CA1256220A - Analytical apparatus - Google Patents

Analytical apparatus

Info

Publication number
CA1256220A
CA1256220A CA000487569A CA487569A CA1256220A CA 1256220 A CA1256220 A CA 1256220A CA 000487569 A CA000487569 A CA 000487569A CA 487569 A CA487569 A CA 487569A CA 1256220 A CA1256220 A CA 1256220A
Authority
CA
Canada
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.)
Expired
Application number
CA000487569A
Other languages
French (fr)
Inventor
Russell D. 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 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 Corp filed Critical BASF Corp
Application granted granted Critical
Publication of CA1256220A publication Critical patent/CA1256220A/en
Expired legal-status Critical Current

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/04Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
    • H01J49/0431Arrangements 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
    • H01J49/044Arrangements 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Electron Tubes For Measurement (AREA)

Abstract

ANALYTICAL APPARATUS
Abstract of the Disclosure The instant invention relates to a mass spec-tometer having an inlet leak and a flow-by sampling arrange-ment. In accordance with the invention, aerosols and solid impurities are removed from the sample 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.

Description

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The present invention relates to a process analyzer apparatus and to a process for analyzing a stream.
In particular, the present invention relates to s process 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 processiny 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. In the flow-by-sample systems where there are multiple sampling points, flow is maintained in all sample lines even though an analysis is taking place from only one line. In the case of multiple sampling, multiple valves, which may be automatically controlled, are employed whereby there may be successive analysis from each flow tube or conduit. In a flow-by-system the sample is obtained through an inlet leak into the mass spectrometer.
These inlet leaks are generally a porous barrier type ~hich may be made of suitable materials such as sintered metal.
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 success-ful operation of such system is dependent on the cleanlinessof 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 capil:lary tubing employed to reduce sample . , ~ .

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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.
Accordingly, it is a purpose of the instant invention to provide a means for preventing the plugging of the capillary and/or inlet leak for the mass spectrometer whereby the time period between shutdowns for cleaning may be inceased substantially.
According to the present invention there is provided a process analyzer apparatus comprisiny a sample conduit having an inlet connected to the sample point on the pro~ess apparatus and an outlet returning the sample to the process apparatus, a mass spectrometer, second conduit means connecting the sample conduit to the mass spectrometer, inlet leak means provided in the second conduit between the sample conduit and the mass spectrometer, a vent provided in the second conduit means substantially adjacent the inlet leak means and between the inlet leak means and the sample conduit means, packing means provided in the sample conduit means between the inlet and the second conduit means comprising particulate material of about 40 to 180 mesh coated with nonvolatile liquid.
According to the present invention, there is also provided a process for analyzing a stream comprising a gas, vaporized liquid, and mixtures thereof containing aerosol impurities by passing the stream along a predetermined path through a conglomeration of irregular solid surfaces in close proximity to one another which surfaces are coated with a nonvolatile liquid, thereby removing the aerosols, and continuing to pass a major portion of the stream from the conglomeration of solid surfaces in a predetermined path :` `
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back to the processing apparatus while passing a small second portion of the stream in a predetermined path to a porous surface, venting off a major portion of the second portion of the stream prior to the porous surface and leaking a minor portion of the second portion into a mass spectometer through the porous surface.
A preferred embodiment will now be described as example without limitative manner with reference to the drawings wherein corresponding parts in the various figures are represented by the same numbers.
Figure 1 is a diagrammatic representation in section of a conventional flow by mass spectrometer sampling tube of the prior art, Figure 2 is a diagrammatic representation of the sampling tube of Figure l incorporating the features of this invention, and Figure 3 is a schematic representation of a mass spectrometer and multiple sampling system incorporating the features of this invention.
Referring now more particularly to Figure 1 illustrating a conventional sampling loop or sampling tube, for sampling from a given point in a processing apparatus, /

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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, pres-sure, 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. Tu~e 5 leads to a roughing vacuum pump (not shown in figure 1). Just beyond tube 5 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.
In accordance with the prior art, as shown in figure 1, 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.

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In accordance with the instant invention, as shown in figure 2, particulate material coated with a nonvolatile liquid 9 is packed into the inlet arm 2 oE 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.
~owever, it must absorb the liquid in the range specified so as not to Eorm droplets or pools of liquid. In a preferred embodiment 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. Other suitable particulate materials include molecular sieves, charcoal, glass fibers, and open cell polymeric foams. Other 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 glass wool or other similar inert packing material ~not - . . .
- . ., . , . . . , . -: . . - . , - . . .

~6~:~0 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 ~ooden stick or pencil. This yields a packing of coated particulate material having uniform density and minimum fine particles By employing the coated particulate material in the inlet arm 2 of tube l the aerosols and solids are removed. While the solids could be collected by simple filtration with conventional filters, aerosols would pass unchanged through filters. When employing coated particulata material 9, 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 l 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. For example, with reference more particularly to Figure 3, four such sample loops or tubes l are illustrated. In accordance with this embodiment of the invention, the tube or capillary 4 from each sample loop or tube 1 is connected through a valve ll of any conventional design and another tube 13 to a tube or header 15. A
suitable tube, capillary, etc., 17 is connected to the - . .. ~ : . , . ~ . - :

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header at one end and is provided with an inlet leak 7 therein beyond which it is connected to the mass spec-trometer 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 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 theréfor, are well known to those skilled in the art and are described in more detail in the manufacturers' literature. The valves ll 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 opera-tion 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.

.
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Claims (13)

The embodiments of the invention in which an exclusive privilege or property is claimed are defined as follows:
1. A process analyzer apparatus comprising a sample conduit having an inlet connected to the sample point on the process apparatus and an outlet returning the sample to said process apparatus, a mass spectrometer, second conduit means connecting said sample conduit to said mass spectrometer, inlet leak means provided in said second conduit between said sample conduit and said mass spec-trometer, a vent provided in said second conduit means substantially adjacent said inlet leak means and between said inlet leak means and said sample conduit means, packing means provided in said sample conduit means between said inlet and said second conduit means comprising particulate material of about 40 to 180 mesh coated with nonvolatile liquid.
2. The apparatus of claim 1 wherein the amount of said nonvolatile liquid is from about 3.0 to 20.0 percent by weight of the particulate material.
3. The apparatus of claim 2 wherein the pressure in the inlet to the mass spectrometer is maintained at about 25 to 100 TORR by means of a roughing pump pulling a vacuum through said vent and the pressure within the mass spec-trometer is maintained at about 10-5 to 10-7 TORR by an ion pump.
4. The apparatus of claim 2 wherein the packing material is diatomaceous earth and said nonvolatile liquid coating material is a silicone.
5. The apparatus of claim 4 wherein said inlet leak is of sintered glass.
6. The apparatus of claim 4 wherein said inlet leak is of sintered metal.
7. The apparatus of claim 5 wherein the pressure in said mass spectrometer inlet is maintained at about 25 to 100 TORR by means of a roughing pump connected to said vent and the pressure within the mass spectrometer is maintained at about 10-5 to 10-7 TORR by an ion pump.
8. The apparatus of claim 6 wherein the pressure in said mass spectrometer inlet is maintained at about 25 to 100 TORR by means of a roughing pump connected to said vent and the pressure within the mass spectrometer is maintained at about 10-5 to 10-7 TORR by an ion pump.
9. The apparatus of claim 7 wherein multiple sample tubes are provided for sampling various points of a processing apparatus, valves are provided in said second conduit means between said sample tubes and said mass spectrometer, said valves being connected to a header means with a single conduit from said header means to said vent, inlet leak and mass spectrometer, and means for sequentially opening and closing said valves.
10. The apparatus of claim 8 wherein multiple sample tubes are provided for sampling various points of a processing apparatus, valves are provided in said second conduit means between said sample tubes and said mass spectrometer, said valves being connected to a header means with a single conduit from said header means to said vent, inlet leak and mass spectrometer, and means for sequentially opening and closing said valves.
11. A process for analyzing a stream comprising a gas, vaporized liquid, and mixtures thereof containing aerosol impurities by passing said stream along a predeter-mined path through a conglomeration of irregular solid surfaces in close proximity to one another which surfaces are coated with a nonvolatile liquid, thereby removing said aerosols, and continuing to pass a major portion of said stream from said conglomeration of solid surfaces in a predetermined path back to the processing apparatus while passing a small second portion of said stream in a predeter-mined path to a porous surface, venting off a major portion of said second portion of said stream prior to said porous surface and leaking a minor portion of said second portion into a mass spectometer through said porous surface.
12. The process of claim 11 wherein said vented portion is returned to said processing apparatus.
13. The process of claim 12 wherein the pressure at the inlet of said mass spectrometer is about 25 and 100 TORR the pressure within said mass spectrometer is about 10-5 to 10-7.
CA000487569A 1984-07-27 1985-07-26 Analytical apparatus Expired CA1256220A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US63517184A 1984-07-27 1984-07-27
US635,171 1984-07-27

Publications (1)

Publication Number Publication Date
CA1256220A true CA1256220A (en) 1989-06-20

Family

ID=24546736

Family Applications (1)

Application Number Title Priority Date Filing Date
CA000487569A Expired CA1256220A (en) 1984-07-27 1985-07-26 Analytical apparatus

Country Status (3)

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

Families Citing this family (19)

* Cited by examiner, † Cited by third party
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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
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
WO2010062151A2 (en) * 2008-11-28 2010-06-03 Sung Jong-Woo Notebook with removable inner sheets
KR102092047B1 (en) 2015-03-06 2020-03-24 마이크로매스 유케이 리미티드 In vivo endoscopic tissue identification tool
EP3671216A1 (en) 2015-03-06 2020-06-24 Micromass UK Limited Imaging guided ambient ionisation mass spectrometry
EP4174906A1 (en) 2015-03-06 2023-05-03 Micromass UK Limited Improved ionisation of gaseous samples
CN108700590B (en) 2015-03-06 2021-03-02 英国质谱公司 Cell population analysis
GB2552430B (en) 2015-03-06 2022-05-11 Micromass Ltd Collision surface for improved ionisation
US10777398B2 (en) 2015-03-06 2020-09-15 Micromass Uk Limited Spectrometric analysis
EP3265820B1 (en) 2015-03-06 2023-12-13 Micromass UK Limited Spectrometric analysis of microbes
WO2016142669A1 (en) 2015-03-06 2016-09-15 Micromass Uk Limited Physically guided rapid evaporative ionisation mass spectrometry ("reims")
WO2016142690A1 (en) 2015-03-06 2016-09-15 Micromass Uk Limited Inlet instrumentation for ion analyser coupled to rapid evaporative ionisation mass spectrometry ("reims") device
US11289320B2 (en) 2015-03-06 2022-03-29 Micromass Uk Limited Tissue analysis by mass spectrometry or ion mobility spectrometry
US10026599B2 (en) 2015-03-06 2018-07-17 Micromass Uk Limited Rapid evaporative ionisation mass spectrometry (“REIMS”) and desorption electrospray ionisation mass spectrometry (“DESI-MS”) analysis of swabs and biopsy samples
GB2551294B (en) * 2015-03-06 2021-03-17 Micromass Ltd Liquid trap or separator for electrosurgical applications
EP3741303A3 (en) 2015-03-06 2020-12-30 Micromass UK Limited Chemically guided ambient ionisation mass spectrometry
EP3265823B1 (en) 2015-03-06 2020-05-06 Micromass UK Limited Ambient ionization mass spectrometry imaging platform for direct mapping from bulk tissue
GB201517195D0 (en) 2015-09-29 2015-11-11 Micromass Ltd Capacitively coupled reims technique and optically transparent counter electrode
EP3443354A1 (en) 2016-04-14 2019-02-20 Micromass UK Limited Spectrometric analysis of plants

Family Cites Families (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 (en) * 1977-03-30 1978-11-10 Street Harold V PROCESS FOR THE PRODUCTION OF DISABLED, INORGANIC, CHROMATOGRAPHIC CARRIER MATERIALS
JPS583592B2 (en) * 1978-09-08 1983-01-21 日本分光工業株式会社 Method and device for introducing sample into mass spectrometer

Also Published As

Publication number Publication date
EP0169469A2 (en) 1986-01-29
JPS6183959A (en) 1986-04-28
EP0169469A3 (en) 1987-10-14

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