|Publication number||USRE30171 E|
|Application number||US 05/914,660|
|Publication date||Dec 18, 1979|
|Filing date||Jun 12, 1978|
|Priority date||Aug 27, 1973|
|Publication number||05914660, 914660, US RE30171 E, US RE30171E, US-E-RE30171, USRE30171 E, USRE30171E|
|Inventors||William P. Kruger, John A. Michnowicz|
|Original Assignee||Hewlett-Packard Company|
|Export Citation||BiBTeX, EndNote, RefMan|
|Patent Citations (8), Non-Patent Citations (3), Referenced by (6), Classifications (5)|
|External Links: USPTO, USPTO Assignment, Espacenet|
This is a continuation of application Ser. No. 391,721 filed Aug. 27, 1973 now U.S. Pat. No. 3,886,365.
Ion sources are employed with mass spectrometers in the analysis of substances. Commonly used sources are the electron impact source and the chemical ionization source. The first one has a large electron entrance, a large ion exit, and an ionization region where the incoming electrons fragment as well as ionize vapor molecules thus providing a large quantity of information which does not necessarily give clear indication of the identity of a substance. The chemical ionization source has, on the other hand, a small electron entrance, a small ion exit, and an ionization region where the pressure can be maintained at such levels that ion-molecule collisions are extremely likely to occur, such collisions leading to ready identification of the molecular weight of a substance.
Operation of a mass spectrometer alternately with electron impact and chemical ionization sources has required many hours of down time during which the operation of the spectrometer stops. An object of this invention is to permit changing between the electron impact and the chemical ionization configurations with minimal interruption of operation of the mass spectrometer.
According to the preferred embodiment, this invention provides an ionization source with two distinct ionization chambers, one which operates as an electron impact ionization source and the other as a chemical ionization source. The invention may be used with a mass spectrometer and changes in configuration can be made easily and quickly. The main elements of the invention include a hollow chamber having a plurality of orifices transverse to the longitudinal axis of the chamber. One of the orifices contains an electron source, and another one is a gaseous sample inlet. A hollow slidable cylindrical member having smaller transverse orifices than those in the hollow chamber fits inside the hollow chamber. At one of its ends, the cylindrical member has two electrode inserts separated from each other along the longitudinal axis and defining a first ionization region between them and the inside walls of the hollow cylindrical member. This region is connected to the sample inlet orifice and to the electron source orifice when the hollow cylinders is in a first position. A second ionization region is defined by the inside walls of the hollow chamber, the outer electrode insert of the cylindrical member, and the open end of the hollow chamber, when the cylindrical member is in a second position. This second region is directly connected to the electron source orifice and to the sample inlet. In this manner, when the cylindrical member is in the first position, the source operates as a chemical ionization source and when the cylindrical member is in the second position, the source operates an an electron impact source. The position of the cylindrical member can be changed quickly and easily by simply pushing or pulling a handle attached to the cylinder.
FIG. 1 shows a cross-sectional view of the preferred embodiment of the present invention in the chemical ionization configuration.
FIG. 2 shows the apparatus of FIG. 1 in the electron impact configuration.
FIGS. 1 and 2 show a vacuum envelope 14 which is connected to an ordinary vacuum pump through a port 9 for evacuating air from the envelope. An ion chamber 16, which may be a stainless steel tube, is supported within envelope 14 by a support member 12 and has orifices 17, 17' and 23 transverse to its longitudinal axis. Orifice 17 contains a filament 18 near the periphery of ion chamber 16 and near an end 19 of ion chamber 16. Orifice 23 is an inlet for samples to be ionized. The ion chamber 16 has a preferably cylindrical bore 24 along the longitudinal axis. Filament orifice 17 intersects bore 24 near end 19.
A hollow member 28 fits slidably inside bore 24, which member may be made of stainless steel tubing. Electrode inserts 35 and 36 are supported by and fastened to the inside of slide member 28 by insulators preferably made of ceramic. Insert 35 is located at end 21 of member 28 and has a passage 34 through it. Insert 36 is spaced apart from insert 35 and has a passage 39 through it. A connector 38 passes through passage 39 and engages passage 34 in insert 35 when member 28 has been moved to the left as shown in FIG. 2. A spring 40 attaches connector 38 to a base block 42, and this block is in turn affixed to but electrically insulated from chamber 16. Slide member 28 has a slot 44 through which base block 42 passes. The external surface of hollow member 28 is preferably hardened to prevent galling or binding with chamber 16. A handle 48 attaches to end 53 of hollow member 28 and is used to displace this member from the first position to the second position as shown in FIGS. 1 and 2 respectively. A bellows 46 surrounds handle 48 and connects the end 53 of hollow member 28 with a wall 55 of vacuum envelope 14. A support member 12 surrounds the bellows 46 and affixes the chamber 16 to wall 55. A pivot axle 75 between a support member 71 and an arm 72 permits pulling or pushing arm 72, which is connected to handle 48, for placing cylinder 28 in either the chemical ionization configuration as shown in FIG. 1 or the electron impact configuration as shown in FIG. 2. Arm 72 is connected to handle 48 by a vernier screw arrangement 73 for making fine alignment adjustments of electron passage 32 with filament orifice 17.
As shown in FIG. 1, electrode inserts 35 and 36 and the inner periphery of hollow member 28 define a first ionization region 30 when hollow member 28 is to the right, as in FIG. 1. A second ionization region 30' is defined by the interior walls of chamber body 16, the electrode insert 35 to the left, and the open end 19 of chamber 16 to the right. A passage 32 through the wall of hollow member 28 permits entry of electrons into the ionization region 30 from orifice 17 when hollow member 28 is to the right. A sample inlet 23 through the walls of ion chamber 16 permits entry of an ionization sample into ionization region 30' when cylinder 28 is to the left as shown in FIG. 2. Sample inlet 23, and sample inlet 20 passing through the walls of hollow member 28, permit entry of an ionization sample into ionization region 30, when hollow member 28 is to the right as shown in FIG. 1. A passage 34 permits exit of ions from the ionization region 30 to an ion lens assembly 26. Both passages 32 and 34 may have a conical configuration to improve entry of the electrons through the first passage and exit of the ions through the second passage. Passages 32 and 34, the electron entrance and ion exit passages respectively of the chemical ionization chamber, are much smaller than the respective passages 17 and 21 of the electron impact chamber. The smaller size of passages 32 and 34 permits maintaining a higher pressure in ionization region 30 than in ionization region 30'.
Magnets 52 and 52' are located adjacent to filament 18 and to an electron collector 50, respectively, which is disposed on the periphery of chamber 16 diametrically opposed to filament 18. The magnets direct an electron beam from the filament to the collector. The ion lens assembly 26, adjacent to end 19, extend away from chamber 16 and, when the appropriate potentials are applied, focuses ions emerging from ionization regions 30 and 30' into a mass filter for analysis (not shown).
A potential source 70 is connected to insert 35 by connector 38 to maintain insert 35 at a potential for repelling ions when the hollow member 28 is to the left, as shown in FIG. 2. When the hollow member 28 is to the right, connector 38 engages only insert 36 to maintain a repelling potential on this insert, which insert now becomes a repeller electrode.
When the hollow cylindrical member is to the left, the ionization source is operating in the electron impact configuration where the pressure inside ionization region 30' is about 10-6 Torr; the ionization electrons have energies of about 70 eV; and mean-free-paths of about 2×103 inches. The electrons in this configuration fragment the sample molecules and produce many ions whose mass-to-charge ratios do not necessarily correspond to the molecular weight of the sample. When the hollow cylindrical member is to the right, the ionization source is operating in the chemical ionization configuration where the pressure in ionization region 30 is up to 1.0 Torr; the ionization electrons have energies of about 100 to 500 eV; and short mean-free-paths of about 2×10-3 inches. The electrons in this configuration do not fragment the sample molecules as much as in the electron impact configuration, but produce an abundance of ions whose mass-to-charge ratio corresponds more accurately to the molecular weight of the sample.
|Cited Patent||Filing date||Publication date||Applicant||Title|
|US3115591 *||May 27, 1960||Dec 24, 1963||Atlas Werke Ag||Ion source for mass spectrometer|
|US3187179 *||Aug 30, 1962||Jun 1, 1965||Ass Elect Ind||Variable slit systems for mass spectrometer ion sources|
|US3355587 *||Mar 3, 1966||Nov 28, 1967||Ludolf Jenckel||Gas analysis apparatus comprising plural ionization chambers with different ionizing electron beam energy levels in the chambers|
|US3405263 *||Jan 14, 1966||Oct 8, 1968||Exxon Research Engineering Co||Dual mass spectrometer ion source comprising field ionization and electron bombardment sources and the method of use|
|US3553452 *||Feb 17, 1969||Jan 5, 1971||Us Air Force||Time-of-flight mass spectrometer operative at elevated ion source pressures|
|US3555272 *||Mar 14, 1968||Jan 12, 1971||Exxon Research Engineering Co||Process for chemical ionization for intended use in mass spectrometry and the like|
|US3582645 *||Nov 7, 1967||Jun 1, 1971||Varian Mat Gmbh||Combined field and impact ionization source for mass spectrometers|
|US3984692 *||Jan 4, 1972||Oct 5, 1976||Arsenault Guy P||Ionization apparatus and method for mass spectrometry|
|1||*||"A Chemical Ionization Mass Spectrometer Source" Fales et al., Rev. of Sci. Ins., vol. 42, No. 11, Nov. 1971, pp. 1578-1584.|
|2||*||"Ionization Sources in Mass Spectrometry" Chait, Anal. Chem., vol. 44, No. 3, Mar. 1972, pp. 77A-88A, 91A.|
|3||*||"Studies in Chemical Ionization Mass Spectrometry", Michnowicz et al., Organic Mass Spectrometry, 1970, vol. 4, pp. 481-492.|
|Citing Patent||Filing date||Publication date||Applicant||Title|
|US5302827 *||May 11, 1993||Apr 12, 1994||Mks Instruments, Inc.||Quadrupole mass spectrometer|
|US6646257||Sep 18, 2002||Nov 11, 2003||Agilent Technologies, Inc.||Multimode ionization source|
|US7091483||Feb 25, 2005||Aug 15, 2006||Agilent Technologies, Inc.||Apparatus and method for sensor control and feedback|
|US7488953||May 31, 2006||Feb 10, 2009||Agilent Technologies, Inc.||Multimode ionization source|
|US7791042||Nov 17, 2006||Sep 7, 2010||Thermo Finnigan Llc||Method and apparatus for selectively performing chemical ionization or electron ionization|
|US20080116369 *||Nov 17, 2006||May 22, 2008||Mccauley Edward B||Method and apparatus for selectively performing chemical ionization or electron ionization|
|U.S. Classification||250/423.00R, 250/427|