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49th ASMS Conference May 2001 |
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Instrumentation Session Poster Paper 019 |
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Bruce N. Laprade, Raymond Cochran and |
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Ronald Starcher |
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BURLE Electro-Optics Inc. |
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Sturbridge MA, 01566 |
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1-800-648-1800 |
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Time of Flight Mass Spectroscopy has become the
most widely used technique for identifying very large organic molecules.
This technique has become the method of choice for most drug discovery and
polymer applications. |
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The Time of Flight technique is frequently
chosen because it is the only technique capable of the high mass
sensitivity needed for many substances. |
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Recently, table top RGA, ICPMS, GC and LCMS
instruments have emerged. |
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The Time-Of-Flight mass spectrometry technique
is an old technique which has seen a resurgence in popularity due to cost
reductions in electronics and the advent of high temporal resolution
detectors. |
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The availability of high temporal resolution
detectors has enabled shorter flight tubes to be used, which lead to
smaller vacuum systems and lower overall instrument costs. |
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In the operation of a typical MALDI TOF
Instrument, analyte molecules, dispersed among matrix material are ionized
by a nitrogen laser. (Figure 1) |
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The resultant ions are held (delayed extraction)
and then ejected down a flight tube through the application of high voltage
pulses. |
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Mass separation occurs during the flight
(typically 1 meter) to the detector, with the lower mass ions arriving
first, followed by progressively larger mass ones. |
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Upon arrival at the detector, the electron
multiplier will produce a charge pulse corresponding to the arrival time of
each ion. (Figure 2) |
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A high speed digitizer is then used to record
the arrival times of the ions, from which the mass of the ion can be
determined. |
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Three types of electron multipliers have been
historically used in TOF-MS. Single Channel Electron multipliers (SEM),
Discrete Dynodes (DD), and Microchannel Plate (MCP) based. Single Channel
Electron Multipliers are not used in modern instruments because of
limitations in temporal resolution (20-30 ns FWHM) and dynamic range.
Discrete dynode electron multipliers exhibit good dynamic range, but are
used in moderate and low resolution applications because of relatively poor
pulse widths (Typically 6-10 ns FWHM). MCP based detectors are used in high
resolution applications because they provide the highest (650 ps) temporal
resolution, however they are limited in dynamic range to about 20 mhz/cm2
of active area. |
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Improving the temporal resolution of the ion
detector will enable resolution of lost peaks (Figure 8) |
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The temporal resolution of a microchannel plate
(Figure 9) based detector is ultimately determined by the electron transit
time (Figure 10) through the channel and the anode impedance. |
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The electron transit time of a microchannel
plate can be decreased by shortening the channel length. In order to
maintain proper operating conditions, the channel diameters must be reduced
proportionally. |
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The Primary Objective of this Development
Project was to Significantly Increase the Temporal Resolution of the
Conventional Time of Flight Mass Spectrometer Detector. |
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In order to increase the temporal resolution,
the MCP pore size must be significantly reduced. Reengineering the
fabrication process was necessary in order to overcome obstacles materials
fiber draw, wafer grind and polish, activation and test. |
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Microchannel Plates are fabricated by a series
of fiber draw operations involving a two glass system. |
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Precision alterations were made to the draw
parameters resulting in the successful fabrication of 18mm active diameter
format MCPs with 2.3 micron (Figure 11) channel diameters. |
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Interdiffusion obstacles were overcome by the
development of a new process. |
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New grinding and polishing techniques were
developed in order to produce microchannel plates as thin as 80 microns. |
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A cartridge assembly (Figure 12) containing two microchannel plates, a grounded
mesh and an output biasing system was developed in order to accommodate the
thin microchannel plates. |
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A low profile, time-of-flight detector for mass
spectrometry incorporating the smallest pore microchannel plates ever
developed has been successfully produced. |
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The temporal resolution of this detector is over
twice that of the best detector currently available. |
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The availability of this detector can
significantly reduce instrument size and cost, while improving mass
resolution. |
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