CN1146474C - Device for tank for cooling contained liquid sample to be analyzed, especially for cooling contained petroleum product - Google Patents

Device for tank for cooling contained liquid sample to be analyzed, especially for cooling contained petroleum product Download PDF

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Publication number
CN1146474C
CN1146474C CNB001374788A CN00137478A CN1146474C CN 1146474 C CN1146474 C CN 1146474C CN B001374788 A CNB001374788 A CN B001374788A CN 00137478 A CN00137478 A CN 00137478A CN 1146474 C CN1146474 C CN 1146474C
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China
Prior art keywords
condenser pipe
compression member
compartment
sample
head end
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Expired - Lifetime
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CNB001374788A
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CN1340382A (en
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�����Ƥ��
皮埃尔·伯顿
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Experimental Instrument Science And Technology S A
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Experimental Instrument Science And Technology S A
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/42Low-temperature sample treatment, e.g. cryofixation
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25DREFRIGERATORS; COLD ROOMS; ICE-BOXES; COOLING OR FREEZING APPARATUS NOT OTHERWISE PROVIDED FOR
    • F25D19/00Arrangement or mounting of refrigeration units with respect to devices or objects to be refrigerated, e.g. infrared detectors
    • F25D19/006Thermal coupling structure or interface
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25BREFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
    • F25B9/00Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point
    • F25B9/14Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point characterised by the cycle used, e.g. Stirling cycle
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25BREFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
    • F25B9/00Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point
    • F25B9/14Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point characterised by the cycle used, e.g. Stirling cycle
    • F25B9/145Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point characterised by the cycle used, e.g. Stirling cycle pulse-tube cycle
    • 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
    • G01N33/26Oils; Viscous liquids; Paints; Inks
    • G01N33/28Oils, i.e. hydrocarbon liquids

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Pathology (AREA)
  • Analytical Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Investigating Or Analyzing Materials Using Thermal Means (AREA)

Abstract

Provided is a refrigerating device includes a stirling cycle or pulse-type cooling unit 10 which is connected to an A.C. power source at one end, provided with a means capable of changing the pressure of a high-pressure operation gas periodically, and is constituted of a compression module 16 which operates with a cold finger 17. An operation chamber subdivided into a plurality of compartments and extended into the compression module 16 and cold finger 17 is filled with helium to enable extremely low temperatures to be obtained at this level by the expansion of the operation gas in the cold compartments placed at the end of the cold finger 17 opposite to the compression module 16 i.e., a first end 18. The refrigerating device includes a dry contact heat- transfer organ 11 on the other side which is mounted on the cold finger 17 at the level of the first end 18, enables a sample to be cooled to necessary temperatures, and operates with a cell containing a sample to be analyzed.

Description

The device of the groove of the Sheng desire is analyzed in the cooling fluid sample, particularly oil product
The present invention relates to contain in a kind of being used for the device of cooling at the groove of viscous liquid sample, the particularly oil product of from+50 to-120 ℃ temperature range analysis.
At some in particular cases, relate to the petroleum product analysis field the experiment of some physical-chemical need with analysis vat and wherein the sample of splendid attire be cooled to temperature until-80 ℃ even-120 ℃; The mensuration of enumerating by nonrestrictive example in these experiments has: temperature, dew point, pour point, cloud point or Tag and Abel (Abel) flash-point can be filtered in the border.
Be this purpose, usually use the device of type as shown in Figure 1, this device is made up of the circulate EGR 2 of this fluid of Rankine (rankine) the formula cryostat 1 collaborative direction with arrow a that has been equipped with one jar of cooling thermal liquid, and this EGR also comprises circulating pump 3.
Closed circuit 2 is to be made of the coil pipe 4 around the groove 5 that is cooled.Its assembling is that coil pipe 4 and the groove 5 that is cooled are put into the heat shield 6 that includes heat-insulating material 7.Hygrosensor 8 can be measured the variations in temperature of groove 5 at any time.
This conventional equipment that is cooled off by the groove of containing sample in contacting with the coil pipe that includes circulation heat transport fluid has many defectives.
What should particularly point out is groove to be cooled to-80 ℃ of temperature need adopt almost-85 ℃~-90 ℃ thermal liquid, and this need use two-stage Rankine (rankine) type generator; Now, this cryogenerator be heavy, be full of noise and flimsy device.
In addition, for cooling bath, must obtain one jar of thermal liquid, it can keep fluid state under very low temperature; At present all used methyl alcohol basically for this purpose, this is because also can consider that other the got liquid that uses is not too expensive, is exactly volatile at ambient temperature.Now, because the toxicity of methyl alcohol will forbid in the near future that probably it uses in the laboratory.
In addition, because the easily damaged relatively property of Rankine (rankine) type cryogenerator does not contain this generator, the adiabatic connecting line that this need be connected with the latter in the analyzer now; Now, these connecting lines are high risk roots of leakage and heat loss, and therefore the whole efficient of this low-temperature receiver type is very low.
Should also be noted that the groove temperature controlling is difficult to carry out owing to can get the thermal shock that does not match and be applied to groove when injecting heat transport fluid of energy and institute's energy requirement at every turn.
The purpose of this invention is to provide a kind of device, this device can accomplish the fluid sample that interior Sheng is to be analyzed particularly the groove of oil product be cooled to very low temperature, and overcome above-mentioned shortcoming.
For reaching this purpose, the present invention relates to a kind of device, it is characterized in that it comprises the Stirling circulation (Stirling cycle) of a pulse gas cooling device on the one hand, also comprise on the other hand one be placed on this cooling device and with the synergistic dry contact of the groove heat transmitter spare that includes analyzed sample so that sample can be cooled to temperature required.Stirling circulation or pulsed gas quench system are for being cooled to electronic component the special design of low-down temperature, this device is pressed shown in the figure and is made up of the collaborative condenser pipe of a compression member, it links to each other with AC power, and be provided with the device that can change high-pressure working gas (particularly helium) pressure periodically, this gas is full of working chamber, and this working chamber is divided into many compartment that stretch into compression member and condenser pipe; So just may working gas be expanded can access the very low temperature of this level in the opposite end of the condenser pipe that is arranged in relative compression member or the chilling room compartment of head end.
According to the present invention, dry contact heat transmitter spare is arranged on the condenser pipe, and concordant with this condenser pipe head end.
The experiment that the structure of these heat transmitter spares is carried out according to needs and changing.
According to a kind of variation of the present invention, defer to European standard pr EN No. 16, the example that oil product border filtrability temperature is measured is illustrated by being suitable for, heat transmitter spare is by metal tube (particularly copper pipe), constitute around the sheath of the groove of the analyzed sample of interior Sheng and the sleeve that is manufactured from the same material on this sheath sidewall, the shape and size of this sheath are corresponding with the head end of condenser pipe, and are installed on this head end.
Change according to this, tubular sheath and energy be installed to the inside that top condenser pipe head end is fixed on the insulated cabinet that includes heat-insulating material with this protective metal shell.
The structure of heat transmitter spare certainly can be different fully, and this depends on the experiment that will carry out and the type of therefore desiring cooling bath.
In all cases, for heat transmitter spare provides hygrosensor, it and Control Component synergy is so that the temperature of regulating tank well.
Or rather, the Stirling cooling back installation generally includes a cylindrical basically compression member and a condenser pipe, and this condenser pipe also is columniform basically, be positioned at the extension of compression member and coaxial with this compression member, but diameter is smaller.
This compression member comprises a main piston at least, and this piston is controlled by the linear or rotary motor of ac power supply, and moves back and forth with compression work gas in compression compartment.Condenser pipe itself contains an oscillating-piston hollow and that fill heat exchange medium (sweeping piston), this piston is flexibly installed, it is with the frequency identical with main piston but with opposite phases motion, and with the pressure of main piston synergy with different interval chamber working gas in the periodic variation working chamber; This oscillating-piston is divided into the compartment that two energy are interconnected by heat exchange medium in condenser pipe inside, promptly one is the cold compartment that is positioned at the head end of condenser pipe, another is the hot compartment that is positioned at this condenser pipe offside one end, and it links to each other with compression compartment.
Such cooling device himself has been known, and for example its structure is open in 8288 aspect file US-A-4894996 and US-A-508, but for for simplicity, just is not described in greater detail in this application.
Consider the vibration that is produced by main piston and oscillating-piston cycle movement, when such cooling device was provided, according to the present invention, this cooling device was necessary and cushions the parts synergy of this vibration.
Be this purpose, according to further feature of the present invention,, cooling device is fixed on (the particularly steel of appropriate mass) on the Weight plate by firmly being installed in the leg of cooling device sidewall, and keep basic parallel, and be placed at least on 3, best 4 dampers with its longitudinal axis.
Device characteristic as the object of the invention will be for a more detailed description according to relevant accompanying drawing:
Fig. 1 is a schematic representation of apparatus of prior art,
Fig. 2 is the schematic diagram with the similar apparatus of the present invention of Fig. 1,
Fig. 3 is suitable for establishing criteria pr EN-116 to measure the sample border be contained in the groove and can filter the exploded perspective view of apparatus of the present invention of temperature,
Fig. 4 is the stereogram that is suitable for measuring apparatus of the present invention of the sample dew point that is contained in the groove,
According to Fig. 2, cooling device is by Stirling circulation or pulse gas cooling device 10 and is used for dry contact assembly 11 be combined intos that heat transmits, so that can be cooled to the groove of the analyzed sample of interior Sheng temperature required.
The member that is made of heat transfer component 11 and groove 12 is positioned at the inside of the insulated cabinet 13 that includes heat-insulating material 14.Hygrosensor 15 can carry out the temperature measuring of groove 12 at any time.
Or rather, cooling device 10 is made of compression member 16 collaborative condenser pipes 17, and the cold junction 18 that is positioned at this condenser pipe 17 of compression member 16 opposite sides is supported dry contact heat transfer component 11.
According to Fig. 3 and 4, cooling-part comprises that is essentially the also cylindrical basically condenser pipe 17 of columned compression member 16 and itself, this condenser pipe 17 be positioned at compression member 16 the extension and with this element coaxial; The diameter of this condenser pipe 17 is less than the diameter of compression member 16.
The cooling device 10 of Xing Chenging is assembled on the Weight plate that the steel 20 of certain mass makes by the leg 19 that is installed on compression member 16 sidewalls thus, the vibration that is produced by the reciprocating motion of the pistons of cooling device 10 inside with balance.
As shown in Figure 3 and Figure 4, Weight plate is parallel with the longitudinal axis of cooling device 10, and is placed on 4 dampers 21.
Referring to Fig. 3, the cold junction 18 of condenser pipe 17 is placed in above the annular copper sleeve 22 of respective diameters.
Annular copper sleeve 22 is installed on the sidewall of tubulose copper sheath 24 of circumferential groove 25, can filter temperature with the border of working sample.
According to European standard pr EN 116, groove 25 is by pipette 26 special shape and that have storeroom, the sample introduction pipe that links to each other with vacuum source and goes out the sample pipe and constitute.The sample introduction pipe passes the stopper 27 that is used for closed tube sheath 24, and links to each other with the container 28 of interior Sheng analytic sample by filter element 29 in its bottom.A middle bracket 30 can keep the sample introduction pipe in the inside of tubular sheath 24.
In addition, hygrosensor 31 also is installed, so that can carry out the mensuration of container 28 internal temperatures at any time on stopper 27.
Referring to Fig. 3, by tubular sheath 24 be positioned at the parts that the annulus 22 on condenser pipe 17 cold junctions 18 forms and form dry contact heat transfer component 11.
This structure 11 is installed on the Weight plate 20, and with top ring 33 that this structure 11 is concordant with the cold junction 18 of condenser pipe 17 by stepping up diagonal brace 32.
Referring to Fig. 4, dry contact heat transfer component 11 ' is made of the metal transmission dish 35 that is installed on the condenser pipe 17, and by clamp 34 clampings.
The inner surface of the bottom 36 by transmitting cover 35 will transmit and cover 35 and affact on the cold junction 18 of condenser pipe 17.
Be the dew point of working sample, the outer surface support slot 37 of 35 bottoms 36 is coiled in transmission, and this outer surface is relative with inner surface on the cold junction 18 that transmission dish 35 is affacted condenser pipe 17.
For this groove 37 is provided with an injection port 38 that is used for analyzed sample and outlet 39 and respectively as two optical pickocffs 40 and 40 ' of transmitter and receiver.Be fixed to temperature sensor 41 working sample temperature at any time on the groove 36 by clamp 39.

Claims (5)

1. device that the groove that is used for the viscous liquid sample that interior Sheng is to be analyzed cools off, can filter temperature on the border of in+50 ℃ to-120 ℃ temperature range, carrying out them, dew point, the mensuration of pour point or cloud point, described device comprises a Stirling circulation or the pulse gas cooling device (10) that is made of the collaborative condenser pipe (17) of compression member (16), this device links to each other with AC power, and provide a high-pressure working gas pressure apparatus that can periodic variation be full of working chamber, this work chamber is divided into many compartment, and in condenser pipe (17) and compression member (16), extend, make to be positioned at and expand with respect to condenser pipe (17) opposite end of compression member (16) or the cold compartment working gas of head end (18), can on this level, obtain low-down temperature
It is characterized in that, dry contact heat transfer component (11) and mutually neat with the head end (18) of this condenser pipe is set on condenser pipe (17), the groove synergy of it and the analyzed sample of interior Sheng, it is temperature required to make that sample can be cooled to; The tubular metal sheath (24) that described heat transfer component (11) is made of copper is formed, this tubular sheath is around the groove of the analyzed sample of interior Sheng, and a sleeve that is manufactured from the same material (22) is set on the sidewall of this tubular sheath, the head end of its shape and size and condenser pipe is corresponding and be arranged on this head end.
2. device as claimed in claim 1 is characterized in that: the head end (18) of heat transfer component (11) and condenser pipe (17) is arranged on the inside of the insulated cabinet (13) that includes heat-insulating material (14).
3. as claim 2 device, it is characterized in that on heat transfer component (11), being provided with a hygrosensor (15).
4. device as claimed in claim 1, it is characterized in that: cooling device comprises a columned basically compression member (16), this compression member comprises one at least by ac power supply and by the main piston of linear or rotary motor control, this main piston moves back and forth with compression work gas in compression compartment, also comprise a condenser pipe (17), this condenser pipe is also cylindrical basically, be positioned at the extension of compression member, and it is coaxial with this compression member, but has littler diameter, this condenser pipe also comprises an oscillating-piston that is full of the hollow of heat exchange medium, this piston is flexibly fixing, it is with the frequency identical with main piston but move with opposite phases, and with main piston synergy pressure with different interval chamber working gas in the periodic variation working chamber, this oscillating-piston is divided into the compartment that two energy are interconnected by heat exchange medium in condenser pipe inside, promptly cold compartment is positioned at the head end (18) of condenser pipe (17), and another hot compartment is positioned at the opposite end of this condenser pipe (17) and link to each other with the compression compartment of compression member (16);
Cooling device (10) is installed on the Weight plate (20) that is formed from steel by the leg (19) that firmly is arranged on its sidewall, and keeps substantially parallel with the longitudinal axis of this Weight plate, and is installed at least 3 dampers (21).
5. device as claimed in claim 4 is characterized in that: the number of described damper (21) is 4.
CNB001374788A 1999-11-18 2000-11-17 Device for tank for cooling contained liquid sample to be analyzed, especially for cooling contained petroleum product Expired - Lifetime CN1146474C (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9914490 1999-11-18
FR9914490A FR2801381B1 (en) 1999-11-18 1999-11-18 DEVICE FOR REFRIGERATING CELLS CONTAINING LIQUID SAMPLES IN PARTICULAR SAMPLES OF PETROLEUM PRODUCTS TO BE ANALYZED

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Publication Number Publication Date
CN1340382A CN1340382A (en) 2002-03-20
CN1146474C true CN1146474C (en) 2004-04-21

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CNB001374788A Expired - Lifetime CN1146474C (en) 1999-11-18 2000-11-17 Device for tank for cooling contained liquid sample to be analyzed, especially for cooling contained petroleum product

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JP (1) JP2001194278A (en)
CN (1) CN1146474C (en)
AT (1) AT412910B (en)
BE (1) BE1013463A3 (en)
CA (1) CA2325773C (en)
DE (1) DE10056131B4 (en)
FR (1) FR2801381B1 (en)
GB (2) GB2360830B (en)
IT (1) IT1321073B1 (en)
NL (1) NL1016581C2 (en)

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FR2846748B1 (en) * 2002-10-30 2005-04-22 I S L METHOD FOR DETERMINING THE DISAPPEARANCE POINT OF CRYSTALS OF PETROLEUM PRODUCTS, AND DEVICE FOR CARRYING OUT SAID METHOD
DE102007028865B3 (en) * 2007-06-22 2009-01-29 Vericold Technologies Gmbh Cryogenic device
US8236168B2 (en) 2009-10-13 2012-08-07 Exxonmobil Research And Engineering Company Onset haze measurement apparatus and procedure
GB201217390D0 (en) * 2012-09-28 2012-11-14 Agplus Diagnostics Ltd Test device and sample carrier
CN103323321A (en) * 2012-11-18 2013-09-25 阿拉山口出入境检验检疫局综合技术服务中心 Inspection and sample feeding device of liquefied petroleum gas
CN107430061B (en) * 2015-02-17 2020-11-06 埃克斯雷姆Ip英国有限责任公司 Techniques for temperature control of polarimeter sample chambers
US11047779B2 (en) * 2017-12-04 2021-06-29 Montana Instruments Corporation Analytical instruments, methods, and components

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ATA19312000A (en) 2005-01-15
GB0223651D0 (en) 2002-11-20
CN1340382A (en) 2002-03-20
GB2360830A (en) 2001-10-03
ITTO20001079A1 (en) 2002-05-17
NL1016581C2 (en) 2001-05-21
IT1321073B1 (en) 2003-12-30
JP2001194278A (en) 2001-07-19
CA2325773A1 (en) 2001-05-18
GB2360830A8 (en) 2002-02-21
DE10056131A1 (en) 2001-05-31
CA2325773C (en) 2007-01-09
FR2801381B1 (en) 2002-01-04
FR2801381A1 (en) 2001-05-25
DE10056131B4 (en) 2011-02-10
GB2360830B (en) 2002-12-18
ITTO20001079A0 (en) 2000-11-17
BE1013463A3 (en) 2002-02-05
GB0028003D0 (en) 2001-01-03
AT412910B (en) 2005-08-25

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