Analytical Chemistry - Module 17: GLOW DISCHARGE ATOMIC EMISSION SPECTROMETRY AND PLASMA EMISSION SPECTROMETRY

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DIRECT-CURRENT PLASMA SOURCE

Experimentally it is arranged for the plasma to be established in a high-velocity gas stream.

PLASMA EMISSION SPECTROMETRY

Is a type of emission spectrometry that uses plasma to produce excited atoms and ions that emit electromagnetic radiation at wavelengths characteristic of a particular event

GLOW DISCHARGE ATOMIC EMISSION SPECTROMETRY (GD-AES)

Is an analytical technique used in the analysis of solid conducting materials

PRISMS and DIFFRACTION GRATINGS

It is a part of the Plasma Emission Spectrometer which is used in the dispersion of the emitted radiation and in the presentation of the analytical signal.

Secondary Ion Mass Spectrometry

It is a technique capable of providing information about the elemental and isotopic composition of samples in situ from a few micrometers down to the sub-micron scale.

Inductively Coupled Plasma Optical Emission Spectrometry

It is a technique in which the composition of elements in samples, mostly water-dissolved, can be determined using plasma and a spectrometer.

Inductively coupled plasma atomic emission spectrometry (ICP-AES)

Its main use in conventional analysis is in the determination of lithium and boron in glass, glazes, borates, petalite, and magnesite.

O-ring

Once a sample is properly prepared, sample introduction consists of simply placing a sample over the ______ at the lamp opening and allowing the vacuum to hold it in place.

Trace Element

Plasma Emission Spectrometry is enormous and is most helpful in almost every field where ______ analysis is carried out

Plasma Emission Spectrometry

The potential for the employment of _____ is enormous and it is finding use in almost every field where trace element analysis is carried out

electric spark ablation laser ablation electrothermal volatilization

There is an obvious attraction in being able to handle a solid directly, and sample volatilization methods using ____, ____, and ____ have also been developed.

GLOW DISCHARGE ATOMIC EMISSION SPECTROMETRY (GD-AES)

This also eliminates the need for lengthy sample preparation steps

Glow Discharge Atomic Emission Spectrometry

This technique is an ideal tool to investigate from the surface down to more than 150 microns with a depth resolution that can be as good as 1 nm.

Direct Current Plasma Source

This type of Plasma Emission Source has a distinct advantage; stability with varying sample matrices, a characteristic which is particularly valuable where the solvent contains a high concentration of dissolved solids.

Inductively Coupled Plasma Torch

This type of Plasma Emission Source uses an ion source that consists of a torch that is surrounded by a radio frequency generator that ionises argon gas inside the torch to form a high-temperature (up to 10,000 K) plasma that can be used to ionise analytes.

GLOW DISCHARGE ATOMIC EMISSION SPECTROMETRY (GD-AES)

This type of analysis is beneficial for studying a material's composition without changing the chemistry of the sample being analyzed

Rocks, soils, waters and biological tissue

____, ____, ____, and ____ are typical of samples to which the plasma emission spectrometry may be applied

GLOW DISCHARGE ATOMIC EMISSION SPECTROMETRY (GD-AES)

combines the advantages of inductively coupled plasma-optical emission spectrometry with the solid sampling of XRF techniques

ICP source

has been applied to provide a source of ions for mass spectrometry

GLOW DISCHARGE ATOMIC EMISSION SPECTROMETRY (GD-AES)

has the ability to accurately and rapidly determine a depth profile of multiple layers of varying composition on a substrate

sputtering

impact on the surface of the cathode leading to vaporization and excitation of atoms from its surface.

DIRECT-CURRENT PLASMA SOURCE

initial heating of an inert gas, usually argon, is produced by a dc-arc.

GD-AES instrument

is a fairly simple piece of equipment to operate, in comparison to other instruments capable of similar analyses.

sputtering

is also the basis of the hollow cathode lamp used in atomic absorption spectrometry

GLOW DISCHARGE ATOMIC EMISSION SPECTROMETRY (GD-AES)

is faster, cheaper and easier to perform than for example Glow Discharge Mass Spectrometry (GD-MS) or SIMS, mainly because it does not require ultrahigh vacuum

Inductively coupled plasma atomic emission spectrometry (ICP-AES)

is the next most important ceramic instrumental method, and is competitive with XRF at minor determination levels and better at trace levels

Plasma emission spectrometry

is well established as a routine method of analysis in these areas.

ICPE-9800 Series Systems

represent the ultimate in ICP atomic emission spectrometry for environmental, pharmaceutical, food, chemical, metal, and other fields

Secondary Ion Mass Spectrometry (SIMS)

technique capable of providing information about the elemental and isotopic composition of samples in situ from a few micrometers down to the sub-micron scale

INDUCTIVELY COUPLED PLASMA-OPTICAL EMISSION SPECTROMETRY

technique in which the composition of elements in samples, mostly water-dissolved, can be determined using plasma and a spectrometer; wide detection range, speed, and lack of interference

PLASMA EMISSION SPECTROMETRY

the gas usually used is argon which is ionized by influence of a strong electrical field either by direct current of by radio frequency

Glow discharge spectrometer

uses a low pressure process to sputter material from the surface of a sample using a gas such as argon

GLOW DISCHARGE ATOMIC EMISSION SPECTROMETRY (GD-AES)

was also routinely used for the bulk analysis of materials that are used in nuclear and uranium enrichment plants.

glow discharge lamp (GDL)

· can be used for the analysis of trace, minor and major constituents in electrically conducting samples, especially metallurgical specimens.

INSTRUMENTATION (PES)

- Emission spectrometer incorporating a sample nebulizer, grating monochromator, photomultiplier detection system and microprocessor controller. - Excitation by dc-arc plasma jet, or inductively coupled plasma. Laser excitation is sometimes used.

PRINCIPLES (GD-AES)

- Emission spectrum generated by bombardment of samples by argon ions in a "sputtering process"

INSTRUMENTATION (GD-AES)

- Glow discharge lamp (GDL) - Analogous to hollow cathode lamp, in which the sample acts as the cathode - Attached to a standard atomic emission spectrometer

DISADVANTAGES (GD-AES)

- Limited scope for sample types

APPLICATIONS (GD-AES)

- Limited to samples that are electrically conducting - Gives high stability signals - Valuable in metallurgy

APPLICATIONS (PES)

- Relative precision 0.5-2%

DISADVANTAGES (PES)

- Samples require dissolution before analysis. - Instrumentation is complex and expensive to purchase and operate.

APPLICATIONS (PES)

- Very widespread for qualitative and quantitative analysis of metals and some non-metals, particularly at trace levels.

Inductively coupled plasma atomic emission spectrometry (ICP-AES)

- the analysis of composition of mortars (BS4551) and concrete (BS1881)

PRINCIPLES (PES)

-Emission of electromagnetic radiation (energy that is transmitted at the speed of light through oscillating electric and magnetic fields) in the visible and ultraviolet regions of the spectrum by atoms and ions after electronic excitation in a high temperature gas plasma - Laser excitation is sometimes used.

ICPE-9800 Series of simultaneous ICP atomic emission spectrometers

-are next-generation systems that offer the superior accuracy necessary to simultaneously and quickly analyze multiple elements regardless of their concentration levels. -They also feature user-friendly software that makes analysis easy. -the systems reduce analysis costs while providing the highest performance levels in the industry

The GD-Profiler 2

-provides fast, simultaneous analysis of all elements of interest including the gases nitrogen, oxygen, hydrogen and chlorine. -It is an ideal tool for thin film characterization and process studies.

glow discharge lamp (GDL)

A recent development in emission spectroscopy has been the ______ as an excitation source

the inductively coupled plasma (ICP) torch

A second plasma emission source which has become the most popular

Inductively coupled plasma atomic emission spectrometry (ICP-AES)

Another major use is for the analysis of liquid samples such as acid- or water-soluble salts from clay or bricks, slip liquors, and ceramic waste-product leachates (for landfill, packaging waste, and special waste regulations).

prisms diffraction gratings

Different combinations of ____ and ____ may be used in the dispersion of the emitted radiation, and in the presentation of the analytical signal

ICP-OES and XRF

GD-AES combines the advantages of ____ AND ______

depth

Glow discharge optical emission spectrometry (GD-OES) is a widely used tool for fast measurements of _____ profiles

Nebulizer

In Sample Introduction for Plasma Sources, sample solution is pumped by a peristaltic pump at a fixed rate and converted into an aerosol by a ______

Argon

In plasma emission spectrometry, the gas usually used is ____ which is ionized by influence of a strong electrical field either by direct current of by radio frequency

By Direct Current By Radio Frequency

In plasma emission spectrometry, the gas usually used is argon which is ionized by influence of a strong electrical field either ____ or _____

GLOW DISCHARGE ATOMIC EMISSION SPECTROMETRY (GD-AES)

a depth profiling technique on samples with varying layers of both conducting and non-conducting materials, it is also capable of rapid bulk analysis of homogenous, solid samples

AUGER ELECTRON SPECTROSCOPY

a surface-specific analytical technique that utilizes a high-energy, finely-focused electron beam as an excitation source

PLASMA

an electrically neutral, highly ionized gas that consists of ions, electrons and atoms

Sophisticated data handling packages

are employed routinely to deal with interferences, and to provide for clarity in data output

Glow discharge spectrometer

are especially useful for their ability to perform rapid analyses on films and coatings


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