Spark source mass spectrometers and sample insertion probe therefor

Claim 2

In an ion source for a mass spectrometer the improved combination comprising: a. structure defining an evacuable ionization chamber and a cleaning station in the chamber, b. an insertion probe for introducing at least one sample to be analyzed into the ionization chamber while it is in an evacuated state; c. a valve connected to the structure and having a closed position for maintaining a vacuum in the evacuable chamber; though also having an open position for admitting the insertion probe; d. cleaning means connected to the structure and adapted to clean a sample when in the sample cleaning station; e. ionization means carried in the chamber and defining an ionization station; and, f. said probe being insertable through the valve to position a sample carried by it selectively and one at a time in the cleaning and ionization statioNs.

Claim 3

The device of claim 1 wherein the cleaning means is within the chamber.

Claim 4

The device of claim 2 wherein the cleaning means is a first electrode means which cleans the sample by etching through ion bombardment.

Claim 5

The apparatus of claim 3 wherein the first electrode means comprises an annular electrode adapted to partially surround the sample and clean the sample by ion bombardment.

Claim 6

The apparatus of claim 1 wherein the ionization means is a laser generator positioned to direct a laser beam at the sample.

Claim 7

The apparatus of claim 1 wherein the insertion probe comprises: i. a tube; ii. a rod axially movable within the tube; and, iii. at least one demountable sample holder connected at one end of the insertion probe.

Claim 8

The apparatus of claim 1 wherein the ionization means includes at least one electrode assembly including movable sample mounting means for holding the sample.

Claim 9

In a mass spectrometer of the spark source type, the combination of: a. structure defining an evacuable ionization chamber; b. an insertion probe for introducing at least one sample of material to be analyzed and a paired member into the chamber, the insertion probe including means for demountably securing such sample and paired member thereto; c. valve means connected to the structure and having a closed position for maintaining a vacuum in the evacuable chamber and an open position for admitting the insertion probe; d. electrode structure within the chamber for receiving the sample and the paired member in an analyzing position; and, e. said combination including a sample positioning means actuatable from outside of the ionization chamber for transferring the sample and the paired member from the probe to the electrode structure.

Claim 10

In a mass spectrometer of the spark source type, the combination of: a. structure defining an evacuable ionization chamber; b. an insertion probe for introducing at least one sample of material to be analyzed and a paired member into the chamber, the insertion probe including means for demountably securing such sample and paired member thereto; c. valve means connected to the structure and having a closed position for maintaining a vacuum in the evacuable chamber and an open position for admitting the insertion probe; d. electrode structure within the chamber for receiving the sample and the paired member in an analyzing position; and, e. said combination including a sample positioning means actuatable from outside of the ionization chamber for transferring the sample and the paired member from the probe to the electrode structure.

Claim 11

The apparatus of claim 8 wherein the sample positioning means is part of the insertion probe and wherein the probe comprises: i. a tube; ii. a control rod movable within the tube; iii. a sealing member disposed in the tube and connected to the control rod; iv. a plate connected to the end of the tube; v. a pair of sample holders pivotally mounted on opposite sides of the plate; vi. the sealing member including projecting elements each overlying a side of the plate for rotating the sample holders; and, vii. the rod being retractable relative to the tube to retract the projecting elements so that the sample may be removed.

Claim 12

In a mass spectrometer of the spark source type including source structure defining an evacuable ionization chamber, the improvement which comprises: a. an insertion lock connected to the source structure; b. said lock having internal surfaces defining a passageway communicating with the chamber and a valve for selectively opening and closing the passageway; c. the internal surfaces including a sealing portion, the valve being positioned between the sealing portion and the chamber; d. an insertion probe including an external sealing surface of the contour of the sealing portion and adapted for sliding movement through said sealing portion while maintaining vacuum sealing engagement therewith; e. said probe including means for carrying a sample and a paired member near one end thereof whereby to position the sample and paired member in the chamber when the probe projects through the passage; f. said valve including an opening sized to receive the probe when the probe positions the sample and paired member in the chamber; g. said probe including structure effecting a seal within the contour generated by said sealing surface whereby to prevent the admission of gases through said probe into said chamber when the probe is in the passageway; and, h. spark means associated with said chamber for establishing a spark between the sample and the paired member when the two are in the ionization chamber.

Claim 13

In a mass spectrometer of the spark source type including source structure defining an evacuable ionization chamber, the improvement which comprises: a. an insertion lock connected to the source structure; b. said lock having internal surfaces defining a passageway communicating with the chamber and a valve for selectively opening and closing the passageway; c. the internal surfaces including a sealing portion, the valve being positioned between the sealing portion and the chamber; d. an insertion probe including an external sealing surface of the contour of the sealing portion and adapted for sliding movement through said sealing portion while maintaining vacuum sealing engagement therewith; e. said probe including means for carrying a sample and a paired member near one end thereof whereby to position the sample and paired member in the chamber when the probe projects through the passage; f. said valve including an opening sized to receive the probe when the probe positions the sample and paired member in the chamber; g. said probe including structure effecting a seal within the contour generated by said sealing surface whereby to prevent the admission of gases through said probe into said chamber when the probe is in the passageway; and, h. spark means associated with said chamber for establishing a spark between the sample and the paired member when the two are in the ionization chamber.

Claim 14

The spectrometer of claim 10 wherein the paired member is a second sample.

Claim 15

The spectrometer of claim 10 wherein the paired member is a counter electrode.

Claim 16

The mass spectrometer of claim 10 wherein the spark means includes a pair of electrode members in the chamber and wherein said probe includes manipulating means for positioning each of the samples and the paired member in a different one of the electrode members.

Claim 19

The method of claim 14 wherein the step of bringing the sample into contact with an electrode and into an analyzing position includes the step of transferring the sample from the probe to the electrode structure.

Claim 20

The method of claim 15 wherein the step of transferring the sample to the electrode structure includes the step of rotating a sample holder from a position longitudinal of the insertion probe to a position transverse with respect to the axis of the insertion probe.

Claim 21

The method of claim 15 wherein the probe is partially withdrawn before a spark is established between the sample and a paired member.

Claim 22

The method of claim 14 wherein the step of cleaning the sample includes admitting a purging flow of inert gas into the chamber and thereafter reestablishing the vacuum.

Claim 23

The method of claim 18 wherein the inert gas is argon.

Claim 24

The method of claim 14 wherein the sample is cleaned with an electrode and the cleaning is accomplished by etching through ion bombardment.

Claim 25

The apparatus of claim 19 wherein the sample positioning means is part of the insertion probe and wherein the probe comprises: i. a tubular body; ii. a control element disposed within the body and movable longitudinally and rotatably relative to the body while in sealing relationship therewith; iii. said body having a central longitudinally extending member at one end thereof; iv. a sample holder mounted on said member; and, v. means on an end of the control element adapted to contact and manipulate the sample holder on movement of said control element to shift the sample holder from a position longitudinal of the probe to a position transverse of the probe.

Claim 26

The method of claim 21 wherein the electrode is an annular electrode and the sample is positioned at least partially within the annular electrode when it is cleaned.

Claim 27

In a mass spectrometers of the spark source type, the combination of: a. structure defining an evacuable ionization chamber; b. an insertion probe for introducing at least one sample of material to be analyzed into the evacuated chamber, the insertion probe including means for demountably securing such sample thereto; c. valve means connected to the structure and having a closed position for maintaining a vacuum in the evacuable chamber and an open position for admitting the insertion prove; d. electrode structure within the chamber for receiving the sample in an analyzing position; e. said combination including a sample positioning means actuable from outside of the ionization chamber for transferring the sample from the probe to the electrode structure; f. said sample positioning means including structure in the probe for maintaining a sample carried by the probe disposed substantially longitudinally of the probe during insertion and for moving the sample support to a position transverse of the probe after insertion; and, g. said sample positioning means also includes movable portions of said electrode structure adapted to transfer a sample from the probe.

Claim 28

In a mass spectrometers of the spark source type, the combination of: a. structure defining an evacuable ionization chamber; b. an insertion probe for introducing at least one sample of material to be analyzed into the evacuated chamber, the insertion probe including means for demountably securing such sample thereto; c. valve means connected to the structure and having a closed position for maintaining a vacuum in the evacuable chamber and an open position for admitting the insertion prove; d. electrode structure within the chamber for receiving the sample in an analyzing position; e. said combination including a sample positioning means actuable from outside of the ionization chamber for transferring the sample from the probe to the electrode structure; f. said sample positioning means including structure in the probe for maintaining a sample carried by the probe disposed substantially longitudinally of the probe during insertion and for moving the sample support to a position transverse of the probe after insertion; and, g. said sample positioning means also includes movable portions of said electrode structure adapted to transfer a sample from the probe.

Claim 29

The combinatioN of claim 23 wherein the sample support is moved from its longitudinal to its transverse position by rotation of the sample support member.

Claim 32

In a mass spectrometer, the improved combination comprising: a. structure establishing an evacuable chamber and a sample insertion passage communicating with the chamber; b. ionization means establishing a sample ionization stain within the chamber and including means to ionize a sample positioned at the ionization station; c. valve means connected to the structure for selectively closing said passage to maintain a vacuum within the space; d. said structure establishing a path of sample travel from external of said structure through said valve means to said ionization station; e. an insertion probe adapted to transport a sample from a position external of said structure along said path to said ionization station; and, f. cleaning means along said path and within said chamber for cleaning a sample within said chamber after it has been moved along said path past said valve means by the insertion probe.

Claim 33

In a mass spectrometer, the improved combination comprising: a. structure establishing an evacuable chamber and a sample insertion passage communicating with the chamber; b. ionization means establishing a sample ionization stain within the chamber and including means to ionize a sample positioned at the ionization station; c. valve means connected to the structure for selectively closing said passage to maintain a vacuum within the space; d. said structure establishing a path of sample travel from external of said structure through said valve means to said ionization station; e. an insertion probe adapted to transport a sample from a position external of said structure along said path to said ionization station; and, f. cleaning means along said path and within said chamber for cleaning a sample within said chamber after it has been moved along said path past said valve means by the insertion probe.

Claim 34

The mass spectrometer of claim 26 wherein said cleaning means establishes a cleaning station between the valve means and the ionization station.

Claim 35

The combination of claim 26 wherein said cleaning means includes means to admit a purging flow of gas after a sample has been cleaned.

Claim 36

The combination of claim 26 wherein the cleaning means includes an electrode adapted to clean a sample by ion bombardment.

Claim 37

The device of claim 29 wherein the electrode is an annular electrode adapted to partially surround the sample and clean the sample by ion bombardment.

Claim 40

The method of claim 31 including the step of transferring the sample and paired member from the probe to electrode structures within the evacuated chamber prior to establishing a spark.

Claim 41

The method of claim 31 wherein the paired member is a second sample.

Claim 42

An insertion probe comprising: a. a tube; b. a control rod movable within the tube; c. a sealing member disposed in the tube and connected to the control rod; d. a plate connected to the end of the tube; e. a pair of sample holders pivotally mounted on opposite sides of the plate; f. the sealing member including projecting elements each overlaying a side of the plate for rotating the sample holders; and g. the rod being retractable relative to the tube to retract the projecting elements so that the sample may be removed.

Claim 43

An insertion probe comprising: a. a tube; b. a control rod movable within the tube; c. a sealing member disposed in the tube and connected to the control rod; d. a plate connected to the end of the tube; e. a pair of sample holders pivotally mounted on opposite sides of the plate; f. the sealing member including projecting elements each overlaying a side of the plate for rotating the sample holders; and g. the rod being retractable relative to the tube to retract the projecting elements so that the sample may be removed.

Claim 44

An insertion probe comprising: a. a tubular body; b. a control element disposed within the body and movable longitudinally and rotatably relative to the body while in sealing relationship therewith; c. said body having a central longitudinally extending member at onE end thereof; d. a sample holder mounted on said member; and, e. means on an end of the control element adapted to contact and manipulate the sample holder on movement of said control element to shift the sample holder from a position longitudinal of the probe to a position transverse of the probe.

Claim 45

An insertion probe comprising: a. a tubular body; b. a control element disposed within the body and movable longitudinally and rotatably relative to the body while in sealing relationship therewith; c. said body having a central longitudinally extending member at onE end thereof; d. a sample holder mounted on said member; and, e. means on an end of the control element adapted to contact and manipulate the sample holder on movement of said control element to shift the sample holder from a position longitudinal of the probe to a position transverse of the probe.