Elemental surveys

SSMS provides complete elemental surveys for a wide range of sample types and allows the determination of elemental concentrations with detection limits in the range 10-50 parts per billion atomic (ppba). 

Complete trace elemental survey of solid materials with accuracy to within a factor of 3 without standards... 

Most applications of LIMS are in failure analysis. A typical microanalytical failure analysis problem, for example, may involve determinating the cause of corrosion in a metallization line of an integrated circuit. One can achieve this by performing an elemental survey analysis of the corroded region. Since it is not always known which elements are normal constituents of the material in question and which are truly contaminants, the vast majority of these analyses are performed by comparing the elemental make-up of the defective region to that of a control region. The com-... 

Although SSMS cannot be considered a surface technique due to the 1-5 rm penetration of the spark in most materials, few other techniques can provide a trace elemental survey analysis of surfaces consisting of films or having depths of interest... 

Inductively Coupled Plasma-Optical (ICP-optical) methods and ICPMS are extremely sensitive elemental survey techniques that also are described in this volume. ICP methods, however, require a solution for analysis, so that the direct... 

Figure 4 SSMS surface analysis. The point-to-plane technique allows ppma elemental surveys over a depth of 1-5 xm.

Abel, Trace Elemental Survey Analysis of TNT , PATR 4257 (1975) 76) T.H. Maugh,... 

H. Kramer, S. Semel J.E. Abel, Trace Elemental Survey Analysis of Trinitrotoluene , PATR 4767 (1975) (An evaluation of the applicability of spark source mass spectrometry and thermal neutron activation for the detn of origin-related trace elemental impurities in TNT) 10) C. Ribando J. Haber-man, Origin-Identification of Explosives Via Their Composite Impurity Profiles I. The... 

Abstract The basic principles of astronomical spectroscopy are introduced and the main types of dispersing element surveyed. The principles behind two modem spectroscopic techniques, multiple object and integral held spectroscopy, are also discussed. 

Trends in element analysis are multi-element (survey) analysis, lower concentration levels, micro/local element analysis and speciation (coupling with chromatography). An overview of the determination of elements in polymeric materials is available [7], Reviews on sample preparation for trace analysis are given in refs [8-10]. Quality assurance of analytical data in routine elemental analysis has been discussed [11], Organic analysis is obviously much more requested in relation to polymer/additive matrices than elemental analysis. 

Applications Real applications of spark-source MS started on an empirical basis before fundamental insights were available. SSMS is now considered obsolete in many areas, but various unique applications for a variety of biological substances and metals are reported. Usually, each application requires specific sample preparation, sparking procedure and ion detection. SSMS is now used only in a few laboratories worldwide. Spark-source mass spectrometry is still attractive for certain applications (e.g. in the microelectronics industry). This is especially so when a multi-element survey analysis is required, for which the accuracy of the technique is sufficient (generally 15-30% with calibration or within an order of magnitude without). SSMS is considered to be a... 

Response to both metallic and nonmetallic elements (survey elemental scans)... 

The technique is referred to by several acronyms including LAMMA (Laser Microprobe Mass Analysis), LIMA (Laser Ionisation Mass Analysis), and LIMS (Laser Ionisation Mass Spectrometry). It provides a sensitive elemental and/or molecular detection capability which can be used for materials such as semiconductor devices, integrated optical components, alloys, ceramic composites as well as biological materials. The unique microanalytical capabilities that the technique provides in comparison with SIMS, AES and EPMA are that it provides a rapid, sensitive, elemental survey microanalysis, that it is able to analyse electrically insulating materials and that it has the potential for providing molecular or chemical bonding information from the analytical volume. 

Steinnes, E., Rambaek, J. P., and Hansson, J. E. (1992). Large scale multi-element survey of atmospheric deposition using naturally growing moss as biomonitor. Chemosphere 25, 735—752. 

C. A. Weeks, M. Croasdale, M. A. Osborne, L. Hewitt, P. F. Miller, P. Robb, M. J. Baxter, P. D. Warriss, T. G. Knowles, Multi-element survey of wild edible fungi and blackberries in the UK, Food Addit. Contam., 23 (2006), 140D147. 

Micro-PIXE with a 20 micron beam spot has proved to be a versatile tool for investigations of water and electrical trees, as well as a variety of other samples. This system is simple to operate and does not require complex target preparation, so that multi-element surveys of a variety of samples can be rapidly performed. 

The elements surveyed in Table 4 could all be measured at their Threshold Limit Value (TLV) by the methods suggested in this chapter. If the TLV is... 

Trace Element Survey Analyses by Spark Source Mass Spectrography... 

LEIPZIGER AND GUIDOBONI Trace Element Survey Analyses... 

XPS analyses was performed on a Quantum 2000 Scanning SK Microprobe instrument. For the XPS analyses the samples were mounted on a sample plate, introduced into the XPS chamber and evacuated to <2x10 Pa. Elemental surveys and narrow scans were conducted with A1 KD X-rays on the uncalcined samples after which the temperature was increased to 573 K and 873 K (heating rate = 20 K min" ). Semi-quantitative data were calculated from the survey scans. The peak area ratios reported in this paper are fractions, which were calculated from the areas under the XPS peaks. The narrow scan data were used to determine probable compounds for the Co and C peaks. This was accomplished from a Gauss-Lorenzian peak fit of the appropriate photoelectron peaks. Wide spectra were recorded to obtain a semi-quantitative analyses of all elements present on the surface (except H and He) and high-resolution narrow spectra were recorded to identify the oxidation states and/or compounds. 

Fig. 31. Qualitative elemental survey scan of the surface of a yellow leaf. Reprinted with permission from T. L. Barr, S. Seal, S. E. Hardcastle, M. A. Maclauran, L. M. Chen, and J. Klinowski, Bull. Pol. Acad. Sci. 45, 1 (1997).

Assignments of intensities and calculation of concentrations can be performed by general element survey and specified software. Precision (RSD) below 5% is commonly achieved for elements present at 25pgl . To correct for matrix-induced ion signal variation and instrumental drift, rhodium or indium in combination with panoramic analysis, based on full mass-spectra scan methods, is used as the internal standard (IS). Spectroscopic effects due to Cl, Na, Ca, Mg, S, and C were corrected with interference factors (IF) on the basis of a set of correction equations (see Table 5). 

VG Isotopes Ltd., is another leading manufacturer of ICP-MS equipment. The special features of their VG Plasmaquad PQ2 includes a multi-channel analyser which ensures rapid data acquisition over the whole mass range. The multi-channel analyser facilities include 4096 channels, 300 m facility for spectral analysis, user-definable number of measurements per peak in peak jumping mode, and the ability to monitor data as they are acquired. A multi-channel analyser is imperative for acquiring short-lived signals from accessories such as flow injection, electrothermal vaporisation, laser ablation, and so on, or for fast multi-element survey scans (typically 1 minute). 

Evans, C.A. and G.H. Morrison, 1968, Trace element survey analysis of biological materials by spark source mass spectrometry. Anal. Chem. 40, 869. 

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