Furnace atomic absorption, direct analysis

Nowka R, Muller H (1997) Direct analysis of solid samples by graphite furnace atomic absorption spectrometry with a transversely heated graphite atomizer and D2-background correction system (SS GF-AAS). Fresenius J Anal Chem 359 132-137. 

In the determination of cadmium in seawater, for both operational reasons and ease of interpretation of the results it is necessary to separate particulate material from the sample immediately after collection. The dissolved trace metal remaining will usually exist in a variety of states of complexation and possibly also of oxidation. These may respond differently in the method, except where direct analysis is possible with a technique using high-energy excitation, such that there is no discrimination between different states of the metal. The only technique of this type with sufficiently low detection limits is carbon furnace atomic absorption spectrometry, which is subject to interference effects from the large and varying content of dissolved salts. 

H. Muller. Direct Analysis of Solid Samples by Graphite Furnace Atomic Absorption Spectrometry, Fresenius J. Anal. Chem. 1997,359, 132. 

Kueeuest U (1998d) Direct solid sampling with graphite furnace atomic absorption spectrometry (GF-AAS). In Kurfiirst U, ed. Solid Sample Analysis, Direct Slurry Sampling using GF-AAS and ETV-ICP, pp. 129-190. Springer-Verlag, Berlin. 

Inductively coupled plasma-mass spectrometry is one of the most sensitive techniques available for trace analysis. Analyte ions produced in the plasma are directed into the inlet of a mass spectrometer, which separates ions by their mass-to-charge ratio. Ions are measured with a sensitive detector that is similar to a photomultiplier tube. The linear range listed in Table 20-4 extends over eight orders of magnitude, and the detection limit is 100-1 000 times lower than that of furnace atomic absorption. 

Graphite furnace atomic absorption spectrometry (GFAAS) is an excellent method to provide sub-ng/mL minimum detection limits [110]. Continuing advancements such as Zeeman correction, and stabilized temperature platform furnaces, have made GFAAS an effective analytical method for magnesium determination. Depending on the sample matrix, pretreatment can vary from direct analysis of fluids, to wet mineralization, dry ash, acid extraction, and by using PPRs (e.g., Triton X-100). 

De Schrijver, I., Aramendia, M., Resano, M., Dumoulin, A., Vanhaecke, F (2008) Novel strategies for rapid trace element analysis of polyamide by graphite furnace atomic absorption spectrometry and inductively coupled plasma mass spectrometry. Dissolution in an organic solvent versus direct solid sampling approaches. /. Anal. At. Spectrom., 23, 500-507. 

Analytical methods of atomic spectroscopy have been used in forestry and wood product research since their earliest development. Nowadays, almost all of the spectroscopic techniques available are employed in the analysis of metals and trace elements in diverse samples of industrial and environmental origin. The techniques that find most regular application include flame atomic absorption spectroscopy (F-AAS), graphite furnace atomic absorption spectroscopy (GF-AAS), inductively coupled plasma atomic emission spectroscopy (ICP-AES) and, occasionally, also direct current plasma atomic emission spectroscopy (DCP-AES). In many applications F-AAS is a sufficiently sensitive and precise technique however, in the analysis of some environmental samples for trace elements (forest soils, plant material and water) where concentrations may be very low (of the order of 100 ng mL" ) the greater sensitivity of GF-AAS and ICP/DCP-AES is required. In considering the applications of atomic spectroscopy to forestry and... 

Highly sensitive iastmmental techniques, such as x-ray fluorescence, atomic absorption spectrometry, and iaductively coupled plasma optical emission spectrometry, have wide appHcation for the analysis of silver ia a multitude of materials. In order to minimize the effects of various matrices ia which silver may exist, samples are treated with perchloric or nitric acid. Direct-aspiration atomic absorption (25) and iaductively coupled plasma (26) have silver detection limits of 10 and 7 l-lg/L, respectively. The use of a graphic furnace ia an atomic absorption spectrograph lowers the silver detection limit to 0.2 l-ig/L. 

Atomic absorption spectroscopy is an alternative to the colorimetric method. Arsine is stiU generated but is purged into a heated open-end tube furnace or an argon—hydrogen flame for atomi2ation of the arsenic and measurement. Arsenic can also be measured by direct sample injection into the graphite furnace. The detection limit with the air—acetylene flame is too high to be useful for most water analysis. 

Trace element analysis of foods can be carried out to check for contamination by toxic elements, such as lead and cadmium, or to determine beneficial micronutrients, or as an aid to distinguishing geographical origin. In fats, small numbers of trace elements are measured after digestion of the sample in acid followed atomic absorption spectrophotometry (AAS) or by direct graphite furnace vaporization. An AAS procedure for measuring lead in edible oils and fats has been collaboratively trialed with cocoa butter as a test material (Firestone, 1994). 

The few articles currently available regarding trace analysis without preconcentration, use in general the graphite furnace technique [102,120, 138] with sample sizes of the order of microliters, and deal with the elements Sb [47, 83], Pb and Bi [48-50], As, Sb, Bi, Sn, Cd, Pb [10, 57, 116] as well as Al, Cr, Sn [6, 62], Co, and Mg [104]. Alkaline earths can be determined directly with the flame method [122, 147], Further techniques of atomic absorption by flame use concentration methods, for example for the determination of small concentrations of tin [17], Te [26], Co, Pb, and Bi [104], and W [106]. From the analytical viewpoint, it is only useful to remove the iron matrix. The extraction of the elements to be determined from the matrix always carries with it the danger of losses and therefore results showing concentrations that are too low. 

Electrodeposition onto solid electrodes or mercury cathodes is a long established pre-treatment capable of large concentration factors, and provided the cathode potential is carefully controlled it is also of considerable selectivity. When atomic absorption is used as the finish, selective deposition is not usually required. There have been recent reports of electrodeposition of trace metals from water samples directly onto special graphite furnace tubes [8] and this technique should prove to be just as applicable to the analysis of reagents, where the chemical conditions can be more carefully controlled. The utility of electrodeposition for electrothermal atomisation... 

Thermal evaporation of the analyte elements from the sample has long been used in atomic spectrometry. For instance, it had been applied by PreuE in 1940 [170], who evaporated volatile elements from a geological sample in a tube furnace and transported the released vapors into an arc source. In addition, it was used in so-called double arc systems, where selective volatilization was also used in direct solids analysis. Electrothermal vaporization became particularly important with the work of L vov et al. [171] and Massmann in Dortmund [172], who introduced elec-trothermally heated sytems for the determination of trace elements in dry solution residues by atomic absorption spectrometry of the vapor cloud. Since then, the idea has regularly been taken up for several reasons. 

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