires the preparation and measurement of 100 individual calibration standards (five point calibration per element). It would be impracticable for an analyst to calibrate the instrument daily. The instrument is calibrated at regular intervals (say fortnightly) by the analyst. In the intervening time, the calibration for each metal ion is checked by the use of a set of drift correction standard solutions. Minor corrections can then be made to the calibration to allow for day-to-day drift. 

The surface area of the catalysts was measured by conventional BET methods (nitrogen physisorption at -196°C using a Quanta Chrome-NOVA 1000 instrument). The actual metal loading was measured by inductively-coupled plasma / optical emission spectroscopy (ICP/OES). The acidity and basicity of the synthesized catalysts were measured by NHj and COj thermoprogrammed desorption, respectively, using an AMI-100 (Zeton-Altamira, Pittsburgh, PA) characterization system. The catalyst samples were reduced in 10% H /Ar at 450°C for 8 hours, followed by treatment in 10% NH,/He or 10% COj/He at 35°C and then by desorption up to 400°C with a heating rate of 10°C/min. 

The analytical performance of ICP-MS is compared with other analytical techniques for the determination of trace metal oxide particulates after the simulated detonation of an RDD [10]. Table 20.9 shows a comparison of the instrumental parameters used in inductively coupled plasma optical emission spectroscopy (ICP-OES) and an ICP-MS instrument. These two techniques were used to analyze Sr, Ti, and Ce in ceramic oxides that may be used in RDDs. ICP-MS provided lower detection limits for the metals than ICP-OES. Overall method performance was comparable with ICP-OES and instrumental neutron activation analysis (INAA), another well-established nuclear and radiological analytical technique. 

Because light emitted from inductively coupled plasma torches is characteristic of the elements present, the torches were originally introduced for instruments that optically measured the frequencies and intensities of the emitted light and used them, rather than ions, to estimate the amounts and types of elements present (inductively coupled plasma atomic emission spectroscopy. 

Since the introduction of the first commercially available atomic absorption spectrophotometer (AAS) in the early 1960s, there has been an increasing demand for better, faster, easier-to-use, and more flexible trace element instrumentation. A conservative estimate shows that today s market for atomic spectroscopy (AS)-based instruments, such as atomic absorption (AA), inductively coupled plasma optical emission (ICP-OES), and inductively coupled plasma mass spectrometry (ICP-MS), represents over 700 million in annual revenue. After market sales and service costs are added to this number, it is probably close to 1 billion. As a result of this growth, we have seen a rapid emergence of more sophisticated equipment and easier-to-use software. Moreover, with an increase in the number of manufacturers of both instrumentation and sampling accessories, the choice of which technique to use is often unclear. 

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. 

Numerous methods have been published for the determination of trace amounts of tellurium (33—42). Instrumental analytical methods (qv) used to determine trace amounts of tellurium include atomic absorption spectrometry, flame, graphite furnace, and hydride generation inductively coupled argon plasma optical emission spectrometry inductively coupled plasma mass spectrometry neutron activation analysis and spectrophotometry (see Mass SPECTROMETRY Spectroscopy, OPTICAL). Other instrumental methods include polarography, potentiometry, emission spectroscopy, x-ray diffraction, and x-ray fluorescence. 

With the exception of better optical resolution needed, the basic instrument used for atomic emission is very similar to that used for atomic absorption with the difference that no primary light source is used for atomic emission. One of the most critical components for this technique is the atomisation source because it must also provide sufficient energy to excite the atoms as well as atomise them. The earliest energy sources for excitation were simple flames, but these often lacked sufficient thermal energy to be truly effective sources. The development in 1963 and the introduction in 1970 of the first commercial inductively coupled plasma (ICP) as a source for atomic emission dramatically changed the use and the utility of emission spectroscopy (Thompson Walsh 1983). 

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