Surface analytical methods, comparison

Table 9.18 Comparison of analytical methods for surface analysis. 

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. 

Example 5.3 The Semi-infinite Solid with Variable Thermophysical Properties and a Step Change in Surface Temperature Approximate Analytical Solution We have stated before that the thermophysical properties (k, p, Cp) of polymers are generally temperature dependent. Hence, the governing differential equation (Eq. 5.3-1) is nonlinear. Unfortunately, few analytical solutions for nonlinear heat conduction exist (5) therefore, numerical solutions (finite difference and finite element) are frequently applied. There are, however, a number of useful approximate analytical methods available, including the integral method reported by Goodman (6). We present the results of Goodman s approximate treatment for the problem posed in Example 5.2, for comparison purposes. 

Layer charges can be calculated from mineral and chemical composition. Mineral composition can be determined by the comparison of x-ray diffraction and thermal analytical and surface area studies. Chemical composition is determined by a total chemical analysis of the sample. In the classical method, chemical analysis is made after acidic dissolution (Ross and Hendricks 1945). Nowadays, nondestructive analytical methods (e.g., electron microscopy, prompt gamma activation analysis, etc.) are also applied. Chemical composition is usually given as oxides (e.g., Si02, A1203, etc.). The cations are divided into three groups ... 

The opponents of fundamental studies with idealized electrocatalysts and reactions cannot deny the unique insight into surface molecular and electronic or energetic interactions that new surface and mechanistic techniques generate. A combination of surface spectrometries, isotopic reactions, and conventional electrode kinetics could help unravel some of the surface mysteries. The application of such methods in electrocatalysis is limited at present to hydrogen and oxygen reactants on simple catalytic surfaces. Extension to a variety of model and complex reactions should be attempted soon. The prospective explorer, however, should strive and attend with care the standardization of analytical methods for meaningful interpretations and comparisons. 

Advanced analytical methods enable an in-depth study of chemical and morphological characteristics of micro- and nanografted polymer materials. Often, the combination of several techniques is necessary to obtain a detailed picture. Investigations of simplified model systems such as nonstructured grafted surfaces, brushes produced on nonpoly-meric substrates, or selectively derivatized or stained samples are needed for comparison or as standards. Furthermore, the adaptation of biochemical and chemical assay techniques is useful to complete the picture of the produced structures and their functionalities. 

Yakes BJ, Deeds J, White K, DeGrasse SL. Evaluation of surface plasmon resonance biosensors for detection of tetrodotoxin in food matrices and comparison to analytical methods. J Agri Food Chem 2011 59 839—46. 

At X-ray fluorescence analysis (XRF) of samples of the limited weight is perspective to prepare for specimens as polymeric films on a basis of methylcellulose [1]. By the example of definition of heavy metals in film specimens have studied dependence of intensity of X-ray radiation from their chemical compound, surface density (P ) and the size (D) particles of the powder introduced to polymer. Have theoretically established, that the basic source of an error of results XRF is dependence of intensity (F) analytical lines of determined elements from a specimen. Thus the best account of variations P provides a method of the internal standard at change P from 2 up to 6 mg/sm the coefficient of variation describing an error of definition Mo, Zn, Cu, Co, Fe and Mn in a method of the direct external standard, reaches 40 %, and at use of a method of the internal standard (an element of comparison Ga) value does not exceed 2,2 %. Experiment within the limits of a casual error (V changes from 2,9 up to 7,4 %) has confirmed theoretical conclusions. 

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