An Agilent Technologies’
Presentation at VinaLab 2013
22 March 2013
VinaLab 2013 1
Innovative
Breakthroughs in
Atomic Spectrochemical
Analysis
Contents
1. Introduction
2. Breakthrough #1
Running on Air - Myth or Reality?
3. Breakthrough #2
World’s First Functional ICP-QQQ
featuring Tandem MS/MS
Technology
4. Conclusions
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Introduction Plasma Spectrochemical Analysis
• Chemical analysis of a mixture of
substances or a complex of substance
by a study of spectra (plasma based
atomic spectroscopy)
• Ions (atomic) generated can be
extracted and quantified using a
suitable mass spectrometer (plasma
based mass spectrometry)
• With properly prepared reference
standards, allows for accurate
quantitation from ultratrace to % levels
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Ref: http://www.merriam-webster.com/dictionary/spectrochemical%20analysis, viewed 21 May 2012.
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Agilent Atomic Spectroscopy Portfolio
(from Jan 2012 onwards…)
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AAS
7700 Series
ICP-MS
Instrument Price
P
erf
orm
an
ce
700 Series
ICP-OES
4100 MP-AES
Agilent 8800
ICP-QQQ
• Academic
• Difficult samples in
Semicon.
Life Science
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Ground State Excited State Relaxation
Sample
Microwave excited Plasma
Monochromator
& Detector
Quantitation
Atom Formation
EXCITATION
Emission
Microwave Plasma-Based Spectrochemical Analysis Fundamentals
Analysis is based upon Well-Proven Atomic
Emission Spectroscochemical Principles!
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Agilent 4100 Microwave Plasma-Atomic Emission
Spectrometer (MP-AES)
New technique for elemental determination using atomic emission
• Microwave excited plasma source
• Nitrogen based plasma - runs on air (using a N2 generator)
Improved performance compared with flame AA:
• Higher sample throughput with fast sequential measurement
– More than 2x faster than conventional flame AA
• Superior detection limits and improved dynamic range
Easy to use: • New generation software featuring automated
optimization and software applets that load a preset method
• One piece torch with easy torch removal and replacement – no alignment
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Agilent 4100 Microwave Plasma-Atomic Emission
Spectrometer (MP-AES)
Reduced operating costs: • Runs on air – eliminates need for
Acetylene, Argon, etc.
• Eliminates need for source/hollow
cathode lamps
• Simple installation – no chiller, 10 A
supply
Improved Safety: • Eliminates need for flammable gases and
cylinder handling
• Safe, reliable unattended multi-element
overnight operation
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Accessory Options for the 4100 MP-AES
• Automate and simplify analysis with the SPS-3 Autosampler (for unattended overnight operation)
Page 9
• To enable low ppb level detection of As, Se or
Hg, use the Multimode Sample Introduction
System (MSIS). Can be used to analyse hydride
and non-hydride forming elements at the same
run!
• For organic applications, the External Gas
Control Module (EGCM) bleeds air into the
plasma minimizing Carbon build-up and reducing
background
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Page 10
IDL’s in ppb, clean water samples
**3 sigma IDLs using a 10 second integration time with dewar nitrogen
*30 second integration time used for these elements
Performance Comparison Typical Instrument Detection Limits**
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Application Notes Available
(downloadable from the Agilent website)
Page 11
Geochemical
• New methodology for analysis of gold and precious metals
• Analysis of base metals in geochemical samples
Chemical & Petrochemical
• Analysis of wear metals and contaminants in engine oils
• Analysis of lubricating oil additives
• Analysis of trace elements in petroleum and diesel fuels
Food & Agriculture
• Analysis of soil extracts
• Cost-effective analysis of major, minor, and trace elements in foodstuffs
Environmental
• Determination of metals in industrial wastewaters
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Cost savings based on reductions in gas expenses ONLY!.
Assumes measuring 9 elements (4 nitrous-oxide elements) in batches of 100 samples,
3 days/week using the N2 generator. For a detailed cost comparison, consult your local Agilent representative
Reduced Cost of Ownership
Page 12 LabVietnam 2012
The Agilent 4100 MP-AES
Key Features
o Runs on air – the most significant advance in Atomic Spectroscopy
o Lowest running cost of any atomic spectroscopy technique due to capability to run on air – ideal for remote and at site operation
o Improved safety – capability to run on air means no flammable gases and no manual handling of cylinders
o Easy-to-use software with MP applets and plug and play torch which simplify operation and maximize uptime
o Superior performance to flame AA, with capability to run unattended overnight
o An even greener technology, displacement of fuel gas (acetylene) reduces carbon footprint, aids CSR initiatives of many organisations (People, Planet, Profit)
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Breathrough #2
World’s First Functional ICP-QQQ featuring
Tandem MS/MS Technology
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Agilent 8800 ICP-QQQ
Agilent 7700
Single-Quad ICP-MS
Agilent 8800
ICP-QQQ
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World’s first Triple Quadrupole ICP-MS (ICP-QQQ)
New modes of operation and performance not possible with quadrupole ICP-MS
The highest performing quadrupole ICP-MS system
Unique capabilities, based on proven technology of world’s best selling ICP-MS
(7700)
8800 ICP-QQQ Key Product Hardware
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Low flow
sample
introduction
system
High matrix
introduction
(HMI)
technology
Fast, frequency-
matching 27MHz
RF generator Efficient twin-turbo
vacuum system
Dual conical Extraction and
Omega lens focuses ions
across the mass range
9 orders
dynamic range
electron
multiplier (EM)
detector
Analyzer quad Q2:
High frequency
hyperbolic quadrupole
– selects ions that
pass to detector
High-transmission,
matrix tolerant interface
First quad Q1: High frequency
hyperbolic quadrupole mass filter –
selects ions that enter the cell
3rd generation collision/
reaction cell (ORS3)
with 4 cell gas lines
Peltier-
cooled
spray
chamber
Robust, high-temperature
plasma ion source
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ICP-QQQ: How Does it Work?
ICP (plasma) and Interface:
Forms and extracts ions from
the sample (just like the 7700)
EM (detector): Measures the
ions that are scanned by Q2
(just like the 7700)
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Q1 – controls ions
that enter the cell
• Consistent reactions
even if sample
composition changes.
ORS3 – collision/
reaction gas added
• Ions react and are
neutralized or moved.
• Product ions are formed.
Q2 – selects the
target analyte mass
• Interference-free analyte
ions passed to EM
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Q1 – controls ions
that enter the cell
• Consistent reactions
even if sample
composition changes
ORS3 – collision/
reaction gas added
• Ions react and are
neutralized or moved
• Product ions are formed
Q2 – selects the
target analyte mass
• Interference-free analyte
ions passed to EM
ICP-QQQ: How Does it Work?
ICP (plasma) and Interface:
Forms and extracts ions from
the sample (just like the 7700)
EM (detector): Measures the
ions that are scanned by Q2
(just like the 7700)
Unique aspect of ICP-QQQ is Q1.
• Controls the ions that enter the cell
Reaction processes in the cell are
consistent and predictable, even if
sample composition is complex or
variable.
• Consistent cell conditions means
reaction mode method development
is easier than on single quad (same
method can be used for different
samples).
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Scan Type on ICP-QQQ
• Single Quad mode
• MS/MS mode
– On-Mass mode
– Mass-Shift mode
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Q2 cell Q1
Cell gas
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ICP-QQQ can function in Single-Quad Mode.
Q1 operates like an ion guide (just like single quad ICP-MS).
ICP-QQQ has typically 2x higher sensitivity and >5x lower background
than 7700, so DLs are better even in single-quad mode.
Single Quad Mode
Q2 (scanned) cell Q1 (ion guide)
Cell gas
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Parameters 7700x ICP-MS 8800 ICP-QQQ #100
Low mass (7Li) > 50 Mcps/ppm > 100 Mcps/ppm
Mid mass (89Y) > 160 Mcps/ppm > 350 Mcps/ppm
High mass (205Tl) > 80 Mcps/ppm > 200 Mcps/ppm
No Gas Background < 2 cps (m = 9) < 0.3 cps (m = 9)
Mass-Shift Measurement: Reactive analyte reacts with chosen cell
gas, is moved to a new product ion mass and can be separated from
unreactive interferences. No existing ions can overlap new analyte
product ion, as all non-target masses are rejected by Q1
With ICP-MS/MS, Q1 rejects all non-target masses, ensuring no existing
ions (analyte, matrix, or polyatomic) can overlap new analyte product ion
How Reaction Mode Works in ICP-MS/MS Mode
Original
interfering ion
On-mass
interference
Analyte
Off-mass
interference
Reaction
gas
Analyte
M+ MR+
Q2 set to analyte product
ion mass – rejects original
interfering ions
Analyte
product ion
Analyte reacts to
form product ion Q1 set to analyte
mass – rejects all
non-target masses
All non-target
masses
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• Q1 is set to precursor ion mass, controlling the ions that enter ORS.
• Q2 is set to mass of reaction product ion (Q1+16amu in O2 mode):
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Example: S with O2 Cell Gas
Q2 (Q1+16)
(scanned) cell Q1 (m/z= 32)
(scanned)
O2
32S+
48Ca+, 48Ti+
36Ar12C +
48SO+ 32S+ 48SO+
48Ca+, 48Ti+
36Ar12C +
Single-quad reaction cell ICP-MS can also do SO mass-
shift to move S (as SO+) away from the O2+ interference.
BUT single quad reaction cell ICP-MS cannot remove
the 48Ca/48Ti and 36Ar12C overlaps on 48SO+.
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8800 Abundance Sensitivity in Single-Quad Mode
- Trace 55Mn is overlapped by 56Fe in 1000ppm Fe
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Abundance Sensitivity (AS) is
the degree of peak “tailing” – the
contribution a peak makes to the
adjacent (-1 and +1amu) masses
7700 specification is 5 x 10-7 on the
low mass side
Note: log intensity scale 55Mn
56Fe
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QQQ Abundance Sensitivity is
the product of Q1 AS x Q2 AS,
so overlaps to adjacent peaks
are virtually eliminated.
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8800 Abundance Sensitivity in MS/MS Mode - 55Mn is free from overlap by 56Fe in 1000ppm Fe
55Mn
56Fe
8800 QQQ AS is almost too
good to measure (<10-10).
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Agilent 8800 ICP-QQQ – Key Features
• World’s first functional ICP-QQQ with Tandem MS/MS capability
• Outperforms single quadrupole ICP-MS for conventional applications
• Provides unique, high-performance MS/MS mode
• ICP-QQQ ensures control of ions that enter the cell; controlled reaction
processes deliver reliable results
• Offers ultimate flexibility for problem solving and advanced research
• Utilizes proven 7700 hardware and same MassHunter software platform
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Factory in Tokyo
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