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TRANSCRIPT
Atomic Spectroscopy Basics
Fergus Keenan Thermo Fisher Scientific
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Not measurable
ICP-MS
Unstable elements
AA/ICP/ICP-MS ICP/ICP-MS
H
Na
Li
K
Rb
Cs
Fr
Mg
Be
Ca
Sr
Ba
Ra
Sc
Y
La
Ac
Ti
Zr
Hf
V
Nb
Ta
Cr
Mo
W
Mn
Tc
Re
Fe
Ru
Os
Co
Rh
Ir
Ni
Pt
Cu
Ag
Au
Zn
Cd
Hg
Al
B
Ga
In
Tl
Si
C
Ge
Sn
Pb
P
N
As
Sb
Bi
S
O
Se
Te
Po
Cl
F
Br
I
At
He
Ar
Ne
Kr
Xe
Rn
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th Pa U Pu Am Cm Bk Cf Es Fm Md No Lw Np
Pd
The Periodic Table; Our Common Language
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Elemental Analysis
H
Li
Fr Ra
Sc
Ac
Zr
Hf
Nb
Ta
Tc
Re
Ru
Os
Rh
Ir Hg
In
Tl
Ge
Sb
Bi
S
Te
Po
Cl
F
At
He
Ar
Ne
Kr
Xe
Rn
Pa Pu Am Cm Bk Cf Es Fm Md No Lw Np
Not measurable
ICP-MS
Unstable elements
AA/ICP/ICP-MS ICP/ICP-MS
IC
Na
K
Rb
Cs
Be
Mg
Ca
Sr
Ba
Y
La
Ti V Cr
Mo
W
Mn Fe Co Ni
Pd
Pt
Cu
Ag
Au
Zn
Cd
Al
Ga
Sn
Pb
B C O N
Br
I
Si P
As Se
Ce Pr
Th
Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
U
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Perf
orm
ance
Investment
Trace Elemental Analysis Product Range
iCE 3000 Series AA
iCAP 6000 Series ICP
X-Seriesll ICP-MS
Element 2 ICP-MS
AA, ICP and ICP-MS…
Redefined…
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Quadrupole ICP-MS
ICP-OES
Furnace AA
Flame AA
Performance Characteristics
1 ppq 1 ppt 1 ppb 1 ppm 1,000 ppm 100%
Magnetic Sector ICP-MS
Detection Limit / Range
ICP-OES Technology
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Atomic Emission Theory
• This high-temperature atomisation source provides sufficient energy to promote the atoms into high energy levels. When the atoms decay back to lower levels, they simultaneously emit light in the form of a photon
M M+ Atom Ion
+ photon
State I State II
+ photon
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Atomic Emission explained
• Atomic Emission – the wavelength regions
Spectral Region
Vacuum UV Ultra-Violet Visible Near IR
Wavelength = nm 160 190 360 760 900
Lower wavelengths are shorter and have more energy, higher wavelengths e.g. in the Visible region, are longer and have less energy
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Inductively Coupled Plasma (ICP)
• Quartz torch surrounded by induction coil
• Magnetic coupling to ionized gas
• High temperature – equivalent to 10,000k
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Plasma Advantages
• High Temperature – allows for full dissociation of sample components
• Argon is Inert – non reactive with sample • Linearity – analysis of samples from ppb to ppm range in the same
method • Matrix tolerance – robust and flexible design with Duo and Radial
options
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Sample Transport
MX M M+
M*
+ photon + photon M+*
State I State II
Solid Solution Gas
Atom Ion
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Simultaneous Optics – Echelle Spectrometer
ICP-Source
Detector
Prism Grating
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What you get
Full, continuous wavelength coverage; never miss an analyte
Inductively Coupled Plasma Mass Spectrometry
Fergus Keenan Thermo Fisher Scientific
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ICP-MS Process: Quadrupole ICP-MS
Ion Lens Quad Detector M+
Li-U
M+
Li, Be, B. Pb, Bi, U. M+ detected
3. 4. 5.
Plasma
Sample
M+
Li-U
1.
Interface
2.
• 5 Basic Stages • 1. Sample Introduction and Ion Generation • 2. Ion Extraction • 3. Ion Focussing • 4. Separation of Analyte Ions in Quadrupole Mass Filter • 5. Ion Detection
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ICP Ion optics and mass spectrometer
Ion detection
ICP-MS in a nutshell
Sampling interface
Sample intro
• Most elements possible (around 80)
• Elemental and isotopic information given
• Concentration range ppq (pg/L) to mid-ppm (100s mg/L)
• Rapid analysis – 2-6 minutes per sample
• Good precision – ~2% RSDs
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ICP-MS: characteristic mass spectrum
• Simple spectra (primarily M+ ions) - Simple interpretation
• Very high signal to background - Low detection limits
ICP-MS Spectrum - Vanadium (51V) ICP-AES Spectrum - Vanadium 10 mg/L
• Many emission lines • High continuum background
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Characteristics of ICP-MS
• Elemental and isotopic information
56Fe
54Fe 57Fe
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• Low limits of detection • Wide dynamic range
X Series ICP-
ICP-AES
GFAAS
AAS
ICP-AES
GFAAS
AAS
XSERIES 2 ICP-MS
1 ppq 1 ppt 1 ppb 1 ppm 1,000 ppm 100%
Characteristics of ICP-MS
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History of ICP-MS
VG Elemental~1980
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First commercial ICP-MS
VG Elemental PlasmaQuad – Pittcon 1983
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1995 Fully Automated ICP-MS
VG Elemental PQ3 – Winter Plasma Conference 1995
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First commercial Collision Cell ICP-MS
VG Elemental PQ ExCell – Winter Plasma Conference 1999
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XSERIES 2
• Routine Trace Element Analysis • ppt to ppm levels
• Smallest ICP-MS • Collision Cell Technology
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Typical Application Areas
• Environmental • Drinking Water • Sludges & Soils
• Semiconductor • Process Chemicals • Organics, Gasses, VPD
• Nuclear • Hot Waste • Uranium Fuel Production
• Nuclear-Environmental • Ground Water, Soils & Air • Urine & Blood,
• Metals, Materials and Chemicals • High Temperature Alloys • High Purity Metals and Solid
Sampling • Earth Science
• Igneous Rocks • Climatology, • Sediments, Seawater, Biological
(plants) • Life Sciences
• Blood, Urine • Drugs • Tissues, Food/Agriculture