Agilent 7700 Series. The Smallest, Most Powerful ICP MS Ever Made

Transcription

1 The All New Agilent 7700 Series The Smallest, Most Powerful ICP MS Ever Made

2 Inductively Coupled Plasma Mass Spectrometry ICP MS is a fast, multi element, high sensitivity trace metals analysis technique Key applications are: Environmental Foods Semiconductor Clinical Chemical/Petrochemical Pharmaceutical Consumer Goods Forensic Geological Nuclear Academic/Research ICP MS market continues to grow as technology improves and GFAA and ICP OES instruments are replaced with ICP MS

3 Agilent ICP MS Instrument Development Agilent 7700 Series Agilent 4500 Series Thenew face of ICP MS Agilent 7500 Series

4 Agilent s History of Innovation in ICP MS 1987 to PMS 100 introduced First computer controlled ICP MS 1988 PMS 200 introduced Second generation ICP MS with off axis Qpole lens st 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 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 Series 100, 200 & 300 introduced: 1st applications specific ICP MS Agilent 7500 Series introduced 7500a, 7500i and 7500s the next generation in ICP MS instrumentation. 9 orders detector range 2001 Agilent 7500c launched 1 st generation ORS for high matrix samples New digital generators and LAN control introduced. First commercial GC ICP MS interface Agilent 7500cs launched 2 nd generation ORS for high purity semicon samples Agilent 7500ce launched 2 nd generation ORS for high matrix samples Low flow cell gas MFC s for Xe NH 3, O 2, etc added to 7500ce/cs 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 system, for ultra high throughput analysis Agilent 4500 Series ShieldTorch System Octopole Reaction System Agilent 7500 Series Agilent 7700 Series

5 7700 Series New Product Highlights New ORS 3 Collision/Reaction Cell Longer, narrower rods, higher cell pressure and frequency MUCH better performance in He mode New RF Generator Fast tuning 27MHz generator, for better tolerance to changing matrix (incl. organics) Increased Matrix Tolerance High Matrix Introduction (HMI) standard on 7700x model Much smaller cabinet >30% smaller footprint than any other ICP MS Simple software; reliable Auto Tuning MassHunter software intuitive and easy to learn. Pre set plasma conditions and fast lens auto tuning

6 Two 7700 Models 7700x High productivity system Third generation ORS HMI Environmental, food, clinical, pharmaceutical and general purpose applications 7700s Clean room ready Third generation ORS Cool plasma Mineral acids, silicon matrices, organics, DIW, process chemicals

7 Agilent 7700 ICP MS System in Detail High matrix introduction (HMI) dilution gas inlet Off axis ion lens Cell gas inlet 3 rd generation Octopole Reaction System (ORS 3 ) Fast, simultaneous dual mode detector (9 orders dynamic range) Low flow Sample Introduction Peltier cooled spray chamber High frequency (3MHz) hyperbolic quadrupole High performance vacuum system Fast, frequencymatching 27MHz RF generator High transmission, matrix tolerant interface

8 Inorganic Analysis Techniques in a Typical Laboratory % ICP OES for majors and high matrix samples ppm Multi element, ~2 min/ sample 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 LOD GFAAS Single element, ~6min/ sample 10 s ppt to 100 s ppb Hydride/AFS ppb Few elements, ppt ~2min/ sample Single ppt to 10 s ppb Few Elements/Samples In many inorganic labs, several analytical techniques are used, to cover the range of analytes, matrices and detection limits required. This is encouraged by some vendors, who want to sell multiple instruments to each lab! Many Elements/Samples

9 Inorganic Analysis Techniques in a Typical Laboratory % ICP OES ppm LOD 7700 ICP-MS Multi element, ~2 min/ sample Multi-element 10 s ppb to 1000 s ppm Single ICP MS cell gas for mode trace and elements productivity and clean tools samples reduce run time Multi element, ~4min/ sample HMI for samples with % level solids Single ppt to 10 s ppm Single ppt (incl. hydride and Hg) to 100 s ppm (1000 s ppm with HMI) GFAAS Single element, ~6min/ sample 10 s ppt to 100 s ppb Hydride/AFS ppb Few elements, ppt ~2min/ sample Single ppt to 10 s ppb Uniquely, the Agilent 7700 can replace all these separate techniques, providing high throughput, matrix tolerance, wide elemental coverage and low LODs in a single run Few Elements/Samples Many Elements/Samples

10 7700 Smaller Cabinet; Longer Ion Path!! The 7700has >30% smaller footprint than any other ICP MS, but access for maintenance has been improved (all service from front) Despite much smaller external cabinet size, the ion path of the 7700 is actually 30mm longer than the 7500 Extra length due to redesigned cell (longer octopole rods) and lens 30% smaller footprint 30mm longer ion path

11 Unique Performance of the 7700 Better matrix tolerance than any other ICP MS Higher plasma temperature (lower CeO/Ce ratio) under standard conditions than any other system Best performance with Helium cell gas eliminates need for reaction gases in all common applications 7700 ORS 3 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

12 7700 Series Sample Introduction Low flow (typically 0.15mL/min) Temperature stabilized (Peltier cooled spray chamber) Wide Torch Injector ID (2.5mm) No O rings in spray chamber end cap reduced risk ofcontamination Auto alignment of torch after maintenance Fast frequency matching RF generator Simple setup, using pre set plasma conditions and auto tuning Provides most robust plasma of any ICP MS under standard conditions

13 All New RF Generator The new RF generator of the 7700 operates using a unique computer controlled fast tuning design, to instantly match to changing load. This means that the 7700 can switch from pure water to volatile organics without disturbing the plasma

14 Interface area

15 Comparison of Plasma Loading/Cooling ICP MS plasma must produce ions neutral atoms cannot be measured (unlike ICP OES where many of the best emission lines are atomic) Sample introduction must maintain high plasma temperature monitored using CeO + /Ce + ratio Hottest part of Sample channel is Residence time is a plasma ~ 8000K at ~6700K few milliseconds By sample cone, analytes present as M + ions Aerosol is Dried Particles are decomposed and dissociated Conventional ICP MS Optimized ICP MS (7700) mL/min, mm Injector, no water vapor removal Low central channel temperature + Highest M + population should correspond to lowest polyatomic population Atoms are formed and then ionised mL/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

16 CeO/Ce Ratio Effect on Matrix Suppression Whena highsample matrix (e.g.1/10seawater) is introduced,thethe plasma is overloaded and analyte signal drops (suppression). Suppression is worse when the CeO/Ce ratio is higher (plasma temperature is lower) Signal Suppression in 0.3% NaCl % Rec covery Sc-45 Cr-52 Fe-56 Zn-66 Mo-95 In -115 Elements 1% CeO/Ce 1.7 % CeO/Ce Spike recovery in a high matrix is better with a robust plasma (low CeO/Ce ratio) 7700 has the lowest CeO/Ce ratio in standard conditions of any ICP MS (<1%)

17 Other Benefits of High Plasma Temp. Reducing CeO + /Ce + ratio from 3.0% to 1.0% (3x reduction) removes ~70% of many 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 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 Sub ppt Be detection limit! 30ppt Hg BEC (ppt) LOD (ppt) ppt 10ppt Be BEC (ppt) LOD (ppt)

18 High Matrix Introduction (HMI) How it Works HMI is a sample dilution technique but, uniquely, it dilutesthe the sample inthe gas state, using aerosol dilution. This removes the main problems of liquid sample dilution: Time Reagents ErrorsE Contamination

19 HMI Automatic Setup of Plasma Conditions Principle of HMI is simple hardware comprises extra gas line to dilute aerosol. However, requires very sophisticated software algorithm to map plasma conditions, and very reproducible hardware to allow conditions to be recalled consistently

20 HMI Robust Plasma Low Oxide Interferences Recovery of a 1 ppb Cd spike in increasing Mo concentration (0, 2, 5 ppm Mo). Comparison of standard 7700x (1% oxides) and 7700xunder HMI conditions (0.2% oxides)

21 HMI Effect on Matrix Suppression % Recovery of 10 0ppb Spike Elements HMI dilutes aerosol density & water vapour, as well as sample matrix. +/- 15% Gives much higher plasma temp; much better matrix decomposition. Matrix suppression is almost eliminated. 2% CeO/Ce 1% CeO/Ce 0.2% CeO/Ce Plot shows % recovery in undiluted d seawater vs aqueous calibrations. With HMI, ALL results are within +/ 15% recovery (shaded area) Without HMI, ALL results are below 60% recovery

22 Other Benefits of HMI HMI increases sample throughput Reduces sample prep time (no manual or auto dilution) Reduces number of over range range samples which have to be repeated HMI decreases routine maintenance HMI dilution reduces the matrix loading on the plasma This decreases the amount of matrix which reaches the interface cones and so less maintenance (cone cleaning) is required Lower matrix loading also asoimproves poeslong term stability, ty, which decreases eases the need to run repeated calibrations Further increases sample throughput

23 7700 Series Interface New interface provides simple access for maintenance remove and refit cone without any tools Provides good ion transmission i and matrix tolerance 7700 Series standard interface provides high sensitivity and good matrix tolerance as standard no need for a separate set of lowsensitivity cones for high matrix samples!

24 7700 Series Ion Lens Ion Lens focuses ions into the cell, and rejects photons and neutrals 7700 uses a combined Extraction/Off axis Lens located outside high vacuum region, so easy to access for maintenance Provides ideal combination of high transmission across the mass range, low random background, and protection from matrix contamination in the high vacuum region No need to set up variable voltages to increase ion transmission at specific masses 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

25 All New Octopole Reaction System (ORS3) The 7700 uses a completely new collision/ reaction cell, with: 18% longer rods 15% smaller ID and operates at 16% higher pressure 20% higher frequency 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

26 Se Calibration (in 2% HCl + 100ppm Ca) Calibration for 78, 80, 82Se at 0, 0.5, 1, 10ppb LOD shows 0ppb Blank was 2cps +/ 0cps Probably <5ppt LOD Sub ppb LOD shows interference removal on all Se isotopes essential for accurate isotope ratio or isotope dilution measurement Isotope BEC (ppt) LOD (ppt) <5ppt Improved performance for Se with ORS 3 in He mode eliminates i the need for reaction mode in routine applications. No SeH or BrH formation (affects all reaction gases)

27 High Frequency Hyperbolic Quadrupole 7700 Series retains the renowned research grade hyperbolic quadrupole of the 7500 Series. Still the only hyperbolic quadrupole used in any commercial ICP MS. Provides excellent peak separation, for the best abundance sensitivity specification: Low Mass: 5 x 10 7 High Mass: 1 X 10 7

28 7700 Quadrupole & Abundance Sensitivity 3MHz, hyperbolic quadrupole withalignment tolerance to 1 micron Winner of 2006 Bill Hewlett Innovation Award U.S. Patent #6,926,783: Manufacturing Precision Multipole Guides and Filters "This invention is the most significant advance in quadrupole mass filter technology in 40 years." Jerry Dowell, Ail Agilent Senior Staff ffsi Scientisti Best Abundance Sensitivity Specification of any ICP MS no need to set up custom resolution to separate adjacent peaks all peaks are separated 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) p g Quadrupole with alignment mandrel

29 9 Orders Dynamic Range Detector Unique Discrete Dynode Electron Multiplier (DDEM) detector, providing 9 orders dynamic range (6 orders in pulse mode, and 3 further orders in analog). 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 same run as trace elements at ppt, without operator having to change conditions or hardware configuration. Calibration i shows Na in 1:10 110and 1:5 15diluted d seawater top point is 2360ppm

30 7700x Largest Analytical Range of any ICP MS These 4 plots were obtained under the same analytical conditions Calibration ranges on the 7700x only the gas mode (NoGas for Hg) changed Hg (10 200ppt) NoGas Mode As ( ppt) He Mode Se ( ppt) He Mode Hg As Na ( ppm) He Mode As Overall calibration range 10ppt (Hg, As, Se) to 1000 ppm (Na) in a single method without attenuating ion transmission to increase working range 10 ppt Mercury 10 ppt Arsenic Na Typically, ICP MS cannot measure above 200ppm Na without changing quad resolution or ion lens settings Hg Hg LOD on 7700x is about 2ppt 7700x can QUANTIFY at 10ppt! Se Se 10 ppt Selenium Na 1000 ppm Sodium Good fit at 0.2ppm 7700x can do both of the above in the same run!

31 Orders Detector Dynamic Range Original ICP MS pulse count detectors gave 6 orders dynamic range (up to 2Mcps) 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 Upper range is even higher for mineral elements in He mode, as low mass signal is reduced when cell is pressurized electronics increase detector lifetime to >2 years (around 6 months on other ICP-MS) 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 overrange on other detectors, requiring manual signal attenuation or dilution for these concentrations to be measured on other ICP MS instruments. 1) 7700 Series detector 9 orders dynamic range, from 0 to 500ppm 2) Typical ICP MS detector 8 orders dynamic range, from 0 to 50ppm 3) Older, pulse count only detector 6 orders dynamic range, from 0 to 0.5ppm

32 New hardware New x-lens New sampling cone New RF generator ORS 3 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)

33 Build Quality The renowned build quality, durability and reliability of the 7500 has been further improved This photo shows the high quality finish of the 7700 ICP MS even the rear panel that is not seen by users

34 Even Cleaner than the s takes clean room operation even further Single Singleexhaustexhaust duct (no need for optional duct kit) No external air exhaust vents into clean room Lower exhaust flow requirement (5 7m 3 /min, down from 7 8m 3 /min) Much lower pressure drop (140Pa for 7500, to 40Pa for 7700), simplifies clean room installation and reduces air handling costs

35 Chromatographic Applications Simple link to Ail Agilent LC Direct sequence control from ICP MS sample log table Method setup for LC/GC from ICP MS PC Predefined application packs available, as for 7500 Data Analysis software now integrated into main suite Same service support for all units

36 MassHunter Software for 7700 Series ICP MS

37 Overview of Data Analysis Window (MassHunter) Batch View Data table with real time update during sequence, on screen display of outlier/qc failures (e.g. flag for results outside calibration range)

38 Calibration Plots 12 Plots or Single Plot 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 g shows element with outlier (e.g. over calib range) Current sample result shown on calib plot

39 ISTD Stability and LabQC Plots 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 chromatographic hi data can be expanded to full screen, or minimised to default layout

40 Spectrum MassHunter Simple tools to view, zoom and scroll spectra, overlay files and tune steps, and process spectra to give semi quant data Peak ID no limit to number of elements Overlay spectra or tune mode, to quickly compare data

41 Chromatographic Data Analysis MassHunter Chromatographic Data Analysis option is fully integrated into main Batch table view, including real time update, calib display and outlier flags. FamiliarGUI (similarto LC/MS)

42 Chromatographic Data Analysis Manual Integration Manual lintegration, ti with update dt of method/report t with manually integrated t peak(s)

43 Chromatographic Data Analysis Signal/Noise Noise region selected in lower pane applies to selected compound and mass only Signal/Noise result displayed as peak label and printed in report 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. Noise region can be selected for all compounds and all analyte masses, for all compounds of the selected mass, or just for the selected compound

44 MassHunter Software Significant improvement in ease of use and functionality Easier to learn Faster learning cycle = improved productivity. New software capabilities for speciation Chromatographic data analysis software integrated with main data table Excel based reporting Common SW platform with other Agilent instruments GC/MS, GC/MS/MS, / LC/MS, and LC/MS/MS / Reduced staff training costs

45 7700 Environmental Impact Reduction Lower electrical lpower 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 Increaseduseof recyclablematerials materials, suchasplasticcomponents components At only 110Kg, the 7700 mainframe weighs 30% less than the 7500 Series, so significantly reduced CO2 emissions from transportation The 7700 is the first environmentally friendly fi ICP MS

46 Agilent 7700 with ORS 3 The Most Powerful ICP MS for the Routine or Research Lab Effective removal of polyatomic interferences using He mode only, even in unknown and variable sample matrices Simple method development same conditions used for all elements and all sample types No new interferences and no loss of analyte signal by reaction Highest data integrity inunknown matrices Unmatched sensitivity across the mass range Widest dynamic range low ppt to 1000ppm The 7700x simplifies ICP MS operation, while improving matrix tolerance and providing unparalleled interference removal in complex and variable samples

47 Is it ready to ship.?