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GB2157485A - A method of mass spectrometer analysis - Google Patents
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GB2157485A - A method of mass spectrometer analysis - Google Patents

A method of mass spectrometer analysis Download PDF

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Publication number
GB2157485A
GB2157485A GB08431285A GB8431285A GB2157485A GB 2157485 A GB2157485 A GB 2157485A GB 08431285 A GB08431285 A GB 08431285A GB 8431285 A GB8431285 A GB 8431285A GB 2157485 A GB2157485 A GB 2157485A
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GB
United Kingdom
Prior art keywords
sputtered
specimen
electrons
ofthe
bombarding
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
GB08431285A
Other versions
GB8431285D0 (en
Inventor
Joseph Franks
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ion Tech Ltd
Original Assignee
Ion Tech Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ion Tech Ltd filed Critical Ion Tech Ltd
Publication of GB8431285D0 publication Critical patent/GB8431285D0/en
Publication of GB2157485A publication Critical patent/GB2157485A/en
Withdrawn legal-status Critical Current

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Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/10Ion sources; Ion guns
    • H01J49/14Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

In order to increase the sensitivity of mass spectrometer analysis, the generation of ions to be analysed is increased by ionising those particles sputtered from the specimen in an uncharged state. This can be done by bombarding the sputtered material in the gaseous state with electrons, which may be excited secondary electrons, produced for example by bombardment of the specimen with neutral particles, or chemical ionisation methods can be used. The sensitivity can also be increased by making a solution of the material to be analysed and increasing the diffusion rate of the material to the surface of the solution, for example by ultrasonic agitation or electric fields.

Description

SPECIFICATION A method of mass spectrometer analysis The analysis of material by mass spectrometry depends on the production of free ionic species ofthe material under examination. Various methods have been developed to ionize specimens such as electron bombardment of evaporated material, chemical ionization and field desorption. Classes of materials exist which are difficultto analyse by these techniques such as refractories and thermally labile materials including many organic compounds.
Many of such difficult materials have been analysed using a FAB (fast atom bombardment) source (seeM.
Barber, R. S. Bordoli, R. D. Sedgwick & A. N. Tyler, J.
Chem. Soc., Chem. Commun., 325(1981), and D. J.
Surman,J. C. Vickerman Ibid 324(1981)), in which a suitably prepared specimen is bombarded with fast atoms e.g., of argon orxenon.
Sputtered molecules and fragments may be found to be positively or negatively charged and, therefore, capable of being detected and mass analysed. The method is often successful with polar compounds but structurally informative ions have not been obtained with non polar hydrocarbons (seeD. H. Williams, C.
Bradley, G. Bojesen, S. Santikarn & L. C. E. Taylor, J.
Am. Chem. Soc. 103,5700(1981).
It is proposed that the sensitivity ofthe FAB method may be improved by ionizing the sputtered material in the gaseous state. One method isto sputterthe specimen using e.g., a neutral saddle field source and bombarding the sputtered material with electrons.
Another method is to apply a RFfield to the specimen probe to excite secondary electrons produced during neutral bombardment. The unexcited secondary electrons have energies generally in the range 0-5eV, which are insufficientto cause any appreciable ionization on coliision with the sputtered material.
Excitation ofthe electrons by RFwill supply sufficient energyfor electrons to ionize the sputtered material.
Of course, combinations ofvarious ionizing methods may be used such as chemical ionization. By introducing a suitable reactive gas in the FAB source with or without an inert gas, chemical ionization is promoted, i.e., by proton exchange.
The sensitivity can also be increased by increasing the rate of diffusion ofthe material to the surface where it will be sputtered. For example, to analyse many ofthe organic materials it has been found necessaryto disscolve them in a suitable liquid such as glycerol. The material to be analysed diffuses to the surface, is sputtered and replaced by fresh material from the interior. The sensitivity reaches a limit when the sputtering rate equals the rate of surface replenishment by diffusion. The sensitivity may been hanced therefore by increasing the diffusion rate for example by ultrasonic agitation ofthe specimen or by applying an electronicfield across the specimen.
1. A method of mass spectroscopy comprising bombarding a specimen with pa rticles to produce sputtered material, ionising the sputtered material in the gaseous state and analysing the ions.
2. A method as claimed in claim 1 comprising ionising the sputtered material by bombarding with electrons.
3. A method as claimed in claim 2 wherein said electrons are secondary electrons excited by the application of an RFfield.
4. A method as claimed in claim 3 wherein the secondary electrons are produced by bombarding the specimen with neutral particles.
5. A method as claimed in anyone of claims 1 to 4 comprising ionising by chemical methods.
6. A method of mass spectroscopy comprising dissolving material to be analysed in a solvent, bombarding the solution with particles to produce ions, analysing the ions, and enhancing the rate of diffusion of the material to the surface of the solution.
7. A method as claimed in claim 6 comprising enhancing the diffusion rate by ultrasonic agitation.
8. A method as claimed in claim 6 comprising enhancing the diffusion rate by applying an electric field across the solution.
9. A method of mass spectroscopy as claimed in claim 1 or claim 6 substantially as herein described.
**WARNING** end of DESC field may overlap start of CLMS **.

Claims (9)

**WARNING** start of CLMS field may overlap end of DESC **. SPECIFICATION A method of mass spectrometer analysis The analysis of material by mass spectrometry depends on the production of free ionic species ofthe material under examination. Various methods have been developed to ionize specimens such as electron bombardment of evaporated material, chemical ionization and field desorption. Classes of materials exist which are difficultto analyse by these techniques such as refractories and thermally labile materials including many organic compounds. Many of such difficult materials have been analysed using a FAB (fast atom bombardment) source (seeM. Barber, R. S. Bordoli, R. D. Sedgwick & A. N. Tyler, J. Chem. Soc., Chem. Commun., 325(1981), and D. J. Surman,J. C. Vickerman Ibid 324(1981)), in which a suitably prepared specimen is bombarded with fast atoms e.g., of argon orxenon. Sputtered molecules and fragments may be found to be positively or negatively charged and, therefore, capable of being detected and mass analysed. The method is often successful with polar compounds but structurally informative ions have not been obtained with non polar hydrocarbons (seeD. H. Williams, C. Bradley, G. Bojesen, S. Santikarn & L. C. E. Taylor, J. Am. Chem. Soc. 103,5700(1981). It is proposed that the sensitivity ofthe FAB method may be improved by ionizing the sputtered material in the gaseous state. One method isto sputterthe specimen using e.g., a neutral saddle field source and bombarding the sputtered material with electrons. Another method is to apply a RFfield to the specimen probe to excite secondary electrons produced during neutral bombardment. The unexcited secondary electrons have energies generally in the range 0-5eV, which are insufficientto cause any appreciable ionization on coliision with the sputtered material. Excitation ofthe electrons by RFwill supply sufficient energyfor electrons to ionize the sputtered material. Of course, combinations ofvarious ionizing methods may be used such as chemical ionization. By introducing a suitable reactive gas in the FAB source with or without an inert gas, chemical ionization is promoted, i.e., by proton exchange. The sensitivity can also be increased by increasing the rate of diffusion ofthe material to the surface where it will be sputtered. For example, to analyse many ofthe organic materials it has been found necessaryto disscolve them in a suitable liquid such as glycerol. The material to be analysed diffuses to the surface, is sputtered and replaced by fresh material from the interior. The sensitivity reaches a limit when the sputtering rate equals the rate of surface replenishment by diffusion. The sensitivity may been hanced therefore by increasing the diffusion rate for example by ultrasonic agitation ofthe specimen or by applying an electronicfield across the specimen. CLAIMS
1. A method of mass spectroscopy comprising bombarding a specimen with pa rticles to produce sputtered material, ionising the sputtered material in the gaseous state and analysing the ions.
2. A method as claimed in claim 1 comprising ionising the sputtered material by bombarding with electrons.
3. A method as claimed in claim 2 wherein said electrons are secondary electrons excited by the application of an RFfield.
4. A method as claimed in claim 3 wherein the secondary electrons are produced by bombarding the specimen with neutral particles.
5. A method as claimed in anyone of claims 1 to 4 comprising ionising by chemical methods.
6. A method of mass spectroscopy comprising dissolving material to be analysed in a solvent, bombarding the solution with particles to produce ions, analysing the ions, and enhancing the rate of diffusion of the material to the surface of the solution.
7. A method as claimed in claim 6 comprising enhancing the diffusion rate by ultrasonic agitation.
8. A method as claimed in claim 6 comprising enhancing the diffusion rate by applying an electric field across the solution.
9. A method of mass spectroscopy as claimed in claim 1 or claim 6 substantially as herein described.
GB08431285A 1984-03-28 1984-12-12 A method of mass spectrometer analysis Withdrawn GB2157485A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB848408043A GB8408043D0 (en) 1984-03-28 1984-03-28 Mass spectrometer analysis

Publications (2)

Publication Number Publication Date
GB8431285D0 GB8431285D0 (en) 1985-01-23
GB2157485A true GB2157485A (en) 1985-10-23

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Family Applications (2)

Application Number Title Priority Date Filing Date
GB848408043A Pending GB8408043D0 (en) 1984-03-28 1984-03-28 Mass spectrometer analysis
GB08431285A Withdrawn GB2157485A (en) 1984-03-28 1984-12-12 A method of mass spectrometer analysis

Family Applications Before (1)

Application Number Title Priority Date Filing Date
GB848408043A Pending GB8408043D0 (en) 1984-03-28 1984-03-28 Mass spectrometer analysis

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GB (2) GB8408043D0 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2239985A (en) * 1989-12-21 1991-07-17 Vg Instr Group Method and apparatus for surface analysis

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1210218A (en) * 1967-02-08 1970-10-28 Ass Elect Ind Improvements relating to ion probe target analysis
US3984692A (en) * 1972-01-04 1976-10-05 Arsenault Guy P Ionization apparatus and method for mass spectrometry
GB1463795A (en) * 1974-06-28 1977-02-09 Anvar Local surface analysis

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1210218A (en) * 1967-02-08 1970-10-28 Ass Elect Ind Improvements relating to ion probe target analysis
US3984692A (en) * 1972-01-04 1976-10-05 Arsenault Guy P Ionization apparatus and method for mass spectrometry
GB1463795A (en) * 1974-06-28 1977-02-09 Anvar Local surface analysis

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2239985A (en) * 1989-12-21 1991-07-17 Vg Instr Group Method and apparatus for surface analysis
US5146088A (en) * 1989-12-21 1992-09-08 Vg Instruments Group Limited Method and apparatus for surface analysis

Also Published As

Publication number Publication date
GB8408043D0 (en) 1984-05-10
GB8431285D0 (en) 1985-01-23

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WAP Application withdrawn, taken to be withdrawn or refused ** after publication under section 16(1)