Graphite Furnace 2 CEE 772 #7 David Reckhow 1 CEE 772 - - PDF document

CEE 772 Lecture #7 9/21/2014 1

Lecture #7

Atomic Spectroscopy: Sample Treatment and Methodology

(Skoog, Chapts. 8 & 9; pp.192-203, 206-227)

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CEE 772: Instrumental Methods in Environmental Analysis

Updated: 21 September 2014

Print version

(Harris, Chapt. 22) (pp.615-635)

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Graphite Furnace

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Platform position

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Graphite Furnace

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Temperature Programming

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 Dry

 Remove solvent

 Char

 Remove organic matter and other

volatiles  Atomize

 Convert analyte to an atom vapor

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Signals

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 Analysis of Molybdenum

 A: uncoated tube  B: pyro-coated tube

Use of Matrix Modifiers

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 Thermal pretreatment for Cd using different matrix

modifiers

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Matrix Modifiers, cont.

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 Impact of K on

calibration curve for Sr

Thermal Progression

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Pretreatment/Atomization 1

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 Case for Iron

 Pretreatment

 First losses just below melting

point  Atomization

 Probably directly from metal as

many salts decompose at lower temps Pretreatment Step Atomization Step

Pretreatment/Atomization 2

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 Case for Antimony

 Pretreatment

 First losses just below

melting point  Atomization

 Probably delayed due to

high temp of salt decomposition Pretreatment Step Atomization Step

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Standard Addition

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 Use of standard

addition to compensate for matrix effects

Photomultiplier

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Plasma source

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The sample is nebulized and entrained in the flow of plasma support gas, which is typically Ar. The plasma torch consists of concentric quartz tubes, with the inner tube containing the sample aerosol and Ar support gas and the outer tube containing an Ar gas flow to cool the tubes (see schematic). A radiofrequency (RF) generator (typically 1-5 kW @ 27 MHz or 41 MHz) produces an

• scillating current in an induction coil that wraps

around the tubes. The induction coil creates an

• scillating magnetic field, which produces an oscillating

magnetic field. The magnetic field in turn sets up an

• scillating current in the ions and electrons of the

support gas. These ions and electrons transfer energy to

• ther atoms in the support gas by collisions to create a

very high temperature plasma.

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Element Wavelength (nm) Estimated Detection Limit (µg/L) Aluminum 308.215 45 Antimony 206.833 32 Arsenic 193.696 53 Barium 455.403 2 Beryllium 313.042 0.3 Boron 249.773 5 Cadmium 226.502 4 Calcium 317.933 10 Chromium 267.716 7 Cobalt 228.616 7 Copper 324.754 6 Iron 259.940 7 Lead 220.353 42 Magnesium 279.079 30 Manganese 257.610 2 Molybdenum 202.030 8 Nickel 231.604 15 Potassium 766.491 See note c Selenium 196.026 75 Silicon 288.158 58 Silver 328.068 7 Sodium 588.995 29 Thallium 190.864 40 Vanadium 292.402 8 Zinc 213.856 2

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Atomization and MS

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Quadrupole

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Plasma MS

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ICP-MS

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 To next lecture