Preparation surface analysis

Nineteen bone samples were prepared for analysis of the trace elements strontium (Sr), rubidium (Rb), and zinc (Zn). The outer surface of each bone was removed with an aluminum oxide sanding wheel attached to a Dremel tool and the bone was soaked overnight in a weak acetic acid solution (Krueger and Sullivan 1984, Price et al. 1992). After rinsing to neutrality, the bone was dried then crushed in a mill. Bone powder was dry ashed in a muffle furnace at 700°C for 18 hours. Bone ash was pressed into pellets for analysis by x-ray fluorescence spectrometry. Analyses were carried out in the Department of Geology, University of Calgary. 

This equation predicts a value of 26.8%ofor the zebra at Turkana assuming an average value of 6%o for Lake Turkana water. This predicted value is l%o less than the actual value of 27.8%o. Given the variation in methods of sample preparation and analysis, variation between bone and tooth enamel (Stuart-Williams and Schwarcz 1997), and uncertainty in surface water oxygen isotopic composition, these values are extraordinarily close. Alternatively, if the equation is solved for using the actual value of the Turkana zebra. 

Castro RJ, Cabrera CR (1997) Photovoltammetry and surface analysis of MoSea thin films prepared by an intercalation-exfoliation method. J Electrochem Soc 144 3135-3140... 

A typical sample would have a surface area of the order 10 x 20 mm. The preparation of the surface for examination is the subject of an ASTM standard (ASTM E1078-97), and the objective is to ensure that the surface to be analysed has not been contaminated or altered prior to analysis. The techniques of surface analysis are sensitive to surface layers only a few atoms thick, so the degree of cleanliness required will be much greater than for other forms of analysis. Nothing must be allowed to touch the surface to be analysed. 

ASTM (1997) Standard Guide for Procedures for Specimen Preparation and Mounting in Surface Analysis E1078-97. 

Figure 6. Plan of the target preparation facilities consisting of UHV preparation chamber (a), (reactive) ion etching chamber (b), ion etching gun (c), laser (d), photon detector (e), transfer arms (f), Auger system for surface analysis (g), sample manipulator and annealing facility (h), load lock and optical microscope for viewing sample (i), evaporator (j), transmission diffractometer (k), and vacuum tank for main spectrometer (1).

Desorption Electrospray Ionization (DESI). DESI is a novel gentle ionization method for surface analysis (Figure 2.6).[19,20] Like classical ESI, it operates at atmospheric pressure. No sample preparation is required. A solvent passes through the capillary of the electrospray source charged droplets are produced (primary ions) and they are directed to a solid sample. Their impact with the surface causes sample molecules to be ionized and... 

Mass spectrometric measurements of ions desorbed/ionized from a surface by a laser beam was first performed in 1963 by Honig and Woolston [151], who utilized a pulsed mby laser with 50 p,s pulse length. Hillenkamp et al. used microscope optics to focus the laser beam diameter to 0.5 p,m [152], allowing for surface analysis with high spatial resolution. In 1978 Posthumus et al. [153] demonstrated that laser desorption /ionization (LDI, also commonly referred to as laser ionization or laser ablation) could produce spectra of nonvolatile compounds with mass > 1 kDa. For a detailed review of the early development of LDI, see Reference 154. There is no principal difference between an LDI source and a MALDI source, which is described in detail in Section 2.1.22 In LDI no particular sample preparation is required (contrary to... 

MALDI, which is LDI utilizing a particular sample preparation). Although the performance of MALDI is superior to LDI in the analysis of many groups of compounds, LDI is still the perferred choice in some important applications, including cmde oil analysis [155], fullerene detection in rocks [156], atmospheric aerosol analysis [157], semiconductors, and surface analysis [158]. Reference 21 is a comprehensive review of the use of LDI (and several other ion sources) in analysis of inorganics. 

Membrane morphology is studied with scanning electron microscopy (SEM) thereby providing an Insight into the relationship between asymmetric membrane preparation, structure, and performance (29,3A). The extent of ion exchange of the salt form of the SPSF membranes is studied with atomic absorption spectroscopy (AAS), neutron activation analysis (NAA), and ESCA. AAS is used for solution analysis, NAA for the bulk membrane analysis, and ESCA for the surface analysis. 

UHV surface preparation and analysis chamber, a variable pressure STM chamber, and a load lock and sample transfer system. Fig. 11 shows a schematic of the system. 

The surface of a solid sample interacts with its environment and can be changed, for instance by oxidation or due to corrosion, but surface changes can occur due to ion implantation, deposition of thick or thin films or epitaxially grown layers.91 There has been a tremendous growth in the application of surface analytical methods in the last decades. Powerful surface analysis procedures are required for the characterization of surface changes, of contamination of sample surfaces, characterization of layers and layered systems, grain boundaries, interfaces and diffusion processes, but also for process control and optimization of several film preparation procedures. 

Although laser-ablation sample preparation and analysis are conducted with relative ease, quantification of data can prove challenging. With liquid samples, the amount of material introduced into the ICP-MS remains relatively constant, and instrument drift is usually corrected through the use of internal standards. However, in LA-ICP-MS, conditions such as the texture of the sample, ablation time, the location of the sample within the laser cell, surface topography, laser... 

The compositions of the ceramic glazes were examined using laser-ablation inductively coupled-mass spectroscopy (LA-ICP-MS) at the University of Missouri Research Reactor (MURR). LA-ICP-MS is a surface analysis technique requiring little sample preparation. Because of its small spot size, areas of weathered glaze could be avoided during analysis (24). 

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