Solids atomic absorption spectrometry

Direct atomic absorption spectrometry (AAS) analysis of increasing (e 0,10 g) mass of solid samples is the great practical interest since in a number of cases it allows to eliminate a long-time and labor consuming pretreatment dissolution procedure of materials and preconcentration of elements to be determined. Nevertheless at prevalent analytical practice iS iO based materials direct AAS are not practically used. 

Electrothermal vaporization can be used for 5-100 )iL sample solution volumes or for small amounts of some solids. A graphite furnace similar to those used for graphite-furnace atomic absorption spectrometry can be used to vaporize the sample. Other devices including boats, ribbons, rods, and filaments, also can be used. The chosen device is heated in a series of steps to temperatures as high as 3000 K to produce a dry vapor and an aerosol, which are transported into the center of the plasma. A transient signal is produced due to matrix and element-dependent volatilization, so the detection system must be capable of time resolution better than 0.25 s. Concentration detection limits are typically 1-2 orders of magnitude better than those obtained via nebulization. Mass detection limits are typically in the range of tens of pg to ng, with a precision of 10% to 15%. 

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. 

Pauwels J. De Angelis L, Grobecker KH (1991) Solid sampling Zeeman atomic absorption spectrometry in production and use of certified reference materials. Pure Appl Chem 63 1199-1204. 

Solid Sampling Atomic Absorption Spectrometry ICP Optical Emission Spectrometry ICP Mass Spectrometry... 

Backmank S, Karlsson RW (1979) Determination of lead, bismuth, zinc, silver and antimony in steel and nickel-base alloys by atomic-absorption spectrometry using direct atomization of solid samples in a graphite furnace. Analyst 104 1017-1029. 

Hinds MW (1993) Determination of gold, palladium and platinum in high purity silver by different solid sampling graphite furnace atomic absorption spectrometry methods, Spectrochim Acta 48B 435-445. 

Hofmann C, Vandecasteele C, Pauwels ] (1992) New calibration method for solid sampling Zeeman atomic absorption spectrometry (SS-ZAAS) for cadmium. Fresenius J Anal Chem 342 936-940. 

LtiCKER E, Konig H, Gabriel G, Rosopulo A (1992) Analytical quality control by solid sampling graphite furnace atomic absorption spectrometry in the production of animal tissue reference materials. Fresenius J Anal Chem 342 941-949. 

Pauwels J, Hofmann C, Vandbcasteele C (1994) Calibration of solid sampling Zeeman atomic absorption spectrometry by extrapolation to zero matrix. Fresenius J Anal Chem 348 418-421. 

Magnesium deficiency has been long recognized, but hypermagnesia also occurs (Anderson and Talcott 1994). Magnesium can be determined in fluids by FAAS, inductively coupled plasma atomic emission spectrometry (ICP-AES) and ICP-MS. In tissue Mg can be determined directly by solid sampling atomic absorption spectrometry (SS-AAS) (Herber 1994a). Both Ca and Mg in plasma/serum are routinely determined by photometry in automated analyzers. 

Amoli, H. S. and Simpson, P. Development of an ion chromatography-solid phase extraction atomic absorption spectrometry method for the determination of low level ions in aqueous phase, Biomed. Chromatogr., 12, 304, 1998. 

Table 8.20 Main characteristics of solid sampling in atomic absorption spectrometry...

For the majority of applications, the sample is taken into solution and introduced into the plasma as an aerosol in the argon stream. The sample solution is pumped by a peristaltic pump at a fixed rate and converted into an aerosol by a nebulizer (see atomic absorption spectrometry). Various designs of nebulizer are in use, each having strengths and weaknesses. The reader is directed to the more specialist texts for a detailed consideration of nebulizers. There is an obvious attraction in being able to handle a solid directly, and sample volatilization methods using electric spark ablation, laser ablation and electrothermal volatilization have also been developed. 

Five liquid membrane electrodes (Table 13.3) are now commercially available and have found wide application in the testing of electrolytes in biological and technological systems. All five electrodes perform well in the concentration range over which the Nernstian slope is maintained, i.e., from 10 -10 moldm . These electrodes to a certain extent have replaced in both chemical and clinical laboratories the more traditional instrumental methods of analysis, such as flame photometry and atomic absorption spectrometry. There are, of course, many more liquid membrane electrodes, but the availability of satisfactory solid electrodes has greatly restricted their development and practical application. 

M. J. Cal-Prieto, M. Felipe-Sotelo, A. Carlosena, J. M. Andrade, P. Lopez-Mahia, S. Muniategui and D. Prada, Slurry sampling for direct analysis of solid materials by electrothermal atomic absorption spectrometry (ETAAS). A literature review from 1990 to 2000, Talanta, 56, 2002, 1-51. 

M. C. Yebra and A. Moreno-Cid, On-line determination of manganese in solid seafood samples by flame atomic absorption spectrometry, Anal. Chim. Acta, 477(1), 2003, 149-155. 

A. F. Barbosa, M. G. Segatelli, A. C. Pereira, A. De Santana Santos, L. T. Kubota, P. O. Luccas and C. R. T. Tarley, Solid-phase extraction system for Pb(n) ions enrichment based on multiwall carbon nanotubes coupled on-line to flame atomic absorption spectrometry, Talanta, 71(4), 2007, 1512-1519. 

U. Schaffer and V. Krivan, Analysis of High Purity Graphite and Silicon Carbide by Direct Solid Sampling Electrothermal Atomic Absorption Spectrometry, Fresenius J. Anal. Chem. 2001,371, 859 R. Nowka and... 

Experiments were performed in Teflon-lined titanium autoclaves, submerged in a thermostated oil bath. The supernatant liquors were analyzed using atomic absorption spectrometry. Solid residues were washed with water, dried and examined by the following surface analytical methods ... 

Tawali, A.B. and Schwedt, G. (1997) Combination of solid phase extraction and flame atomic absorption spectrometry (FAAS) for differentiated analyses of labile iron (II) and iron (III) species. Fresenius J. Anal. Chern., 357, 50-55. 

Latif, E., A.K. Aslihan, and S. Mustafa. 2008. Solid phase extraction method for the determination of iron, lead and chromium by atomic absorption spectrometry using Amberite. J. Hazard. Mater. 153 454-461. 

Anthemidis, A.N. and K.-I.G. Ioannou. 2006. Evaluation of polychlorotrifluoroethylene as sorbent material for on-line solid phase extraction systems Determination of copper and lead by flame atomic absorption spectrometry in water samples. Anal. Chim. Acta 575 126-132. 

Soylak, M., L. Elci, and M. Dogan. 2003. Uses of activated carbon columns for solid phase extraction studies prior to determinations of traces heavy metal ions by flame atomic absorption spectrometry. Asian J. Chem. 15 1735-1738. 

A. S. Ribeiro, M. A. Vieira, A. F. Silva, D. L. G. Borges, B. Welz, U. Heitmann, A. J. Curtius, Determination of cobalt in biological samples by line-source and high-resolution continuum source graphite furnace atomic absorption spectrometry using solid sampling or alkaline treatment, Spectrochim. Acta, 60B (2005), 693. 

Graphite Furnace Atomic Absorption Spectrometry Graphite furnace atomic absorption spectrometry (GFAAS), the most popular form of ET-AAS, is today a common technique widely used in routine laboratories and has become a powerful tool for the analysis of trace and ultratrace elements in clinical and biological samples [61]. The main advantages of this technique are low cost, simplicity, excellent detection power, and the fact that it allows very low sample volumes to be used (5-20 p,L). In this sense, this technique allows LoDs for many elements in the order of 0.01 pgl-1 in solution or 1 pg g-1 in solid samples to be achieved [62]. However, the technique is prone to spectral and matrix interferences. 

R. C. Campos, A. J, Curtius, H. Bemdt, Combustion and volatilisation of solid samples for direct atomic absorption spectrometry using silica or nickel tube furnace atomisers, J. Anal. Atom. Spectrom., 5 (1990), 669-673. 

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