EP0169469A2 - Analysegerät - Google Patents

Analysegerät Download PDF

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Publication number
EP0169469A2
EP0169469A2 EP85108792A EP85108792A EP0169469A2 EP 0169469 A2 EP0169469 A2 EP 0169469A2 EP 85108792 A EP85108792 A EP 85108792A EP 85108792 A EP85108792 A EP 85108792A EP 0169469 A2 EP0169469 A2 EP 0169469A2
Authority
EP
European Patent Office
Prior art keywords
mass spectrometer
inlet
sample
conduit
pressure
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Withdrawn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
EP85108792A
Other languages
English (en)
French (fr)
Other versions
EP0169469A3 (de
Inventor
Russel David Ring
Roger Bourg Iii
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.)
BASF Corp
Original Assignee
BASF Wyandotte Corp
BASF Corp
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 BASF Wyandotte Corp, BASF Corp filed Critical BASF Wyandotte Corp
Publication of EP0169469A2 publication Critical patent/EP0169469A2/de
Publication of EP0169469A3 publication Critical patent/EP0169469A3/de
Withdrawn legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—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
    • H01J49/0431—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for liquid samples
    • H01J49/044—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for liquid samples with means for preventing droplets from entering the analyzer; Desolvation of droplets

Definitions

  • This invention relates to a method and apparatus for use in the analysis of gases and vaporized substances by means of a mass spectrometer.
  • the mass spectrometer is a well known apparatus for on-line analysis and control of processing equipment in the chemical and other process industries. Such an apparatus is described in U. S. Patent 3,648,047.
  • the samples from the processing equipment may be taken from multiple points or locations employing a flow-by- inlet system. Flow within the sample system is established by a pressure head in the process and the unused portion of the sample may be returned to the process or a common sump. These are continuous flow type systems, no batch sampling technique is required.
  • the flow-by path from each sample point may suitably take the form of a U-shaped tube going from the sample point to the inlet for the mass spectrometer and returning back to the process stream or sump.
  • the successful operation of such system is dependent on the cleanliness of the vaporized liquid or gas entering the analyzer. In many processes aerosols and/or solids are produced which are then present in the sample stream whereby they may plug either the capillary tubing employed to reduce sample pressure or plug the inlet leak to the mass spectrometer itself. If either of these problems occur, the analyzer must be shut down and the problem corrected. In a given conventional apparatus known to the inventor, it was - necessary to shut down the apparatus every three to seven days.
  • the above purposes of the instant invention are accomplished by packing a portion of the flow-by tubing, prior to the inlet capillaries or the inlet leak of the mass spectrometer with a packing material coated with a suitable nonvolatile liquid.
  • the packing must have the spaces between the particles thereof small enough to remove fine particles while still permitting adequate flow. With this apparatus the solids are collected by simple.filtration through the packing material while the aerosols flowing into the packing are partitioned into the nonvolatile liquid coating the particles and are released at a later time into the sample stream as a vapor or gas.
  • FIG. 1 illustrating a conventional sampling loop or sampling tube, for sampling from a given point in a processing apparatus, which comprises a tube 1 preferably about 3/32 to 1/2" internal diameter of material which is unaffected by the components normally present in the process streams being analyzed. It must also be physically and chemically stable under the processing conditions, i.e., temperature, pressure, etc. Typical materials would include stainless steel, glass lined metal tubing and polymeric tubing.
  • Tube 1 comprises an inlet arm 2 and an outlet or return arm 3.
  • a small tube or capillary 4 of suitable material such as for tube 1 leads from the end of the loop or tube 1 to the mass spectrometer.
  • a venting means such as a tube 5 of suitable material as previously described is provided between tube 4 and the mass spectrometer.
  • Tube 5 leads to a roughing vacuum pump (not shown in figure 1).
  • an inlet leak 7 is provided for leaking a small amount of gas to the mass spectrometer.
  • the inlet leak 7 is generally of a porous material such as sintered glass or sintered metal.
  • the gas samples passing through the tube 1 often contain aerosols and solids which flow through the tube and back to the process or sump and also through tube 4 to the inlet leak 7 whereby they have the effect of plugging the inlet leak 7.
  • particulate material coated with a nonvolatile liquid 9 is packed into the inlet arm 2 of sample loop or tube 1.
  • Any packing or liquid support material could be used as the particulate material which is physically and chemically stable when exposed to the process stream. However, it must absorb the liquid in the range specified so as not to form droplets or pools of liquid.
  • the coated particulate material 9 consists of diatomaceous earth with a particle mesh size of from about 40 to 180 coated with a nonvolatile liquid such as a silicone-type liquid. The percentage by weight of the silicone liquid based on the total weight of the particulate material is about 3 to 15 percent.
  • the packing must be air- sized to remove the fine particles having a mesh size greater than 180 which might also plug the sample capillary 4 or the inlet leak 7.
  • suitable particulate materials include molecular sieves, charcoal, glass fibers, and open cell polymeric foams.
  • suitable coating materials % include any substance that is liquid at the operating temperature of the device and having a low vapor pressure such as polyethers, hydrocarbons and derivatives thereof.
  • the coated particulate material 9 is secured within the arm 2 of tube 1 by means of small wads of inert 5 glass wool or other similar inert packing material (not shown).
  • the packing of the particulate material 9 into the arm 2 of tube 1 is done in such a way as not to form fine particles. This is accomplished by adding the packing to the tubing while gently tapping on the tubing with a 1/4" diameter wooden stick or pencil. This yields a packing of coated particulate material having uniform density and minimum fine particles.
  • the aerosols and solids are removed. While the solids could be collected by simple filtration with conventional filters, aerosols would pass unchanged through filters.
  • the aerosols pass into the packed material 9 and are partitioned into the non-volatile liquid coating the particles and are released at a later time into the sample stream as a vapor or gas.
  • a single tube or loop 1 may be connected to a mass spectrometer or a plurality of sample loops or tubes 1 may be connected through a suitable valving arrangement to a single mass spectrometer.
  • a suitable valving arrangement to a single mass spectrometer.
  • the tube or capillary 4 from each sample loop or tube 1 is connected through a valve 11 of any conventional design and another tube 13 to a tube or header 15.
  • a suitable tube, capillary, etc., 17 is connected to the header at one end and is provided with an inlet leak 7 therein beyond which it is connected to the mass spectrometer 19.
  • a vacuum generally from about 25 to 100 TORR is maintained in the sample inlet system by provision of a roughing pump 21 connected to the vent tube 5.
  • An ion pump 23 maintains a vacuum within the mass spectrometer apparatus of about 10 -5 to 10 Torr. All of such apparatus, i.e., the mass spectrometer 19, ion pump 23, roughing pump 21, vent tube 5 and the arrangement therefor, are well known to those skilled in the art and are described in more detail in the manufacturers' literature.
  • the valves 11 may be controlled to open in sequence thus providing samples from each source in turn, i.e., from each sample loop or tube 1 for a short period of time after which the one valve is closed and the next valve is opened, only one valve being open at a time generally speaking. This sequencing operation can be accomplished by any conventional control apparatus (not shown). In most cases the discharge from the roughing pump is returned to the process apparatus at or near the point where the sample is removed.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Electron Tubes For Measurement (AREA)
EP85108792A 1984-07-27 1985-07-13 Analysegerät Withdrawn EP0169469A3 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US63517184A 1984-07-27 1984-07-27
US635171 1984-07-27

Publications (2)

Publication Number Publication Date
EP0169469A2 true EP0169469A2 (de) 1986-01-29
EP0169469A3 EP0169469A3 (de) 1987-10-14

Family

ID=24546736

Family Applications (1)

Application Number Title Priority Date Filing Date
EP85108792A Withdrawn EP0169469A3 (de) 1984-07-27 1985-07-13 Analysegerät

Country Status (3)

Country Link
EP (1) EP0169469A3 (de)
JP (1) JPS6183959A (de)
CA (1) CA1256220A (de)

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002044684A2 (en) * 2000-11-28 2002-06-06 Mds Inc. Sample introduction device for mass spectrometry using a fast fluidic system to synchronize multiple parallel liquid sample streams
US6841774B1 (en) 2000-11-28 2005-01-11 Mds Inc. Sample introduction device for mass spectrometry using a fast fluidic system to synchronize multiple parallel liquid sample streams
US10777397B2 (en) 2015-03-06 2020-09-15 Micromass Uk Limited Inlet instrumentation for ion analyser coupled to rapid evaporative ionisation mass spectrometry (“REIMS”) device
US10777398B2 (en) 2015-03-06 2020-09-15 Micromass Uk Limited Spectrometric analysis
US10916415B2 (en) 2015-03-06 2021-02-09 Micromass Uk Limited Liquid trap or separator for electrosurgical applications
US10978284B2 (en) 2015-03-06 2021-04-13 Micromass Uk Limited Imaging guided ambient ionisation mass spectrometry
US11031222B2 (en) 2015-03-06 2021-06-08 Micromass Uk Limited Chemically guided ambient ionisation mass spectrometry
US11031223B2 (en) 2015-09-29 2021-06-08 Micromass Uk Limited Capacitively coupled REIMS technique and optically transparent counter electrode
US11037774B2 (en) 2015-03-06 2021-06-15 Micromass Uk Limited Physically guided rapid evaporative ionisation mass spectrometry (“REIMS”)
US11139156B2 (en) 2015-03-06 2021-10-05 Micromass Uk Limited In vivo endoscopic tissue identification tool
US11239066B2 (en) 2015-03-06 2022-02-01 Micromass Uk Limited Cell population analysis
US11264223B2 (en) 2015-03-06 2022-03-01 Micromass Uk Limited Rapid evaporative ionisation mass spectrometry (“REIMS”) and desorption electrospray ionisation mass spectrometry (“DESI-MS”) analysis of swabs and biopsy samples
US11270876B2 (en) 2015-03-06 2022-03-08 Micromass Uk Limited Ionisation of gaseous samples
US11282688B2 (en) 2015-03-06 2022-03-22 Micromass Uk Limited Spectrometric analysis of microbes
US11289320B2 (en) 2015-03-06 2022-03-29 Micromass Uk Limited Tissue analysis by mass spectrometry or ion mobility spectrometry
US11342170B2 (en) 2015-03-06 2022-05-24 Micromass Uk Limited Collision surface for improved ionisation
US11367605B2 (en) 2015-03-06 2022-06-21 Micromass Uk Limited Ambient ionization mass spectrometry imaging platform for direct mapping from bulk tissue
US11454611B2 (en) 2016-04-14 2022-09-27 Micromass Uk Limited Spectrometric analysis of plants
CN118225520A (zh) * 2024-05-23 2024-06-21 烟台至公生物医药科技有限公司 一种质谱仪的气体取样装置

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010062151A2 (ko) * 2008-11-28 2010-06-03 Sung Jong-Woo 속지 탈부착 가능한 수첩

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3648047A (en) * 1970-07-13 1972-03-07 Perkin Elmer Corp Sensitivity control for mass spectrometer
US4008388A (en) * 1974-05-16 1977-02-15 Universal Monitor Corporation Mass spectrometric system for rapid, automatic and specific identification and quantitation of compounds
AT346286B (de) * 1977-03-30 1978-11-10 Street Harold V Verfahren zur herstellung von deaktivierten, anorganischen, chromatographischen traegermaterialien
US4298795A (en) * 1978-09-08 1981-11-03 Japan Spectroscopic Co. Ltd Method and apparatus for introducing samples to a mass spectrometer

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3648047A (en) * 1970-07-13 1972-03-07 Perkin Elmer Corp Sensitivity control for mass spectrometer
US4008388A (en) * 1974-05-16 1977-02-15 Universal Monitor Corporation Mass spectrometric system for rapid, automatic and specific identification and quantitation of compounds
AT346286B (de) * 1977-03-30 1978-11-10 Street Harold V Verfahren zur herstellung von deaktivierten, anorganischen, chromatographischen traegermaterialien
US4298795A (en) * 1978-09-08 1981-11-03 Japan Spectroscopic Co. Ltd Method and apparatus for introducing samples to a mass spectrometer

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
GEC JOURNAL OF SCIENCE & TECHNOLOGY, vol. 42, no. 1, 1975, pages 16-20, London, GB; J.R. WILCOX: "Advances in organic mass spectrometry - Resolutions up to 150 000 " *
JOURNAL OF CHROMATOGRAPHY, vol. 42, 1969, pages 319-335, Amsterdam, NL; W.A. AUE et al.: "Preparation and chromatographic uses of surface-bonded silicones" *

Cited By (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002044684A2 (en) * 2000-11-28 2002-06-06 Mds Inc. Sample introduction device for mass spectrometry using a fast fluidic system to synchronize multiple parallel liquid sample streams
WO2002044684A3 (en) * 2000-11-28 2003-02-27 Mds Inc Sample introduction device for mass spectrometry using a fast fluidic system to synchronize multiple parallel liquid sample streams
US6841774B1 (en) 2000-11-28 2005-01-11 Mds Inc. Sample introduction device for mass spectrometry using a fast fluidic system to synchronize multiple parallel liquid sample streams
AU2002223343B2 (en) * 2000-11-28 2007-01-18 Mds Inc. Sample introduction device for mass spectrometry using a fast fluidic system to synchronize multiple parallel liquid sample streams
US11289320B2 (en) 2015-03-06 2022-03-29 Micromass Uk Limited Tissue analysis by mass spectrometry or ion mobility spectrometry
US11282688B2 (en) 2015-03-06 2022-03-22 Micromass Uk Limited Spectrometric analysis of microbes
US10916415B2 (en) 2015-03-06 2021-02-09 Micromass Uk Limited Liquid trap or separator for electrosurgical applications
US10978284B2 (en) 2015-03-06 2021-04-13 Micromass Uk Limited Imaging guided ambient ionisation mass spectrometry
US11031222B2 (en) 2015-03-06 2021-06-08 Micromass Uk Limited Chemically guided ambient ionisation mass spectrometry
US11367605B2 (en) 2015-03-06 2022-06-21 Micromass Uk Limited Ambient ionization mass spectrometry imaging platform for direct mapping from bulk tissue
US11037774B2 (en) 2015-03-06 2021-06-15 Micromass Uk Limited Physically guided rapid evaporative ionisation mass spectrometry (“REIMS”)
EP3265821B1 (de) * 2015-03-06 2021-06-16 Micromass UK Limited Flüssigkeitsfalle oder separator für elektrochirurgische anwendungen
US11367606B2 (en) 2015-03-06 2022-06-21 Micromass Uk Limited Rapid evaporative ionisation mass spectrometry (“REIMS”) and desorption electrospray ionisation mass spectrometry (“DESI-MS”) analysis of swabs and biopsy samples
US11139156B2 (en) 2015-03-06 2021-10-05 Micromass Uk Limited In vivo endoscopic tissue identification tool
US11239066B2 (en) 2015-03-06 2022-02-01 Micromass Uk Limited Cell population analysis
US11264223B2 (en) 2015-03-06 2022-03-01 Micromass Uk Limited Rapid evaporative ionisation mass spectrometry (“REIMS”) and desorption electrospray ionisation mass spectrometry (“DESI-MS”) analysis of swabs and biopsy samples
US11270876B2 (en) 2015-03-06 2022-03-08 Micromass Uk Limited Ionisation of gaseous samples
US10777398B2 (en) 2015-03-06 2020-09-15 Micromass Uk Limited Spectrometric analysis
US10777397B2 (en) 2015-03-06 2020-09-15 Micromass Uk Limited Inlet instrumentation for ion analyser coupled to rapid evaporative ionisation mass spectrometry (“REIMS”) device
US11342170B2 (en) 2015-03-06 2022-05-24 Micromass Uk Limited Collision surface for improved ionisation
US11133164B2 (en) 2015-09-29 2021-09-28 Micromass Uk Limited Capacitively coupled REIMS technique and optically transparent counter electrode
US11031223B2 (en) 2015-09-29 2021-06-08 Micromass Uk Limited Capacitively coupled REIMS technique and optically transparent counter electrode
US11454611B2 (en) 2016-04-14 2022-09-27 Micromass Uk Limited Spectrometric analysis of plants
CN118225520A (zh) * 2024-05-23 2024-06-21 烟台至公生物医药科技有限公司 一种质谱仪的气体取样装置

Also Published As

Publication number Publication date
EP0169469A3 (de) 1987-10-14
CA1256220A (en) 1989-06-20
JPS6183959A (ja) 1986-04-28

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Effective date: 19890530

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Inventor name: RING, RUSSEL DAVID

Inventor name: BOURG III, ROGER