Destructive analysis

Beyond these issues of concern to all archaeologists, there are some specific topics particularly relevant to archaeometry and archaeological chemistry. We discuss two of these - destructive analysis and the study of human remains - in more detail below. 

Our position as archaeological scientists is that materials from the past are collected, 

At the same time, only a small, usually a tiny, amount of material is needed. 

It is also the case that some materials require a bit more material in order to obtain an accurate analysis. For homogeneous materials, a few milligrams will suffice, but for heterogeneous materials such as pottery and some rocks, one must take a sample that represents the whole, as an average. For coarsely tempered pottery, this might require a gram or more, regardless of the instrument used for analysis. 

This issue of destructive analysis also involves the question of human remains, since small amounts of bone and other tissues are often destroyed when scientific analysis is undertaken. Human remains are the subject of the next section. 

Determination of nuclear material content and, if required, of the isotopic composition of 

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A comprehensive program that includes predictive maintenance techniques to monitor and analyze critical machines, equipment, and systems in a typical plant. Techniques include vibration analysis, ultrasonics, thermography, tribology, process monitoring, visual inspection, and other non-destructive analysis methods. 

Various destructive and non-destructive methods of analysis have been tested and H-l and C-13 NMR have, among other techniques provided valuable structural information on soluble humic acids and fulvic acids 48, Humin, on the other hand has withstood detailed non-destructive analysis. 

A flat surface required for best depth resolution and for ion microscopy Destructive analysis. 

Analysis by the Detection of X-rays or y rays. EPMA is a fully qualitative and quantitative method of non-destructive analysis of micrometre-sized volumes at the surface of materials, with sensitivity at the level of ppm. All elements from Be to U can be analysed, either in the form of point analysis, from line scans and also as X-ray distribution maps. Current software allows the combination of elemental data in the latter, so that, for example, the digital data for those elements that corresponds to a selected phase will produce an X-ray map of the distribution of that phase in a given microstructure. 

Gratuze, B., J. N. Barrandon, K. A1 Isa, and M. C. Cauvin (1993), Non-destructive analysis of obsidian artefacts using nuclear techniques Investigation of provenance of Near Eastern artefacts, Archaeometry 35,11-21. 

E. Darque Ceretti and M. Aucouturier, Secondary ion mass spectrometry. Application to archaeology and art objects, in Non destructive Analysis of Cultural Heritage Materials, K. Janssens and R. Van Grieken (eds), Comprehensive Analytical Chemistry XLII, Elsevier BV, Amsterdam, 2004, pp. 397 461. 

Non-destructive analysis is especially valuable in an on line situation. X-ray fluorescence has above all become of major importance for the analysis of inorganic process streams. Cement production is an example of the successful application of this technique. The X-ray analyser can be used for the simultaneous assay of the various feedstocks (iron ore, clay and limestone) for Fe203, A1203, Si02 and CaO. In turn the signals from the analyser are used to control the feedstock supplies to the blending mill and to maintain an optimum product composition. 

ABSTRACT The aim of this study was to test portable infrared spectroscopy for non-destructive analysis of ancient construction mortar. Mortar samples from the House of the Vestals, in Pompeii, Italy, were initially examined with traditional analytical techniques, including X-ray fluorescence, X-ray diffraction and thin section analysis. These techniques were used to establish mineralogical and chemical profiles of the samples and to verify the results of experimental field methods. Results showed the lime-based binder was composed of calcite, and the volcanic sand aggregate contained clinopyroxene, plagioclase, sanidine and olivine crystals. 

The high sensitivity of modem instrumental techniques such as ICP-MS (Chapter 9) means that in many cases only small samples (typically, a hundred milligrams or less) need be taken for destructive analysis. However, this also means that the amounts of some individual elements may be very low, and problems of contamination can be significant. Common external contaminants include A1 from deodorants, Pb from paint or car exhausts, Zn from skin particles (and therefore from dust), and Na from sweat. The levels of contamination for each batch of samples will be revealed by the sample... 

Williams-Thorpe, O., Potts, P. J., and Webb, P. C. (1999). Field-portable non-destructive analysis of lithic archaeological samples by X-ray fluorescence instrumentation using a mercury iodide detector Comparison with wavelength-dispersive XRF and a case study in British stone axe provenancing. Journal of Archaeological Science 26 215-237. 

Elemental analysis of sample digests Non-destructive analysis of solid samples... 

A number of conclusions may be drawn from this discussion of the destructive analysis of samples. 

Destructive analysis will continue to be necessary, for many types of samples, owing to the nature of certain samples. The complexity of the composition of some samples often imposes use of a separation step prior to the analysis itself. Furthermore, the classical techniques are... 

Destructive analysis is also necessary when there is a need to concentrate the components of a given sample, the components being present at very low concentrations (or in traces), often in a very complex matrix. 

The techniques of destructive analysis involve taking some special precautions concerning the sampling in general, and the dissolution-decomposition process in particular, in order to avoid the risk of contamination. 

The techniques of destructive analysis may lead to reliable analytical results only if the analytical process is correctly planned, by taking into account the interdependence of all the operational parameters of the process. 

Considering these conclusions, it is apparent that, destructive analysis still has a place in the analysis of soils and sediments—and for this very reason, we should correlate the necessary knowledge so as to simplify as much as possible the analytical process. Such an action is necessary in order to shorten the analysis time. 

There is no such thing as a completely non-destructive analysis. Upon interaction of the beam with the sample, a series of surface-disruption phenomena can occur. This fact is illustrated in Table 14.10 for the four major surface analysis techniques mentioned above. The least surface disruption occurs in ESCA and the measurements are characteristic of the surface. However, when charged particles such as electrons and ions are... 

Collaborative Testing. A second approach to assessing accuracy, when no certified reference material is available, may be used in conjunction with analysis by independent methods and in-house materials. Sample exhanges with other laboratories can help establish the existence or absence of systematic errors in a method. Collaborative tests are most useful in this regard when some of the participating laboratories use different sample preparation and quantification. The utility of independent analysis methods and comparisons between destructive and non-destructive analysis is again emphasized here. 

A number of methods can assist in identifying and characterizing enol intermediates (as well as eneamine and carbanion intermediates) in enzyme-catalyzed reactions. These include (1) proton isotope exchange (2) oxidation of the intermediate (3) coupled elimination (4) spectrophotometric methods (5) use of transition-state inhibitors (6) use of suicide inhibitors (7) isolation of the enol and (8) destructive analysis. 

Dey, AK, Ghose AK, ShuMa DK (1981) A modified ring electrographic method for the non-destructive analysis of metaUic artefacts. Mikrochim Acta 11 175-181. 

Gordus, A. A., Non-Destructive Analysis of Parthian, Sasanian, and Umay-... 

In 2006, a table-top energy-dispersive XRF (ED-XRF) spectrometer was acquired by the Archaeometry Lab to facilitate non-destructive analysis of obsidian and other types of artifacts. One of the first projects performed on the new XRF spectrometer was the re-analysis of the geological samples from sources in Peru. As a result, it is now possible for the Archaeometry Lab to use either XRF or NAA to successfully determine the provenance of obsidian artifacts from Peru. Due to its light weight, the spectrometer also has the potential to be transported from the laboratory to museums and to archaeological sites for in situ analysis. 

Since MURR acquired the Elva-X ED-XRF spectrometer, investigations of its capability with respect to Andean obsidian have been ongoing. Although the measurement precision for XRF is less than NAA, when a rapid, non-destructive analysis is required XRF can be used quite successfully. As shown in Figures 5 and 6, the elements Rb, Sr, and Fe indicate no overlap at the 95% confidence level. Thus, these elements are then the most powerful discriminating elements available by XRF for the sources in this region. 

Balas, K. 8c Pelecoudas, D. Imaging Method and Apparatus for the Non-Destructive Analysis of Paintings and Monuments US Patent Application Publication 2003/0117620 Al Filed in 2000. 

The rapid and non-destructive analysis features of NIR make it an ideal method to investigate film-coated tablets. Kirsch and Drennen101 analyzed theophylline tablets... 

NIR in the diffuse reflectance mode is a technique that also allows non-destructive analysis of polymers with very little or no sample preparation [80, 81]. NIR is based on measurement of light reflected by the sample when exposed to electromagnetic radiation in the range from 780 nm (12820 cm-1) to 2500 nm (4000 cm-1). Qualitatively this is the region be-... 

In order to overcome these problems, interest was focussed on that portion of the organic matter trapped in mineral precipitates which formed synchronously with sedimentation. In these cases, the material is hermetically sealed in the crystalline matter and may survive with relatively little subsequent alteration. Such preservation is common in cherts which are chemical precipitates of silica and now comist of fine grained quartz. These rocks offer the best chance for successful preservation of truely Precambrian molecular fossils. Modem microprobes and spectrophotometer microscopes allow the non-destructive analysis of organic matter enclosed in mineral crystals. Laser bombardment of microscopic... 

The use of 14 MeV neutron activation principally for major elements, Ge(Li) detectors for trace elements following thermal neutron irradiations, and gamma-gamma coincidence techniques for positron or cascade gamma-ray emitters as discussed in the previous sections, provide the analyst with powerful tools for devising schemes for non-destructive analysis. A few additional activation techniques which may be useful in special applications are discussed briefly below. In most of these cases rather sophisticated instrumentation is required. It is unlikely, therefore, that these techniques will be in routine use in a facility devoted principally to analytical applications. In some cases, however, arrangements may be made for part time use of a more extensive nuclear facility for a specific analytical problem. 

Summarizing, XPS is a very powerful surface technique, analyzing specifically the upper layer (0.3 - 3 nm) of the substrate. It is a non-destructive analysis tool, detecting any element (except hydrogen) that is present above 0.1%. Quantitative as well as qualitative information can be obtained. 

Megaelectron volt (MeV) ion beam techniques offer a number of non-destructive analysis methods that allow to measure depth profiles of elemental concentrations in material surfaces. Elements are identified by elastic scattering, by specific nuclear reaction products or by emission of characteristic X-rays. With nuclear microprobes raster images of the material composition at the surface can be obtained. Particle-induced gamma-ray emission (PIGE) is especially suited for fluorine detection down to the ppm concentration level. 

Analytical technique Non-destructive analysis possible (conservation of the sample after analysis) Sample quantity required Sample preparation Analysis type Spatial resolution Limit of detection... 

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