Multi-element analytical technique

For the above reasons, indoor air filters often yield particle masses that are orders of magnitude below the mass requirements for quantitative ED-XRF analysis - the multi-element detection method traditionally used for air analysis. Researchers are currently seeking alternative multi-element analytical techniques with adequate sensitivity for indoor air samples. Indoor and outdoor air concentration data, from a variety of studies which employed different sampling and analytical approaches, are summarized in Table 11.3. Van Winkle and Scheff (2001) used high-volume samplers equipped with 37-mm quartz fiber filters and an air flow rate of 25 L min to monitor 10 homes in... 

In principle, XRE analysis is a multi-element analytical technique and, in particular, the simultaneous determination of all the detectable elements present in the sample is inherently possible with EDXRE. In WDXRF both sequential and simultaneous detection modes are possible. 

Multi-Element Analytical Scheme The 76 elements analyzed include 39 elements originally analyzed in the RGNR Projects, and 37 new elements. The analytical scheme is based largely on ICPMS, ICPAES and XRF, supplemented with other techniques (Table 1). The lower levels of detection of all elements are less than their crustal abundances (Table 2). 

There are several factors which make neutron activation analysis (NAA) an appropriate technique for investigating potential pollutants in coal and the combustion process. First, the multi-element nature of NAA is useful because of the large number of potential elemental pollutants, such as Se, Hg, As, Zn, Ni, Sb, and Cd. Also, the use of elemental ratios made possible by the multi-element capability facilitates the understanding of chemical behavior during the combustion process. Elemental ratios have been used previously in urban (15) and upper atmospheric (26) studies. Secondly, the sensitivity and selectivity of NAA allows determination of many elements present at very low concentrations (ppm or lower), and the results are unaffected by matrix interferences. This sensitivity also allows analysis of very small samples. Finally, the cost of NAA when conducted as a multi-element analytical tool is competitive with more conventional and less sensitive techniques on the cost-per-element-per-sample basis. 

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. 

It should be pointed out that no other analytical technique has the capability to provide multi-element data non-destructively, often with good detection limits and... 

Table 8.29 shows the main characteristics of ICP-AES as a fast multi-element technique. Analytical figures of merit for ICP emission spectrometers are... 

Activation analysis is based on a principle different from that of other analytical techniques, and is subject to other types of systematic error. Although other analytical techniques can compete with NAA in terms of sensitivity, selectivity, and multi-element capability, its potential for blank-free, matrix-independent multielement determination makes it an excellent reference technique. NAA has been used for validation of XRF and TXRF. 

The introduction of EU directives on Waste Electrical and Electronic Equipment and Reduction of Hazardous Substances has highlighted the need for precise and repeatable elemental analysis of heavy metals in the plastics production process. X-ray fluorescence (XRF) spectroscopy has emerged as the most economical and effective analytical tool for achieving this. A set of certified standards, known as TOXEL, is now available to facilitate XRF analyses in PE. Calibration with TOXEL standards is simplified by the fact that XRF is a multi-element technique. Therefore a single set of the new standards can be used to calibrate several heavy elements, covering concentrations from trace level to several hundred ppm. This case study is the analysis of heavy metals in PE using an Epsilon 5 XRF spectrometer. 

Hydride/vapour generation techniques provide extremely good sensitivity. When coupled to continuous flow methodologies for use in routine analysis, simple and reliable analytical techniques are provided. TTie extension of chemistries and sample transfer systems to provide analytical protocols to cope with a wider range of elemental analyses should be pursued in the search for lower detection levels. While multi-element techniques offer very low levels of detection, the use of specific single element analytical instruments with detection capabihties similar to those described above may be the best route for routine laboratories with high sample throughput. 

Elements chosen from the limited NURE multi-element geochemical packages that may be pathfinders for porphyry-style deposits (Lefebure Ray 1995) include Ba, Co, Cu, Mn, Pb, Ti, V, and Zn. Under the NURE program, two analytical techniques were used energy dispersive x-ray fluorescence (Cu and Pb) and neutron activation (Ba, Co, Mn, Ti, V, and Zn). Single element plots and element association plots were generated. Geochemical data for pond sediments collected over the Pebble deposit in 2008... 

LA-ICP-MS was used for in situ determination of ultratrace elements in quartz. The analytical protocol included the following elements Al, Ba, Be, Cr, Ee, Ge, K, Li, Mg, Mn, Pb, Rb, Sr, Th, Ti and U . Apphcation of the LA technique to heterogeneous samples usually requires preparing a homogeneous glass by fusing with lithium borate . A difficulty encountered with multi-element LA-ICP-MS analysis is the absence of standards... 

While it is to be expected that the effects of these disadvantages will continue to diminish as more becomes known about electrothermal atomization, currently it can be said that if there is sufficient sample for flame or ICP analysis, and that these techniques offer sufficient sensitivity, then they should be used in preference. Plasma techniques should be used in preference to the flame if more than one analyte is to be determined. Recently a multi-element, simultaneous electrothermal instrument has been developed. These spectrometers still use a suite of hollow cathode lamps as sources. At present, a maximum of six analytes can be determined simultaneously. This area is likely to expand very rapidly, which may lead to a resurgence in the technique. If the sensitivity of a flame or ICP-AES is insufficient, and ICP-MS cannot be afforded, electrothermal atomization comes into its own, and is invaluable when either high sensitivity is required or when only small amounts of sample are available. 

In spite of the excellent capability and advantages (high selectivity and sensitivity) of RIMS for the ultratrace analysis of isotopes with naturally rare abundance in environmental, geological, medical and nuclear samples, no commercial instrumentation is available to date. In contrast to AMS and RIMS as mono-elemental (element-specific) analytical techniques, ICP-MS and LA-ICP-MS possess, in analogy to GDMS and SIMS, have the ability for multi-element analysis and thus could have the widest fields of application. 

For many decades, TIMS was the isotope analytical technique of choice, but due to instrumental developments in ICP-MS, especially with multiple ion collectors (MC-ICP-SFMS), and the advantages of ICP-MS in comparison to TIMS (e.g., higher element sensitivities, faster isotope ratio measurements, comparable precision and accuracy, practically no restriction on the ionization potential of chemical elements, time independent mass fractionation and the possibility of additional multi-element analysis at trace and ultratrace level and fewer, less time-consuming sample preparation steps75), TIMS will be replaced in future by powerful ICP-MS to an ever greater extent. 

The most frequently applied analytical methods used for characterizing bulk and layered systems (wafers and layers for microelectronics see the example in the schematic on the right-hand side) are summarized in Figure 9.4. Besides mass spectrometric techniques there are a multitude of alternative powerful analytical techniques for characterizing such multi-layered systems. The analytical methods used for determining trace and ultratrace elements in, for example, high purity materials for microelectronic applications include AAS (atomic absorption spectrometry), XRF (X-ray fluorescence analysis), ICP-OES (optical emission spectroscopy with inductively coupled plasma), NAA (neutron activation analysis) and others. For the characterization of layered systems or for the determination of surface contamination, XPS (X-ray photon electron spectroscopy), SEM-EDX (secondary electron microscopy combined with energy disperse X-ray analysis) and... 

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