14.13
电感耦合等离子体(ICP)是原子发射光谱(AES)中常用的等离子体源,是一种检测和分析样品中各种元素的技术。这种方法通常称为电感耦合等离子体原子发射光谱法 (ICP-AES)。
电感耦合等离子体原子发射光谱仪(ICP-AES) 主要有三种类型:顺序式光谱仪、多通道光谱仪和傅里叶变换光谱仪,其中,傅里…
等离子体发射光谱法使用三种基本类型的仪器。
顺序等离子体发射光谱仪一次仅测量一条发射谱线,而多通道和傅里叶变换仪器可同时测量多条发射谱线。
顺序光谱仪通常使用光栅单色仪,通过旋转光栅将不同波长的光聚焦到出射狭缝上。
例如,在扫描式光谱仪中,单色器会快速旋转至接近某一条发射谱线的波长,然后以微小步长逐步扫描该谱线。
相比之下,扫描式埃舍尔光谱仪在狭缝板后方设有可移动的光电倍增管,埃舍尔光栅将波长散射成一个宽广的阵列,可逐次通过单个狭缝进行检测。
一些多通道仪器采用光栅多色仪,并在固定出射狭缝后方放置光电倍增管,以同时测量多条发射谱线。
其他多通道仪器采用光谱仪进行同时测量,并使用二维电荷注入器件或电荷耦合器件作为换能器。
尽管傅里叶变换光谱仪具有宽波长覆盖范围,但由于其多种局限性,在原子发射光谱分析中并未得到广泛应用。
View the full transcript and gain access to JoVE Core videos
Q1: What are the three main types of ICP-AES instruments?
ICP-AES instruments fall into three categories: sequential, multichannel, and Fourier transform types. Sequential instruments measure one emission line at a time by rotating a monochromator to focus different wavelengths on an exit slit. Multichannel instruments simultaneously measure multiple emission lines using either a polychromator with photomultiplier tubes or a spectrograph with charge-coupled devices. Fourier transform spectrometers offer wide wavelength coverage but are rarely used in atomic emission spectroscopy due to various limitations.
Q2: How does a grating monochromator work in sequential spectrometers?
A grating monochromator uses a holographic grating with 2400 or 3600 grooves per millimeter. A digitally controlled stepper motor rotates the grating to focus different wavelengths sequentially and precisely on the exit slit. This allows sequential spectrometers to measure one emission line at a time by positioning the grating so that each desired wavelength aligns with the exit slit for intensity measurement.
Q3: What is the difference between slew-scan and scanning echelle spectrometers?
Slew-scan spectrometers rapidly rotate the monochromator to a wavelength near an emission line, then scan across that line in small steps to minimize time spent in non-useful wavelength regions. Scanning echelle spectrometers use a different approach: they employ an echelle grating that scatters wavelengths in a broad array, with a moving photomultiplier tube behind an aperture plate detecting wavelengths one slit at a time.
Q4: How do multichannel instruments measure multiple elements simultaneously?
Multichannel instruments use either a polychromator or spectrograph for simultaneous detection. Polychromators contain multiple photomultiplier tubes positioned behind fixed exit slits along the focal curve of a grating, each detecting a different emission line. Spectrographs employ two-dimensional charge-injection devices or charge-coupled devices as transducers to capture multiple wavelengths at once, enabling rapid analysis of multiple elements.
Q5: What are the advantages and disadvantages of sequential versus multichannel ICP-AES?
Sequential instruments are more straightforward and cost-effective initially but require more time and sample consumption since they measure each element individually. Multichannel instruments measure multiple elements simultaneously or nearly so, reducing analysis time and sample usage, making them more efficient for routine analyses. The choice depends on analytical throughput needs and budget constraints for specific applications.
Q6: Why are Fourier transform spectrometers rarely used in atomic emission spectroscopy?
Although Fourier transform spectrometers offer significant advantages including wide wavelength coverage, high speed, high resolution, accurate wavelength measurements, large dynamic range, compact size, and large optical throughput, they are not widely used in atomic emission spectroscopy due to various limitations. These limitations outweigh their benefits for most AES applications, making traditional grating and echelle spectrometers more practical choices.
Q7: What detection devices are used in multichannel spectrographs?
Multichannel spectrographs employ two-dimensional transducers for simultaneous wavelength detection. The primary devices used are charge-injection devices and charge-coupled devices, which capture multiple emission lines across a broad wavelength range at once. These two-dimensional detectors enable rapid, simultaneous measurement of multiple elements, making spectrographs ideal for high-throughput analytical applications.