Another consideration is the emission line's intensity. Atomic spectroscopy includes a number of analytical techniques used to determine the elemental composition of a sample (it can be gas, liquid, or solid) by observing its electromagnetic spectrum or its mass spectrum. An ionization interference occurs when thermal energy from the flame or the electrothermal atomizer is sufficient to ionize the analyte, \[\mathrm{M}(s)\rightleftharpoons \ \mathrm{M}^{+}(a q)+e^{-} \label{10.1}\]. 1. Spectrosc. The most important factor in choosing a method of atomization is the analyte’s concentration. For this reason, only the introduction of solution samples is considered in this chapter. All rights reserved. When possible, a quantitative analysis is best conducted using external standards. The description here is based on Bhattacharya, S. K.; Goodwin, T. G.; Crawford, A. J. Anal. Whereas atomic absorption spectroscopy is the study of how light and energy interact with matter, atomic absorption spectrometry refers to the techniques and methodology used to apply this study to real-world practices. Each element in a hollow cathode lamp provides several atomic emission lines that we can use for atomic absorption. The result is an apparent increase in the sample’s absorbance. Alternatively, we can extract the analyte using a Soxhlet extractor. maryville.edu. Read: pp. Converting an aqueous analyte into a free atom requires that we strip away the solvent, volatilize the analyte, and, if necessary, dissociate the analyte into free atoms. Have questions or comments? Atomic absorption is used for the analysis of over 60 elements at concentrations at or below the level of μg/L. A protecting agent reacts with the analyte to form a stable volatile complex. Qualitative analysis gives an indication of the amount of one or more of these components. Because the absorption spectra for M and M+ are different, the position of the equilibrium in reaction \ref{10.1} affects the absorbance at wavelengths where M absorbs. Alternatively, if the background is due to a known matrix component, then we can add that component in excess to all samples and standards so that the contribution of the naturally occurring interferent is insignificant. Inside the lamp, the cathode is coated with a metal... 2. In the unit shown here, the aqueous sample is drawn into the assembly by passing a high-pressure stream of compressed air past the end of a capillary tube immersed in the sample. The radiation source for atomic absorption spectroscopy should emit stable, intense radiation of the element to be determined, useually a resonance line of the element.. a. By fashioning the cathode from the metallic analyte, a hollow cathode lamp provides emission lines that correspond to the analyte’s absorption spectrum. Flame and electrothermal atomization require that the analyte is in solution. For more information contact us at info@libretexts.org or check out our status page at https://status.libretexts.org. There is, however, an important additional need in atomic absorption spectroscopy: we first must covert the analyte into free atoms. The hollow cathode is coated with the element you wish to measure. The cost of a new instrument ranges from between $10,000– $50,000 for flame atomization, and from $18,000–$70,000 for electrothermal atomization. Accurate quantitative work, therefore, requires a suitable means for computing the calibration curve from a set of standards. 1983, 37, 411–418]. A serum sample, for instance, is difficult to aspirate when using flame atomization and may produce an unacceptably high background absorbance when using electrothermal atomization. Flame Absorption Spectroscopy The determination of potassium using an atomic absorption spectrophotometer requires a light source (wavelength for K = 766.5 nm) and an atomization source (flame). Attosecond transient absorption spectroscopy (ATAS) is used to observe photoexcited dynamics with outstanding time resolution. In addition, it is the most intense emission line, which decreases the uncertainty in the measured absorbance. The hottest part of the flame typically is 2–3 cm above the primary combustion zone. Absorption spectroscopy refers to spectroscopic techniques that measure the absorption of radiation, as a function of frequency or wavelength, due to its interaction with a sample.The sample absorbs energy, i.e., photons, from the radiating field. For example, continuously aspirating a sample that has a high concentration of dissolved solids—sea water, for example, comes to mind—may build-up a solid de- posit on the burner head that obstructs the flame and that lowers the absorbance. \[A=-0.0002+0.0661 \times \frac{\mu \mathrm{g} \ \mathrm{Cu}}{\mathrm{mL}} \nonumber\], Substituting the sample’s absorbance into the calibration equation gives the concentration of copper as 0.351 μg/mL. The small volume requirement for electrothermal atomization or for flame microsampling, however, makes practical the analysis of micro and ultramicro samples. 7-Oct-14 Pharmaceutical Analysis 4 5. Of these, ICP-OES and ICP-MS are very linear; that is, a plot of concentration vs. intensity forms a straight line over a wide range of concentrations (Figure 1). Although each method is unique, the following description of the determination of Cu and Zn in biological tissues provides an instructive example of a typical procedure. Only the background, therefore, absorbs radiation from the D2 lamp. Flame microsampling allows us to introduce a discrete sample of fixed volume, and is useful if we have a limited amount of sample or when the sample’s matrix is incompatible with the flame atomizer. A Cu hollow cathode lamp has several emission lines, the properties of which are shown in the following table. The most common means for introducing a sample into a flame atomizer is a continuous aspiration in which the sample flows through the burner while we monitor absorbance. The three most common atomic spectroscopy techniques . An increase in sensitivity may be realized by adding a low molecular weight alcohol, ester, or ketone to the solution, or by using an organic solvent. These gases are removed by the inert gas flow. With electrothermal atomization, sensitivity is influenced by the drying and ashing stages that precede atomization. For the light source, arc discharge lamps may be … Commercial instruments were in place by the early 1960s, and the importance of atomic absorption as an analytical technique soon was evident. Atomic Absorption Spectroscopy Learning Module. Some of the sputtered atoms are in the excited state and emit radiation characteristic of the metal(s) from which the cathode is manufactured. Flame or Electrothermal Atomization? Report the amount of copper in the sample as μg Cu/g FFDT. It was the problem of how small concentrations of metallic elements could be measured more exactly by spectroscopy. After drying and extracting the sample, a 11.23-mg FFDT tissue sample gives an absorbance of 0.023. The primary combustion zone usually is rich in gas combustion products that emit radiation, limiting is useful- ness for atomic absorption. Distinct elements will absorb these wavelengths differently. The interzonal region generally is rich in free atoms and provides the best location for measuring atomic absorption. The analyte’s concentration in the resulting vapor phase is as much as \(1000 \times\) greater than in a flame atomization [Parsons, M. L.; Major, S.; Forster, A. R. Appl. The inert gas is ionized as a high voltage potential difference is created between the tungsten anode and use-specific cylindrical cathode. This is the case for Zn, but not for Cu. A few elements are atomized by using a chemical reaction to produce a volatile product. 1991, 63, 1033A–1038A]. Unfortunately, matrix interferences are a frequent problem, particularly when using electrothermal atomization. Flame. Hollow cathod lamp. To limit ionization we add a high concentration of an ionization suppressor, which is a species that ionizes more easily than the analyte. Analytical Chemistry 1991, 63 (2) , 151-159. An intense field of radiation provides ionization and excitation of the metal to produce a spectrum. The most useful radiation source for atomic absorption spectroscopy is the hollow-cathode lamp (HCL). As shown in Figure \(\PageIndex{4}\), the graphite tube is housed in an sealed assembly that has an optically transparent window at each end. The result is a transient absorbance peak whose height or area is proportional to the absolute amount of analyte injected into the graphite tube. Vertical adjustments change the height within the flame from which absorbance is monitored. The matrix for the standards and the blank should match the matrix of the samples; thus, an appropriate matrix is 0.75 M HNO3. Atomic absorption spectroscopy is ideally suited for the analysis of trace and ultratrace analytes, particularly when using electrothermal atomization. Most instruments include several different algorithms for computing the calibration curve. Applying a potential across the electrodes ionizes the filler gas. Unless otherwise noted, LibreTexts content is licensed by CC BY-NC-SA 3.0. Missed the LibreFest? Figure 9-13a. Chem. When the sample exits the nebulizer it strikes a glass impact bead, which converts it into a fine aerosol mist within the spray chamber. Developing a quantitative atomic absorption method requires several considerations, including choosing a method of atomization, selecting the wavelength and slit width, preparing the sample for analysis, minimizing spectral and chemical interferences, and selecting a method of standardization. When analyzing a lake sediment for Cu, Zn, and Fe, for example, we bring the analytes into solution as Cu2+, Zn2+, and Fe3+ by extracting them with a suitable reagent. In the final stage the sample is atomized by rapidly increasing the temperature to between 2000–3000oC. Other methods of background correction have been developed, including Zeeman effect background correction and Smith–Hieftje background correction, both of which are included in some commercially available atomic absorption spectrophotometers. 5). To reiterate the above statement, atomic absorption spectrometry can be conducted with either solid or liquid samples. These additional lines are a potential source of stray radiation that could result in an instrumental deviation from Beer’s law. EPA methods for determination of metals by direct aspiration. This is most widely used as a light source. 3. Atomic absorption is used widely for the analysis of trace metals in a variety of sample matrices. Background correction using a D2 lamp is necessary for zinc. A stable flame minimizes uncertainty due to fluctuations in the flame. The sensitivity of a flame atomic absorption analysis is influenced by the flame’s composition and by the position in the flame from which we monitor the absorbance. Potassium and cesium frequently are used as an ionization suppressor because of their low ionization energy. Usually the wavelength that provides the best sensitivity is the one we choose to use, although a less sensitive wavelength may be more appropriate for a sample that has higher concentration of analyte. Chem. On the other hand, if our interest is biologically available metals, we might extract the sample under milder conditions using, for example, a dilute solution of HCl or CH3COOH at room temperature. b. Electrode less Discharge lamp. There are two common atomization methods: flame atomization and electrothermal atomization, although a few elements are atomized using other methods. The temperature and time at each stage is optimized for each type of sample. Structurally, this is an air-tight lamp filled with argon or neon and kept at around 1 to 5 torr. St. Louis, Missouri 63141 Results are reported as μg of Cu or Zn per gram of FFDT. A significant improvement in sensitivity is achieved by using the resistive heating of a graphite tube in place of a flame. The flame’s thermal energy then volatilizes the particles, producing a vapor that consists of molecular species, ionic species, and free atoms. 650 Maryville University Drive St. Louis, Missouri 63141 314.529.9466 After centrifuging at 2500 rpm for 10 minutes, the supernatant is transferred to a 5-mL volumetric flask. Modern atomic absorption spectroscopy has its beginnings in 1955 as a result of the independent work of A. C. Walsh and C. T. J. Alkemade [(a) Walsh, A. Anal. Sample Introduction. Elements such as As, Se, Sb, Bi, Ge, Sn, Te, and Pb, for example, form volatile hydrides when they react with NaBH4 in the presence of acid. Optical Atomic Spectroscopy Optical Spectrometry Absorption Emission Fluorescence Source: R. Thomas, “Choosing the Right Trace Element Technique,” Today’s Chemist at … The signal for flame microsampling is a transitory peak whose height or area is proportional to the amount of analyte that is injected. Copper and zinc are isolated from tissue samples by digesting the sample with HNO3 after first removing any fatty tissue. In short, flame photometry (FP) is an atomic technique which measures the wavelength and intensity of light emitted by atoms in a flame resulting from the drop from the excited state (formed due to absorption of energy from the flame) to lower states. The aerosol mist is swept through the spray chamber by the combustion gases—compressed air and acetylene in this case—to the burner head where the flame’s thermal energy desolvates the aerosol mist to a dry aerosol of small, solid particulates. 1991, 63, 1024A–1031A; (c) Slavin, W. Anal. Although this method of background correction is effective, it does assume that the background absorbance is constant over the range of wavelengths passed by the monochromator. Minimizing Chemical Interferences. If several emission lines meet our requirements for sensitivity, we may wish to use the emission line with the largest relative P0 because there is less uncertainty in measuring P0 and PT. Electrothermal atomization requires substantially more time per analysis, with maximum sample throughputs of 20–30 determinations per hour. 1. There are two categories of sources, line and continuum. One of these concerns the radiation source. Mercury is determined by the cold-vapor method in which it is reduced to elemental mercury with SnCl2. In the second stage, which is called ashing, the temperature is increased to between 350–1200oC. The digestion is repeated two more times, for 2–4 hours each, using 0.9-mL aliquots of 0.75 M HNO3. 650 Maryville University Drive
A power supply is used to pass a current through the graphite tube, resulting in resistive heating. Flame microsampling is accomplished using a micropipet to place 50–250 μL of sample in a Teflon funnel connected to the nebulizer, or by dipping the nebulizer tubing into the sample for a short time. Atomic absorption spectrophotometers use the same single-beam or double-beam optics described earlier for molecular absorption spectrophotometers (see Figure 10.3.2 and Figure 10.3.3). As atoms approach the flame’s secondary combustion zone, the decrease in temperature allows for formation of stable molecular species. The slot burner in Figure \(\PageIndex{1}\)a provides a long optical pathlength and a stable flame. If the sample is a solid, then we must bring the analyte into solution before the analysis. This effect arises because atoms will have different components of velocity along the line of observation. Any interferences from other components of the sample matrix are minimized by background correction. Guystav Kirchoff and Robert Bunsen first used atomic absorption—along with atomic emission—in 1859 and 1860 as a means for identify atoms in flames and hot gases. For years Alan Walsh, a tall and wiry Lancashire-born physicist of oceanic moods, had weathered despair in trying to find an answer to a problem that had defeated other scientists since the last century. The more time an analyte spends in the flame the greater the atomization efficiency; thus, the production of free atoms increases with height. Consequently, as much as 95% of the sample never reaches the flame, which is the reason for the waste line shown at the bottom of the spray chamber in Figure \(\PageIndex{1}\). Doppler effect. Standardizing the Method. When it comes to Atomic Absorption, there are a couple important factors to note. Continuum sources are typically used for background correction, to eliminate the matrix so only the signal of the analyte is observed. Dilute solutions of Cd2+, Co2+, Cu2+, Fe3+, Pb2+, Ni2+, and Zn2+, for example, are concentrated by extracting with a solution of ammonium pyrrolidine dithiocarbamate in methyl isobutyl ketone. Structurally, this is an air-tight lamp filled with argon or neon and kept at around 1 to 5 torr. For this reason the method of standard additions often is used. There are many commercially available models of HCLs, some can possess multiple metal cathodes for analysis of several metals. Horizontal adjustments ensure the flame is aligned with the instrument’s optical path. The best way to appreciate the theoretical and the practical details discussed in this section is to carefully examine a typical analytical method. Different Types of Light Sources Tungsten Halogen light sources are mostly used to do measurements in the […] .. Atomic absorption spectroscopy deals with the absorption of specific wavelength of radiation by neutral atoms in the ground state. 2. The concentration of copper in the tissue sample, therefore, is, \[\frac { \frac{0.351 \mu \mathrm{g} \ \mathrm{Cu}}{\mathrm{mL}} \times 5.000 \ \mathrm{mL}} {0.01123 \text{ g sample}}=156 \ \mu \mathrm{g} \ \mathrm{Cu} / \mathrm{g} \ \mathrm{FDT} \nonumber\]. Copper is analyzed at a wavelength of 324.8 nm with a slit width of 0.5 nm, and zinc is analyzed at 213.9 nm with a slit width of 1.0 nm. In order to analyze a sample for its atomic constituents, it has to be atomized. The monochromator’s slit width is set as wide as possible to improve the throughput of radiation and narrow enough to eliminate these sources of stray radiation. Chem. On the other hand, a molecule’s broad absorption band or the scattering of source radiation is a potentially serious spectral interference. Different Atomization Sources for Atomic Spectroscopy Typical Source Temperature Source Type Combustion Flame ° C Electrothermal ° C Vaporization (ETV) on graphite platform Inductively coupled ° C plasma (ICP( Direct-current plasma ° C (DCP) Microwave induced ° C plasma (MIP) Atomic absorption spectroscopy is an absorption spectroscopic method where radiation from a source is absorbed by non-excited atoms in the vapour state. If the identity of the matrix interference is unknown, or if it is not possible to adjust the flame or furnace conditions to eliminate the interference, then we must find another method to compensate for the background interference. Preparing the Sample. 1. The concentrations of Cu and Zn in the diluted supernatant are determined by flame atomic absorption spectroscopy using an air-acetylene flame and external standards. A typical electrothermal atomizer, also known as a graphite furnace, consists of a cylindrical graphite tube approximately 1–3 cm in length and 3–8 mm in diameter. A rotating wheel is interposed between the hollow cathod lamp and the flame. An important consideration when using a flame as an atomization source is its effect on the measured absorbance. Since unique elements have characteristic (signature) spectra, atomic spectroscopy, specifically the electromagnetic spectrum or mass spectrum, is applied for determination of elemental compositions.It can be divided by atomization source or by the type of spectroscopy used. Liquid samples are analyzed directly or the analytes extracted if the matrix is in- compatible with the method of atomization. The intensity of the absorption varies as a function of frequency, and this variation is the absorption spectrum. 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