US3618363A - Calibration arrangement for an apparatus for measuring the gas content of material - Google Patents

Calibration arrangement for an apparatus for measuring the gas content of material Download PDF

Info

Publication number
US3618363A
US3618363A US25937A US3618363DA US3618363A US 3618363 A US3618363 A US 3618363A US 25937 A US25937 A US 25937A US 3618363D A US3618363D A US 3618363DA US 3618363 A US3618363 A US 3618363A
Authority
US
United States
Prior art keywords
gas
pump system
calibration
arrangement
source
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 - Lifetime
Application number
US25937A
Inventor
Thaddaus Kraus
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.)
Balzers Patent und Beteiligungs AG
Original Assignee
Balzers Patent und Beteiligungs AG
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 Balzers Patent und Beteiligungs AG filed Critical Balzers Patent und Beteiligungs AG
Application granted granted Critical
Publication of US3618363A publication Critical patent/US3618363A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N7/00Analysing materials by measuring the pressure or volume of a gas or vapour
    • G01N7/14Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/20Metals
    • G01N33/202Constituents thereof
    • G01N33/2022Non-metallic constituents
    • G01N33/2025Gaseous constituents

Definitions

  • An arrangement for the quantitative analysis of gases which are liberated from the gas source includes a pump system connected to the source, to collect the gas to be analyzed, a gas collecting space connected to the pump system discharge, and a device for inserting measured amounts of calibration gas, from a source thereof, into the gas collecting space.
  • the pump system comprises a two-stage or multi-stage pump system, with the stages being interconnected by connection lines.
  • the calibrating gas insertion device is connected into the connecting line between two successive pump stages.
  • Arrangements for the analysis of gases liberated from a gas source customarily comprise a pump system connected to the gas source and a gas collecting space into which the gases to be analyzed are pumped, the gases subsequently being analyzed, such as quantitatively, by means of suitable measuring devices.
  • a calibration system has hitherto been connected at the location of the source of the gas to be analyzed or, in other words, at the suction side of the pump system and, through the pump system, a predetermined amount of the calibration gas is inserted into the gas collection space.
  • the calibration gas has been inserted directly into the vacuum extraction furnace.
  • This known procedure or arrangement has the disadvantage that the required calibration gas connecting lines, with their shut-off valves, enlarge the volume on the suction side of the pump system. This has an unfavorable consequence during the subsequent analysis of the gases liberated from the gas source, particularly if the pumps used have a small suction capacity.
  • the reason for this is that, if the extraction of the sample is to take place sufiiciently complete within a predetermined period, such as, for example, one second, with the analysis being complete to a degree of, for example, 99%, then the quotient formed from the free volume, which is connected at the suction side of the pump system, and the suction capacity of the pump, is not supposed to exceed a predetermined amount. In the example given above, this amount is 0.22 s.
  • This invention relates to the quantitative analysis of gases liberated from a gas source and, more particularly, to an improved and simplified arrangement of this type 1n which the disadvantageous effect of the dead volume of the dosage system is eliminated.
  • An arrangement for the quantitative analysis of gases liberated from a gas source embodying the invention, has, in common with the prior art, a pump system which is connected to the gas source for collecting the gas to be determined. Furthermore, the invention arrangement has a gas collecting space connected to the exhaust of the pump system, as well as an arrangement for the insertion of a dosed amount of calibration gas into the gas collectmg space.
  • the arrangement is characterized in that the pump system is arranged as a two-stage or multi-stage system, and the calibration gas dosage device merges or discharges into the connecting line between two pump stages.
  • An object of the invention is to provide an improved arrangement for the quantitative analysis of gases liberated from a gas source.
  • Another object of the invention is to provide such an arrangement in which a pump system, connected to the source, is designed as a plural-stage pump system with an insertion device for calibration gas being connected into a connecting line between two successive pump stages.
  • a further object of the invention is to provide such an arrangement which is simple, inexpensive, and efficient.
  • Another object of the invention is to provide such an arrangement in which the disadvantageous effect of the dead volume of the dosage system is prevented.
  • a source which liberates or gives off the gas to be analyzed, is indicated at 1.
  • the source will liberate the gases under subatmospheric pressure conditions, for example, the source may be a vacuum hot extraction furnace.
  • a two-stage mechanical pump system is connected to gas source 1 for the purpose of collecting the gas to be analyzed and for supplying this gas to the gas measuring device 2.
  • Measuring device 2 may be of any suitable kind and may, for example, be based on measuring the infrared absorption of the has, its heat conducting capacities, or other physical or chemical characteristics.
  • the two-stage pump system comprises rotary vane type vacuum pump stages 3 and 4.
  • the first pump stage 3 compresses gas from the pressure of source 1 to an average pressure.
  • the second stage 4 compresses the gas from this average pressure to the pressure prevailing in the gas collecting space 2.
  • This last-mentioned pressure usually is also a subatmospheric pressure, and the gas collecting space, prior to starting the analysis, is evacuated or exhausted by an additional pump which has not been illustrated.
  • a calibration gas inlet or insertion means is provided and, in accordance with the invention, communicates with the space connecting pump stages 3 and 4, specifically, it communicates with connecting line 6.
  • the drawing illustrates a shut-off valve 7 in the calibration gas connecting line, the measuring volume 8 for the calibration gas, and a second shut-off valve 10 which permits insertion, from the calibration gas supply 9, of a predetermined amount of calibration gas into the calibration gas measuring volume 8. Subsequently, upon opening valve 7, this measured volume of calibration gas flows into the gas collecting space 2.
  • the invention arrangement in which two-stage or multi-stage pump systems are provided, has the advantage that, in the connecting line between two pump stages, the pressure is so low that the calibration gas amount can be quantitatively inserted into the system.
  • the pressure may, if desired, already be so high that the calibration gas is no longer completely drawn into the gas collecting chamber or space 2.
  • the gas collected in space 2, in accordance with the invention, is then subjected to analysis and investigation by means of measuring devices which are connected to the gas collecting chamber 2 or which form, with the gas collecting chamber 2, a structural unit.
  • v1 In an arrangement for the quantitative analysis of gases which are liberated from a gas source, and including a pump system connected to the source, to collect the gas to be analyzed, a gas collecting chamber connected to the pump system discharge, and a device for inserting measured amounts of calibration gas into the gas collecting chamber, the improvement comprising, in combination, said pump system including plural pump stages interconnected by connection lines; and means connecting said insertion device into the connecting line between two pump stages.

Landscapes

  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

AN ARRANGEMENT FOR THE QUANTITATIVE ANALYSIS OF GASES WHICH ARE LIBERATED FROM THE GAS SOURCE INCLUDES A PUMP SYSTEM CONNECTED TO THE SOURCE, TO COLLECT THE GAS TO BE ANALYZED, A GAS COLLECTING SPACE CONNECTED TO THE PUMP SYSTEM DISCHARGE, AND A DEVICE FOR INSERTING MEASURED AMOUNTS OF CALIBRATION GAS, FROM A SOURCE THEREOF, INTO THE GAS COLLECTING SPACE. THE PUMP SYSTEM COMPRISES A TWO-STAGE OR MULTI-STAGE PUMP SYSTEM, WITH THE STAGES BEING INTERCONNECTED BY CONNECTION LINES. THE CALIBRATING GAS INSERTION DEVICE IS CONNECTED INTO THE CONNECTING LINE BETWEEN TWO SUCCESSIVE PUMP STAGES.

Description

Nov. 9, 197] KRAUS 3,618,363
CALIBRATION ARRANGEMENT FOR AN APPARATUS FOR MEASURING THE GAS CONTENT OF MATERIAL Filed April 6, 1970 CM. lB/QA 7/0 i ME1I5UQ/IV6 V04 UME MEASUE/IVG INVENTOR. 77/400403 KRAUS ATTORNEYS United States Patent 3,618,363 CALIBRATION ARRANGEMENT FOR AN APPARA- TUS FOR MEASURING THE GAS CONTENT OF MATERIAL Thaddaus Kraus, Vaduz, Liechtenstein, assignor to Balzers Pateutund Beteiligungs-Aktiengesellschaft, Balzers, Liechtenstein Filed Apr. 6, 1970, Ser. No. 25,937 Claims priority, application Switzerland, Apr. 8, 1969, 5,397/ 69 Int. Cl. G01n 7/14 US. Cl. 73-1 A 4 Claims ABSTRACT OF THE DISCLOSURE An arrangement for the quantitative analysis of gases which are liberated from the gas source includes a pump system connected to the source, to collect the gas to be analyzed, a gas collecting space connected to the pump system discharge, and a device for inserting measured amounts of calibration gas, from a source thereof, into the gas collecting space. The pump system comprises a two-stage or multi-stage pump system, with the stages being interconnected by connection lines. The calibrating gas insertion device is connected into the connecting line between two successive pump stages.
BACKGROUND OF THE INVENTION Arrangements for the analysis of gases liberated from a gas source, for example, gases which are liberated from a metal sample which is heated in a hot vacuum extraction furnace, customarily comprise a pump system connected to the gas source and a gas collecting space into which the gases to be analyzed are pumped, the gases subsequently being analyzed, such as quantitatively, by means of suitable measuring devices. For the purpose of calibrating such an arrangement, a calibration system has hitherto been connected at the location of the source of the gas to be analyzed or, in other words, at the suction side of the pump system and, through the pump system, a predetermined amount of the calibration gas is inserted into the gas collection space. For example, the calibration gas has been inserted directly into the vacuum extraction furnace.
This known procedure or arrangement has the disadvantage that the required calibration gas connecting lines, with their shut-off valves, enlarge the volume on the suction side of the pump system. This has an unfavorable consequence during the subsequent analysis of the gases liberated from the gas source, particularly if the pumps used have a small suction capacity. The reason for this is that, if the extraction of the sample is to take place sufiiciently complete within a predetermined period, such as, for example, one second, with the analysis being complete to a degree of, for example, 99%, then the quotient formed from the free volume, which is connected at the suction side of the pump system, and the suction capacity of the pump, is not supposed to exceed a predetermined amount. In the example given above, this amount is 0.22 s. For this reason also, the furnace volume cannot exceed a predetermined value which, in the illustrated example, is 60 cm. if a pump is used which has a predetermined suction capacity such as, for example, 1 m /h.=280 cmfi/s. Since, however, valves of the kind which are required for insertion of exactly those calibration gas amounts have already a dead volume of the same magnitude, such an arrangement is not feasible from a practical standpoint.
Therefore, new solutions must be sought.
ice
SUMMARY OF THE INVENTION This invention relates to the quantitative analysis of gases liberated from a gas source and, more particularly, to an improved and simplified arrangement of this type 1n which the disadvantageous effect of the dead volume of the dosage system is eliminated.
An arrangement for the quantitative analysis of gases liberated from a gas source, embodying the invention, has, in common with the prior art, a pump system which is connected to the gas source for collecting the gas to be determined. Furthermore, the invention arrangement has a gas collecting space connected to the exhaust of the pump system, as well as an arrangement for the insertion of a dosed amount of calibration gas into the gas collectmg space.
In accordance with the invention, the arrangement is characterized in that the pump system is arranged as a two-stage or multi-stage system, and the calibration gas dosage device merges or discharges into the connecting line between two pump stages.
With the invention arrangement, there can be obtained a quick and quantitative emptying of the calibrated volume of the calibration system, and furthermore a rapid and quantitative degassing of the sample in the furnace space, without requiring expensive additional arrangements.
An object of the invention is to provide an improved arrangement for the quantitative analysis of gases liberated from a gas source.
Another object of the invention is to provide such an arrangement in which a pump system, connected to the source, is designed as a plural-stage pump system with an insertion device for calibration gas being connected into a connecting line between two successive pump stages.
A further object of the invention is to provide such an arrangement which is simple, inexpensive, and efficient.
Another object of the invention is to provide such an arrangement in which the disadvantageous effect of the dead volume of the dosage system is prevented.
For an understanding of the principles of the invention, reference is made to the following description of a typical embodiment thereof as illustrated in the accompanying drawing.
BRIEF DESCRIPTION OF THE DRAWING In the drawing, the single figure is a somewhat schematic diagram of a quantitative analysis arrangement embodying the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT Referring to the drawing, a source, which liberates or gives off the gas to be analyzed, is indicated at 1. In many cases, the source will liberate the gases under subatmospheric pressure conditions, for example, the source may be a vacuum hot extraction furnace. In accordance with the invention, a two-stage mechanical pump system is connected to gas source 1 for the purpose of collecting the gas to be analyzed and for supplying this gas to the gas measuring device 2. Measuring device 2 may be of any suitable kind and may, for example, be based on measuring the infrared absorption of the has, its heat conducting capacities, or other physical or chemical characteristics.
In the illustrated example, the two-stage pump system comprises rotary vane type vacuum pump stages 3 and 4. The first pump stage 3 compresses gas from the pressure of source 1 to an average pressure. The second stage 4 compresses the gas from this average pressure to the pressure prevailing in the gas collecting space 2. This last-mentioned pressure usually is also a subatmospheric pressure, and the gas collecting space, prior to starting the analysis, is evacuated or exhausted by an additional pump which has not been illustrated.
In order to supply to the arrangement a calibration gas, for calibration purposes, a calibration purposes, a calibration gas inlet or insertion means is provided and, in accordance with the invention, communicates with the space connecting pump stages 3 and 4, specifically, it communicates with connecting line 6.
The drawing illustrates a shut-off valve 7 in the calibration gas connecting line, the measuring volume 8 for the calibration gas, and a second shut-off valve 10 which permits insertion, from the calibration gas supply 9, of a predetermined amount of calibration gas into the calibration gas measuring volume 8. Subsequently, upon opening valve 7, this measured volume of calibration gas flows into the gas collecting space 2.
As compared to insertion of the calibration gas directly into the gas collecting space 2, the invention arrangement, in which two-stage or multi-stage pump systems are provided, has the advantage that, in the connecting line between two pump stages, the pressure is so low that the calibration gas amount can be quantitatively inserted into the system. At the discharge side of the pump system, on the other hand, the pressure may, if desired, already be so high that the calibration gas is no longer completely drawn into the gas collecting chamber or space 2.
The gas collected in space 2, in accordance with the invention, is then subjected to analysis and investigation by means of measuring devices which are connected to the gas collecting chamber 2 or which form, with the gas collecting chamber 2, a structural unit.
While a specific embodiment of the invention has been shown and described in detail to illustrate the application of the principles of the invention, it will be understood that the invention may be embodied otherwise without departing from such principles.
What is claimed is:
v1. In an arrangement for the quantitative analysis of gases which are liberated from a gas source, and including a pump system connected to the source, to collect the gas to be analyzed, a gas collecting chamber connected to the pump system discharge, and a device for inserting measured amounts of calibration gas into the gas collecting chamber, the improvement comprising, in combination, said pump system including plural pump stages interconnected by connection lines; and means connecting said insertion device into the connecting line between two pump stages.
2. The improvement claimed in claim 1, in which said insertion device is connected into the connecting line between two successive pump stages.
3. The improvement claimed in claim 1, in which said pump system is a two-stage pump system.
4. The improvement claimed in claim 3, in which the first stage compresses the gas to be analyzed to an intermediate pressure and the second stage compresses the gas to be analyzed into the final pressure of the gas collecting space.
References Cited UNITED STATES PATENTS 2,795,132 6/1957 Boehme et al. 7319 3,222,133 12/1965 Ballou et al 73-19 3,229,500 1/1966 Kraus 7319 S. CLEMENT SWlSHER, Primary Examiner US. Cl. X.R. 7319
US25937A 1969-04-08 1970-04-06 Calibration arrangement for an apparatus for measuring the gas content of material Expired - Lifetime US3618363A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CH539769A CH490673A (en) 1969-04-08 1969-04-08 Arrangement for the quantitative determination of the gases given off by a gas source

Publications (1)

Publication Number Publication Date
US3618363A true US3618363A (en) 1971-11-09

Family

ID=4292882

Family Applications (1)

Application Number Title Priority Date Filing Date
US25937A Expired - Lifetime US3618363A (en) 1969-04-08 1970-04-06 Calibration arrangement for an apparatus for measuring the gas content of material

Country Status (6)

Country Link
US (1) US3618363A (en)
CH (1) CH490673A (en)
DE (1) DE2009004C3 (en)
FR (1) FR2038314B1 (en)
GB (1) GB1282197A (en)
NL (1) NL6909218A (en)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3885414A (en) * 1972-10-24 1975-05-27 Gen Electric Package for calibration fluids and process
US4287750A (en) * 1978-10-06 1981-09-08 Dragerwerk Ag Device for checking the functioning of gas measuring apparatus
US4723436A (en) * 1985-06-15 1988-02-09 Dragerwerk Aktiengesellschaft Process for calibrating a gas metering instrument
FR2627285A1 (en) * 1988-02-16 1989-08-18 Pechiney Analysing gas quantity and composition in metallic samples - using heated metallic cross connected to vacuum pump and quartz tube where gas is extracted from sample and analysed in container
US5033286A (en) * 1990-06-18 1991-07-23 Westinghouse Electric Corp. On-line instrument for measuring effective partial pressure of dissolved gases in a liquid
US5369977A (en) * 1992-09-30 1994-12-06 Lundahl Instruments, Inc. Gaseous detection system
US5394730A (en) * 1993-01-29 1995-03-07 Eli Lily And Company Method and apparatus for generating a vapor/gas mixture, and uses therefor
EP1666877A1 (en) * 2003-09-10 2006-06-07 Astellas Pharma Inc. Method of analyzing vaporization pattern of solvent and solvent vacuum vaporization device
CN108387691A (en) * 2018-04-02 2018-08-10 杭州赛威斯真空技术有限公司 A kind of material air-breathing deflation rate test device

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3885414A (en) * 1972-10-24 1975-05-27 Gen Electric Package for calibration fluids and process
US4287750A (en) * 1978-10-06 1981-09-08 Dragerwerk Ag Device for checking the functioning of gas measuring apparatus
US4723436A (en) * 1985-06-15 1988-02-09 Dragerwerk Aktiengesellschaft Process for calibrating a gas metering instrument
US4793173A (en) * 1985-06-15 1988-12-27 Dragerwerk Aktiengesellschaft Process for calibrating a gas metering instrument
AU585618B2 (en) * 1985-06-15 1989-06-22 Dragerwerk Aktiengesellschaft Process for calibrating a gas metering instrument
FR2627285A1 (en) * 1988-02-16 1989-08-18 Pechiney Analysing gas quantity and composition in metallic samples - using heated metallic cross connected to vacuum pump and quartz tube where gas is extracted from sample and analysed in container
US5033286A (en) * 1990-06-18 1991-07-23 Westinghouse Electric Corp. On-line instrument for measuring effective partial pressure of dissolved gases in a liquid
US5369977A (en) * 1992-09-30 1994-12-06 Lundahl Instruments, Inc. Gaseous detection system
US5394730A (en) * 1993-01-29 1995-03-07 Eli Lily And Company Method and apparatus for generating a vapor/gas mixture, and uses therefor
EP1666877A1 (en) * 2003-09-10 2006-06-07 Astellas Pharma Inc. Method of analyzing vaporization pattern of solvent and solvent vacuum vaporization device
US20060288604A1 (en) * 2003-09-10 2006-12-28 Astellas Pharma Inc. Method of analyzing vaporization pattern of solvent and solvent vacuum vaporization device
EP1666877A4 (en) * 2003-09-10 2009-09-02 Astellas Pharma Inc Method of analyzing vaporization pattern of solvent and solvent vacuum vaporization device
US7758317B2 (en) 2003-09-10 2010-07-20 Astellas Pharma Inc. Method of analyzing vaporization pattern of solvent and solvent vacuum vaporization device
CN108387691A (en) * 2018-04-02 2018-08-10 杭州赛威斯真空技术有限公司 A kind of material air-breathing deflation rate test device
CN108387691B (en) * 2018-04-02 2023-08-22 杭州赛威斯真空技术有限公司 Material gassing rate testing arrangement that breathes in

Also Published As

Publication number Publication date
DE2009004B2 (en) 1974-07-25
NL6909218A (en) 1970-10-12
CH490673A (en) 1970-05-15
DE2009004A1 (en) 1970-10-15
GB1282197A (en) 1972-07-19
DE2009004C3 (en) 1975-03-20
FR2038314A1 (en) 1971-01-08
FR2038314B1 (en) 1974-05-03

Similar Documents

Publication Publication Date Title
US3618363A (en) Calibration arrangement for an apparatus for measuring the gas content of material
US5317900A (en) Ultrasensitive helium leak detector for large systems
CN107014156A (en) Dried object moisture measurement method, Minton dryer and its control method
CN102494741B (en) Static sampling introduction device and method of calibrating pressure leak hole
CA2484455A1 (en) Leak testing of hermetic enclosures for implantable energy storage devices
US3968675A (en) Method and apparatus for preparing a mass spectrometer leak detector system for operation
CN101696923A (en) Dual testing room measured material outgassing rate measuring device and method
US20080048663A1 (en) Apparatus for and method of measuring composition and pressure of the discharged gas from ion gauge using residual gas analyzer
EP1769226A1 (en) Gas sensor and method for operating a getter pump
JP6934239B2 (en) High-sensitivity temperature rise desorption gas analyzer
US4709579A (en) Measurement of moisture content
US4683749A (en) Process and system for detecting and measuring a tritium gas leak
CN107578979A (en) The quantitative enrichment method sampling device and method of a kind of Proton-Transfer Reactions ion gun
CN110648898A (en) Mass spectrum device and method for detecting multi-component gas in freeze-drying process
US3229500A (en) Gas metering and analyzing apparatus
CN209784116U (en) system for measuring solubility of solid sample in supercritical carbon dioxide
CN210037512U (en) System for measuring solubility of solid sample in supercritical carbon dioxide
CN106841482A (en) A kind of gas chromatograph application process of vacuum sampling device
JPS58105032A (en) Helium mass analyzing type leakage tester
JPS6066127A (en) Testing apparatus of helium leakage
CN201122153Y (en) Flue gas humidity detection apparatus
CN2165441Y (en) Integrative hydrogen permeability parameter measuring apparatus
SU1663511A1 (en) Device for analysis of gases in metals
CN213022857U (en) Gas path structure for gas detection
CN218628823U (en) NECL parameter testing device of gas leak detector