The All New The All New Agilent 7700 g Series The Smallest, Most - - PowerPoint PPT Presentation
The All New The All New Agilent 7700 g Series The Smallest, Most Powerful ICP MS Ever Made Inductively Coupled Plasma Mass Spectrometry ICP MS is a fast, multi element, high sensitivity trace metals analysis technique Key applications
ICP‐MS is a fast, multi‐element, high sensitivity trace metals analysis technique Key applications are:
Consumer Goods
ICP‐MS market continues to grow as technology improves and GFAA and ICP‐OES instruments are replaced with ICP‐MS
Agilent 7500 Series Agilent 4500 Series
1987 – PMS 100 introduced – First computer‐controlled ICP‐MS p 1988 – PMS 200 introduced – Second generation ICP‐MS with off‐axis Qpole lens 1989 – 1st ETV accessory for semicon analysis by ICP‐MS 1990 – PMS 2000 introduced – Omega off‐axis lens. Lowest random background ICP‐MS 1992 – ShieldTorch interface developed ‐ Ar interferences virtually eliminated in cool plasma enabling ppt analysis of K Ca Fe by ICP MS plasma, enabling ppt analysis of K, Ca, Fe by ICP‐MS 1994 – 4500 Series introduced ‐ World's first benchtop system. Hyperbolic profile quad, motorized torch XYZ, cool plasma 1998 – First real time ICP‐MS chromatographic software – PlasmaChrom. T‐mode reaction interface introduced
Agilent 4500 Series ShieldTorch System Octopole Reaction
1999 – 4500 Series 100, 200 & 300 introduced: 1st applications‐specific ICP‐MS. 2000 – Agilent 7500 Series introduced ‐ 7500a, 7500i and 7500s ‐ the next generation in ICP‐MS instrumentation. 9 orders detector range 2001 – Agilent 7500c launched – 1st generation ORS for high matrix samples. 2002 – New digital generators and LAN control introduced First commercial GC‐ICP‐MS
Octopole Reaction System
2002 New digital generators and LAN control introduced. First commercial GC‐ICP‐MS interface. 2003 – Agilent 7500cs launched – 2nd generation ORS for high purity semicon samples. 2004 – Agilent 7500ce launched – 2nd generation ORS for high matrix samples. 2005 – Low flow cell gas MFC’s for Xe NH3, O2, etc added to 7500ce/cs.
Agilent 7500 Series
2006 – Agilent acquires 100% of Agilent/Yokogawa joint venture 2007 – Agilent 7500cx introduced: He only mode ICP‐MS 2008 – High Matrix Interface developed – enables 2% TDS samples to be run by ICP‐MS 2009 – Agilent 7700 Series introduced – replaces 7500 Series. MassHunter Software introduced ‐ common platform with other Agilent MS. ISIS‐DS Discrete sampling introduced common platform with other Agilent MS. ISIS DS Discrete sampling system, for ultra high throughput analysis
Agilent 7700 Series
Longer, narrower rods, higher cell pressure and frequency – MUCH better
performance in He mode
Fast tuning 27MHz generator, for better tolerance to changing matrix (incl.
High Matrix Introduction (HMI) standard on
7700x model
>30% smaller footprint than any other ICP‐MS
MassHunter software – intuitive and easy
to learn. Pre‐set plasma conditions and p fast lens auto‐tuning
7700x 7700s 7700x
pharmaceutical and general purpose
7700s
DIW h i l pharmaceutical and general purpose applications DIW, process chemicals
Off‐axis ion lens 3rd generation High matrix introduction (HMI) dilution gas inlet Off axis ion lens Cell gas inlet Fast, simultaneous dual mode detector (9 orders d i ) g Octopole Reaction System (ORS3) gas inlet Low‐flow Sample Introduction dynamic range) Peltier‐cooled spray chamber High‐frequency (3MHz) hyperbolic quadrupole p y High‐performance Fast, frequency‐ matching 27MHz RF generator vacuum system High‐transmission, matrix tolerant matrix tolerant interface
%
ICP‐OES – for majors and high matrix samples
Multi‐element, ~2 min/ sample 10’s ppb to 1000’s ppm
f l d l l ICP‐MS – for trace elements and clean samples
Multi‐element, ~4min/ sample Single ppt to 10’s ppm
ppm
GFAAS
Single element, ~6min/
ppb
Hydride/AFS
Few elements,
LOD
In many inorganic labs, several analytical techniques are used, to cover the range f l i d d i
6min/ sample 10’s ppt to 100’s ppb
pp
, ~2min/ sample Single ppt to 10’s ppb
limits required. This is encouraged by some vendors, who want to sell multiple instruments to each lab!
Few Elements/Samples ppt Many Elements/Samples Few Elements/Samples Many Elements/Samples
%
ICP‐OES
Multi‐element, ~2 min/ sample 10’ b t 1000’
f l d l l
7700 ICP-MS
Multi-element
10’s ppb to 1000’s ppm
ICP‐MS – for trace elements and clean samples
Multi‐element, ~4min/ sample Single ppt to 10’s ppm
ppm
Single cell gas mode and productivity tools reduce run time HMI for samples with % level solids Single ppt (incl. hydride and Hg) to 100’s ppm (1000’s ppm ith HMI) GFAAS
Single element, ~6min/
ppb
Hydride/AFS
Few elements,
LOD
with HMI)
Uniquely, the Agilent 7700 can
6min/ sample 10’s ppt to 100’s ppb
pp
, ~2min/ sample Single ppt to 10’s ppb
q y, g replace all these separate techniques, providing high throughput, matrix tolerance, wide elemental coverage Few Elements/Samples ppt Many Elements/Samples and low LODs in a single run Few Elements/Samples Many Elements/Samples
30% smaller footprint 30mm longer ion path
than any other system y y
7700 ORS3 improvements ‐ removes all 7700 ORS improvements removes all
polyatomics in He mode, giving accurate results in complex or variable sample types – impossible on ICP‐MS systems that use i ll i reactive cell gases or mixtures
Full 9 orders dynamic range at the detector
– linear to 500ppm without changing conditions or hardware
cooled spray chamber) p y )
cap – reduced risk of contamination cap – reduced risk of contamination
maintenance F f hi RF
generator
l d d plasma conditions and auto‐tuning Provides most robust plasma of any ICP‐MS under standard conditions
The new RF generator of The new RF generator of the 7700 operates using a unique computer controlled fast tuning design to instantly match design, to instantly match to changing load. This means that the 7700 can switch from pure water to volatile organics without disturbing the plasma
Hottest part of Sample channel is Residence time is a
ICP‐MS plasma must produce
plasma ~ 8000K By sample cone, analytes present as M+ ions p at ~6700K few milliseconds
ICP MS plasma must produce ions – neutral atoms cannot be measured (unlike ICP‐OES where many of the best
+ Highest M+ population should correspond to lowest polyatomic population
emission lines are atomic) Sample introduction must maintain high plasma
Conventional ICP MS Optimized ICP‐MS (7700)
Particles are decomposed and dissociated Aerosol is Dried Atoms are formed and then ionised
temperature – monitored using CeO+/Ce+ ratio
+ +
Conventional ICP‐MS
0.5 ‐ 1.0mL/min, 1.8‐2.0 mm Injector, no water vapor removal Low central channel temperature
Optimized ICP‐MS (7700)
0.10 ‐ 0.25mL/min, 2.5mm Injector, water vapor removed High central channel temperature + + + + + + + + + + + + + High sample load, narrow central channel poor matrix decomposition Low sample load, wide central channel good matrix decomposition
When a high sample matrix (e.g. 1/10 seawater) is introduced, the plasma is When a high sample matrix (e.g. 1/10 seawater) is introduced, the plasma is
the CeO/Ce ratio is higher (plasma temperature is lower)
Signal Suppression in 0.3% NaCl
90.0 100.0 50.0 60.0 70.0 80.0 covery 1% CeO/Ce 10 0 20.0 30.0 40.0 % Rec 1.7 % CeO/Ce
Spike recovery in a high matrix is better with a robust
0.0 10.0 Sc-45 Cr-52 Fe-56 Zn-66 Mo-95 In -115 Elements
plasma (low CeO/Ce ratio) 7700 has the lowest CeO/Ce ratio in standard conditions
Reducing CeO+/Ce+ ratio from 3.0% to 1.0% (3x reduction) removes ~70% of many g / ( ) y matrix‐based interferences (ArCl+, ClO+, CaO+, etc) Hotter plasma is less affected by a variable matrix (more robust) Better matrix decomposition reduces interface and lens contamination and therefore p reduces maintenance Hotter plasma improves the ionization of poorly ionized elements, so MUCH lower LODs possible for Be (right), B, As, Se, Cd, Hg (below), etc
S b t B Sub ppt Be detection limit! 30ppt 30ppt 10ppt 5ppt
Hg BEC (ppt) LOD (ppt) 201 9.49 1.51 Be BEC (ppt) LOD (ppt) 9 0.465 0.235
Principle of HMI is simple – hardware comprises extra hardware comprises extra gas line to dilute aerosol. However, requires very sophisticated software sophisticated software algorithm to map plasma conditions, and very reproducible hardware to reproducible hardware to allow conditions to be recalled consistently
HMI dilutes aerosol density & water vapour, as well as sample matrix. Gives much higher
100 120
+/- 15%
Gives much higher plasma temp; much better matrix
suppression is almost
80 100 0ppb Spike
/ 15%
suppression is almost eliminated. Plot shows % recovery in dil d
40 60 Recovery of 10 2% CeO/Ce 1% CeO/Ce
undiluted seawater vs aqueous calibrations. With HMI, ALL results are within +/‐ 15%
20 % R 0.2% CeO/Ce
/ recovery (shaded area) Without HMI, ALL results are below 60% recovery
Elements
g p
less maintenance (cone cleaning) is required
at
p o es o g te stab ty, c dec eases t e need to run repeated calibrations
– Further increases sample throughput
7700 Series standard interface provides high sensitivity and good matrix tolerance as standard – no need for a separate set of low‐ sensitivity cones for high matrix samples!
rejects photons and neutrals
Lens – located outside high‐vacuum region, so easy to access for maintenance
transmission across the mass range, low random background, and protection from matrix contamination in the high vacuum i region
increase ion transmission at specific masses ll i d ll h i ! – all masses are transmitted all the time! 7700 Series has the highest ion transmission across the mass range of any ICP‐MS, in standard, matrix tolerant conditions
The 7700 uses a completely new collision/ reaction cell, with: 18% longer rods 18% longer rods 15% smaller ID and operates at 16% higher pressure 20% higher frequency ORS3 also operates with a much larger energy ORS3 also operates with a much larger energy discrimination step. Result is much more effective removal of interferences in He mode with KED Major improvement compared to 7500 Series, which already offered by far the best He mode performance of any ICP‐MS
Sub‐ppb LOD shows interference removal on all Se isotopes – essential for accurate isotope ratio or isotope dilution measurement
LOD shows 0ppb Isotope BEC (ppt) LOD (ppt) 78 7.95 <5ppt 80 301 133 82 252 210
dilution measurement
pp
Blank was 2cps +/‐ 0cps Probably <5ppt LOD
82 252 210
Improved performance for Se with ORS3 in He mode – li i t th d f eliminates the need for reaction mode in routine applications. No SeH or BrH formation (affects all reaction gases) No SeH or BrH formation (affects all reaction gases)
7700 Series retains the renowned research‐grade hyperbolic quadrupole of the 7500 Series Still the only 7500 Series. Still the only hyperbolic quadrupole used in any commercial ICP‐MS. Provides excellent peak ti f th b t separation, for the best abundance sensitivity specification: Low Mass: 5 x 10‐7 High Mass: 1 X 10‐7
f
Multipole Guides and Filters
quadrupole mass filter technology in 40 years." J D ll A il S i S ff S i i Jerry Dowell, Agilent Senior Staff Scientist
Best Abundance Sensitivity Specification of any ICP‐ MS – no need to set up custom resolution to separate adjacent peaks – all peaks are separated p j p p p under standard conditions! (Factory performance certificate ships with every 7700 Series instrument)
Agilent 7700 Low Mass Side 5x10‐7 (Cs) High Mass Side 1x10‐7 (Cs)
Quadrupole with alignment mandrel
High Mass Side 1x10 (Cs)
p g
Unique Discrete Dynode Electron Multiplier (DDEM) detector, providing 9 orders dynamic range (6 orders in pulse mode, and 3 further
Also has shortest minimum dwell time 0.1ms in both pulse and analog modes Genuine 9 orders dynamic range so major elements at 100’s ppm can be measured in the elements at 100 s ppm can be measured in the same run as trace elements at ppt, without
configuration. C lib i h N i 1 10 d 1 5 dil d Calibration shows Na in 1:10 and 1:5 diluted seawater – top point is 2360ppm
Calibration ran es These 4 plots were obtained under the same analytical conditions Calibration ranges Hg (10 – 200ppt) – NoGas Mode As (10 – 200 ppt) – He Mode Se (10 – 200 ppt) – He Mode Na (0 05 1000 ppm) He Mode
As
Hg
p y
As
Na (0.05 – 1000 ppm) – He Mode Overall calibration range 10ppt (Hg, As, Se) to 1000 ppm (Na) in a single method
As 10 ppt Mercury 10 ppt Arsenic
method ‐ without attenuating ion transmission to increase working range Na
Arsenic
Na Typically, ICP‐MS cannot measure above 200ppm Na without changing quad resolution or ion lens settings Hg
1000 ppm Sodium Se
Na Se
Good fit at 0.2ppm
Hg Hg LOD on 7700x is about 2ppt – 7700x can QUANTIFY at 10ppt! 7700x can do both of the above in the
10 ppt Selenium
f same run!
Original ICP MS pulse count
Detector range comparison: The entire green‐shaded area is within the measurement range of the 7700 Series detector, but 90% of these concentrations would be over‐ range on other detectors, requiring manual signal attenuation or dilution for these concentrations to be measured on other ICP‐MS instruments.
Original ICP‐MS pulse‐count detectors gave 6 orders dynamic range (up to 2Mcps) Analog mode typically adds a
1) 7700 Series detector – 9 orders dynamic range, from 0 to 500ppm
Analog mode typically adds a further 2 orders dynamic range (up to 400Mcps), equivalent to about 50ppm Agilent 7700 Series detector adds another order of dynamic range in analog mode – up to 4,000Mcps or around 500ppm
2) Typical ICP‐MS detector – 8 orders dynamic range, from 0 to 50ppm
around 500ppm Upper range is even higher for mineral elements in He mode, as low‐mass signal is reduced when
3) Older, pulse‐count only detector – 6
g cell is pressurized.
7700 electronics increase detector lifetime to >2 years (around 6 months on other ICP MS) months on other ICP-MS)
New x-lens New sampling cone ORS3 New RF generator
Size – Foot print is more than 30% smaller than Agilent 7500
Agilent 7500 D600 ( 720 w/ plug ) x W 1100 ( 1210 included SC) x H575 ( 645 with Chimney) Agilent 7700 D620 ( 720 w/ plug ) x W 730 ( 860 included SC) x H595 ( 655 with Chimney)
Weight ‐ more than 30% lighter 115kg (Agilent 7700 ) vs 175kg ( Agilent 7500)
Data Analysis software now integrated into main suite Same service support for all units
– Batch View Data table with real‐time update during sequence, on‐screen display of
– Calibration view can show 12 plots, single plot, or single plot with calib table – Elements with outlier flags are highlighted with calib plot shading – Current element in currently selected sample line is shown on calib curve Highlight shows g g element with outlier (e.g. over calib range) Current sample result shown on calib plot shown on calib plot
G hi l – Graphical pane shows ISTD Plot (recovery) – Can also show LabQC recovery (up to 3 can be defined) – Same pane can be used to show spectrum or h t hi chromatographic data – can be expanded to full screen or screen, or minimised to default layout
– Simple tools to view, zoom and scroll spectra, overlay files and tune steps, and process spectra to give semi quant data spectra to give semi‐quant data Overlay spectra or tune mode to tune mode, to quickly compare data Peak ID – no limit to number of elements
– Chromatographic Data Analysis option is fully integrated into main Batch table view, including real time update calib display and outlier flags Familiar GUI (similar to LC/MS) including real‐time update, calib display and outlier flags. Familiar GUI (similar to LC/MS)
M l i t ti ith d t f th d/ t ith ll i t t d k( ) – Manual integration, with update of method/report with manually integrated peak(s)
Signal to Noise Calculation (per compound, per analyte or per sample) Screen shows S/N for compound AB = S/N is shown above the selected peak. selected peak. Noise region can be selected for all compounds and all
Noise region – selected in l li
analyte masses, for all compounds of the selected mass, or just for the selected
lower pane – applies to selected compound and mass only Signal/Noise result displayed as peak label and printed in report
for the selected compound
L l t i l i t d t t d i Lower electrical power requirement, due to new rotary pump design Lower heat output and reduced exhaust vent flow (for 7700s), with redesigned cooling air‐flow management system All stainless‐steel outer panels, requiring less paint and associated solvents Reduction of toxic compounds in Printed Circuit Boards Increased use of recyclable materials such as plastic components Increased use of recyclable materials, such as plastic components At only 110Kg, the 7700 mainframe weighs 30% less than the 7500 Series, so significantly reduced CO2 emissions from transportation Th 7700 i th fi t i t ll f i dl ICP MS The 7700 is the first environmentally friendly ICP‐MS