Name: aes sample handling and detection
Uploaded: 2024-12-05T18:32:15.000Z
Duration: 1 min 22 s
Channel: JoVE

K12 Standards

Pennsylvania State Academic Standards

9-12

Earth and Space Science

Space Systems

3.3.9-12.B

atomic-emission-spectroscopy-instrumentation

Atomic Emission Spectroscopy: Instrumentation

Das Atomemissionsspektrometer besteht aus einem Probenvernebler, einer Plasmaquelle, einem wellenlängenisolierenden Gerät, Wandlern und einer Mikroprozessorsteuerung.
Die Probe wird mit einer Schlauchpumpe entnommen und zu einem Vernebler transportiert, der die Probenlösung in feine Tröpfchen umwandelt.
Größere Tröpfchen werden in einen Abfluss geleitet, während die feinen Tröpfchen durch Argongas zum Plasma transportiert werden – üblicherweise Gleichstromplasma oder induktiv gekoppeltes Plasma.
Im Plasma werden die Proben zu Gasphasenatomen und Ionen zerstäubt und bei weiterer Kollision angeregt.
Die atomare oder ionische Emission aus dem Plasma wird dann durch einen Monochromator, Polychromator oder Spektrografen getrennt.
Monochromatoren trennen einzelne Wellenlängen nacheinander durch einen einzigen Ausgangsspalt, während Polychromatoren mit mehreren Ausgangsschlitzen mehrere Wellenlängen gleichzeitig isolieren.
Alternativ ermöglicht ein Spektrograf die gleichzeitige Überwachung eines Bereichs von Wellenlängen.
Die isolierte Strahlung wird durch einzelne oder mehrere Photomultiplier-Wandler oder Array-Detektoren in elektrische Signale umgewandelt und weiter analysiert.

atomemissionsspektroskopie: instrumentierung

Die Instrumentierung der Atomemissionsspektrometrie (AES) umfasst verschiedene Komponenten, darunter Atomisierungsgeräte, die Proben in gasförmige Atome und Ionen umwandeln. Es gibt zwei Haupttypen von Verneblern: kontinuierliche und diskrete Atomisierer. Kontinuierliche Atomisierer, wie Plasmen und Flammen, führen Proben in einem konstanten Strom ein, während diskrete Atomisierer einzelne Proben mithilfe von Spritzen oder Autosamplern injizieren. Der am häufigsten verwendete diskrete Atomisierer ist der elektrothermische Atomisierer.

Unter Vernebelung versteht man das Einbringen von Proben in Form von Aerosolen. Ein Vernebler erzeugt einen feinen Sprühnebel aus Tröpfchen der flüssigen Probe und ermöglicht so eine effiziente Atomisierung. Nach der Atomisierung bildet die Probe in einer Flamme oder einem Plasma eine stationäre Population von Atomen, Molekülen und Ionen. Die Emission des Plasmas wird dann mit Hilfe eines Wellenlängenisolators, z. B. eines Monochromators, Polychromators oder Spektrographen, in die einzelnen Wellenlängen zerlegt. Die isolierte Strahlung wird von Wandlern oder Array-Detektoren in elektrische Signale umgewandelt, die dann von Computersystemen verarbeitet und analysiert werden. 

Bei induktiv gekoppelten Plasmaemissionssystemen (ICP) wird anstelle einer Flamme ein Hochtemperaturplasma, ein so genannter Argonplasmabrenner, verwendet. Dies ermöglicht eine breitere Anwendung und eine schnelle Multielementanalyse. Bei der Gleichstromplasmaquelle (DCP) wird das Inertgas durch einen Gleichstrombogen erhitzt, der das Plasma in einem Hochgeschwindigkeitsgasstrom erzeugt. Bei der DCP wird in der Regel eine umgekehrte V-förmige Elektrodenanordnung verwendet, bei der sich der Anregungsbereich an der Kreuzung der Argonströme befindet.

Für die Bestimmung mehrerer Elemente stehen verschiedene Instrumente zur Verfügung, darunter sequentielle Spektrometer, die verschiedene Emissionslinien nacheinander scannen, und simultane Spektrometer, die Polychromatoren oder Spektrographen verwenden, um mehrere Wellenlängen gleichzeitig zu messen. Die Instrumentierung der Atomemissionsspektrometrie bietet verschiedene Optionen für optische Pfade, darunter sequentielle optische Pfade mit Monochromatoren zur sequentiellen Wellenlängenmessung und simultane direkt ablesbare Polychromatoren mit mehreren Austrittsspalten und Photoröhren zur gleichzeitigen Messung mehrerer Emissionslinien.

Atomemissionsspektroskopie: Instrumentierung

Die Instrumentierung der Atomemissionsspektrometrie (AES) umfasst verschiedene Komponenten, darunter Zerstäubungsvorrichtungen, die Proben in Gasphasen- und ...

Education

Lehre

JoVE Core

Analytical Chemistry

Analytische Chemie

Unit 1

Einheit 1

Atomic Spectroscopy

Atomspektroskopie

KEY TERMS AND CONCEPTS

WICHTIGE BEGRIFFE UND KONZEPTE

aes sample handling and detection

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 liquid samples are introduced by nebulization. A nebulizer makes a fine spray of droplets, called an aerosol, from the liquid sample. This helps the sample atomize efficiently. After atomization, the sample in a flame or plasma forms a steady mix of atoms, molecules, and ions.

The emitted light must then be separated by wavelength. Instruments use a monochromator, polychromator, or spectrograph to isolate the radiation. Transducers or array detectors turn the light into electrical signals. A computer system then processes and analyzes the data.

Some AES systems use inductively coupled plasma, or ICP, instead of a flame. An argon plasma torch creates a very hot plasma, which supports a wider range of uses and fast multi-element analysis. Direct-current plasma, or DCP, uses a DC arc to heat an inert gas in a high-velocity stream. Its design often includes an inverted V-shaped electrode setup, and the nebulizer injects the sample at the point where the argon streams meet.

AES instruments can also measure one wavelength at a time or several at once. Sequential spectrometers scan emission lines in order. Simultaneous spectrometers use polychromators or spectrographs to measure multiple wavelengths at the same time. In sequential optical paths, a monochromator measures one wavelength after another. In simultaneous direct-reading systems, multiple exit slits and phototubes collect several emission lines together.

AES Sample Handling and Detection

atomic spectroscopy: absorption, emission, and fluorescence

atomic-spectroscopy-absorption-emission-and-fluorescence

Element Analysis with Atomic Light Spectra

Atomic spectroscopy is used to identify and measure elements by their light signals. It supports both qualitative analysis, which tells what is present, and quantitative analysis, which tells how much is present. The optical methods in this group are atomic absorption spectroscopy, atomic emission spectroscopy, and atomic fluorescence spectroscopy. These methods begin with atomization. In this step, a solid, liquid, or solution sample is changed into gas-phase atoms and ions. Once the sample...

atomic spectroscopy: effects of temperature

atomic-spectroscopy-effects-of-temperature

How Heat Changes Atomic Spectra

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

Atomic Absorption Spectroscopy for Trace Metals

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

atomic-absorption-spectroscopy-instrumentation

Atomic Absorption Spectroscopy: Key Parts

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

atomic-absorption-spectroscopy-radiation-and-light-sources

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-atomization-methods

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...

atomic absorption spectroscopy: interference

atomic-absorption-spectroscopy-interference

Correcting Errors in Atomic Absorption Spectroscopy

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

Atomic Emission Spectroscopy for Element Analysis

Atomic emission spectroscopy is used to identify the elements in a sample by measuring the light they emit. Atoms are first excited to higher energy levels by thermal energy from hot sources such as plasma, arcs, or sparks. When they fall back to lower energy levels, they give off light at specific wavelengths. Each element produces its own set of lines, so the emission spectrum can show both what is present and how much is there. AES instruments are similar to atomic absorption spectrometers,...

atomic emission spectroscopy: instrumentation

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...

atomic emission spectroscopy: interference

atomic-emission-spectroscopy-interference

Reducing Interference in AES Signals

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...

inductively coupled plasma atomic emission spectroscopy: principle

inductively-coupled-plasma-atomic-emission-spectroscopy-principle

ICP-AES Torch and Sample Analysis

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

inductively-coupled-plasma-atomic-emission-spectroscopy

ICP-AES Instrument Types and Detection

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 atomic emission spectrometry uses atomizers, nebulizers, ICP and DCP sources, and detectors to separate and measure emitted light from samples.

AES Sample Handling and Detection | JoVE K12

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3.3.9-12.D

AES Sample Handling and Detection

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