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Inductively Coupled Plasma. Plasma. A Plasma consists of a collection of free-moving electrons and ions and is very hot. Energy must be continually applied to sustain the plasma. For an ICP torch, the plasma is initiated by application of sparks from a Tesla coil.
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Plasma • A Plasma consists of a collection of free-moving electrons and ions and is very hot. Energy must be continually applied to sustain the plasma
For an ICP torch, the plasma is initiated by application of sparks from a Tesla coil. • The plasma is propagated by means of an induction coil. • The applied rf produces a fluctuating magnetic field. • Ions flow and their resistance to flow generates heat. • Temperataures can reach 6,000 k – 10,000 K. • Argon cooling is absolutely imperative.
Three Ar flows are introduced to the torch: 1) Cool Gas - the outer flow ~ 14 l min-1 keeps the sides of thetorch from melting; 2) Auxilliary Flow - this is the intermediate flow through the torch that keeps the plasma away from the end of the torch at a rate of 0.5-1.5 l min-1; 3) Sample Flow - this central flow introduces the sample to the plasma at ~ 0.7-1.0 l min-1. The cool sample injected through the center of the plasma cools it to ~ 7,000 K which reduces the abundance of Ar+ but still maximizes sample ionization.
ICP is used for EmissionSpectroscopy • Occasionally used for fluorescence • Not used for absorption because the high temperatures means the atoms are in excited states • Also coupled with Mass spectrometry
ICP Torch • Plasma forms in and above inductive coil in a shape like a flame • Temperature of Plasma varies with height • PREHEATING ZONE – where sample first enters plasma • evaporation of solvent • melting and vaporization of salt • INITIAL RADIATIVE ZONE (IRZ) • atoms formed and excited • atomic emission takes place
NORMAL ANALYTICAL ZONE (NAZ) • ion formation occurs • usually +1 and +2 • TAIL OR PLUME • atoms can recombine to polyatomics • An yttrium salt can be used to visually locate these regions of the plasma • IRZ – red NAZ – blue tail – red
Optimal sensitivity for different elements occurs at different heights • But similar enough that you can successfully do simultaneous analysis using an ‘average’ height • Usually measure emission from 15-25 mm above coil-low background where there are few Ar lines • Below this height the plasma is brilliant white and transparent – a continuum with the atomic spectrum for Ar superimposed
Advantages of ICP • 6000 – 10000 K – gives better atomization • Long residence times (~2 ms) ~2 × flame • Chemically inert environment (no radicals as found in flames) prevents oxide formation • Get a lot of lines – helps identify • (also a disadvantage because spectra get so complicated)
Temperature cross-section of plasma is relatively uniform • no self absorption problems • can get linear calibration curves over several orders of magnitude • One set of conditions is close to optimum for many elements – so can do multielement analysis
ICP-AES • One can obtain a simple Li spectrum at low temperatures, for example with an air-propane flame (2000 K) • Other elements such as Uranium require higher temperatures • At higher temperatures you get a complex spectrum and you need a high resolution spectrometer to separate the lines • Interference corrections are essential
Spectrum of Mixture of Elements t 200 300 400 500 600 700 800 Pb Hg Mg Cu Zr Ca Ba Na U K