Name: atomic absorption spectroscopy: sample atomization
Uploaded: 2024-12-05T18:32:14.000Z
Duration: 1 min 25 s
Channel: JoVE

AAS usually atomizes samples through flame or electrothermal atomization.
Flame atomization typically uses a nebulizer to continuously aerosolize the sample and a spray chamber assembly to mix it with fuel and oxidant.
Only about five percent of the aerosol droplets are fine enough to reach the flame, where they desolvate in the primary combustion zone, leaving behind bare particles that are atomized in the inner flame.
The gaseous atoms, ions, and molecular species swiftly flow through the interzonal region for analysis and out of the flame.
Because very little of the sample is successfully atomized and detected, flame atomization isn&#39;t good for samples with low analyte concentrations or limited volumes.
On the other hand, electrothermal atomization, also known as graphite-furnace atomization, uses a graphite tube to capture and concentrate analytes from small, discrete samples, which are dried, charred, and atomized at high temperatures.
Alternatively, some elements under milder chemical conditions convert to volatile hydride products first and then can be atomized. Additionally, mercury determination can use a unique cold-vapor method because of its natural volatility.&#160;

atomaire absorptiespectroscopie: atomiseringsmethoden

Atomic Absorption Spectroscopy: Atomization Methods

Atomaire absorptiespectroscopie (AAS) atomiseert monsters door vlamatomisering of elektrothermische atomisering. Vlamatomisering omvat doorgaans een vernevelaar en een sproeikamer om het monster te combineren met een brandstof-oxidantmengsel, waardoor een fijne aerosolmist ontstaat die een brander binnengaat. Meestal worden de brandstof en de oxidant gecombineerd in een ongeveer stoichiometrische verhouding. Voor atomen die gemakkelijk oxideren, kan een brandstofrijk mengsel echter voordeliger zijn. Slechts ongeveer 5% van de aerosoldruppels bereikt de vlam, waar ze desolvatatie ondergaan in de primaire verbrandingszone, waardoor kale deeltjes in de binnenste vlam worden geatomiseerd. De gasvormige atomen, ionen en moleculaire soorten passeren snel het interzonale gebied voor analyse voordat ze de vlam verlaten. Vlamatomiseringsapparaten hebben een lage atomiseringsefficiëntie vanwege grote aerosoldruppels die de vlam niet bereiken en aanzienlijke monsterverdunning door verbrandingsgassen. De efficiëntie van vlamverstuiving kan echter worden verbeterd door het monster continu te aspireren, de brandstof-tot-oxidantverhoudingen te optimaliseren, de stroomsnelheden van de vernevelaar aan te passen en de branderhoogte in te stellen.

 Vlamverstuiving is niet geschikt voor monsters met lage analytconcentraties of beperkte volumes vanwege het kleine aantal monsters dat succesvol is verstoven en gedetecteerd. Daarentegen gebruikt elektrothermische verstuiving, ook bekend als grafietovenverstuiving, een grafietbuis om de analyten op te vangen en te concentreren en werkt goed voor kleine, discrete monsters. Bij deze techniek wordt het monster gedroogd en verkoold voordat het bij hoge temperaturen wordt verstoven.

 Elementen zoals As, Se, Sb, Bi, Ge, Sn, Te en Pb kunnen onder mildere omstandigheden worden verstoven door ze chemisch om te zetten in vluchtige hydriden voordat ze naar de vlam worden gebracht. Bovendien kan kwikbepaling een unieke koudedampmethode gebruiken vanwege de natuurlijke vluchtigheid ervan.

Atomaire absorptiespectroscopie: atomiseringsmethoden

Atomic Absorption Spectroscopy (AAS) atomizes samples through flame atomization or electrothermal atomization. Flame atomization typically involves a ...

atomic-absorption-spectroscopy-atomization-methods

Education

JoVE Core

Analytical Chemistry

Analytische chemie

Unit 1

Atomic Spectroscopy

Atoomspectroscopie

KEY TERMS AND CONCEPTS

BELANGRIJKE TERMEN EN CONCEPTEN

atomic absorption spectroscopy: sample atomization

Atomic absorption spectroscopy uses sample atomization to turn a liquid specimen into free atoms for analysis. The two main approaches are flame atomization and electrothermal atomization. Both methods prepare the sample so its atoms can be measured by the instrument.

Flame atomization uses a nebulizer and spray chamber to mix the sample with a fuel-oxidant mixture. This creates a fine aerosol mist that enters the burner. The fuel and oxidant are usually close to a stoichiometric ratio, but a fuel-rich mixture can work better for atoms that oxidize easily.

Only about 5% of the aerosol droplets reach the flame. In the primary combustion zone, these droplets undergo desolvation, which means the solvent is removed. The bare particles are then atomized in the inner flame. The gaseous atoms, ions, and molecular species move through the interzonal region for analysis before leaving the flame.

Flame atomizers have low atomization efficiency. Large droplets do not reach the flame, and combustion gases also dilute the sample. Efficiency can be improved by continuously aspirating the sample, adjusting the fuel-to-oxidant ratio, changing the nebulizer flow rate, and setting the burner height. Flame atomization is not a good choice for samples with very low analyte levels or small sample volumes.

Electrothermal atomization, also called graphite furnace atomization, uses a graphite tube to collect and concentrate the analytes. It works well for small, discrete samples. The sample is first dried and charred, then atomized at very high temperatures.

Some elements, including As, Se, Sb, Bi, Ge, Sn, Te, and Pb, can be handled under milder conditions by forming volatile hydrides before they are carried to the flame. Mercury can also be measured with a cold-vapor method because it is naturally volatile.

Atomic Absorption Spectroscopy: Sample Atomization

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Heat changes atomic spectra by affecting atomization, excitation, ionization, and line shape. In atomic spectroscopy, atomization means converting a sample into gas-phase atoms and ions. The flame temperature needed for this step changes how efficiently the method works and shifts the balance between excited and ground-state atoms. At thermal equilibrium, the relative numbers of excited and ground-state atoms can be estimated with the Maxwell-Boltzmann distribution. A small temperature rise...

atomic absorption spectroscopy: overview

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Atomic absorption spectroscopy (AAS) measures trace metals by tracking how atoms absorb electromagnetic radiation (EMR). The absorbed light makes atoms move to a higher-energy orbit. In AAS, the key step is atomization, which converts the sample into gas-phase atoms. A flame or a furnace is typically used for this step. Inside the flame, some atoms become thermally excited. Most stay in the ground state, which is the lowest-energy state. These ground-state gas-phase atoms absorb EMR only when...

atomic absorption spectroscopy: instrumentation

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Atomic absorption spectrophotometry uses a set of key parts to measure light absorbed by atoms. The main components are a radiation source, an atomizer, a monochromator, and a detector. Each part has a specific job in the instrument. The radiation source is usually a hollow-cathode lamp, or HCL, or an electrodeless-discharge lamp, or EDL. Both produce a narrow emission line at the needed wavelength. Some instruments instead use continuum sources with high-resolution monochromators to narrow...

atomic absorption spectroscopy: radiation and light sources

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Choosing Light Sources for AAS Measurements

Atomic absorption spectroscopy (AAS) uses a light source that emits a very narrow range of wavelengths. This is needed because the source must match the absorption behavior of the analyte atom. The choice of source also depends on giving a precise, intense emission at the right wavelength for accurate detection. Two common line sources in AAS are hollow-cathode lamps (HCLs) and electrodeless-discharge lamps (EDLs). These lamps are selected based on the element being analyzed and the level of...

atomic absorption spectroscopy: atomization methods

Atomic absorption spectroscopy uses sample atomization to turn a liquid specimen into free atoms for analysis. The two main approaches are flame atomization and electrothermal atomization. Both methods prepare the sample so its atoms can be measured by the instrument. Flame atomization uses a nebulizer and spray chamber to mix the sample with a fuel-oxidant mixture. This creates a fine aerosol mist that enters the burner. The fuel and oxidant are usually close to a stoichiometric ratio, but a...

atomic absorption spectroscopy: interference

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Atomic absorption spectroscopy interference can create systematic error by making the analytical signal or the background look stronger or weaker than it should be. In atomic absorption measurements, these errors are usually grouped as spectral interference, chemical interference, and physical interference. Spectral interference happens when signals from other elements or molecules overlap with the analyte signal, the substance being measured. This overlap can falsely raise or hide the analyte...

atomic absorption spectroscopy: lab

AAS Sample Prep and Calibration

Atomic absorption spectroscopy (AAS) depends on careful sample preparation and calibration. Samples must be turned into clear solutions before measurement. That often means extra treatment to dissolve materials such as soils, animal tissues, and minerals. Common sample prep methods include hot mineral acids, wet ashing, combustion in closed containers, high-temperature ashing, and fusion with reagents. These steps help make the sample suitable for AAS analysis. Solutions that contain organic...

atomic emission spectroscopy: overview

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Atomic emission spectrometry (AES) uses sample handling, atomization, and detection parts to measure emitted light from atoms and ions. The sample must first be changed into a gas-phase form so it can produce a measurable signal. AES uses two main atomizer types. Continuous atomizers, such as flames and plasmas, feed the sample in a steady stream. Discrete atomizers add one sample at a time with syringes or autosamplers. The electrothermal atomizer is the most common discrete type. Many...

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Atomic emission spectroscopy (AES) can produce interfering signals when atoms and molecules in a flame or plasma emit overlapping light. High-temperature atomizers excite many species at once, including oxides, hydroxides, and flame combustion products. These extra emissions can make the analyte signal harder to read. Spectral interference happens when emission lines or bands overlap. One way to reduce it is to improve instrument resolution. Another is to choose a different emission line for...

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Inductively coupled plasma atomic emission spectroscopy uses a plasma torch to analyze elements in a sample. This method is also called inductively coupled plasma optical emission spectroscopy, or ICP-OES. It is widely used because the plasma creates a strong environment for elemental analysis. The ICP source, or torch, contains three concentric quartz tubes. Argon gas flows through the tubes. A spark from a Tesla coil starts the ionization of argon and creates a high-temperature plasma. The...

inductively coupled plasma atomic emission spectroscopy: instrumentation

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Inductively coupled plasma atomic emission spectroscopy, or ICP-AES, uses an inductively coupled plasma to detect and analyze elements in a sample. The method measures the light given off by atoms, which helps identify and compare different elements. It is a common approach in atomic emission spectroscopy. ICP-AES instruments are built in three main forms: sequential, simultaneous multichannel, and Fourier transform instruments. Fourier transform designs are less commonly used, but they are...

atomic emission spectroscopy: lab

Plasma Sources in Atomic Emission Spectroscopy

Atomic emission spectroscopy uses plasma sources to identify elements by their light. The method creates abundant spectra with characteristic emission lines. Inductively coupled plasma, or ICP, is especially useful because it gives strong quantitative data. It works well under stable conditions, with low noise, low background, and few interferences. Newer air-operated microwave sources are also being studied. These sources may be more cost-effective than conventional ICP systems. Atomic...

atomic fluorescence spectroscopy

Measuring Elements by Atomic Fluorescence

Atomic fluorescence spectroscopy measures elements by detecting the light atoms give off after they are excited by electromagnetic radiation. The atoms are first placed in a flame, furnace, or plasma. They absorb energy, become excited, and then release that energy as they return to their original state. The emitted light is called fluorescence. The fluorescence is observed at a right angle to the incoming beam. This setup helps separate the emitted light from the light used to excite the...

flame photometry: overview

Flame Emission Spectrometry Basics

Flame emission spectrometry uses a flame to excite elements in a sample so their light can be measured. It is also called flame photometry. The method can be used for both qualitative and quantitative analysis of elements. The idea became established in the early 1860s when Kirchhoff and Bunsen showed that specific elements give off characteristic radiation in a flame. The first instrument for this purpose measured sodium in plant ash with a Bunsen flame. A major problem was how to add the...

flame photometry: lab

Flame Photometry and Metal Detection

Flame photometry is a method for detecting metals by measuring the light they emit in a flame. A solution such as potassium chloride is aspirated into the flame. The solvent evaporates first. The remaining salt becomes dehydrated and then dissociates into free gaseous atoms in the ground state. Some of these atoms absorb energy from the flame and move to an excited state. When they return to the ground state, they emit photons at characteristic wavelengths. These emissions are very narrow...

key terms and concepts

Learn how AAS atomizes samples with flame and graphite furnace methods, plus hydride and cold-vapor techniques for specific elements.

Atomic Absorption Spectroscopy: Sample Atomization | JoVE K12

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Atomic Absorption Spectroscopy: Sample Atomization

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