Trace element spectroscopy

Trace-element analysis of metals can give indications of the geographic provenance of the material. Both emission spectroscopy (84) and activation analysis (85) have been used for this purpose. Another tool in provenance studies is the measurement of relative abundances of the lead isotopes (86,87). This technique is not restricted to metals, but can be used on any material that contains lead. Finally, for an object cast around a ceramic core, a sample of the core material can be used for thermoluminescence dating. 

Trace-element analysis, using emission spectroscopy (107) and, especially, activation analysis (108) has been appHed in provenance studies on archaeological ceramics with revolutionary results. The attribution of a certain geographic origin for the clay of an object excavated elsewhere has a direct implication on past trade and exchange relationships. 

Chemical Properties. Elemental analysis, impurity content, and stoichiometry are determined by chemical or iastmmental analysis. The use of iastmmental analytical methods (qv) is increasing because these ate usually faster, can be automated, and can be used to determine very small concentrations of elements (see Trace AND RESIDUE ANALYSIS). Atomic absorption spectroscopy and x-ray fluorescence methods are the most useful iastmmental techniques ia determining chemical compositions of inorganic pigments. Chemical analysis of principal components is carried out to determine pigment stoichiometry. Analysis of trace elements is important. The presence of undesirable elements, such as heavy metals, even in small amounts, can make the pigment unusable for environmental reasons. 

The boron nitride obtained in this study was characterized by infrared spectroscopy, powder x-ray diffractometry and transmission electron microscopy. Trace elemental analyses were also performed by energy dispersive x-ray analysis and carbon arc emission spectroscopy. Representative spectra are displayed in Figures 2-4. 

Chemical Analysis. The chemical composition of ancient objects is important for their authentication. The nature as well as the relative amounts of major, minor, and trace elements in any object are of use for determining the authenticity or otherwise of ceramics, glass, or alloys. A wide range of analytical techniques, depending on the nature of the material studied, have been used for this purpose, including X-rays fluorescence analysis, mass spectrometry, atomic absorption spectroscopy, and neutron activation analy-... 

Vol. 51 Trace Element Analysis of Geological Materials. By Roger D. Reeves and Robert R. Brooks Vol. 52 Chemical Analysis by Microwave Rotational Spectroscopy. By Ravi Varma and Lawrence... 

Chong et al. [742] have described a multielement analysis of multicomponent metallic electrode deposits, based on scanning electron microscopy with energy dispersive X-ray fluorescence detection, followed by dissolution and ICP-MS detection. Application of the method is described for determination of trace elements in seawater, including the above elements. These elements are simultaneously electrodeposited onto a niobium-wire working electrode at -1.40 V relative to an Ag/AgCl reference electrode, and subjected to energy dispersive X-ray fluorescence spectroscopy analysis. Internal standardisation... 

Stump, I.G., J. Kearney, J.M. D Auria, and J.D. Popham. 1979. Monitoring trace elements in the mussel, Mytilus edulis using X-ray energy spectroscopy. Mar. Pollut. Bull. 10 270-274. 

The Association of Official Analytical Chemists is utilizing atomic absorption spectroscopy for the determination of several trace elements. McBride 274>27s), has conducted collaborative and ruggedness studies for a number of elements in fertilizers. He dissolves the sample in hydrochloric acid, filters, and dilutes to vo-... 

Nixon277 compared atomic absorption spectroscopy, flame photometry, mass spectroscopy, and neutron activation analysis as methods for the determination of some 21 trace elements (<100 ppm) in hard dental tissue and dental plaque silver, aluminum, arsenic, gold, barium, chromium, copper, fluoride, iron, lithium, manganese, molybdenum, nickel, lead, rubidium, antimony, selenium, tin, strontium, vanadium, and zinc. Brunelle 278) also described procedures for the determination of about 20 elements in soil using a combination of atomic absorption spectroscopy and neutron activation analysis. 

Concentrations of major cations in all samples were determined by acetylene flame Atomic Absorption Spectroscopy at the Trace Element Analytical Laboratories (TEAL) of McGill University. Analyses of trace element concentrations were canied out using Inductively Coupled Plasma Quadrupole Mass Spectrometry (also at TEAL). Concentrations of anions were determined by Ion Chromatography at the Hydrogeology Laboratory at McGill University. 

Casetta, B., Giaretta, A., and Mezzacasa, G. (1990). Determination of rare earth and other trace elements in rock samples by ICP-mass spectrometry comparison with other techniques. Atomic Spectroscopy 11 222-228. 

Trace Analysis Spectroscopic Methods for Elements. Edited by J. D.Winefordner Contamination Control in Trace Element Analysis. By Morris Zief and James W. Mitchell Analytical Applications of NMR. By D. E. Leyden and R. H. Cox Measurement of Dissolved Oxygen. By Michael L. Hitchman Analytical Laser Spectroscopy. Edited by Nicolo Omenetto... 

Studies of the inorganics in cotton dust have incorporated the use of a wide variety of techniques. These include X-ray fluorescence spectroscopy, atomic absorption spectroscopy, electron microscopy, energy dispersive analysis of X-rays, X-ray diffraction, atomic absorption spectroscopy, neutron activation analysis and petrographic microscopy. It is necessary to use a wide array of techniques since no single technique will permit the measurement of all trace elements. Steindard chemical techniques to determine the ash content of samples and of various extracts have also been used. In most of these studies the ash fraction has been considered to be a reasonably accurate measure of the inorganic content. 

In the other study. X-ray fluorescence spectroscopy was used to analyze trace element concentrations by observing dusts on 37 ram diameter cellulose acetate filters (20). Twenty-three elutriator and twenty-three area samples from 10 different bales of cotton were analyzed. The average fraction of total dust accounted for by the elements analyzed was 14.4% amd 7.6% for vertical elutriator and area samples, respectively. Although the variation in absolute quantity of atn element was high, the relative abundance of an element was consistent for measurements within a bale. Averaged over all the samples analyzed, calcium was the most abundant element detected (3.6%), followed by silicon (2.9%), potassium (2.7%), iron (1.1%), aluminum (1.1%), sulfur (1.0%), chlorine (0.8%) and phosphorous (0.6%). Other elements detected in smaller aunounts included titanium, manganese, nickel, copper, zinc, bromine, rubidium, strontium, barium, mercury amd lead. 

Major and trace element concentrations in the acidified samples were determined via ICP-MS (inductively coupled plasma mass spectrometry) and ICP-OES (inductively coupled plasma optical emission spectroscopy) at the GSC s Geochemistry Research Laboratory. Dissolved anion concentrations were measured by 1C (ion chromatography) on the unacidified samples, also at the GSC s Geochemistry Research Laboratory. Characterization of the sediment mineralogy and texture by XRD (X-ray diffraction), SEM (scanning electron microscopy) and TEM (transmission electron microscopy) is ongoing. 

Chapters 7 and 8 describe two major techniques for the monitoring of trace elements in environmental samples atomic absorption (AA) and inductively coupled plasma-atomic emission spectroscopy (ICP). AA is most ideally suited for analyses where a limited number of trace metal concentrations are needed with high accuracy and precision. ICP has the advantage of multielement analysis with high speed. 

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