ARI Aerosol Mass Spectrometer Operation Manual AERODYNE RESEARCH, Inc. Billerica, Massachusetts 01821-3976 978-663-9500 Fax 978-663-4918 www.aerodyneresearch.com AERODYNE RESEARCH, Inc. 978-663-9500 10/19/05 Page 2 Table of Contents Instrument Description................................................................................................................................5 SPECIFICATIONS...................................................................................................................................5 Performance..........................................................................................................................................5 Physical.................................................................................................................................................6 THEORY OF OPERATION.....................................................................................................................7 Particle Beam Formation......................................................................................................................7 Particle Detection..................................................................................................................................9 Electron Multiplier..............................................................................................................................11 Volumetric Sampling (Flow) Rate......................................................................................................17 Particle Size/Velocity..........................................................................................................................18 System Set-Up.............................................................................................................................................20 AMS HARDWARE................................................................................................................................20 Vacuum System..................................................................................................................................20 ELECTRONICS......................................................................................................................................23 Computer/Data System.......................................................................................................................23 Balzers QMG 422 Quadrupole Controller..........................................................................................24 AMS Power Supply............................................................................................................................24 Turbo Pump Control (TPC) Box.........................................................................................................27 Electronics Box (EB)..........................................................................................................................31 Operational Procedures.............................................................................................................................36 START-UP..............................................................................................................................................36 SHUT-DOWN.........................................................................................................................................37 Controlled Shut-Down Procedure.......................................................................................................37 Emergency Shut-Down Procedure......................................................................................................38 Calibrations.................................................................................................................................................39 SYSTEM CALIBRATIONS THAT AFFECT SIGNAL INTENSITIES...........................................40 SYSTEM CALIBRATIONS THAT AFFECT ACCURATE REPORTING......................................41 OF AEROSOL MASS VALUES........................................................................................................41 ELECTRON MULTIPLIER CALIBRATION........................................................................................42 QUADRUPOLE MASS AND RESOLUTION CALIBRATION...........................................................48 Peak Shapes in Quadrupole Mass Spectra..........................................................................................48 Peak Shape Calibration.......................................................................................................................50 Peak Position Calibration....................................................................................................................51 PROCEDURE FOR MS CALIBRATION:........................................................................................53 IONIZATION EFFICIENCY (IE) CALIBRATION...............................................................................54 Automated IE Calibration...................................................................................................................56 FLOW RATE CALIBRATION..............................................................................................................58 AERODYNAMIC LENS ALIGNMENT................................................................................................61 PARTICLE-SIZING CALIBRATION....................................................................................................63 SERVO MOTION/POSITION CALIBRATION....................................................................................67 Acquisition and Analysis Software Overview..........................................................................................70 DATA ACQUISITION MODES............................................................................................................70 TOF Mode...........................................................................................................................................71 MS Mode............................................................................................................................................71 Alternate Mode...................................................................................................................................72 Special Modes.....................................................................................................................................73 DATA ANALYSIS OVERVIEW...........................................................................................................73 Maintenance................................................................................................................................................74 CLEANING.............................................................................................................................................75 LEAK TEST............................................................................................................................................75 FILAMENT REPLACEMENT...............................................................................................................76 AERODYNE RESEARCH, Inc. 978-663-9500 MULTIPLIER REPLACEMENT...........................................................................................................85 Troubleshooting/Diagnostics.....................................................................................................................88 NO ION SIGNAL....................................................................................................................................88 LOW ION SIGNAL................................................................................................................................89 NO VARIATION IN ION SIGNALS DURING QUADRUPOLE AUTO-TUNE PROCEDURE........89 CHOPPER WHEEL NOT SPINNING....................................................................................................90 CHOPPER SERVO NOT MOVING.......................................................................................................90 NO MS SIGNAL.....................................................................................................................................92 FILAMENT DOES NOT LIGHT...........................................................................................................92 TROUBLESHOOTING, CONTINUED….............................................................................................93 FILAMENT DOES NOT STAY LIT, TURNS ON BUT SHUTS OFF.................................................93 NO OR LOW AIR BEAM SIGNAL.......................................................................................................93 AIR BEAM DECREASING BUT IONIZATION EFFICIENCY IS OK...............................................93 Safety...........................................................................................................................................................95 Glossary.......................................................................................................................................................96 References...................................................................................................................................................98 Aerodyne Research, Inc. (ARI)......................................................................Error! Bookmark not defined. ARI Staff..........................................................................................................Error! Bookmark not defined. Technical Support and Training Resources..................................................Error! Bookmark not defined. Index............................................................................................................................................................99 11/17/05 Page 2 AERODYNE RESEARCH, Inc. 978-663-9500 Figures Figure 1: Aerosol Mass Spectrometer............................................................................................................7 Figure 2: Calculated Particle Trajectories......................................................................................................9 Figure 3: Signal Train in AMS.....................................................................................................................10 Figure 4: Multi-stage Discrete Dynode Multiplier.......................................................................................11 Figure 5: Setting Electron Multiplier Threshold to Detect Individual Ions..................................................13 Figure 6: Pulse Height vs. Time...................................................................................................................14 Figure 7: Pulse Height DistributionIonization Efficiency............................................................................15 Figure 8: Setting Electron Multiplier Threshold to Detect Individual Particles...........................................16 Figure 9: Relationship Between Single Ion and Single Particle Pulses........................................................17 Figure 10: Cross-Section of Vacuum Chamber............................................................................................20 Figure 11: Chamber Distances and Apertures..............................................................................................22 Figure 12: AMS Power Supply, front and rear views...................................................................................26 Figure 13: Turbo Pump Control, front panel controls..................................................................................28 Figure 14: Turbo Pump Control, rear panel connectors...............................................................................30 Figure 15: Electronics Box, front panel controls..........................................................................................32 Figure 16: Electronics Box, rear panel controls...........................................................................................34 Figure 17: Pin Description for I/O Connectors.............................................................................................35 Figure 18: Screens: Electron Multiplier Calibration.....................................................................................44 Figure 19: Multiplier Gain Curve.................................................................................................................48 Figure 20: Screen: MS Calibration...............................................................................................................53 Figure 21: Flow Curve..................................................................................................................................59 Figure 22: Lens Alignment...........................................................................................................................61 Figure 23: Lens Position Adjustment...........................................................................................................63 Figure 24: Particle Times of Flight...............................................................................................................64 Figure 25: Velocities plotted against Particle Aerodynamic Diameter.........................................................65 Figure 26: Screen: Data Acquisition Program Menu....................................................................................67 Figure 27: Screen: Servo Motion/Position Calibration.................................................................................68 Figure 28: Screen: AMS Software................................................................................................................70 Figure 29: Screen: Example, MS Mode.......................................................................................................72 Figure 30: Filament Replacement.................................................................................................................76 Figure 31: Detail, Quadropole Removal: Hand Position..............................................................................77 Figure 32: Filament Replacement: Quadrupole Mounting...........................................................................77 11/17/05 Page 3 AERODYNE RESEARCH, Inc. 978-663-9500 Figure 33: Filament Replacement.................................................................................................................78 Figure 34: Replacement Filament Assembly................................................................................................78 Figure 35: Filament Replacement.................................................................................................................79 Figure 36: Servo in Beam Block Position....................................................................................................83 Figure 37: Servo in Beam Chop Position.....................................................................................................84 Figure 38: Servo in Beam Open Position.....................................................................................................84 Figure 39: Electron Multiplier Replacement................................................................................................86 Figure 40: Electron Multiplier Replacement................................................................................................87 Figure 41: Balzers Cross-Beam Ionizer Voltage Table................................................................................94 11/17/05 Page 4 AERODYNE RESEARCH, Inc. 978-663-9500 Instrument Description The ARI Aerosol Mass Spectrometer provides real-time size resolved composition analysis of volatile and semi-volatile particulate matter. The combination of size and chemical analysis of sub-micron aerosol mass loading with fast time resolution makes the ARI AMS unique. Aerosol particles in the size range ~ 0.04 to ~1.0 micrometers are sampled into a high- vacuum system where they are aerodynamically focused to a narrow beam (~ 1mm diameter). The particle beam is directed onto a resistively heated surface where volatile and semi-volatile chemical components are thermally vaporized and detected by electron impact ionization quadrupole mass spectrometry. Particle aerodynamic diameter is determined from particle time-of-flight (TOF) velocity measurements using a beam-chopping technique. An optional optical module makes it possible to correlate light scattering, aerodynamic diameter and chemical composition analysis on a particle-by-particle basis for particles larger than 200 nm diameter. Specifications Performance • Size-resolved mass analysis of non-refractory aerosol components. (cid:127) Chemical analysis by thermal vaporization and electron impact ionization mass spectrometry (unit mass resolution to 340 AMU, scan rate 1 msec/amu). Single ion detection ability. (cid:127) Real-time mass spectral analysis of inorganic (nitrate, sulfate, ammonium) and organic mass (OM). 11/17/05 Page 5 AERODYNE RESEARCH, Inc. 978-663-9500 o o (cid:127) Particle vaporization temperature adjustable from 200 C to 900 C. (cid:127) Single-particle detection diameter approximately 100 nm. (cid:127) Sensitivity of ~ 0.01 mg/m3 in several minutes. (cid:127) Sampling flow rate: 100 cc min-1. (cid:127) Aerodynamic particle size measurement in the range of 40 nm to ~1 µm. Size resolution of 5 to 10 (D /∆D , FWHM) over that size range. aero aero (cid:127) Quantitative particle collection efficiency (~ 100%) in the range of 50 to 500 nanometers in diameter. Collection extends to particles about a factor of 2-3 smaller and larger with reduced efficiency. (cid:127) Fast time resolution of seconds. Maximum data rate ~100 Hz. (cid:127) Data output format: ASCII, HDF. Wavemetrics© Igor program license supplied. Physical (cid:127) Size: Approximately 41" wide x 24" deep x 53" high. (cid:127) Weight: Approximately 170 kg. (cid:127) Power: Approximately 600 W. Universal power 110VAC/60Hz or 220VAC/50Hz. Vacuum system fully operational on 24 VDC. (cid:127) Packaging: Shipped in one reusable container. Total shipping weight ~280 kg. Approx. outside dimensions 30" wide x 51" long x 63" high on forklift skids. 11/17/05 Page 6 AERODYNE RESEARCH, Inc. 978-663-9500 Theory of Operation Particle Beam Formation The ARI Aerosol Mass Spectrometer measures the size and chemical composition of volatile/semi-volatile submicron aerosols. It provides composition information on ensembles of particles, with limited single-particle information. The instrument combines standard vacuum and mass spectrometric techniques with aerosol sampling techniques. Figure 1: Aerosol Mass Spectrometer 11/17/05 Page 7 AERODYNE RESEARCH, Inc. 978-663-9500 Aerosols enter the AMS through a particle-sampling inlet that restricts the flow with a 100 mm (or similar diameter) critical orifice. They proceed through a lens1 that focuses the aerosols into a tight beam of approximately one millimeter in diameter, using 6 apertures. Gas is removed later by differential pumping. As the aerosols exit the lens, they are accelerated in a supersonic expansion caused by the difference in pressure between the aerosol-sampling chamber and the aerodynamic particle-sizing chambers. This expansion gives different velocities to aerosols of different sizes. After passing through the lens, the aerosols enter the particle-sizing chamber. A rotating chopper wheel, with two radial slits located 180o apart, intercepts the focused particle beam. The chopper can be placed in any of three positions: completely blocking the beam so that no particles pass through (beam closed); not blocking the beam so that all particles pass through (beam open), and a chopping position that allows particles to pass through the radial slits only (beam chopped). The time of flight (TOF) between the chopper and the detector is the measurement of a particle's velocity; from this measurement the particle's aerodynamic diameter (D ) can be determined. aero The particles passing through the flight chamber are directed onto a resistively heated surface. Upon collision with this heated surface, non-refractory particles flash vaporize under high-vacuum conditions. The vaporization process occurs directly inside an electron impact ionizer where the vaporized constituents are converted to positive ions, which can then be detected by the mass spectrometer.2 The electron impact ionization process is a universal process; therefore, any species in the gas phase will be detectable. The AMS does not efficiently detect low-volatility materials such as black carbon, NaCl, crustal oxides and certain metals. However, lower volatility species adsorbed on such material can be detected. 1 Following the design in Liu et al [1995]. 2 "Non-refractory" refers to any material that rapidly vaporizes (on the time scale of <100 µs) at 600 oC temperature. 11/17/05 Page 8