nuevo icp-qms 7900 de agilent technologies · single ppt to 10’s ppb range inorganic analysis...
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Nuevo ICP-QMS 7900 de Agilent Technologies. Redefiniendo los límites de la técnica.
Rubén García
Especialista de Producto, Agilent
Technologies
Agenda ICP-MS Presentation
• Basic of ICP-MS
• High Matrix Interface
• Interference Removal with Collission Mode
• The New Agilent 7900 ICP-MS
What is ICP-MS?
Inductively Coupled Plasma Mass Spectrometry
Elemental analysis with:
• Wide elemental coverage (up to 75 elements)
• Very low detection limits (sub ppt level)
• Fast analysis times (all elements at once)
• Wide analytical working range (up to 11 orders)
- Simple spectra
• High matrix tolerance
• Isotopic information
7700x Detection Limits in Standard mode
Li Be B C
Na Mg Al Si P S Cl
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi
Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Th U
10 – 100 ppt
0.1-1 ppb
1-10 ppb
< 0.1ppt
0.1 – 1 ppt
1 – 10 ppt
26 Years of Agilent ICP-MS Innovation
1987 2000 2009 1994
First computer-controlled ICP-MS
PMS 100
4500 Series
7500 Series
7700 Series
Pioneering
ICP-MS
technology
Enabling routine
robust ICP-MS
analysis
Setting new levels
to ICP-MS
Performance
World's first benchtop system. Hyperbolic profile quad, motorized torch XYZ, cool plasma
Bringing ease of use
and reliability in ICP-
MS
9 orders detector range Octopole Reaction System
HMI, ISIS-DS, 3rd Generation ORS MassHunter SW #1 selling ICP-MS
A new era in ICP-MS
analysis
8800 ICP-QQQ
World’s first ICP-QQQ for unparalleled interference removal and sensitivity
2012
7700 had:
Better matrix tolerance than any other ICP-MS
• More robust plasma (lower CeO/Ce ratio) than any other system under standard tuning conditions , plus HMI for routine analysis of % level dissolved solids
Best interference removal with Helium cell gas – eliminates need for reaction gases in all common applications
• 7700 ORS3 improvements - removes all polyatomics in He mode, giving accurate results in complex or variable sample types – impossible on ICP-MS systems that use reactive cell gases or mixtures
Wider dynamic range than any other quadrupole ICP-MS
• Full 9 orders dynamic range at the detector – linear to 500ppm without changing conditions or hardware
Why Introduce another new ICP-MS? Building on the success of the Agilent 7700 Series:
The Agilent HMI for Aerosol Dilution
Argon
Dilution Gas
The flow of fine aerosol from the
spray chamber is diluted with argon
before delivery to the torch.
The HMI allows manual or auto
setup of robust plasma
conditions for matrix tolerance.
Automatic Setup of Plasma Conditions
• Requires sophisticated software algorithm to map plasma conditions, and
hardware to allow conditions to be replicated.
• US Patent 7,671,329 B2
The Agilent HMI for Ease-of-Use
• And it is very easy to set up!
Lowest Oxide AND Double-Charged Ratios
Figure-of-Merit Agilent Agilent
HMI BrandX
Oxide ratio % CeO+/Ce+ < 1.2* 0.2 - 1.0 < 2.5
Double-Charged ratio
% Ce2+/Ce+ < 2* < 2 < 3
No other ICP-MS can achieve these
low Oxide AND double-charged ratios
HMI
* Demonstrated at Installation
45Sc 52Cr 56Fe 63Cu 66Zn 111Cd 115In 136Ba
100
50
0
% Recovery of a 10ppb mixed standard spiked into undiluted NASS-5 Seawater
0.2% CeO+/Ce+ 1 % CeO+/Ce+ 2 % CeO+/Ce+
Greater Matrix Tolerance = Lower Oxides
Interferences in Complex Matrices
Some manufacturers claim that ICP-MS
has only a few interferences, and that
reaction gases can be used to remove
them.
That’s true in a simple sample, but in a
complex sample there are many
interferences, and no reaction gas can
remove all of them
But He mode on the Agilent ICP-MS
can!!
Isotope Principal Interfering Species (mixed matrix)45Sc 13C16O2,
12C16O2H, 44CaH, 32S12CH,
32S13C, 33S12C47Ti 31P16O, 46CaH, 35Cl12C, 32S14NH, 33S14N49Ti 31P18O, 48CaH, 35Cl14N, 37Cl12C, 32S16OH, 33S16O50Ti 34S16O, 32S18O, 35Cl14NH, 37Cl12CH51V 35Cl16O, 37Cl14N, 34S16OH52Cr 36Ar16O, 40Ar12C, 35Cl16OH, 37Cl14NH, 34S18O53Cr 36Ar16OH, 40Ar13C, 37Cl16O, 35Cl18O, 40Ar12CH54Fe 40Ar14N, 40Ca14N, 23Na31P55Mn 37Cl18O, 23Na32S, 23Na31PH56Fe 40Ar16O, 40Ca16O57Fe 40Ar16OH, 40Ca16OH58Ni 40Ar18O, 40Ca18O, 23Na35Cl59Co 40Ar18OH, 43Ca16O, 23Na35ClH60Ni 44Ca16O, 23Na37Cl61Ni 44Ca16OH, 38Ar23Na, 23Na37ClH63Cu 40Ar23Na, 12C16O35Cl, 12C14N37Cl, 31P32S, 31P16O2
64Zn 32S16O2, 32S2,
36Ar12C16O, 38Ar12C14N, 48Ca16O
65Cu 32S16O2H, 32S2H, 14N16O35Cl, 48Ca16OH66Zn 34S16O2,
32S34S, 33S2, 48Ca18O
67Zn 32S34SH, 33S2H, 48Ca18OH, 14N16O37Cl, 16O235Cl
68Zn 32S18O2, 34S2
69Ga 32S18O2H, 34S2H, 16O237Cl
70Zn 34S18O2, 35Cl2
71Ga 34S18O2H, 35Cl2H, 40Ar31P72Ge 40Ar32S, 35Cl37Cl, 40Ar16O2
73Ge 40Ar32SH, 40Ar33S, 35Cl37ClH, 40Ar16O2H74Ge 40Ar34S, 37Cl275As 40Ar34SH, 40Ar 35Cl, 40Ca 35Cl, 37Cl2H77Se 40Ar 37Cl, 40Ca 37Cl78Se 40Ar 38Ar80Se 40Ar2,
40Ca2, 40Ar40Ca, 32S2
16O, 32S16O3
Low flow sample
introduction system
High temperature 27MHz
plasma generator
Multi-element interference removal by
on-axis octopole reaction cell
High frequency hyperbolic
quadrupole
Fast simultaneous dual
mode detector
(9 orders dyn. range)
Agilent ICP-MS System with Collision Reaction Cell (CRC)
Helium interactions in an Octopole Reaction Cell Collision: Energy discrimination
He
Collision
Ar
Cl
Ar
Cl
As
As
Electrical potential (Octopole)
Reaction cell
Electrical potential (Q-pole)
Molecular interference(ArCl) has larger cross
section than the analyte (As).
More frequent interactions with He.
A significant reduction in kinetic energy relative to
the analyte (As). Energy filtering can be used to
ensure only the analyte
enters the quadrupole analyzer.
2E5
cps
45 50 55 60 65 70 75 80 Mass
Blank Acid Matrices and IPA in No Gas Mode
No Gas Mode
Unspiked 5% HNO3 + 5% HCl + 1% H2SO4 + 1% IPA Matrix
Unspiked Matrix – ALL peaks are due to polyatomic interferences
Multiple polyatomic interferences affect almost every
mass – Interferences are matrix-dependent
45 50 55 60 65 70 75 80 Mass
2E5
cps
He Mode
ALL polyatomic interferences are removed
in He Mode
Unspiked 5% HNO3 + 5% HCl + 1% H2SO4 + 1% IPA Matrix
ALL polyatomic interferences are removed in He Mode (same cell conditions)
Blank Acid Matrices and IPA in He Mode
Color of spectrum indicates which matrix gave each interfering peak
2E5
cps
45 50 55 60 65 70 75 80 Mass
10ppb Spike in 5% HNO3 + 5% HCl + 1% H2SO4 + 1% IPA Matrix
Consistent high sensitivity for all isotopes of all elements in He Mode
Matrix Mix with Spike (10ppb) in He Mode
He Mode
Good signal for all spike
elements at 10ppb Spike.
Perfect template fit for all
elements – no residual
interferences and no loss of
analyte signal by reaction
Consistent sensitivity and perfect template match for all elements
9 Orders Dynamic Range Detector
Genuine 9 orders dynamic range so major elements at 100’s ppm can be measured in the same run as trace elements at ppt, without operator having to change conditions or hardware configuration.
Calibration shows Na in 1:10 and 1:5 diluted seawater – top point is 2360ppm
ICP-OES
Multi-element, ~2 min/ sample
10’s ppb to 1000’s ppm
Few Elements/Samples
ppt
ICP-MS – for trace elements and clean samples
Multi-element, ~4min/ sample
Single ppt to 10’s ppm
GFAAS
Single element, ~6min/ sample
10’s ppt to 100’s ppb
Many Elements/Samples
%
ppm
ppb Hydride/AFS
Few elements, ~2min/ sample
Single ppt to 10’s ppb
Range
Inorganic Analysis Techniques in a Typical Laboratory
7700 ICP-MS
Multi-element
Single cell gas mode and productivity tools reduce run time
HMI for samples with up to 2% dissolved solids
Single ppt (incl. hydride and Hg) to 100’s ppm (1000’s ppm
with HMI)
The Power of 10!
What if the world’s best quadrupole ICP-MS gets 10 times better?
The new Agilent 7900 opens up a new dimension
in ICP-MS capability.
7700 Series ICP-MS
How to Improve on the Best ICP-MS?
How about NEW
detector technology for
unprecedented
11 orders measurement
range and Fast TRA
Acquisition at 0.1msec
dwell time.?
How about a NEW Interface &
Ion Lens for up to 15x Signal
to Noise improvement?
How about a NEW ORS4
for ultra fast gas switching
in less than 3 seconds?
25% NaCl Brine Solutions Without Dilutions?
How about a NEW Ultra HMI for analysis of up to
25% NaCl brine solutions without dilutions?
11 Orders?
Higher sensitivity & lower background than 7700x Comparison to 7700x actual performance
Plasma mode
Sensitivity (7900/7700x)
7Li 89Y 205Tl
No Gas
Normal x1.2 x1.9 x1.9
Low Matrix x1.0 x1.6 x1.6
General Purpose x1.0 x1.5 x1.8
HMI-high x1.3 x1.6 x1.8
Model Sensitivity [kcps/ppb] Off Mass Bkgnd [cps] S/N [x1E3]
7Li 89Y 205Tl 7amu 89amu 205amu 7Li 89Y 205Tl
7700x 100 320 320 0.7 1.5 5.4 140 210 60
7900 120 620 600 0.2 0.2 1.2 600 3100 500
7900/7700x 1.2 1.9 1.9 0.28 0.13 0.22 4 15 8
~2x higher sensitivity at mid- and high-mass
>3x to 5x lower background
Average ~10x better signal to noise (S/N)
Agilent 7900 Capable of Very High Sensitivity Tuned like competitor’s ICP-MS – CeO/Ce <2.5%
Calibration
Level Conc. Calc Conc. CPS Det. RSD
1 0 0 1 P 86.6
2 10 9.89 13676 P 0.6
3 50 49.984 69112 P 0.9
4 100 100.019 138295 P 0.4
Uranium calibration in No
Gas mode:
Ultra-high sensitivity
1.38 GHz/ppm
Ultra-low background:
MDL: 1.3ppq; BEC: 0.48ppq;
NEW 7900 Ultra High Matrix Introduction (UHMI)
• Increased dilution range to x100 – even higher matrix capability
• Less matrix loading to interface, so better long-term stability
• Maintain high carrier gas flow through spray chamber,
so faster gas replacement and washout
7700 HMI 7900 UHMI
HMI-4 (HMI-L) 0.6 L/min 0.8 L/min
HMI-8 (HMI-M) 0.35 0.68
HMI-25 (HMI-H) 0.23 0.5
HMI-50 N.A. 0.4
HMI-100 N.A. 0.33
UHMI
Dilution
Port
Matrix Tolerance Vastly Superior to Any Other ICP-MS - Analysis of Brine (25% NaCl) with UHMI (HMI-50)
• Better DL than OES
• No maintenance required for cones after 8 hours continuous introduction.
50
60
70
80
90
100
110
120
130
140
150
25%
NaC
l + 1
00p
pb
25%
NaC
l + 1
00p
pb
25%
NaC
l + 1
00p
pb
25%
NaC
l + 1
00p
pb
25%
NaC
l + 1
00p
pb
25%
NaC
l + 1
00p
pb
25%
NaC
l + 1
00p
pb
25%
NaC
l + 1
00p
pb
25%
NaC
l + 1
00p
pb
25%
NaC
l + 1
00p
pb
25%
NaC
l + 1
00p
pb
25%
NaC
l + 1
00p
pb
25%
NaC
l + 1
00p
pb
25%
NaC
l + 1
00p
pb
25%
NaC
l + 1
00p
pb
9 Be [ no ]27 Al [ no ]51 V [ no ]51 V [ He ]52 Cr [ no ]52 Cr [ He ]55 Mn [ no ]55 Mn [ He ]56 Fe [ He ]59 Co [ no ]59 Co [ He ]60 Ni [ no ]60 Ni [ He ]63 Cu [ He ]66 Zn [ no ]66 Zn [ He ]68 Zn [ no ]68 Zn [ He ]75 As [ He ]78 Se [ He ]107 Ag [ no ]107 Ag [ He ]111 Cd [ no ]111 Cd [ He ]205 Tl [ no ]205 Tl [ He ]208 Pb [ no ]208 Pb [ He ]238 U [ no ]238 U [ He ]
4 hrs Quant Recovery
(25% NaCl matrix + 100µg/L spike)
OES
DL
(μg/L)
7900
DL
(μg/L)
Ag 0.7 0.07
Al 0.5 0.6
Be 0.07 0.03
Cd 0.4 0.16
Co 1 0.04
Cr 1 0.05
Fe 1.7 0.33
Mn 0.2 0.12
Ni 2.5 0.12
Pb 6 0.73
Se 10 1.2
Tl 9 0.22
V 1 0.09
Zn 0.5 0.39
7700: H2: 6.0 0 mL/min
10 sec.
7900: H2: 6.0 0 mL/min
2 sec.
Fast Cell Gas Switching – ORS4
NEW 7900 Orthogonal Detector System Improved dynamic range
Extended upper limit of detector range
Analog range increased from 3 Gcps 10 Gcps
Up to 11 orders dynamic range - ~0.1 cps to 10 Gcps
Far Wider Measurement Range Than Any Other ICP-MS 11 orders - low and high level calibrations in a single run
Cd (1ppt - 1ppb) and Na (100ppb - 10,000ppm (1%)) in the same run
Concentration range (11 orders)
and upper measurement limit
(>1%) are at least 10x better
than any other ICP-MS
Both calibrations are linear.
Total concentration range
covered from Cd blank (BEC
of <0.1ppt) to is 11 orders
Na
1%
Cd
BEC: <0.1ppt
Faster TRA mode for Transient Signal Analysis Minimum dwell time is shortened from 3 msec. on the 7700 Series
to 0.1 msec to allow faster sampling of transient signals.
0.1 msec This enables the
measurement of the
single NP peak signal
arriving on the detector.
30 nm Au Nanoparticle
New Integrated Sample Introduction System (ISIS 3) Fully compliant multi-mode EPA 6020 analysis* in <1 minute
7 port valve (incl.
online
ISTD port)
Piston
pump
3-way
valve
New features in ISIS 3
• Close-coupled valve – very short tube length so minimal stabilization/rinse delay
• Piston pump for faster sample uptake
• 3-way valve to switch between on-line ISTD or tune solution
• ISIS is now compatible with Startup auto-optimization functions and full autotune
* EPA 6020 includes 23 analytes, plus 8 recommended ISTDs, so up to ~30 analytes (2 gas modes gives optimum data in terms of sensitivity and interference removal)
New Integrated Sample Introduction System (ISIS 3)
Increase sample throughput: 30% faster
26+ elements analysis in soils, etc. (e.g. EPA 6020):
• 7700+ISIS 2: ~75 sec.
• 7900+ISIS 3: <60 sec.
MassHunter 4.1: Simpler and More Powerful Software Dashboard with Gadgets replaces old mixed UI concept
Instrument status monitor (right) can be
displayed on top of DA window, to show status
and access top level functions without the need
to open entire Top Level Application.
• Gadget icons are “live”; change appearance
depending on current status
• Also have short pull-down menus for quick
access to most common functions
Software so Powerful it Can Write Your Methods! A new era in simple method setup and ease of use
Method Wizard – Develops a complete method in three steps!
1. Select pre-set method template and choose matrix level
2. Confirm analytes and internal standards…
Software so Powerful it Can Write Your Methods! A new era in simple method setup and ease of use
Method Wizard – Develops a complete method in three steps!
3. Choose whether to optimize method for speed or DLs
…and click “Optimize”
Select “Speed” or “Low DL”
The new batch is ready to run It can be edited or save as a template for future use
unit DL BEC
Speed Low DL Speed Low DL
Be ppt 2.7 0.3 0.5 0.2
V ppt 1.4 0.0 0.3 0.0
Cr ppt 4.2 1.7 27.8 22.8
Co ppt 1.4 0.4 5.3 5.5
Cu ppt 3.7 2.2 9.3 8.8
As ppt 7.2 0.8 1.4 0.6
Mo ppt 0.8 0.3 0.7 0.4
Ag ppt 1.3 0.7 6.8 5.8
Cd ppt 0.0 0.0 0.0 0.1
Sb ppt 0.2 0.1 0.3 0.2
Ba ppt 7.4 1.8 21.7 17.6
Pb ppt 1.9 0.5 3.6 3.0
U ppt 0.0 0.0 0.0 0.0
Acquisition time
Speed: 2.4min
Low DL: 5.7 min
Remote Monitor App (iOS and Android devices) View instrument status and perform basic system control
An Industry First!
Improving Installation & Familiarization Installation
• Intuitive Installation Checkout
• Site Prep tool for Software Installation
Familiarization tools
• Familiarization Tutorials
- Familiarization Guide
- Familiarization Video
- Familiarization Slide Set
Plus:
Remote Advisor Now available
for ICP-MS!
ICP-OES
Multi-element, ~2 min/ sample
10’s ppb to 1000’s ppm
Few Elements/Samples
ppt
ICP-MS – for trace elements and clean samples
Multi-element, ~4min/ sample
Single ppt to 10’s ppm
GFAAS
Single element, ~6min/ sample
10’s ppt to 100’s ppb
Many Elements/Samples
%
ppm
ppb Hydride/AFS
Few elements, ~2min/ sample
Single ppt to 10’s ppb
Range
Inorganic Analysis Techniques in a Typical Laboratory
7700 ICP-MS
Multi-element
Single cell gas mode and productivity tools reduce run time
HMI for samples with up to 2% dissolved solids
Single ppt (incl. hydride and Hg) to 100’s ppm (1000’s ppm
with HMI)
Agilent 7900 Multi-element
Faster analysis with ISIS3 and fast cell gas switching
UHMI for samples with up to 25% dissolved solids
Single ppt (incl. hydride and Hg) to 10,000’s ppm with new 11
orders concentration range detector
Eliminates the need for additional techniques for high-matrix
levels and high concentration/major elements
Raise Your Expectations A New Dimension in Quadrupole ICP-MS
Making the world’s best selling ICP-MS ten
times better
• 10x Higher Matrix Tolerance (25%TDS)
• 10x Wider Dynamic Range (11 orders)
• 10X Better Signal-to-Noise
• Plus SW so powerful it can write methods
for you
ICP-MS Redefined. Again.
10x