Name: flame emission spectrometry basics
Uploaded: 2024-12-05T18:32:16.000Z
Duration: 1 min 2 s
Channel: JoVE

K12 Standards

Pennsylvania State Academic Standards

9-12

Earth and Space Science

Space Systems

3.3.9-12.C

Flame Photometry: Overview

A fotometria de chama, ou espectrometria de emissão de chama, usa uma chama para excitar uma solução de amostra.
As chamas devem possuir energia suficiente para atomização, baixa emissão e absorção em comprimentos de onda relevantes e a capacidade de operar em baixas velocidades do gás.
As chamas de ar propano são normalmente usadas, pois as chamas de ar butano e gás natural são menos sensíveis devido a temperaturas mais baixas.
Os fotômetros de chama usam um sistema de nebulizador-queimador para transformar a solução da amostra em uma névoa ou aerossol. Existem dois tipos principais de queimadores.
Os queimadores de pré-mistura ou fluxo laminar geram uma névoa fina em uma câmara de vaporização, que é então misturada com combustível e gases oxidantes antes de atingir o cabeçote do queimador.
Os queimadores de consumo total ou fluxo turbulento consistem em três tubos concêntricos que transportam a solução de amostra, gás combustível e gás oxidante separadamente, permitindo que eles se misturem apenas na ponta do queimador.

fotometria de chama: visão geral

A fotometria de chama, também conhecida como espectrometria de emissão de chama, é uma técnica usada para a análise qualitativa e quantitativa de elementos presentes em uma amostra usando uma chama como fonte de energia de excitação. O conceito de fotometria de chama foi realizado no início da década de 1860 por Kirchhoff e Bunsen, que descobriram que elementos específicos emitem radiação característica quando excitados em chamas. O primeiro instrumento desenvolvido para esse propósito foi usado para medir o sódio (Na) em cinzas de plantas usando uma chama de Bunsen. No entanto, o desafio estava em encontrar a maneira mais eficaz de introduzir a amostra na chama. Foi somente em 1929, quando Lundegardh introduziu um nebulizador, que um avanço significativo foi feito, permitindo uma introdução reproduzível da amostra na chama.

Na espectrometria de emissão de chama, o nebulizador converte uma amostra líquida em uma névoa fina ou aerossol. Isso é obtido passando um fluxo de gás de alta pressão sobre a extremidade de um tubo capilar contendo a amostra e aspirando-a para uma câmara de pulverização. O aerossol produzido é então passado para o queimador, onde o calor da chama o dessolvata, formando partículas secas que se volatilizam e produzem átomos livres para análise.

Os primeiros instrumentos utilizavam espectrógrafos de prisma de quartzo e gravação fotográfica para dispersar e capturar linhas de emissão atômica. No entanto, avanços em filtros ópticos e fotodetectores elétricos substituíram esses componentes, melhorando a precisão e a conveniência.

A fotometria de chama envolve a introdução da solução da amostra em um nebulizador, que a converte em uma névoa fina ou aerossol. A amostra atomizada então entra na chama, junto com ar ou oxigênio e um gás combustível, como propano ou acetileno. A chama fornece a excitação térmica necessária para energizar os átomos na amostra. À medida que esses átomos excitados relaxam, sua radiação emitida é detectada por uma fotocélula ou fotomultiplicador.

A fotometria de chama é particularmente eficaz na medição de elementos de sódio, potássio, lítio e cálcio. A chama usada na fotometria de chama é tipicamente uma chama de propano-ar com uma faixa de temperatura de 1900-2000 °C, embora chamas alternativas como butano-ar ou gás natural-ar também possam ser usadas. A fotometria de chama tem algumas limitações que podem ser superadas usando temperaturas mais altas e chamas mais redutoras, como ar-acetileno, juntamente com detecção espectrométrica de alta resolução. No entanto, essas abordagens não são competitivas em termos de custo em comparação com a técnica de espectrometria de absorção atômica por chama ou AAS, a qual é mais amplamente aplicável.

Fotometria de Chama: Visão Geral

A fotometria de chamas, também conhecida como espectrometria de emissão de chamas, é uma técnica utilizada para a análise qualitativa e quantitativa de elementos presentes em um ...

Education

JoVE Core

Analytical Chemistry

Química Analítica

Unit 1

Unidade 1

Atomic Spectroscopy

Espectroscopia Atômica

KEY TERMS AND CONCEPTS

TERMOS E CONCEITOS-CHAVE

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 sample to the flame in a steady way.

That problem changed in 1929, when Lundegardh introduced a nebulizer. A nebulizer turns a liquid sample into a fine mist, or aerosol. A high-pressure gas stream passes over a capillary tube, draws the sample into a spray chamber, and sends the aerosol to the burner.

At the burner, flame heat removes the solvent and leaves dry particles. These particles volatilize and form free atoms for analysis. Early instruments used quartz prism spectrographs and photographic recording to separate and capture the atomic emission lines. Later, optical filters and electrical photodetectors replaced those parts and made the method more precise and easier to use.

In a flame photometry setup, the sample solution enters the nebulizer and then the flame with air or oxygen and a fuel gas such as propane or acetylene. The flame supplies the thermal energy needed to excite the atoms. When the atoms return to a lower energy state, they emit radiation that is measured by a photocell or photomultiplier.

This method is especially useful for sodium, potassium, lithium, and calcium. A propane-air flame is commonly used and reaches about 1900 to 2000 degrees Celsius. Butane-air and natural gas-air flames can also be used. Some limits can be reduced with higher temperatures and more reducing flames, such as air-acetylene, together with higher-resolution spectrometric detection. Even so, these options are not as cost-competitive as flame atomic absorption spectrometry, also called AAS.

Flame Emission Spectrometry Basics

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-spectroscopy-instrumentation

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...

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 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 flame emission spectrometry uses a nebulizer, flame excitation, and photodetectors to measure elements like sodium, potassium, lithium, and calcium.

Flame Emission Spectrometry Basics | JoVE K12

analytical chemistry

JoVE Core Analytical Chemistry simplifies complex chemical principles by breaking them down into clear, engaging animations, making topics from SI Units to NMR spectroscopy more accessible and straightforward. Additionally, the scientist-in-action videos highlight the application of these concepts in real-world research conducted in laboratories globally.

Arizona Science Standards

High School

Physical Science

HS+C.P1

HS+C.P1U1.2

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3.3.9-12.A

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3.3.9-12.D

Flame Emission Spectrometry Basics

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