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Agilent 7500 Series ICP-MS An Introduction. Presented By: Ferdi Ferdian Kusnadhi. 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...)

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slide1

Agilent 7500 Series ICP-MS

An Introduction

Presented By:

Ferdi Ferdian Kusnadhi

what is icp ms
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

What is ICP-MS?

An inorganic (elemental) analysis technique

ICP-MS has the detection limits of GFAA and the sample throughput of ICP-OES

agilent 7500ce icp ms system with collision reaction cell crc
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

Plasma

Octopole

Off-axis Lens

High frequency hyperbolic quadrupole

Low flow sample introduction system

agilent 7500 series icp ms
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, R&D.
    • Ultra low BECs at high plasma power
    • Cool plasma also available
different ways of acquiring information from a sample

Different ways of acquiring information from a sample

Qualitative scan

Semiquantitative Analysis

Fully quantitative data

primary agilent icp ms team in asia pacific
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

factory trained agilent icp ms service engineers ap region only excluded jpn
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

application notes of interest to the semiconductor market
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
agilent icp ms in asia pacific big growth big rewards
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!
what is

M  M+

M  M-

M+

M+

M+

M+

M+

M+

M+

M+

M+

M+

M+

M+

What is ….

A Mass Spectrometer

DETECTOR

MASS FILTER

ION SOURCE

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)

what else can be measured using ms
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

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

Advantages of ICP-MS
slide13

Hg

As

Se

Na

1180 ppm Sodium

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!

elemental coverage of icp ms
Elemental Coverage of ICP-MS

Almost every element can be measured by ICP-MS (including actinides), mostly at extremely low limits of detection

the majority of elements have ppt and below detection limits
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
overview of inorganic analysis techniques
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.

SequentialSimultaneous

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

overview of inorganic analysis techniques1
Overview of Inorganic Analysis Techniques

SequentialSimultaneous

Criteria1 FAAS GFAAS ICP-OES ICP-OES ICP-MS

Detection Limits +10ppb +50 ppt 1 ppb <1 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)

who uses agilent icp ms ww
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
comparison of metals techniques speed vs detection power
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

agilent 7500 3 sigma detection limits

<0.1 ppt

1 - 10 ppt

>10 ppt

Agilent 7500 - 3 Sigma Detection Limits

Standard pneumatic nebuliser

3 sec/mass integration time

* Class 1000 cleanroom with ShieldTorch

0.1 - 1ppt

extending the capabilities of icp ms
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
laser ablation icp ms

Agilent 7500 ICP-MS

Merchantek UP 213 Laser Ablation system

Laser

Ar Gas with ablated material

Sample

Laser Ablation ICP-MS
  • Pulsed Nd:YAG 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 !
agilent gc icp ms interface
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

key benefits of icp ms
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 <0.5ppt to >500ppm
  • 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
semiquantitative analysis
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
example semiquantitative analysis ieae soil 7 standard
Example Semiquantitative Analysis IEAE Soil - 7 standard

Values marked with an asterix * are not fully certified and for information only

typical application areas for icp ms
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

Pharmaceutical

Routine heavy metal contamination

Drug discovery

Clinical trials

HPI

R&D

QA/QC

Semiconductor

Process Chemicals

Contaminants in Si Wafers

Photoresists & Strippers

Nuclear

Fuel production

Measurement of Radioisotopes

Primary Cooling Water

Typical Application Areas for ICP-MS
  • Geological
  • Soil, Rocks, Sediments
  • Hydrology
  • Isotope Ratio Studies
  • Laser Sampling
  • Archaeological
  • Artifact analysis, proof of origin
  • Tooth, bone, tusk, shell, coral analysis
  • Forensics
  • Gun Shot Residue
  • Materials Characterization
  • Point of Origin
  • Poisoning
metals analysis can be performed by 4 different techniques
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

graphite furnace atomic absorption spectroscopy gfaas
Advantages

good detection limits for some elements - e.g. Cr in whole blood

well documented methods

good tolerance to dissolved solids

unattended operation

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

Graphite Furnace Atomic Absorption Spectroscopy (GFAAS)
icp oes simultaneous
Advantages

multielement, fast

flexible element selection

well documented methods

very good tolerance to dissolved solids

good linear dynamic range

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

ICP-OES - Simultaneous
icp ms
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

Disadvantages

dissolved solids/matrix effects - need to dilute samples more than other techniques

capital cost high

requires knowledgeable operator

ICP-MS

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!

price performance how does icp ms compare with other inorganic techniques
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 US$k

Inductively Coupled Plasma Optical Emission Spectroscopy

Typically 1ppb to >1000ppm (Simultaneous)

100

Graphite Furnace Atomic Absorption Typically 10ppt to 100ppb

50

Flame Atomic Absorption

Typically 50ppb to 500ppm

1ppt

10ppt

100ppt

1ppb

10ppb

100ppb

1ppm

10ppm

100ppm

1000ppm

Typical measurement range

agilent 7500 series icpms features
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 <10ppt Hg and >1000ppm 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)
summary
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!