Graphite-furnace atomic absorption

A technique is any chemical or physical principle that can be used to study an analyte. Many techniques have been used to determine lead levels. For example, in graphite furnace atomic absorption spectroscopy lead is atomized, and the ability of the free atoms to absorb light is measured thus, both a chemical principle (atomization) and a physical principle (absorption of light) are used in this technique. Chapters 8-13 of this text cover techniques commonly used to analyze samples. 

Finally, analytical methods can be compared in terms of their need for equipment, the time required to complete an analysis, and the cost per sample. Methods relying on instrumentation are equipment-intensive and may require significant operator training. For example, the graphite furnace atomic absorption spectroscopic method for determining lead levels in water requires a significant capital investment in the instrument and an experienced operator to obtain reliable results. Other methods, such as titrimetry, require only simple equipment and reagents and can be learned quickly. 

Trace metals in sea water are preconcentrated either by coprecipitating with Ee(OH)3 and recovering by dissolving the precipitate or by ion exchange. The concentrations of several trace metals are determined by standard additions using graphite furnace atomic absorption spectrometry. 

L Vov, B. V. Graphite Furnace Atomic Absorption Spectrometry, AuflZ. Chem. 1991, 63, 924A-931A. 

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%. 

Figure 15-12 is a schematic illustration of a technique known as acid volatile sulfides/ simultaneously extracted metals analysis (AVS/SEM). Briefly, a strong acid is added to a sediment sample to release the sediment-associated sulfides, acid volatile sulfides, which are analyzed by a cold-acid purge-and-trap technique (e.g., Allen et ai, 1993). The assumption shown in Fig. 15-12 is that the sulfides are present in the sediments in the form of either FeS or MeS (a metal sulfide). In a parallel analysis, metals simultaneously released with the sulfides (the simultaneously extracted metals) are also quantified, for example, by graphite furnace atomic absorption spectrometry. Metals released during the acid attack are considered to be associated with the phases operationally defined as "exchangeable," "carbonate," "Fe and Mn oxides," "FeS," and "MeS."... 

In order to derive a quantitative relation between emission Intensity as measured by EMI and actual metal content, cell samples were subjected to graphite furnace atomic absorption (GFAA) analysis (14). Atomic absorption experiments were performed both on cells which had been stained with a fluorescent reagent and on cells not exposed to a lumlnophore. After EMI analysis, 50 fiL of cell suspension were withdrawn from the 0.30 mL of sample used for EMI and were digested In 150 iiL of concentrated HNO3 for 90 minutes at 85° . These solutions were then diluted to 1/10 of their concentration with deionized water, and the 150 liL of these diluted... 

Vol. 149. A Practical Guide to Graphite Furnace Atomic Absorption Spectrometry. By David J. Butcher and Joseph Sneddon... 

R. W. "Determination of Lead In Whole Blood by Graphite Furnace Atomic Absorption Spectrophotometry". Amer. Ind. Hyg. Assoc. J. (1974), 566-570. 

D. Wienke, T. Vijn and L. Buydens, Quality self-monitoring of intelligent analyzers and sensor based on an extended Kalman filter an application to graphite furnace atomic absorption spectroscopy. Anal. Chem., 66 (1994) 841-849. 

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. 

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. 

Klemm W, Baumeach G (1995) Trace element determination in contaminated sediments and soils by ultrasonic slurry sampling and Zeeman graphite furnace atomic absorption spectrometry. Fresenius J Anal Chem 353 12-15. 

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. 

Dabeka, R. W. and McKenzie, A. D. (1991). Graphite furnace atomic absorption spectromet-ric determination of selenium in foods after sequential wet digestion with nitric acid, dry ashing and coprecipitation with palladium. Can. J. Appl. Spectrosc. 36,123-126. 

Kelko-Levai, A., Varga, I., Zih-Perenyi, K., and Lasztity, A., Determination of trace elements in pharmaceutical substances by graphite furnace atomic absorption spectrometry and total reflection X-ray fluorescence after flow injection ion-exchange preconcentration, Spectrochim. Acta Pt. B, 54, 827, 1999. 

FIM Field ion microscopy GFAAS Graphite furnace atomic absorption... 

ZGFAAS Zeeman graphite furnace atomic absorption spectrometry... 

Aroza I, Bonilla M, Madrid Y, et al. 1989. Combination of hydride generation and graphite furnace atomic absorption spectrometry for the determination of lead in biological samples. J Anal Atmos Spectra 4 163-166. 

ASTM. 1998a. ASTME1613. Standard test method for analysis of digested samples for lead by inductively coupled plasma atomic emission spectrometry (ICP-AES). Flame Atomic Absorption (FAAS), or Graphite Furnace Atomic Absorption (GFAA) Techniques. American Society for Testing and Materials. 

Ellen G, Van Loon JW. 1990. Determination of cadmium and lead in foods by graphite furnace atomic absorption spectrometry with Zeeman background correction Test with certified reference materials. Food Addit Contam 7 265-273. 

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