US3722872A - Combined specimen removal and vacuum distillation apparatus - Google Patents

Combined specimen removal and vacuum distillation apparatus Download PDF

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Publication number
US3722872A
US3722872A US00085320A US3722872DA US3722872A US 3722872 A US3722872 A US 3722872A US 00085320 A US00085320 A US 00085320A US 3722872D A US3722872D A US 3722872DA US 3722872 A US3722872 A US 3722872A
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US
United States
Prior art keywords
cover
vessel
chamber
tube
specimen
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
US00085320A
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English (en)
Inventor
H Jentges
O Burz
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Siemens AG
Siemens Corp
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Siemens Corp
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Publication date
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    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21C—NUCLEAR REACTORS
    • G21C17/00—Monitoring; Testing ; Maintaining
    • G21C17/02—Devices or arrangements for monitoring coolant or moderator
    • G21C17/022—Devices or arrangements for monitoring coolant or moderator for monitoring liquid coolants or moderators
    • G21C17/025—Devices or arrangements for monitoring coolant or moderator for monitoring liquid coolants or moderators for monitoring liquid metal coolants
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/10—Devices for withdrawing samples in the liquid or fluent state
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00—Investigating or analyzing materials by the use of thermal means
    • G01N25/14—Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0093—Radioactive materials
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/10—Devices for withdrawing samples in the liquid or fluent state
    • G01N2001/1031—Sampling from special places
    • G01N2001/1037—Sampling from special places from an enclosure (hazardous waste, radioactive)
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4022—Concentrating samples by thermal techniques; Phase changes
    • G01N2001/4033—Concentrating samples by thermal techniques; Phase changes sample concentrated on a cold spot, e.g. condensation or distillation
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/30—Nuclear fission reactors

Definitions

  • the apparatus comprises a ves sel of stainless steel forming a processing chamber and [21] Appl. No.: 85,320 having wall-temperature control means and a removable top cover, means for positionally securing the cover on the vessel against excess pressure in the [30] Foreign Application Pnomy Dam chamber, a plurality of removable specimen con- Nov.7, 1969 Germany ..P 1955 988.7 tainers, holder devices mounted on the cover in suspended relation thereto for supporting the respec- 521 U.S.Cl. ..266/34 R, 23/253 R, 356/36 five specimen containers, the holder means having [51] Int.
  • liquid-metal systems especially liquid-metal circulation systems for the conveyance of heat
  • chemical analysis of the liquid-metal melts to detect impurities, especially oxides is of the highest importance since the rate of corrosion of structural materials depends essentially on the degree of purity of the melt. Since reliablyoperating continuous apparatus for determining and recording such impurities do not exist, such determinations can be effected only by discontinuous processes of chemical analysis.
  • radioactive'radiation is also present, allowing a chemical analysis of a few cubic centimeters of the melt only after the metal has been removed.
  • Distillation of the liquid metal is therefore a most promising process as a pre-stage for such chemical analyses, since with total vaporization of metal no further metallic oxide can be generated through oxygen, and radioactive radiation due predominantly to the radioactivity of liquid metal is substantially reduced.
  • the residue of such samples can then be investigated for the types and amounts of impurities by means of 'chemical analysis or flame-spectrometric methods.
  • Another object of the present invention is to conserve the distillation residue, if necessary, for subsequent investigation before it comes into contact with oxygen.
  • a removable top cover which prevents excess pressure when in position, and serves as a base for a number of movable sample tanks which include respective holding devices provided with heating means and temperature sensors. Furthermore, a lifting duct is arranged above the cover and tightly joined to the vessel chamber for lifting the cover together with the sample tanks through a glove box and an outwardly discharging sluice.
  • This apparatus contains no glass components and can be arranged in such a manner that the distillation chamber itself together with the liquid-metal circulation systems which can also be contaminated with radioactivity are installed behind a suitable shield, such as cement, while the distillation residue can be taken away in a glove box situated outside the protected area, for further examination outside the chamber. To some extent the further investigation can take place inside the glove box, but the samples can also be taken out through a sluice. Renewed oxygen contamination can be avoided by using a suitably pure protective gas. Since a shield is provided between the glove box and the distillation chamber itself, a further distillation cycle can commence during the examination of the residue.
  • the present invention provides for time saving which is a particular advantage when charging such apparatus on the industrial scale, for instance, in sodium-cooled nuclear reactor installations.
  • FIG. 1 shows our apparatus. in conjunction with a nuclear reactor circulation system 8 for a liquid-metal coolant.
  • System 8 comprises a reactor 81, a pump 82 and a heat exchanger 83.
  • the supply conduits to the distillation apparatus further include a a pump 84 and reflux tank 85.
  • the distillation chamber 1 is connected with the liquid-metal circulation system through first and second outlet lines 16 and 17 and inlet line 3, with the reactor plant lying behind a shield 9 of concrete.
  • a glove box 6 and lift tube 7 wherein is mounted a windlass 71 having a rope 72, whereby a cover 13 of chamber 1 with the distillation residues suspended therefrom can be lifted by means of the rope through the concrete shield into the glove box for further treatment.
  • the distillation residues contain only very little radioactivity and therefore are easily manipulated without fear of contamination.
  • a vacuum pump 5 connected to chamber 1 through a liquid-metal condenser 51, and a storage .tank 181 for the protective gas.
  • the high-vacuum slide 64 can also be closed when charging or discharging the system, thus providing a two-fold protection against an unwanted supply of air, (for instance, the handling gloves 68 becoming ripped).
  • chamber 1 consists of a longitudinal steel vessel 11, which is provided with an external heating means 14. Since changes of temperature of this vessel are required for accomplishing the distillation process, heating means 14 is capable of cooling, working, for example, through a flow of liquid-metal having a temperature capable of being adjusted, whose circulation system is not shown in FIG. 2. Intensive cooling produces a short distillation time andcondensation of the highly radioactive sodium vapor inside the chamber.
  • Chamber 1 is closed by cover 13 having a sealing seat I 12 provided with its own heating or cooling means 15 which reenters into the chamber space 1 to balance the thermal stress.
  • the seat 12 has an upward tubular extension on which the cover 13 is maintained in a tightly sealed position by wing screws 74. The screwing down of the cover is accomplished inside glove box 6 and can be loosened by hand outside the concrete shield.
  • Cover 13 also serves as a carrier for the sample tanks 23.
  • a holder frame 2 which is formed by three rigid supporting frames projecting downwardly, onto which the specimen holding devices 21 with heating means 22 for the sample tanks 23 rigidly fastened.
  • the cylindrical shape of sample tanks 23 combined with the rounded transfer from the base to side wall and the cylindrical heating conductor assemblies 22 promotes the heat input by short heat conducting paths and intensive convection to the liquid level such that the shoft distillation time is achieved without retardation of boiling.
  • the electrical connections for the heating devices 2 run through the holder frame 2 as do the connecting lines for temperature sensors 24 mounted beneath the sample tanks 23 inside the holding devices 21. These lines are carried upward above cover 13 in the form of a flexible, helical-wound cable 73, and drawn out (in a manner not shown in drawings) through vacuum-tight lead-in means from the lift tube 7 to the height ofdrum or windlass 71 and connected to respective measuring devices and/or sources of power (not shown).
  • Chamber 1 is furthermore provided with an inlet 18 for the delivery of protective gas and is connected through supply tubes 31 with a liquid-metal supply 3 merging with the reactor circulartion system.
  • the tubes 31 terminate in the interior of chamber 1 in the form ofjets and feed the liquid metal to be investigated to respective ones of the sample tanks 23.
  • Chamber 1 is further linked through outlet 16 to vacuum pump 5, the outlet line 16 supplying liquidmetal into a reflux tank 85 when there is an overflow.
  • the sealing seat is cooled down by the cooling and/0r heating means 15 to 30 to 40C beneath the freezing or solidifying' temperature of the liquid metal, so that with heat conduction, the sealing cone resting on the sealing seat is at 20 to 30C above the freezing point.
  • the liquid metal or the vapor thereof condenses on the bulging bottom of the sealing cone, runs down to the closure gap of the cone and freezes on the sealing seat itself.
  • the frozen gasket is melted by warming heating coils 15. The condensate runs off outwardly and is prevented from dripping into the crucibles 23.
  • this apparatus is not subjected to any special pressure load, but if some unforeseen blockage of overflow 16 were to occur, a maximum excess or overpressure of 16 atmospheres might occur which, as already mentioned, will be absorbed by the cover-fastening screws 74.
  • chamber 1 is evacuated by means of pump 5 and thoroughly baked under the heating and/or cooling means 44.
  • the heating and/or cooling fluid must be fluid and stable in the range from 0 to 650C and impervious to radioactive radiation which might be emitted from the contents of the chamber. Potassiumsodium melt is suitable, for instance. Subsequently, pu-
  • rified argon is poured into the chamber as the protective gas and the liquid metal, sodium, for example, for examination is squirted through lines or tubes 31 from the reactor circulation system into the sample tanks 23.
  • the overflowing metal through outlet line 17 forms a freezing plug in the gasket 171, so that the liquid-metal level in chamber 1 rises up to the overflow level.
  • the overflowing melt flows back into the reflux tank and from the reflux tank through pump 84 into the reactor circulation system.
  • the liquid metal initially flows through chamber 1, which is at a temperature of between 500 and 600C, residual gases especially 0xygen are chemically combined and washed away by the liquid-metal or vapor, and therefore no longer interfere with the sample after the metal commences being distilled.
  • the tightsealing of the cover seating is, as mentioned above, secured by the metal condensate.
  • the chamber cooling circulation flow is now commenced.
  • the tubes of heating means 14 are supplied with coolant fluid and vacuum pump 5 is energized as soon as the wall temperatures drop to below C and the crucible temperatures to about 350C, as sensed by means of the temperature sensors 24.
  • the required vacuum is obtained, the
  • Glove compartment 6 and lift tube 7 have been filled during the above processes with the protective gas, enabling cover 13 with the sample-tanks 23 dependent thereon to be raised manually or by an electrically operated winch turning drum 71.
  • the sample tanks are taken off the holder devices 21, given further treatment there and/or conveyed through sluice 62 to further testing equipment (not shown).
  • a samplings carrier under protective gas is required only if the samples are to be analyzed for elements present in the atmosphere and which react with the residuum.
  • the crucible carrier is subsequently charged with fresh sampling tanks and again set in movement.
  • the next filling and distillation process can immediately start, since a renewed bakeout of wall partitions of chamber 1 is no longer required.
  • the walls of the vessel 11 can be cleansed in rotation through rinsing means 33, connected through an inlet pipe 34 with a liquid-metal storage tank. Possible residues in the holding devices 21 can be rinsed clean without sample tanks.
  • sampling tanks they can be made, for example, of superpure nickel,
  • the same end is served also by the direct heating shown in FIG. 2 for the sampling tanks, on the surfaces of the shell, and their indirect heating in the fissure filled with liquid metal between the container base and holder device 21.
  • This interstice is dimensioned in such manner that on distillation the sampling tank 23 boils first and then the fissure.
  • the vacuum thermocouple 24 senses the temperature of the liquid metal in this fissure.
  • the sodium throughput time will be about 4 hours as previously mentioned and the-distillation time about one-half an hour, so that the examination of the distillation residue and likewise of the liquid metal circulating in the circulation system can be effected during this period. It is thus possible, with the plant, to survey the condition of the liquid-metal circulation systems and other continuously-working metering equipment and/or readjust the same.
  • a combined specimen removal and vacuum distillation apparatus for discontinuously checking liquid metal for purity, such as used as a heat carrier in nuclear reactor plants, comprising a vessel of stainless steel forming a processing chamber and having walltemperature control means and a removable top cover, means for positionally securing said cover on said vessel against excess pressure in said chamber; a plurality of removable specimen containers; holder devices mounted on said cover in suspended relation thereto for supporting said respective specimen containers, said holder means having respective heating means and respective temperature sensors; a lifting device having a tube vertically extending above said cover and tightly joined with said vessel chamber, a lifting mechanism disposed insaid tube and connected to said cover for lifting said cover and said specimen containers; and a glove box and a specimen sluice interposed between said vessel and said tube of said lifting device.
  • said vessel having a liquid-metal inlet, a first liquid-metal overflow outlet, a second liquid-metal overflow outlet and a protective gas connection duct; a vacuum pump connected to said first overflow outlet, and a condenser interposed betweensaid vacuum pump and said first overflow outlet.
  • Apparatus according to Claim 1 comprising a vacuum-tight shut-off slide between said vessel and said glove box for closing and opening said chamber relative to said glove box and sluice.
  • said specimen containers being crucibles
  • said heating means for each of said. crucibles being an electric resistance heater arranged'on said holder device for heating the crucible content through the crucible wall surface.
  • said crucibles having a cylindrical cup shape and a rounded edge portion between the bottom and the cylindrical wall of said cup shape.
  • said lifting mechanism comprising windlass having a rope pull mounted in said tube near the top thereof and having a rope extending from said windlass to said cover.
  • Apparatus according to claim I -comprising flexible helical windings of cables for electrical connection to said heating means and to said temperature sensors, said helical cable windings extending upwardly through said tube in substantially coaxial relation thereto.
  • said vessel having vacuum tight lead-in means for said cables, said lead-in means being lo cated near said windlass.

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  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Pathology (AREA)
  • Immunology (AREA)
  • General Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Analytical Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • General Engineering & Computer Science (AREA)
  • Hydrology & Water Resources (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
US00085320A 1969-11-07 1970-10-30 Combined specimen removal and vacuum distillation apparatus Expired - Lifetime US3722872A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19691955988 DE1955988A1 (de) 1969-11-07 1969-11-07 Kombinierte Probenentnahme- und Vakuumdestillationseinrichtung

Publications (1)

Publication Number Publication Date
US3722872A true US3722872A (en) 1973-03-27

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ID=5750365

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US00085320A Expired - Lifetime US3722872A (en) 1969-11-07 1970-10-30 Combined specimen removal and vacuum distillation apparatus

Country Status (7)

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US (1) US3722872A (fr)
BE (1) BE757692A (fr)
CA (1) CA925814A (fr)
DE (1) DE1955988A1 (fr)
FR (1) FR2082959A5 (fr)
GB (1) GB1292086A (fr)
NL (1) NL7015067A (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070131650A1 (en) * 2001-07-30 2007-06-14 Tokyo Electron Limited Plasma chamber wall segment temperature control

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3145442A1 (de) * 1981-11-16 1983-05-26 Interatom Internationale Atomreaktorbau Gmbh, 5060 Bergisch Gladbach "verfahren und vorrichtung zur entnahme von natriumproben aus dem core eines natriumgekuehlten kernreaktors"
DE4023841A1 (de) * 1990-07-27 1992-02-06 Wiederaufarbeitung Von Kernbre Einrichtung zur entnahme von gas- und/oder fluessigkeitsproben aus einem sicherheitsbehaelter von kernkraftwerken
DE102023104568A1 (de) 2023-02-24 2024-08-29 Deutsches Zentrum für Luft- und Raumfahrt e.V. Probenentnahmevorrichtung zur Entnahme einer Probe aus einem ein flüssiges Medium führenden Anlagenteil sowie Verfahren zur Entnahme einer solchen Probe

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070131650A1 (en) * 2001-07-30 2007-06-14 Tokyo Electron Limited Plasma chamber wall segment temperature control

Also Published As

Publication number Publication date
NL7015067A (fr) 1971-05-11
BE757692A (fr) 1971-04-01
GB1292086A (en) 1972-10-11
DE1955988A1 (de) 1971-05-13
CA925814A (en) 1973-05-08
FR2082959A5 (fr) 1971-12-10

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