SIMS, analytical method Applications

As with any analytical method, the ability to extract semiquantitative or quantitative information is the ultimate challenge. Generally, static SIMS is not used in this mode, but one application where static SIMS has been used successfully to provide quantitative data is in the accurate determination of the coverage of fluropolymer lubricants. These compounds provide the lubrication for Winchester-type hard disks and are direaly related to ultimate performance. If the lubricant is either too thick or too thin, catastrophic head crashes can occur. 

The SIMS analytical ion signal of a specific element or isotope also can be enhanced by selective ionization of particular atoms, and the detection limit for that element thereby improved. This mode of SNMS is important to specific applications, but it lacks the generality inherent in nonselective SNMS methods. The focus of this article will be on the methods for obtaining complete, accurate, and matrix-independent compositions of chemically complex thin-film structures and materials. 

The application of SIMS, SNMS, SSMS and GDMS in quantitative trace analysis for conducting bulk material is restricted to matrices where standard reference materials (SRMs) are available. For quantification purposes, the well characterized multi-element SRMs (e.g., from NIST) are useful. In Table 9.5 the results of the analysis by SNMS and the RSCs (relative sensitivity coefficients) for different elements in a low alloy steel standard (NBS 467) are compared with those of SSMS. Both solid-state mass spectrometric techniques with high vacuum ion sources allow the determination of light non-metals such as C, N, and P in steel, and the RSCs for the elements measured vary from 0.5 to 3 (except C). RSCs are applied as a correction factor in the analytical method used to obtain... 

The penetration mechanism requires the transfer of the aggressive anions from the electrolyte to the metal-oxide interface. The application of surface analytical methods such as X-Ray Photoelectron Spectroscopy (XPS), Auger Electron Spectroscopy (AES), and Secondary Ion Mass Spectroscopy (SIMS) do not clearly support this mechanism. Careful measurements begin with a specimen prepassivated in a solution without any aggressive anions and with their being added later to avoid incorporation during film growth to study their penetration. Eor these conditions. 

Depth concentration measurement is an important application of surface analytical methods. Examples are depth distribution of additives in plastics, or interface analysis where polymers are in contact with metals or ceramics. All surface methods with a good depth resolution (XPS, AES, SIMS) are suitable for depth or profile measurements. Complete multilayer coating systems require analytical methods that are applicable to small sample sizes and low concentrations. Techniques for obtaining chemical composition and component distribution depth profiles for automotive coating systems, both in-plane (or slab) microtomy and cross-section microtomy, include /xETIR, /xRS, ToE-SIMS, optical microscopy, TEM, as well as solvent extraction followed by HPLC, as illustrated by Adamsons et al. [5]. Surface and interface/interphase analysis can now be done routinely on both simple monolayer coatings and complex multicomponent, multilayered... 

Fit the purpose calibration. It is common sense to check instrument performance each day, and GLP requirements simply formalize the performance and documentation of these checks. On the other hand, it is also important to use the right test (full calibration, verification, system suitability test, or instrument and method validation) to verify the performance and to avoid needlessly lengthy procedures. As already discussed (see Sections 13.2.3 and 13.3.1), it is not always necessary to perform a MS full calibration every day. For example, if a particular MS is used only to record complete full-scan mass spectra, a daily calibration or verification of the calibration of the m/z ratio scale is required. However, in the case where a MS is coupled with an LC and utilized primarily for the analysis of one or more analytes in the selected ion monitoring (SIM) mode, it does not always require a daily verification of the calibration. In this specific case it is quite common in LC-MS and LC-MS/MS applications to test only the following performance parameters (a) sensitivity, (b) system precision,... 

This review focuses on the phenomenon of molecular SIMS—that is, the physical and chemical bases for its many analytical applications. The applications themselves are also reviewed. The coverage is somewhat historical, emphasizing progress which has come out of this and other laboratories in the past five years. SIMS is discussed in the context of experiments using related desorption ionization (DI) methods, especially laser desorption (LD) and fast atom bombardment (FAB). 

A sensitive and rapid chromatographic procedure using a selective analytical detection method (electrospray ionization-mass spectrometry in SIM mode) in combination with a simple and efficient sample preparation step was presented for the determination of zaleplon in human plasma. The separation of the analyte, IS, and possible endogenous compounds are accomplished on a Phenomenex Lima 5-/rm C8(2) column (250 mm x 4.6 mm i.d.) with methanol-water (75 25, v/v) as the mobile phase. To optimize the mass detection of zaleplon, several parameters such as ionization mode, fragmentor voltage, m/z ratios of ions monitored, type of organic modifier, and eluent additive in the mobile phase are discussed. Each analysis takes less than 6 min. The calibration curve of zaleplon in the range of 0.1-60.0 ng/ml in plasma is linear with a correlation coefficient of >0.9992, and the detection limit (S/N = 3) is 0.1 ng/ml. The within- and between-day variations (RSD) in the zaleplon plasma analysis are less than 2.4% (n = 15) and 4.7% (n = 15), respectively. The application of this method is demonstrated for the analysis of zeleplon plasma samples [14]. 

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