Agilent 7500 Series ICP-MS

1
Agilent 7500 Series ICP-MS An Introduction
Presented By Ferdi Ferdian Kusnadhi
2
What is ICP-MS?
An inorganic (elemental) analysis technique

• ICP - Inductively Coupled Plasma
• high temperature ion source
• decomposes, atomizes and ionizes the sample

• MS - Mass Spectrometer
• featuring quadrupole mass analyzer
• mass range - 7 to 260 amu (Li to U...)
• separates all elements in rapid sequential scan
• ions measured using dual mode detector
• ppt to ppm levels
• isotopic information available

ICP-MS has the detection limits of GFAA and the
sample throughput of ICP-OES
3
Agilent 7500ce ICP-MS System withCollision
Reaction Cell (CRC)
Multi-element interference removal by on-axis
octopole reaction cell
Fast simultaneous dual mode detector (9 orders
dynamic range)
Reaction Gas Inlet
High temperature 27MHz plasma generator
Octopole
Plasma
Off-axis Lens
High frequency hyperbolic quadrupole
Low flow sample introduction system
4
Agilent 7500 Series ICP-MS

• Agilent 7500ce (G3272A)
• Enviro, foods, biological...
• Robust Octopole Reaction System (ORS)
• Superb capability in the most complex matrix
• Flexibility

• Agilent 7500a (G3271A) Standard ICP-MS
• General purpose that does not require collision
• Standard ShieldTorch System for cool plasma
• Upgradeable to ORS

• Agilent 7500cs (G3273A)
• Semiconductor, RD.
• Ultra low BECs at high plasma power
• Cool plasma also available

5
Different ways of acquiring information from a
sample

• Qualitative scan
• Semiquantitative Analysis
• Fully quantitative data

6
Primary Agilent ICP-MS Team in Asia Pacific
Dedicated Applications Support
Dedicated Sales Support
Asia Pacific Resource
Dr Christopher Tye Asia Pacific Business
Development Manager Based in Singapore
Dr Deng-yun Chen Senior ICP-MS Applications
Specialist Greater China Based in China
Fan Chen ICP-MS Product Specialist SMT
Kung-yu Chen Peak ICP-MS/semiconductor Sales
Greater China Based in Taiwan
David Wilkinson ICP-MSProduct Support Engineer
Asia Pacific Based in Australia
Yu-hong Chen ICP-MS Applications Specialist
Greater China Based in China
Fred Fryer Senior ICP-MS Applications Specialist
South East Asia Based in Australia
Jerry Leu ICP-MS Product Specialist Greater
China Based in Taiwan
7
Factory Trained Agilent ICP-MS Service
Engineers(AP Region Only, excluded JPN)
S Korea - 5
China - 8
Taiwan - 4
Hong Kong - 1
Vietnam - 1
Malaysia - 2
India - 1
Thailand - 1
Australia - 5
Singapore - 2
Country with Agilent ICP-MS installed
New Zealand - 1
No Agilent ICP-MS installed
8
Application Notes of interest to the
Semiconductor Market

• 5989-4348EN Determination of Impurities in
  Semiconductor Grade Hydrochloric Acid Using the
  Agilent 7500cs ICP-MS AN 12/2005
• 5988-8901EN Determination of Trace Metal
  Impurities in Semiconductor Grade Phosphoric Acid
  by High Sensitivity Reaction Cell ICP-MS AN
  11/2004
• 5988-9190EN Analysis of Impurities in
  Semiconductor Grade Sulfuric Acid using the
  Agilent 7500cs ICP-MS AN 11/2004
• 5988-9529EN Characterization of Trace Impurities
  in Silicon Wafers by High Sensitivity Reaction
  Cell ICP-MS AN 11/2004
• 5988-9892EN Analysis of Impurities in
  Semiconductor Grade TMAH using the Agilent 7500cs
  ICP-MS AN 11/2004
• 5989-0629EN Direct Analysis of Photoresist and
  Related Solvents using the Agilent 7500cs ICP-MS
  AN 11/2004
• 5989-0321EN Analysis of Electroceramics Using
  Laser Ablation ICP-MS AN 10/2004

9
Agilent ICP-MS in Asia PacificBig Growth - Big
Rewards!

• In FY06 we sold 84 units (in calendar year 2006
  108!)
• Our market share in 06 is 45!
• Why do we win?
• Our technical advantages (especially the 7500ce)
  and the fact we have the best people supporting
  the field means we win most deals!

10
What is .
A Mass Spectrometer
DETECTOR
ION SOURCE
MASS FILTER
Produces ions
that are
separated according to mass
and
detected
Chemical Ionization (CI)
Electron Impact Ionization (EI)
Time to Frequency (TOFs only)
Time Of Flight (TOF)
Electrospray Ionization (ESI)
Ion Trap
Electron Multiplier
Quadrupole
Atmospheric Pressure Photo Ionization (APPI)
Atmospheric Pressure Chemical Ionization (APCI)
Matrix Assisted Laser Desorption Ionization
(MALDI)
11
What Else Can Be Measured Using MS?

• Many of you have been successful in selling
  organic MS
• Used to get molecular or structural information
  from a sample
• What about inorganic MS?
• For characterising elements
• Only dealing with the Periodic Table
• Only 256 natural isotopes
• Generally only quantitative data required
• The difference between inorganic MS and organic
  MS lies primarily within one component of a mass
  spectrometer..

THE SOURCE
12
Advantages of ICP-MS

• Excellent detection limits
• low ppb - ppt for all elements
• Wide elemental coverage - from Li - U
• over 70 elements measurable
• High throughput
• all elements determined simultaneously
• 20 element run/3 replicates/washout in 3 minutes
• Wide dynamic range
• linear over 9 orders

• Powerful semiquantitative analysis
• no standards needed
• Isotopic analysis
• isotope ratios
• isotope dilution
• Routine technique
• many users run systems overnight
• Small size
• saves lab space
• mobile installations

13
7500ce Widest Analytical Range of ANY ICP-MS-
these 4 calibration plots were generated
simultaneously in a single run
Calibration rangesHg (0.01 2ppb) Std ModeAs
(0.1 200 ppb) He ModeSe (0.1 200 ppb) H2
ModeNa (0.05 1180 ppm) He ModeOverall
calibration range 10ppt (Hg) to 1180 ppm (Na) in
a single method- without attenuating ion
transmission to increase working
rangeNaTypically, ICP-MS cannot measure
above 200ppm Na without changing quad
resolution or ion lens settingsHgHg detection
limit by 7500ce is about 3ppt 7500ce can
QUANTIFY at 10ppt!7500ce can measure both Na
and Hg in the same run!
14
Elemental Coverage of ICP-MS
Almost every element can be measured by ICP-MS
(including actinides), mostly at extremely low
limits of detection
15
The Majority of Elements Have ppt and Below
Detection Limits

• Over 70 elements can be analysed at trace levels
• In the same measurement cycle
• Over a wide dynamic range

16
Overview of Inorganic Analysis Techniques

• Atomic Absorption Spectrometry
• Light having a wavelength characteristic of the
  analyte is passed through the sample. The amount
  of light absorbed is proportional to
  concentration.
• ICP-Optical Emission Spectrometry
• Energy from the plasma promotes an electron to a
  higher energy level (excitation). Electron falls
  back and emits light at a characteristic
  wavelength. Light emission is proportional to
  concentration
• ICP-Mass Spectrometry
• Energy from the plasma ejects electron from shell
  (ionization). Result is a positively charged
  analyte ion. Ions are separated by the mass
  spectrometer and measured. Ions measured are
  directly proportional to analyte concentration.

Sequential
Simultaneous Criteria1 GFAAS ICP-OES ICP-OES ICP-
MS Detection Limits ppt ppb ppb
ppq-ppt Linear Range (orders) 2-3
4-6 4-6 8-9 Interferences
Moderate Many Many Few Speed
Slow Slow Fast Fast Elemental
Coverage Poor Excellent Good
Excellent Multi-element No Yes
Yes Yes Simultaneous
No No Yes Yes Sample Size
uL mL mL uL or mL Capital Cost
Operating Cost

Agilent 7500 Series only - (other ICP-MS - 8
orders) ICP-MS combines the sensitivity of GFAAS
with the speed flexibility of OES while
offering a wider dynamic range and fewer
interferences!
1 ICP-MS The new standard for inorganic
analysis American Laboratory News, Nov.1998
17
Overview of Inorganic Analysis Techniques
Sequential
Simultaneous Criteria1 FAAS GFAAS ICP-OES ICP-OES
ICP-MS Detection Limits 10ppb 50 ppt 1 ppb lt1
ppb sub-ppt Linear Range (orders)
3-4 2-3 4-6 4-6 9 Interferences
Chemical Many Many Some Some Some
Spectral Some Many Some Some Some
Matrix Many Many Some Some Few Speed Moderate
Slow Slow Fast Fast Elemental Coverage Moderate
Poor Good Good Excellent Typical
no. 50 35 55 55 70 Multi-element No
No Yes Yes Yes Simultaneous
N/A N/A No Yes Yes Sample Size mL
uL mL mL uL or mL Capital Cost
Operating Cost
Agilent 7500 Series only - (other ICP-MS 8
orders)
GFAAS operating cost high due to consumables
(furnace tubes) and operator time (sample prep,
many reruns due to small dynamic range)
18
Who Uses Agilent ICP-MS WW ?
Over 2/3 of Agilent ICP-MS users Worldwide are
either environmental or semiconductor, but other
applications and lab types are extremely varied.
Most users are in routine labs
19
Comparison of Metals Techniques - Speed vs
Detection Power
Fast
ICP-OES - most elements single figure ug/L DLs
and good productivity
ICP-MS - most elements single figure ng/L DLs and
very productive
Typical Speed of Analysis
GFAAS is a key target market for ICP-MS!
GFAAS most elements sub-ug/L DLs but poor
throughput
FAAS most elements 10 ug/L DLs
Slow
ug/L (ppb)
ng/L (ppt)
mg/L (ppm)
Typical Detection Limit
20
Agilent 7500 - 3 Sigma Detection Limits
Standard pneumatic nebuliser 3 sec/mass
integration time Class 1000 cleanroom with
ShieldTorch
0.1 - 1ppt
21
Extending the Capabilities of ICP-MS

• ICP-MS instruments can be coupled to different
  sample introduction devices that extend the
  overall usefulness
• Laser Ablation ICP-MS
• Liquid (or Ion) Chromatography ICP-MS
• Gas Chromatography ICP-MS
• Capillary Electrophoresis ICP-MS

22
Laser Ablation ICP-MS

• Pulsed NdYAG laser is used to ablate solid
  samples into the plasma
• Useful for solids
• No dissolution process required
• Useful for bulk analysis and feature analysis
• Oxide levels are much lower
• Interferences less of a problem
• Expensive !

23
Connecting an LC to an ICP-MS
24
Agilent GC-ICP-MS Interface
GC-ICP-MS System used ICP-MS Agilent 7500 GC
Agilent 6890 Interface Agilent G3158A
Fully heated and insulated GC transfer
line Modified torch with heated injector replaces
standard demountable torch. Silicosteel
transfer line and injector liner for inertness GC
capillary can be inserted to tip of injector or
terminated in GC oven GC effluent injected
directly into base of plasma essential for high
boiling point compounds Species decomposed to
atoms - atoms then ionized and passed into MS
25
Key Benefits of ICP-MS

• Wide Elemental Coverage
• Almost every element can be measured
• Very low detection limits ng/L or sub ng/L
• Equivalent to or lower than GFAAS (single-element
  technique)
• Simple Mass spectra
• Only small number of peaks for each element
• Very wide dynamic range
• Agilent systems provide 9 orders range from
  lt0.5ppt to gt500ppm
• High sample throughput
• Multi-element analysis in 3 to 4 minutes
• Relatively few interferences
• Systems optimised to give minimal spectral
  interferences low oxide (measured by CeO/Ce
  ratio) and matrix interferences. Matrix-derived
  spectral interferences can be removed by
  collision/reaction cell

26
Semiquantitative analysis

• Simple process
• spike sample with single internal standard
• acquire data
• software automatically corrects for
• mass bias (mass response)
• natural isotopic abundance
• ionisation potential
• print out data

27
Example Semiquantitative Analysis IEAE Soil - 7
standard
Values marked with an asterix are not fully
certified and for information only
28
Typical Application Areas for ICP-MS

• Pharmaceutical
• Routine heavy metal contamination
• Drug discovery
• Clinical trials
• HPI
• RD
• QA/QC
• Semiconductor
• Process Chemicals
• Contaminants in Si Wafers
• Photoresists Strippers
• Nuclear
• Fuel production
• Measurement of Radioisotopes
• Primary Cooling Water

Geological Soil, Rocks, Sediments Hydrology Isotop
e Ratio Studies Laser Sampling Archaeological Arti
fact analysis, proof of origin Tooth, bone, tusk,
shell, coral analysis Forensics Gun Shot
Residue Materials Characterization Point of
Origin Poisoning

• Environmental
• Drinking Water, Ambient Water, Sea Water
• Soils, Sludges, Solid Waste
• Plant material/agriculture
• Speciation of Hg, As, Pb, and Sn
• Clinical
• Blood, Urine, Serum
• Hair, Tissues
• Toxicology
• Nutrition/deficiency/vitamins
• Food Analysis
• Nutrition
• Toxic element and species monitoring
• QA/QC

29
Metals Analysis can be Performed by 4 Different
Techniques...

• FAAS (Flame Atomic Absorption Spectroscopy)
• Good, cost effective tool for users that do not
  require low detection limits and typically only
  analyze 1 to 5 elements
• Low cost, cheap, ppm measurements
• GFAAS (Graphite Furnace Atomic Absorption
  Spectroscopy)
• Well documented but expensive analysis for users
  that require detection limits at the 50ppt level
  for only 1 to 5 elements
• high cost, low productivity sub ppb measurements
  on a limited number of elements
• high operating cost - consumables (graphite
  tubes) and operator time
• ICP-OES (Inductively Coupled Plasma Optical
  Emission Spectroscopy)
• Good multielement technique for customers that
  require measurements at the ppb level only
• Cost effective multi element analysis at ppb
  levels
• Also known as ICP-AES (Inductively Coupled Plasma
  Atomic Emission Spectroscopy)
• ICP-MS (Inductively Coupled Plasma Mass
  Spectrometry)
• Excellent technique for customers that require to
  measure samples over a wide dynamic range and
  that require low detection limits - can replace
  both GFAA AND ICPOES
• Cost effective, fast multielement analysis from
  low detection limits to high concentrations
  good flexibility

Market in decline
Market in decline
Market flat
Market is growing
30
Graphite Furnace Atomic Absorption Spectroscopy
(GFAAS)

• Disadvantages
• very very slow sample throughput
• poor linear dynamic range (3 orders)
• short term precision not as good as alternatives
• very susceptible to chemical interferences
• strong reliance on background correction hardware
• slow method development
• poor element flexibility
• high running costs

• Advantages
• good detection limits for some elements - e.g. Cr
  in whole blood
• well documented methods
• good tolerance to dissolved solids
• unattended operation

31
ICP-OES - Simultaneous

• Disadvantages
• relatively poor detection limits
• many spectral interferences
• sample consumption high (1 to 5 mL/min)
• element flexibility
• limited in older systems
• speed of analysis compromised in newer systems

• Advantages
• multielement, fast
• flexible element selection
• well documented methods
• very good tolerance to dissolved solids
• good linear dynamic range

32
ICP-MS

• Disadvantages
• dissolved solids/matrix effects - need to dilute
  samples more than other techniques
• capital cost high
• requires knowledgeable operator

• Advantages
• excellent detection limits for most elements
• most elements in Periodic Table available
• good sample throughput
• wide dynamic range (8 to 9 orders)
• much simpler spectra than optical techniques
• low sample volume consumption
• mass spec - so isotopic information available
• flexible quantitation methods
• "semiquantitative"
• external calibrations
• isotope ratios

Due to the wide elemental coverage of ICP-MS or
certain applications e.g. enviro - GFAAS,
ICP-OES and single element detectors have been
replaced by a single 7500!
33
Price/Performance How does ICP-MS Compare With
Other Inorganic Techniques ?
200
Inductively Coupled Plasma Mass Spectrometry
(Quadrupole) Typically 1ppt to 100ppm
150
Typical price range USk
Inductively Coupled Plasma Optical Emission
Spectroscopy Typically 1ppb to gt1000ppm
(Simultaneous)
100
Graphite Furnace Atomic Absorption Typically
10ppt to 100ppb
50
Flame Atomic Absorption Typically 50ppb to 500ppm
1ppb
1000ppm
10ppb
100ppb
1ppm
100ppm
10ppm
100ppt
10ppt
1ppt
Typical measurement range
34
Agilent 7500 Series ICPMS Features

• 1. Unmatched Interference Removal with ORS in He
  ModeSpectral comparison showing removal of ALL
  polyatomic interferences in a complex sample
  matrix only the Agilent ORS can do this, using
  He collision mode. No other ICP-MS can use He
  collision mode requires the focusing power of
  an octopole (applies to 7500ce, 7500cs)
• 2. Detector Dynamic Range
• 9 orders detector range, gives 10x more
  concentration range available all any other
  competitors (applies to all 7500 Series)
• 3. Widest Analytical Measurement Range
• Measurement of lt10ppt Hg and gt1000ppm Na no
  other ICP-MS can do EITHER of these applications
  the 7500ce can do both IN THE SAME RUN (applies
  to 7500ce)
• 4. Lowest Metal Oxides of any ICP-MS
• CeO less than 0.1 - possible due to He
  collision mode removing CeO no other ICP-MS can
  do this (applies to 7500ce, 7500cs)

35
Summary

• Our product line up is perfectly aligned with the
  needs of the market, and is perfectly positioned
  to beat our competition
• Price/performance
• Upgradeability
• Ease of use
• Best design and build quality
• Range of peripherals
• Speciation market is growing fast
• we are the only ICP-MS vendor with expertise in
  LC-ICP-MS and GC-ICP-MS
• all the key speciation labs and opinion leaders
  use Agilent ICP-MS
• We have the best hardware and applications
  support because we have the best people!