Radiant energy – Ionic separation or analysis – Ion beam pulsing means with detector synchronizing means
Reexamination Certificate
2000-08-16
2002-04-09
Berman, Jack (Department: 2881)
Radiant energy
Ionic separation or analysis
Ion beam pulsing means with detector synchronizing means
C250S287000, C250S288000, C436S153000
Reexamination Certificate
active
06369383
ABSTRACT:
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a Time-of-Flight (TOF) mass spectrometer and, more particularly, to a novel ion reflectron useable in, for example, a TOF mass spectrometer and a method of manufacturing same.
2. Description of the Related Art
A spectrometer is an analytical instrument in which an emission (e.g., particles or radiation) is dispersed according to some property (e.g., mass or energy) of the emission and the amount of dispersion is measured. Analysis of the dispersion measurement can reveal information regarding the emission, such as the identity of the individual particles of the emission.
It is well known that energy applied to ionized particles (ions) via an electric field will cause the ions to move. This principle is used in different kinds of spectrometers to accomplish different goals. For example, an ion mobility spectrometer (IMS) is used to detect and analyze organic vapors or contaminants in the atmosphere. As described and shown in U.S. Pat. No. 5,834,771 to Yoon et al., a typical IMS detector cell (also called an ion drift tube) comprises a reaction region for generating ions, a drift region or drift tube for separating ions, and a collector.
A carrier or drift gas along with a sample gas introduced into the IMS are ionized and then the sample is moved through the drift tube by an electric field applied along the drift tube. Different ions in the sample are separated based on their behavior in the drift tube as they collide with the drift gas. Each type of ion exhibits its own identifiable behavior pattern based on its particular structure, e.g., each ion shows unique velocity due to its mass, size, and charge. The separated ions proceed further down the drift tube and collide with the collector, producing a measurable current. The drift velocities and the peak currents of the ions arriving at the collector provide a basis for the approximating the identity of the samples introduced into the reaction region; however, it is not an exacting technique, since two different ion types having similar masses and similar interaction with the drift gas will be difficult, if not impossible, to distinguish from each other.
A variety of methods of generating the electrical field used in the reaction region and the drift tube are available, as described in the previously-mentioned '771 patent. The subject matter of the '771 patent is directed to one such method involving the fixation of a flexible printed circuit board onto the surface of the drift tube. Evenly-spaced parallel conductive bands are patterned on the flexible circuit board and the electrically conductive bands are connected to adjacent bands via resistances. Through proper biasing of the resistors, the conductive bands are placed at potentials relative to their positions along the tube, so that a uniform electric field is developed along the axis of the tube.
Mass spectrometry is another well-known spectrometry method. Mass spectrometers are used to determine, with precision, the chemical composition of substances and the structures of molecules. One type of mass spectrometer, a time-of-flight (TOF) mass spectrometer, is an instrument that records the mass spectra of compounds or mixtures of compounds by measuring the times (usually of the order of tens to hundreds of microseconds) for molecular and/or fragment ions of those compounds to traverse a (generally) field-free drift region within a high vacuum environment. TOF mass spectrometers operate based on the principle that, when ions are accelerated with a fixed energy, the velocity of the ions differ dependant exclusively on mass and charge. Thus, the time-of-flight from point A to point B will likewise differ dependant on the mass of the ion. Using a TOF mass spectrometer, the mass of an ion can be calculated based upon its time of flight. There are no collisions with a carrier gas as occurs in an IMS—only the velocity, and therefore the mass and charge (usually +1), is utilized for the calculation. This allows the molecule to be identified with precision.
TOF mass spectrometers are comprised of a source region, where neutral molecules are ionized, a drift region, followed by an ion reflector (also known as a reflectron) and a detector. In the ion source, ions are formed in a high vacuum environment followed by acceleration down a field free drift region. The ions separate in time dependent only on their mass/charge ratio (normally the charge is +1). Upon entering the opposing field created by the ion reflector, ions gradually slow down, stop, and reverse direction. The detection occurs after the ions are re-accelerated out of the ion reflector. In addition to enabling the calculation of the mass of the ions, ion packet peak widths are sharpened by their passage through the ion reflector, resulting in an enhancement of the instrument's resolving power.
Reflectrons have been in use since the late 1960's and are typically constructed by configuring plural individually manufactured metallic rings along ceramic rods using insulating spacers to separate each ring from the next. This technique is labor intensive, costly, and limits the flexibility of design due to the manufacture and handling of extremely thin rings (a few mils in thickness) of relatively large diameter (1″ or greater). An example of such a configuration is shown in U.S. Pat. No. 4,625,112 to Yoshida. While many permutations of this device exist, the method of construction has been limited to the ring method described above.
Similar to the parallel conductive traces of the '771 patent, the rings are placed at potentials that develop electric fields along the axis of the cylinder. However, in contrast to the IMS method, which develops a uniform electric field along the drift tube and which can only approximate the identity of molecules in a sample, a TOF mass spectrometer is capable of measuring atomic and molecular weights with high precision. Furthermore, to improve performance in a TOF mass spectrometer, reflectrons have been constructed which develop non-uniform fields along the reflectron tube. The non-uniform fields are generated by utilizing a voltage divider network which varies the potential applied to each of the evenly-spaced rings. A detailed explanation of non-linear reflectron theory can be found in U.S. Pat. No. 5,464,985 to Cornish et al., incorporated fully herein by reference.
While the above-described TOF mass spectrometer design has proved quite satisfactory for large reflectors in which the rings are relatively large in diameter and equally spaced, new applications utilizing remote TOF mass spectrometers may require miniaturized components, rugged construction, and/or the use of lightweight materials. Smaller TOF mass spectrometers have reduced drift length, necessitating the use of ideal energy focusing devices (reflectrons) to maximize resolution.
Therefore, it would be desirable to develop new methods of construction to fabricate miniature ion reflectors for TOF's which are smaller, rugged, and lightweight and which provide maximum resolution.
SUMMARY OF THE INVENTION
To this end, a novel technique utilizing the precision of printed circuit board design and the physical versatility of thin, flexible substrates has been devised to produce a new type of ion reflector. In this method, a precisely defined series of thin conductive strips (traces) are etched onto a flat, flexible circuit board substrate. The flexible substrate is then rolled into a tube to form the reflector body, with the conductive strips forming the rings of the ion reflector. The spacing between the traces, and hence the ring spacing, can be readily varied by adjusting the conductor pattern on the substrate sheet during the etching process.
The present invention is a multi-layered reflectron for a time-of-flight (TOF) mass spectrometer, comprising: plural structural layers; and at least one flexible electrode layer, the flexible electrode layer creating an electric field in the reflectron when a vol
Charles Harry K.
Cornish Timothy J.
Wienhold Paul D.
Berman Jack
Fernandez K.
Graf Ernest R.
Krivak Carla M.
The John Hopkins University
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