Surface mass spectrometry, analytical method Applications

There are a variety of HPLC columns and most of them are based on silica particles. The most popular column used today is the reversed-phase Cl8 column that uses a silica support with a bonded organic surface layer. Traditional HPLC analytical columns are usually 4.6 mm x 250 mm with a 5 pm particle size, as used in the USP official method. Modern columns for HPLC-mass spectrometry (LC-MS) applications are more efficient and offer the same or better resolving power in a much smaller package (2.1 mm x 150 mm with a 3.5 pm particle size or smaller). Ultra high-performance liquid chromatography (UHPLC) columns (sub 2pm particle size, 1-2 mm in diameter and 30-100 mm in length) are becoming more and more popular. 

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... 

Use of inductively coupled plasma-mass spectrometry (1CP-MS) coupled to a laser-ablation sample introduction system (LA-ICP-MS) as a minimally destructive method for chemical characterization of archaeological materials has gained favor during the past few years. Although still a relatively new analytical technique in archaeology, LA-ICP-MS has been demonstrated to be a productive avenue of research for chemical characterization of obsidian, chert, pottery, painted and glazed surfaces, and human bone and teeth. Archaeological applications of LA-ICP-MS and comparisons with other analytical methods are described. 

One of the most significant developments in mass spectrometry in the recent years is the introduction of a new class of ionization methods where samples in either solid or liquid state can be directly ionized in their native environment under ambient conditions (rather than inside a mass spectrometer) without any sample preparation. This new class of ionization methods is often referred to as ambient ionization methods [1,2], Because these methods generally ionize analytes on the surface or near the surface of the samples at atmospheric pressure, they have also been called atmospheric pressure surface sampling/ionization methods or direct/open air ionization methods [3], Since the first reports on ambient ionization with desorption electrospray ionization (DESI) [4] and direct analysis in real time (DART) [5], numerous reports have been published on the applications of these new ionization methods as well as the introduction of many related ambient ionization methods such as desorption atmospheric pressure chemical ionization (DAPCI) [6], atmospheric solid analysis probe (ASAP) [7], and electrospray-assisted laser desorption/ionization (ELDI) [8], Recently, two reviews of the various established and emerging ambient ionization methods have been published [2,3],... 

There are numerous other ionization methods, but they have limited applications. Fast atom bombardment (FAB), also known as liquid secondary ion mass spectrometry (LSIMS), was one of the early methods developed for the ionization of polar molecules. FAB is based on bombarding analytes in a matrix of low volatility, such as glycerol, with accelerated energetic neutral atoms (argon or xenon) or ions (cesium) that wiU sputter [M + H]+ ions from the surface. Although of major importance during its heyday, FAB has been superseded by ESI. 

The surface properties of polymers are important in many applications and they are dependent on the structure and composition of the ontermost molecular layers. The surface layer thickness involved is typically of the order of a few nanometers. Understanding surface structure-property relationships therefore requires analytical techniques which have this degree of surface sensitivity (or specificity). Two techniques stand out X-ray photoelectron spectroscopy (XPS) (1), also known as ESCA (electron spectroscopy for chemical analysis), and secondary ion mass spectrometry (SIMS) (2). The information provided by these methods is highly complementary and they are frequently used in combination. This article describes the physical bases and anal5dical capabilities of XPS and SIMS and illustrates their application in polymer surface characterization (3). 

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