Microprobes , lead analysis

The primary methods of analyzing for lead in environmental samples are AAS, GFAAS, ASV, ICP/AES, and XRFS (Lima et al. 1995). Less commonly employed techniques include ICP/MS, gas chromato-graphy/photoionization detector (GC/PID), IDMS, DPASV, electron probe X-ray microanalysis (EPXMA), and laser microprobe mass analysis (LAMMA). The use of ICP/MS will become more routine in the future because of the sensitivity and specificity of the technique. ICP/MS is generally 3 orders of magnitude more sensitive than ICP/AES (Al-Rashdan et al. 1991). Chromatography (GC,... 

The origin of lead present in individual calcite particles could be ascribed by the LAMMA (laser microprobe mass analysis) technique. At low laser irradiances, the desorption mode, information is gathered on metallic species adsorbed on the surface of the particle. At high irradiances the particle is evaporated, revealing the components that coprecipitated with calcite111. 

Eeckhaoudt S, Vandeputte D, Van Praag H, et al. 1992. Laser microprobe mass analysis (LAMMA) of aluminum and lead in fine roots and their ectomycorrhizal mantles of Norway spruce (picea abies (1.) karst.). Tree Physiol 10 209-215. 

A number of techniques are available, including laser microprobe mass analysis (LAMMA) and various microprobes, that are capable of determining within tissues or cell preparations the cellular and subcellular distribution of lead in situ. While these techniques generally require varying levels of sample preparation (e.g., tissue fixation, cell suspensions, etc.), they provide powerful tools for probing different cellular compartments and processes involving lead. Thus, the site-specific distribution of lead can be used to evaluate local toxicity, which can be correlated with pathological alterations in tissues. 

LAMM A. Laser microprobe mass analysis was specifically developed to complement other microanalytical techniques to determine intracellular distributions of physiological cations and toxic constituents in biological tissues. LAMMA is an analytical methodology capable of simultaneous multielement analysis of metals and their distribution on a cellular or subcellular scale, with a measurement sensitivity of 10" to 10" " g for most metals. LAMMA has received somewhat widespread use in the analysis of essential and toxic metals in tissues and cell preparations (Drueke 1980 Goebel et al. 1990 Schmidt and Barckhaus 1991 Schmidt et al. 1980, 1986 Vandeputte et al. 1985 Verbueken et al. 1984 Visser et al. 1984). The detection sensitivity of LAMMA for lead is 5 /rg/g, with a limit of detection of approximately 2 X 10" g (Schmidt and Barckhaus 1991). 

Vandeputte D, Verbueken A, Jacob W, Van Grieken R (1985) Laser microprobe mass analysis (LAMMA) to study lead intoxication at the subcellular level. Acta Pharmacol Toxicol 59(Suppl VII) 617-629. 

Soluble pigments The most important pigments in this class are the metallic chromates, which range in solubilities from 17 0 to 0-00005 g/1 CrO . An examination has recently been carried out of the mechanism of inhibition by chromate ions and it has been shown by chemical analysis of the stripped film, Mdssbauer spectroscopy and electron microprobe analysis that the air-formed film is reinforced with a more protective material in the form of a chromium-containing spinel (Chapter 17). The situation is, however, complicated by the possibility that some chromates, particularly the basic ones, may inhibit through the formation of soaps. There is evidence that lead chromate can function in this way. 

Table V summarizes the data on the lead concentration obtained by electron microprobe analysis of the objects. It was not possible to determine any data on lead from x-ray fluorescence, and NAA cannot be used for lead. The sensitivity of the electron microprobe for lead is poor, and the precision was 15%. These data suggest that the lead content in the silver objects is consistently low and that lead ore refining was well developed.

The presence of small lead inclusions is easily established by using the x-ray modulation method on the microprobe. We believe that a lineal intercept analysis from pictures taken by this method is probably the most accurate if the electron microprobe is used. 

Lead curse tablets from Roman Carthage contain variable amounts of very small metallic inclusions. Electron microprobe analysis confirmed these metallic inclusions were bronze, brass, and a Sn-Sb alloy. This was interpreted as possible evidence of lead metal recycling. Six samples were chosen to represent a range of tablets containing the minimum to the maximum number of inclusions. Thermal ionization mass spectrometry of the Pb isotopes in the curse tablets appear to define a mixing line, with the tablets containing the least number of inclusions plotting closest to the Tunisian lead ore isotope ratios. 

A.D. were found in old mines, and sizable slag deposits suggest at least some level of lead exploitation during Roman times (2). By the careful selection of Roman lead artifacts likely to have been manufactured in Carthage, and the use of lead isotope analysis, it may be possible to confirm the use of Tunisian lead ores during the Roman period. In this preliminary study, analysis of 22 curse tablets by electron microprobe analysis (EMPA) and six tablets by thermal ionization mass spectrometry (TIMS) suggest that these artifacts might be used to better understand Roman lead use and trade. 

For surface structure studies, perhaps the most popular technique has been LEED (373). Elastically diffracted electrons from a monoenergetic beam directed to a single-crystal surface reveal structural properties of the surface that may differ from those of the bulk. Some applications of LEED to electrocatalyst characterization were cited in Section IV (106,148,386). Other, less specific, but valuable surface examination techniques, such as scanning electron microscopy (SEM) and X-ray microprobe analysis, have not been used in electrocatalytic studies. They could provide information on surface changes caused by reaction, some of which may lead to catalyst deactivation (256,257). Since these techniques use an electron beam, they can be coupled with previously discussed methods (e.g. AES or XPS) to obtain a qualitative mapping of the structure and composition of a catalytic surface. 

Silver is reported to segregate to the grain and sub-grain boundaries of lead-calcium-tin alloys [94]. Microprobe analysis of the cross-section of grid wires produced from cast and rolled lead-calcium-tin alloys with a bulk silver content of... 

McKeegan and Leshin, this volume). Typically, spot size is 10-30 pm in diameter and 1-5 pm deep. Over short distances normal to a flat surface, sub-micron spatial resolution is possible by depth profiling (Valley and Graham 1991). The recent development of multiple collectors for ion microprobes has lead to a major reduction in analysis time and promises enhanced accuracy and precision. 

Having made these qualitative observations on the parameters that control poisoning, we subjected the catalysts to detailed analysis. As in our earlier poisoning study (3), electron microprobe analysis revealed that the poison accumulated almost exclusively at the outer edge of the catalyst pellet. The relative concentrations of lead and sulfur, as well as x-ray diffraction, suggest that the lead was primarily in the form of lead sulfate (3, 6). The findings from a typical microprobe analysis of a poisoned catalyst are presented in Figure 6. 

Ma, whereas ion microprobe analyses yielded 934 4 Ma. Zhu et al. (1998) explores potential matrix effects during monazite ion microprobe analysis, but analytical methods outlined in their paper preclude conclusive interpretations. Stem and Sanborn (1998) report that the use of high-Th monazite standards may lead to errors in measuring ages of low-Th grains, and suggest the use of compositionally matched standards and unknowns. 

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