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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

4

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