WO2006123156A2 - Mass spectrometer apparatus - Google Patents

Mass spectrometer apparatus Download PDF

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Publication number
WO2006123156A2
WO2006123156A2 PCT/GB2006/001833 GB2006001833W WO2006123156A2 WO 2006123156 A2 WO2006123156 A2 WO 2006123156A2 GB 2006001833 W GB2006001833 W GB 2006001833W WO 2006123156 A2 WO2006123156 A2 WO 2006123156A2
Authority
WO
WIPO (PCT)
Prior art keywords
compounds
calibration
mixture
ionisation
mixture according
Prior art date
Application number
PCT/GB2006/001833
Other languages
French (fr)
Other versions
WO2006123156A3 (en
Inventor
John George Luke
Richard Sleeman
James Francis Carter
Original Assignee
Mass Spec Analytical 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 Mass Spec Analytical Ltd filed Critical Mass Spec Analytical Ltd
Publication of WO2006123156A2 publication Critical patent/WO2006123156A2/en
Publication of WO2006123156A3 publication Critical patent/WO2006123156A3/en

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/0009—Calibration of the apparatus
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
    • H01J49/0459—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for solid samples
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
    • H01J49/0468—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components with means for heating or cooling the sample
    • H01J49/049—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components with means for heating or cooling the sample with means for applying heat to desorb the sample; Evaporation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/10—Ion sources; Ion guns
    • H01J49/14—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers
    • H01J49/145—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers using chemical ionisation

Definitions

  • This invention relates to mass spectrometer apparatus or to other analytical apparatus whose operation involves atmospheric pressure ionisation of a test sample introduced by thermal desorption, and provides an improved means for the calibration of such apparatus.
  • Mass spectrometry is a known analytical technique which may for example be used to detect trace quantities of harmful or prohibited substances.
  • Samples for test may be subject to thermal activation but, before use on a test sample of unknown composition, the apparatus requires calibration using a range of compounds of known, but different, molecular weights, to ensure that reliable identification information is produced on analysis of a test compound which may, for example, be a suspect narcotic or explosive compound carried on a person's skin or clothing or hi baggage.
  • An objection of the present invention is to provide means for the automated calibration of thermal activation mass spectrometer apparatus or other atmospheric pressure ionisation analytical apparatus.
  • the invention provides a method for the calibration of atmospheric pressure ionisation analytical apparatus including means for ionising a gaseous test sample, the method comprising supplying to the ionising means a mixture of ionizable calibration compounds in solid form, the compounds having respective ionized species of known different molecular weights.
  • the ionisation is chemical ionisation and the apparatus includes means for heating the test sample, the calibration compounds being volatile hi the heating means.
  • the calibration compounds evaporate in the temperature of the heating means and are passed to the transfer conduit through the apparatus, where they are subject to ionization and analysis, for example by measurement of the apparent molecular weights of the ionized species. The apparent molecular weights or other analysis data are then compared with the known values for the compounds concerned, any adjustment necessary then being carried out to calibrate the apparatus accurately.
  • the invention provides a mixture of ionizable calibration compounds in solid form for use in calibration of desorption analytical apparatus, the compounds being volatile and having respective species when ionized of known different molecular weights.
  • volatile capable of evaporation under the temperature regime of the heating means to render them suitable for ionization and analysis, for example by molecular weight determination of the resulting ionized species.
  • the temperature regime of the heating means will depend on the nature of the target compound, that is, the compound being investigated, but typically will be in the range 100-300 0 C.
  • the mixture of calibration compounds may be provided adsorbed or dispersed on a carrier and contained in a housing for location within the heating means and including an exit port for gaseous compounds in communication with the transfer conduit.
  • the housing may comprise a suitable robust tube formed for example from stainless steel and may be lined with glass or other suitable material.
  • the carrier preferably comprises an extended surface area material which is stable under the ambient temperate conditions produced by the heating means and chemically inert to the compounds.
  • Suitable carrier materials comprise vitreous, for example, glass beads, ceramic materials, for example alumina, silica or aluminosilicates, and carbonaceous materials such as graphitised carbon. Such materials may be used alone or in combination.
  • the materials are preferably in particulate form or are otherwise loosely-packed to define pathways therethrough for passage of gaseous or volatilised compounds and may be held in place in the housing by means of porous, for example quartz wool or metal mesh, end plugs.
  • the materials may comprise a unitary block or body of material, such as a ceramic or metallic honeycomb material, defining passageways therethrough.
  • the materials may themselves carry a surface layer uprising a higher surface-area material such as a particular form of alumina, on which the mixture of compounds is adsorbed.
  • the invention provides a container for calibration compounds (as hereinbefore described), the container comprising a housing including an exit port for communicating, in use, with the transfer conduit of thermal activation analytical apparatus, the housing containing a carrier material for supporting the calibration compounds.
  • the calibration compounds should be thermally stable subject to being volatile at the required operating temperatures, available in high purity, capable of ionization and stable on storage for at least six months, preferably for a year or more.
  • the different molecular weights of the ionized species should preferably be incrementally different to cover the detection range of the apparatus or, at least, the range of interest with reference to the target compounds, but nevertheless the molecular weight species should be identifiably different from those of the target compounds, to avoid any possibility of false positive results arising from the residual presence of calibration compounds.
  • each compound should exhibit not only intrinsic stability in the presence of air but also inertness with respect to the other compounds and carrier materials.
  • the calibration compounds are required to be present in an amount to maintain a supply of volatilised compound to the ionizing means of only a few nanograms per second over a time span of, typically, from two to ten minutes.
  • the calibration compounds When the calibration compounds are exhausted from the carrier material, they may be re-charged.
  • the calibration compounds preferably comprise a mixture of esters and/or diesters.
  • the acids forming the esters preferably comprise saturated fatty acids having a carbon chain length of between two and twenty.
  • the alcohol moiety preferably has a carbon chain length of up to twenty and is preferably also saturated, to inhibit reactivity.
  • the molecular weights typically vary from about 120 (for example, methyl hexanoate has a molecular weight of 130) to about 500 (for example, hexadecyl has a molecular weight of 480) and the calibration masses are one mass unit higher, where ionization yields the protonated species.
  • a mixture of calibration compounds comprise an equimolar mixture of the following esters having molecular weights as indicated:
  • a mixture of perfiuorocarbons also known as perfiuorokerosene or PFK
  • PFK perfiuorokerosene
  • Figure 1 is a diagrammatic end view of apparatus according to the invention including a holder for calibration compounds;
  • Figure IA is a fragmentary view of the holder as shown in Figure 1;
  • Figure 2 is a side view of the thermal activation and ionization parts of a mass spectrometry instrument, incorporating the apparatus shown in Figure 1.
  • the apparatus includes upper and lower heated blocks (11, 12) defining between them a transfer line or conduit (13) for passage of calibration and test the ionization means and further through the mass spectrometer.
  • a housing (14) is secured with bolts (15) in thermal contact with the upper block (11); the housing (14) incorporates a cavity (16) for receiving a glass-lined stainless steel tube (17) containing a mixture of calibration compounds absorbed on glass beads (18) held in place by quartz wool plugs (19, 20) at each end.
  • the outer end of the tube (17) carries a sealing end closure (21), made from PTFE 5 which also acts as an insulating handle.
  • the other end of the tube (17) carries a removable end closure (22) which seals that end and prevents ingress of contaminants.
  • the inner end of the chamber or cavity (16) in the housing (14) has an extension passageway (23) in communication with a further passageway (24) formed in upper block (11), itself in communication with the transfer line (13).
  • the upper and lower blocks (11, 12) carry respective cartridge heaters (25, 26); the upper block (11) also carries a thermocouple (27).
  • the upper block (11) also carries an injection port (28) for the transfer line (13). Downstream of the junction of passageway (24) with transfer line (13), the transfer line is attached to the mass spectrometry instrument via ceramic insulators (29) and is connected to brass tube (30) and thence, through a filter (31), to a ceramic tube (32) which passes the compounds to an ionizer needle assembly (33).
  • the calibration compounds contained in tube (17) are heated and evaporated by virtue of the thermal contact between hot block (11) and housing (14) and pass through passageways (23, 24) into transfer line (13), where they are subject to ionization by needle assembly (33) and subsequent molecular weight determination.
  • a gaseous test sample may be introduced in through injection port (28) and itself thermally volatilised between the hot blocks (11, 12), and subsequently ionized and analysed.

Abstract

A method for the calibration of atmospheric pressure ionisation analytical apparatus including means for ionising a gaseous test sample comprises supplying to the ionising means a mixture of ionizable calibration compounds in solid form, the compounds having respective ionized species of known different molecular weights. The ionisation may be chemical ionisation, the apparatus including means for heating the test sample, the calibration compounds being volatile in the heating means. The invention includes a mixture of ionizable calibration compounds in solid form for use in calibration of desorption analytical apparatus, the compounds being volatile and having respective species when ionized of known different molecular weights.

Description

Mass Spectrometer Apparatus
This invention relates to mass spectrometer apparatus or to other analytical apparatus whose operation involves atmospheric pressure ionisation of a test sample introduced by thermal desorption, and provides an improved means for the calibration of such apparatus.
Mass spectrometry is a known analytical technique which may for example be used to detect trace quantities of harmful or prohibited substances. Samples for test may be subject to thermal activation but, before use on a test sample of unknown composition, the apparatus requires calibration using a range of compounds of known, but different, molecular weights, to ensure that reliable identification information is produced on analysis of a test compound which may, for example, be a suspect narcotic or explosive compound carried on a person's skin or clothing or hi baggage.
Conventionally, for calibration purposes, compounds of known molecular weight and having other properties which render them suitable for calibration, such as inertness and stability, are introduced to the apparatus as solutions, for example as ion sprays. The procedure is, however, necessarily requiring of manual operation and hence is inconvenient and time-consuming.
An objection of the present invention is to provide means for the automated calibration of thermal activation mass spectrometer apparatus or other atmospheric pressure ionisation analytical apparatus.
In one aspect, the invention provides a method for the calibration of atmospheric pressure ionisation analytical apparatus including means for ionising a gaseous test sample, the method comprising supplying to the ionising means a mixture of ionizable calibration compounds in solid form, the compounds having respective ionized species of known different molecular weights.
Typically, the ionisation is chemical ionisation and the apparatus includes means for heating the test sample, the calibration compounds being volatile hi the heating means. In use, the calibration compounds evaporate in the temperature of the heating means and are passed to the transfer conduit through the apparatus, where they are subject to ionization and analysis, for example by measurement of the apparent molecular weights of the ionized species. The apparent molecular weights or other analysis data are then compared with the known values for the compounds concerned, any adjustment necessary then being carried out to calibrate the apparatus accurately.
In another aspect, the invention provides a mixture of ionizable calibration compounds in solid form for use in calibration of desorption analytical apparatus, the compounds being volatile and having respective species when ionized of known different molecular weights.
By "volatile" is meant capable of evaporation under the temperature regime of the heating means to render them suitable for ionization and analysis, for example by molecular weight determination of the resulting ionized species. The temperature regime of the heating means will depend on the nature of the target compound, that is, the compound being investigated, but typically will be in the range 100-3000C. The mixture of calibration compounds may be provided adsorbed or dispersed on a carrier and contained in a housing for location within the heating means and including an exit port for gaseous compounds in communication with the transfer conduit. The housing may comprise a suitable robust tube formed for example from stainless steel and may be lined with glass or other suitable material. The carrier preferably comprises an extended surface area material which is stable under the ambient temperate conditions produced by the heating means and chemically inert to the compounds. Suitable carrier materials comprise vitreous, for example, glass beads, ceramic materials, for example alumina, silica or aluminosilicates, and carbonaceous materials such as graphitised carbon. Such materials may be used alone or in combination. The materials are preferably in particulate form or are otherwise loosely-packed to define pathways therethrough for passage of gaseous or volatilised compounds and may be held in place in the housing by means of porous, for example quartz wool or metal mesh, end plugs. However, the materials may comprise a unitary block or body of material, such as a ceramic or metallic honeycomb material, defining passageways therethrough. Optionally, the materials may themselves carry a surface layer uprising a higher surface-area material such as a particular form of alumina, on which the mixture of compounds is adsorbed.
In another aspect, the invention provides a container for calibration compounds (as hereinbefore described), the container comprising a housing including an exit port for communicating, in use, with the transfer conduit of thermal activation analytical apparatus, the housing containing a carrier material for supporting the calibration compounds.
The calibration compounds should be thermally stable subject to being volatile at the required operating temperatures, available in high purity, capable of ionization and stable on storage for at least six months, preferably for a year or more. The different molecular weights of the ionized species should preferably be incrementally different to cover the detection range of the apparatus or, at least, the range of interest with reference to the target compounds, but nevertheless the molecular weight species should be identifiably different from those of the target compounds, to avoid any possibility of false positive results arising from the residual presence of calibration compounds.
The requirement for stability, both at ordinary ambient temperatures during storage and also at the operating temperatures, means that each compound should exhibit not only intrinsic stability in the presence of air but also inertness with respect to the other compounds and carrier materials.
The calibration compounds are required to be present in an amount to maintain a supply of volatilised compound to the ionizing means of only a few nanograms per second over a time span of, typically, from two to ten minutes. When the calibration compounds are exhausted from the carrier material, they may be re-charged.
We have found that the calibration compounds preferably comprise a mixture of esters and/or diesters. The acids forming the esters preferably comprise saturated fatty acids having a carbon chain length of between two and twenty. The alcohol moiety preferably has a carbon chain length of up to twenty and is preferably also saturated, to inhibit reactivity. The molecular weights typically vary from about 120 (for example, methyl hexanoate has a molecular weight of 130) to about 500 (for example, hexadecyl has a molecular weight of 480) and the calibration masses are one mass unit higher, where ionization yields the protonated species.
By way of example, a mixture of calibration compounds comprise an equimolar mixture of the following esters having molecular weights as indicated:
methyl hexanoate - 130 butyl hexanoate - 172 ethyl dodecanoate - 200 diethyl adipate - 202 octyl octanoate - 256 methyl octadecanoate - 298 bis(ethylhexyl) adipate - 370 tetradecyl dodecanoate - 396 bis(butylpentyl) adipate - 398 hexadecyl hexadecanoate - 480
If the atmospheric pressure ionisation analytical apparatus is configured to detect negatively charged ions, a mixture of perfiuorocarbons (also known as perfiuorokerosene or PFK) will be incorporated into the calibration compounds to provide a range of negatively charged ions having a molecular weight range similar to that of those esters listed above, the calibration masses being the same as those of the molecules.
Embodiments of the invention will now be described by way of example with reference to the accompanying drawings, of which:
Figure 1 is a diagrammatic end view of apparatus according to the invention including a holder for calibration compounds;
Figure IA is a fragmentary view of the holder as shown in Figure 1; and
Figure 2 is a side view of the thermal activation and ionization parts of a mass spectrometry instrument, incorporating the apparatus shown in Figure 1.
Referring firstly to Figure 1, the apparatus includes upper and lower heated blocks (11, 12) defining between them a transfer line or conduit (13) for passage of calibration and test the ionization means and further through the mass spectrometer. A housing (14) is secured with bolts (15) in thermal contact with the upper block (11); the housing (14) incorporates a cavity (16) for receiving a glass-lined stainless steel tube (17) containing a mixture of calibration compounds absorbed on glass beads (18) held in place by quartz wool plugs (19, 20) at each end. The outer end of the tube (17) carries a sealing end closure (21), made from PTFE5 which also acts as an insulating handle. As shown in Figure IA, for storage purposes the other end of the tube (17) carries a removable end closure (22) which seals that end and prevents ingress of contaminants.
The inner end of the chamber or cavity (16) in the housing (14) has an extension passageway (23) in communication with a further passageway (24) formed in upper block (11), itself in communication with the transfer line (13).
Turning now to Figure 2, the upper and lower blocks (11, 12) carry respective cartridge heaters (25, 26); the upper block (11) also carries a thermocouple (27). The upper block (11) also carries an injection port (28) for the transfer line (13). Downstream of the junction of passageway (24) with transfer line (13), the transfer line is attached to the mass spectrometry instrument via ceramic insulators (29) and is connected to brass tube (30) and thence, through a filter (31), to a ceramic tube (32) which passes the compounds to an ionizer needle assembly (33).
In use, the calibration compounds contained in tube (17) are heated and evaporated by virtue of the thermal contact between hot block (11) and housing (14) and pass through passageways (23, 24) into transfer line (13), where they are subject to ionization by needle assembly (33) and subsequent molecular weight determination. Once calibration of the apparatus is complete, a gaseous test sample may be introduced in through injection port (28) and itself thermally volatilised between the hot blocks (11, 12), and subsequently ionized and analysed.

Claims

Claims
1. A method for the calibration of atmospheric pressure ionisation analytical apparatus including means for ionising a gaseous test sample, the method comprising supplying to the ionising means a mixture of ionizable calibration compounds in solid form, the compounds having respective ionized species of known different molecular weights.
2. A method according to claim 1, in which the ionisation is chemical ionisation and the apparatus includes means for heating the test sample, the calibration compounds being volatile at temperatures generated by the heating means.
3. A method according to claim 2, in which the heating means is capable of heating the sample to a temperature in the range 100 to 3000C.
4. A mixture of ionizable calibration compounds in solid form for use in calibration of desorption analytical apparatus including transfer means for passage of gaseous calibration compounds, the compounds being volatile and having respective species when ionized of known different molecular weights.
5. A mixture according to claim 4, in which the compounds are adsorbed or dispersed on a carrier and contained in a housing for location within the heating means and including an exit port for gaseous compounds in communication with the transfer means.
6. A mixture according to claim 5, in which the carrier comprises a vitreous, ceramic, and/or carbonaceous material.
7. A mixture according to any of claims 4 to 6, comprising a mixture of esters and/or diesters.
8. A mixture according to claim 7, in which the acids forming the esters comprise saturated fatty acids having a carbon chain length of between two and twenty.
9. A mixture according to claim 7 or claim 8, in which the alcohol moiety of the ester has a carbon chain length of up to twenty and is preferably also saturated.
10. A mixture according to any of claims 7 to 9, in which the molecular weights of the esters and/or diesters vary from about 120 to about 500.
11. A mixture according to any of claims 4 to 10, in which the compounds yield protonated species on ionisation.
12. A mixture according to any of claims 4 to 10, in which a mixture of perfluorocarbons is incorporated with the calibration compounds to provide on ionisation a range of negatively charged ions.
13. A container for a mixture of compounds as claimed in any of claims 4 to 12, the container comprising a housing including an exit port for communicating, in use, with the transfer means of thermal activation analytical apparatus, the housing containing a carrier material for supporting the calibration compounds.
14. Atmospheric pressure ionisation analytical apparatus including means for receiving a mixture of ionizable calibration compounds in solid form, means for ionising said compounds and means for molecular weight determination of ionised species of said compounds in order to calibrate said apparatus for analysis of a test compound.
PCT/GB2006/001833 2005-05-18 2006-05-18 Mass spectrometer apparatus WO2006123156A2 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB0510171A GB0510171D0 (en) 2005-05-18 2005-05-18 Mass spectrometer apparatus
GB0510171.2 2005-05-18

Publications (2)

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WO2006123156A2 true WO2006123156A2 (en) 2006-11-23
WO2006123156A3 WO2006123156A3 (en) 2007-04-26

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4224031A (en) * 1977-11-15 1980-09-23 Mee John M L CI Mass spectrometric analysis of physiologically active compounds
US6207954B1 (en) * 1997-09-12 2001-03-27 Analytica Of Branford, Inc. Multiple sample introduction mass spectrometry
WO2003075772A2 (en) * 2002-03-11 2003-09-18 Pawliszyn Janusz B Micro-devices and analytical procedures for investigation of biological systems

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4224031A (en) * 1977-11-15 1980-09-23 Mee John M L CI Mass spectrometric analysis of physiologically active compounds
US6207954B1 (en) * 1997-09-12 2001-03-27 Analytica Of Branford, Inc. Multiple sample introduction mass spectrometry
WO2003075772A2 (en) * 2002-03-11 2003-09-18 Pawliszyn Janusz B Micro-devices and analytical procedures for investigation of biological systems

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
BECKER J S ET AL: "State-of-the-art in inorganic mass spectrometry for analysis of high-purity materials" INTERNATIONAL JOURNAL OF MASS SPECTROMETRY, ELSEVIER SCIENCE PUBLISHERS, AMSTERDAM, NL, vol. 228, no. 2-3, 15 August 2003 (2003-08-15), pages 127-150, XP004442599 ISSN: 1387-3806 *
LORD H ET AL: "Evolution of solid-phase microextraction technology" JOURNAL OF CHROMATOGRAPHY, ELSEVIER SCIENCE PUBLISHERS B.V. AMSTERDAM, NL, vol. 885, no. 1-2, July 2000 (2000-07), pages 153-193, XP004206006 ISSN: 0021-9673 *
PRZYK E ET AL: "Use of porous glass and silica gel as support media of a surface compound for generation of analytes in gaseous standard mixtures. New method for the determination of the amount of analyte generated" JOURNAL OF CHROMATOGRAPHY A, ELSEVIER, AMSTERDAM, NL, vol. 928, no. 1, 31 August 2001 (2001-08-31), pages 99-108, XP004302029 ISSN: 0021-9673 *
ROBERTS D J ET AL: "APPLICATION OF TANDEM MASS SPECTROMETRY TO THE DETECTION OF DRUGS ON CASH" SPECTROSCOPY EUROPE, WEINHEIM, DE, vol. 9, no. 6, 1997, pages 20,22-24, XP008073637 ISSN: 0966-0941 *
ZHOUYAO ZHANG ET AL: "SOLID-PHASE MICROEXTRACTION" ANALYTICAL CHEMISTRY, AMERICAN CHEMICAL SOCIETY. COLUMBUS, US, vol. 66, no. 17, 1 September 1994 (1994-09-01), pages 844A-853A, XP000466960 ISSN: 0003-2700 *

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GB0510171D0 (en) 2005-06-22
WO2006123156A3 (en) 2007-04-26

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