Heated graphite atomization atomic spectroscopy

Instead of employing the high temperature of a flame to bring about the production of atoms from the sample, it is possible in some cases to make use of either (a) non-flame methods involving the use of electrically heated graphite tubes or rods, or (b) vapour techniques. Procedures (a) and (b) both find applications in atomic absorption spectroscopy and in atomic fluorescence spectroscopy. 

In atomic spectroscopy, analyte is atomized in a flame, an electrically heated furnace, or a plasma. Flames were used for decades, but they have been replaced by the inductively coupled plasma and the graphite furnace. We begin our discussion with flames because they are still common in teaching labs. 

Figure 21-6 An electrically heated graphite furnace for atomic spectroscopy (—38 mm long, in this case). [Courtesy Instrumentation Laboratory, Wiirrington, MA.]...

Figure 21-8 (a) Transversely heated graphite furnace maintains nearly constant temperature over its whole length, thereby reducing memory effect from previous runs. The i vov platform is uniformly heated by radiation from the outer wall, not by conduction. The platform is attached to the wall by one small connection that is hidden from view. [Courtesy Perkin-Bmer Corp., Norwalk, Cl] (to) Heating profiles comparing analyte evaporation from wall and from platform. [From W. Slavin, Atomic Absorption Spectroscopy, Anal. Chem. 1982,54,685A.]... 

Flameless atomic absorption spectroscopy using the heated graphite furnace is a sensitive method for analyzing environ-mental samples for trace metals. High salt concentrations cause interference problems that are not totally correctable by optimizing furnace conditions and/or using background correctors. We determined that samples with identical ratios of major cations have trace metal absorbances directly related to their Na and trace metal concentrations. Equations and curves based on the Na concentration, similar to standard addition curves, can be calculated to overcome the trace element interference problem. Concentrations of Pb, Cd, Cu, and Fe in sea water can be simply (ind accurately determined from the Na concentration, the sample absorbance vs. a pure standard, and the appropriate curve. 

Recommended Air Volume 960 L Recommended Sampling Rate 2.0 L/min Analytical Procedure Air filter samples are digested with nitric acid. After digestion, a small amount of hydrochloric acid is added. The samples are then diluted to volume with deionized water and analyzed by either flame atomic absorption spectroscopy (AAS) or flameless atomic absorption spectroscopy using a heated graphite furnace atomizer (AAS-HGA). 

The air-dried spiked filters were digested and analyzed for their cadmium content by flameless atomic absorption spectroscopy using a heated graphite furnace atomizer following the procedure described in Section 3. A five-fold dilution of the spiked filter samples at 2 times the Action Level TWA was made prior to their analysis. The 0.05 to 20 ng/mL cadmium standards were used in the analysis of the spiked filters. 

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. 

In the application of atomic emission spectroscopy for quantitative analysis, samples must be prepared in liquid form of a suitable solvent unless it is already presented in that form. The exceptions are solids where samples can be analysed as received using rapid heating electro-thermal excitation sources, such as graphite furnace heating or laser ablation methods. Aqueous samples, e.g. domestic water, boiler water, natural spring, wines, beers and urines, can be analysed for toxic and non-toxic metals as received with... 

I) Analytical technique or method, occasionally unfeasible with the Involvement of an operator —this book abounds In Illustrative examples of this kind. Thus, electrothermal vaporization atomic absorption spectroscopy demands the automation of the sample thermal treatment In the graphite tube via a microprocessor programming the different heating stages involved (automation of methodology). Likewise, the use of Image detectors In spectroscopy calls for computerized data acquisition, impossible with manual operators. 

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