WO1991014932A1 - Dispositif de prelevement d'echantillons - Google Patents

Dispositif de prelevement d'echantillons Download PDF

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Publication number
WO1991014932A1
WO1991014932A1 PCT/EP1991/000442 EP9100442W WO9114932A1 WO 1991014932 A1 WO1991014932 A1 WO 1991014932A1 EP 9100442 W EP9100442 W EP 9100442W WO 9114932 A1 WO9114932 A1 WO 9114932A1
Authority
WO
WIPO (PCT)
Prior art keywords
sample
valve
line
sample tube
devices
Prior art date
Application number
PCT/EP1991/000442
Other languages
German (de)
English (en)
Inventor
Robert Krah
Original Assignee
Mütek Gmbh
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 Mütek Gmbh filed Critical Mütek Gmbh
Publication of WO1991014932A1 publication Critical patent/WO1991014932A1/fr

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01F—MEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
    • G01F23/00—Indicating or measuring liquid level or level of fluent solid material, e.g. indicating in terms of volume or indicating by means of an alarm
    • G01F23/22—Indicating or measuring liquid level or level of fluent solid material, e.g. indicating in terms of volume or indicating by means of an alarm by measuring physical variables, other than linear dimensions, pressure or weight, dependent on the level to be measured, e.g. by difference of heat transfer of steam or water
    • G01F23/28—Indicating or measuring liquid level or level of fluent solid material, e.g. indicating in terms of volume or indicating by means of an alarm by measuring physical variables, other than linear dimensions, pressure or weight, dependent on the level to be measured, e.g. by difference of heat transfer of steam or water by measuring the variations of parameters of electromagnetic or acoustic waves applied directly to the liquid or fluent solid material
    • G01F23/296—Acoustic waves
    • G01F23/2966—Acoustic waves making use of acoustical resonance or standing waves
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01F—MEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
    • G01F23/00—Indicating or measuring liquid level or level of fluent solid material, e.g. indicating in terms of volume or indicating by means of an alarm
    • G01F23/22—Indicating or measuring liquid level or level of fluent solid material, e.g. indicating in terms of volume or indicating by means of an alarm by measuring physical variables, other than linear dimensions, pressure or weight, dependent on the level to be measured, e.g. by difference of heat transfer of steam or water
    • G01F23/24—Indicating or measuring liquid level or level of fluent solid material, e.g. indicating in terms of volume or indicating by means of an alarm by measuring physical variables, other than linear dimensions, pressure or weight, dependent on the level to be measured, e.g. by difference of heat transfer of steam or water by measuring variations of resistance of resistors due to contact with conductor fluid
    • G01F23/241—Indicating or measuring liquid level or level of fluent solid material, e.g. indicating in terms of volume or indicating by means of an alarm by measuring physical variables, other than linear dimensions, pressure or weight, dependent on the level to be measured, e.g. by difference of heat transfer of steam or water by measuring variations of resistance of resistors due to contact with conductor fluid for discrete levels
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01F—MEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
    • G01F23/00—Indicating or measuring liquid level or level of fluent solid material, e.g. indicating in terms of volume or indicating by means of an alarm
    • G01F23/22—Indicating or measuring liquid level or level of fluent solid material, e.g. indicating in terms of volume or indicating by means of an alarm by measuring physical variables, other than linear dimensions, pressure or weight, dependent on the level to be measured, e.g. by difference of heat transfer of steam or water
    • G01F23/28—Indicating or measuring liquid level or level of fluent solid material, e.g. indicating in terms of volume or indicating by means of an alarm by measuring physical variables, other than linear dimensions, pressure or weight, dependent on the level to be measured, e.g. by difference of heat transfer of steam or water by measuring the variations of parameters of electromagnetic or acoustic waves applied directly to the liquid or fluent solid material
    • G01F23/296—Acoustic waves
    • G01F23/2966—Acoustic waves making use of acoustical resonance or standing waves
    • G01F23/2967—Acoustic waves making use of acoustical resonance or standing waves for discrete levels
    • 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
    • G01N1/20—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials
    • G01N1/2035—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials by deviating part of a fluid stream, e.g. by drawing-off or tapping

Definitions

  • the invention relates to a sampling device according to the preamble of claim 1.
  • samples of a substance arising or treated in the process have to be taken at relatively short intervals to monitor and / or control them and fed to an analysis device. This can be accomplished by removing an appropriate amount of the substance by hand, which is, however, labor-intensive.
  • a sample quantity suitable for the investigation can also be removed by means of a pump.
  • sampling devices are known, all of which have the disadvantage that at least parts of the sample that can be taken can come from an earlier sampling process.
  • a sampling device is known from US Pat. No. 3,083,577 which comprises a piece of pipe through which a fluid can flow and which can be closed off by valves at the end.
  • Pipes lead into the pipeline in the vicinity of the valves and can be shut off via further valves.
  • To take the sample close the end valves on the pipe section and open the other two valves.
  • the sample can then be conveyed out of the pipe section using compressed air.
  • This sampling device is disadvantageous in that a certain residual volume always remains in the pipe section.
  • the invention has for its object to develop a device of the type mentioned in such a way that an exactly reproducible amount of a current sample can be removed in a simple manner.
  • a device for the controllable removal of samples of fluid substances from a process comprising pump devices which are connected on the input side to a suction line, to which the fluid substances can be supplied and on the output side are connected to a pressure line.
  • controllable valve devices by means of which the pressure line can be connected to a sample container and via which the sample container can be connected to a discharge line, by means of the pump device which is removed from the process by and through feed the sample conveyed material back to the process, and sample ejection devices to discharge the contents of the sample container through a sampling line for further use.
  • This device is characterized by the fact that the sample container is designed as a sample tube, that the sample ejection devices comprise compressed gas devices and that the valve devices comprise two separate valve devices which are designed in this way and are connected to the sample tube, that in a first valve position it is constantly connected to the pressure line and the discharge line and through which the fluid can flow, in a second valve position its first end can be connected to the pressure gas devices and its second end can be connected to the extraction line, so that a volume contained in the sample tube can be blown out through the sampling line.
  • An essential point of the invention lies in the fact that the sample tube has a very large length relative to its clear width (inner diameter). As a result, any residual volumes remaining in the valves are very small in relation to the total volume within the sample tube. Furthermore, the sample tube can be easily wound so that the device does not become too bulky.
  • valve devices each comprise a three-way valve which is connected to the pressure line, the discharge line, the pressure gas device, the sample hose and the sampling line.
  • Figure 1 shows a first preferred embodiment of the invention, in which the valves used are shown in their two positions.
  • Fig. 2 is a schematic diagram of the device according to
  • FIG. 3 shows a circuit diagram of a further preferred embodiment of the invention.
  • FIG. 4 shows the device according to FIG. 1, but in a further constructive embodiment, as well as its mode of operation;
  • Fig. 6 is a schematic representation of part of a
  • Measuring device for observing the filling status of the sample tube
  • Fig. 7 shows another embodiment of a measuring device for
  • the device according to the invention comprises a pump 10 which is connected with its suction line 11 to a process line 20 which contains the fluid substance to be examined.
  • the pump 10 On the pressure side, the pump 10 is connected via a pressure line 12 to a first connection a of a three-way valve 13, the second connection b of which is connected via a sample hose 15 to a second connection b of a second three-way valve 14.
  • the first connection a of the second three-way tils 14 is connected to one end of a discharge line 16, the other end of which is returned to a suitable place in the process.
  • the third connection c of the first three-way valve 13 is connected to one end of a sampling line 19, the other end of which communicates either with an analysis device or with a transport container for the sample to be removed.
  • the third connection c_ of the second three-way valve 14 is connected to a compressed gas source 18 via a compressed gas line 17.
  • the pressurized gas source 18 supplies a pressurized gas which has no or at least no disruptive influence on the nature of the substance to be examined.
  • the substance from the process line 20 is pumped through the sample tube 15 by means of the pump and flows back to the process. If the flow rate, that is to say the time it takes for a partial volume of the substance removed from the process, to pass from the inlet opening of the suction line 11 to the second valve 14 and to fill it completely, is low in comparison to the rate of change of the substance to be monitored, there is a subset of the substance to be investigated in the sample tube 15 and in the valves 13 and 14, the properties of which correspond to those of the substance currently in the process.
  • valves 13 and 14 are switched so that the connections a and b of the valves are no longer connected to one another (see FIG. 1A), but the connections c and b communicate with each other.
  • the compressed gas source 18 is now connected via the compressed gas line 17 to the contents of the sample tube 15 located between the valves 13 and 14.
  • the pressurized gas thus pushes a precisely defined sample volume 1 through the extraction line 19 to the analysis device.
  • the entire remaining contents of the valves 13 and 14 are also carried along or blown out.
  • the variant of the invention shown in FIG. 2 differs from that according to FIG. 1 with regard to its mode of operation only in that the sample volume 1 is not ejected from the sample tube 15 in a direction opposite to the direction of rotation, but rather the direction of rotation is keeps.
  • FIG. 3 differs from that according to FIG. 2 in that two / four-way valves are used instead of two / three-way valves. These are connected via a further circulation line 21 in such a way that when a control 22 switches the valves 13 and 14 in order to supply a sample volume to an analyzer 23, the substance conveyed by the pump 10 passes through the circulation line into the discharge line , so that the pump 10 can continue to promote. This avoids an increased load on the pump 10 and at the same time ensures that the content of the sample tube 15 is "up to date" again immediately when switching back to flow.
  • the sample tube is preferably made very thin and long
  • a sample tube with a clear width (inside diameter) of 3 mm and a length of 1.415 ir is suitable for holding a sample volume of 10 cm.
  • the valves 13 and 14 are equipped with a corresponding flow diameter. If a liquid column of a few mm remains in such a valve, this changes very little in the total sample volume.
  • the hose formed in this way is preferably wound up to save space. By blowing out with compressed gas, a narrow hose wound in this way can also be completely emptied.
  • FIGS. 4 A-C differs from that of FIG. 1 in that a signal transmitter 24 is attached to one valve 13 and a sensor 25 is attached to the other valve 14.
  • the signal transmitter 24 or the sensor 25 are suitable for transmitting or receiving ultrasound.
  • valves 13 and 14 are switched while the pump 10 is running so that the liquid contained therein is removed from the process line 20 and flows through the lines 11, 12, 15 and 16. If a sample is to be taken, a switch is made to the position shown in FIG. 4B, in which the valve 14 the
  • Compressed gas source 18 connects to the sample tube 15.
  • a check valve 39 is provided directly in front of the valve 14 so that no liquid can be pressed into the compressed gas source 18 at this point due to the pumping action of the pump 10. Thus, no liquid flow takes place in the switch position shown in FIG. 4B.
  • the signal generator 24 is now supplied with alternating current at the valve 13, so that the valve 13 is set in vibration. An amount of 5 kHz has been found to be suitable as the oscillation frequency.
  • the vibrations generated in this way are passed on in the liquid within the sample tube 15 and reach the other valve 14.
  • This valve 14 is now set in vibration by the incoming vibrations, so that a corresponding measurement signal can be tapped at the sensor 25. Then, if there is an air bubble within the sample tube 15, that is, the sample tube is not completely filled, the passage of the sound waves from the The signal transmitter to the sensor is damped considerably, since the sound wave resistance in liquids is much lower than in air and reflections also occur at the interfaces. In this way it is very easy to determine whether the sample tube 15 is completely filled or not.
  • a major advantage of this measurement method is that the measurement result is largely independent of the type of liquid examined.
  • valve 27 is provided in the line 17 upstream of the valve 13 instead of the check valve 39.
  • valve 27 is first kept closed, so that the volume contained in sample tube 15 stays there.
  • the measurement described above is then carried out, in which a signal generator 33 excites the signal generator 24 in accordance with signals from the controller 22.
  • the measurement signal from the sensor 25 is amplified via a measurement amplifier 26 and fed to the control 22.
  • the valve 27 is opened so that gas from the pressurized gas source can reach the sample tube 15 through the line 17 and its content into the sampling line 19 and from there to the analyzer.
  • the valves 13 and 14 are switched back again (from the position shown in FIG. 1B to the position shown in FIG. 1A), so that the sample tube is refilled becomes. Then the process described begins again.
  • a valve 13 can either be coupled directly to couple the vibrations into the liquid contained in the sample tube 15 vibrate and the vibrations on the valve 14th
  • FIG. 6 An increased sensitivity of the sensor or an increased efficiency of the signal generator can be achieved if the device shown in FIG. 6 is used.
  • This comprises a pipe socket 32 (eg made of V2A steel) coming from the valve 13 or 14, which has a flattened section.
  • a piezo element 28 piezo disk
  • the other surface of the piezo disk 28 is covered with a contact 29, so that an alternating current can be fed into the piezo element 29 via connecting wires 30, 31 - then the arrangement acts as a signal transmitter - or a corresponding alternating voltage can be removed - then the arrangement acts as a sensor.
  • the greatest possible error in this arrangement which occurs when there is no liquid (in FIG. 6) to the left of the pipe socket 32, is only small, since the length of the unfilled pipe section relative to the total length of the sample hose 15 is very low.
  • the signal generator and the sensor 25 are formed by electrodes.
  • the ohmic resistance between the electrodes is a measure of whether the sample tube 15 is completely filled or not.
  • the resistance between the electrodes depends to a large extent on the liquid being examined, its temperature, etc. In order to compensate for this dependency, it is advantageous to use a bridge circuit as shown in
  • Fig. 7 is shown.
  • a liquid-filled line 38 with electrodes 36 and 37 contained therein is then also used as the reference resistor, this line section forming a loop hanging downward. It can therefore be ensured that the loop is always filled with the liquid to be examined in an air-free manner.
  • the other elements shown in FIG. 7 and their interconnection are known per se.
  • Reference number 34 is one Designated alternating voltage source, with 35 a measuring device which transmits a signal from the control 22 corresponding to the alignment error.

Landscapes

  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Fluid Mechanics (AREA)
  • Acoustics & Sound (AREA)
  • Electromagnetism (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

Un dispositif de prélèvement ajustable d'échantillons de matières fluides, notamment de liquides, en cours de production, comprend une pompe (10) en communication avec un conduit d'aspiration (11) du côté d'admission, qui aspire la matière fluide, et avec un conduit de pression (12) du côté de sortie, qui est à son tour en communication avec un tuyau d'échantillonnage (15) à travers une vanne à trois voies. L'autre extrémité du tuyau d'échantillonnage (15) est en communication à travers une autre vanne à trois voies (14) avec un conduit d'évacuation (16), de sorte que l'on peut prélever la matière à examiner en cours de production au moyen de la pompe (10), la transporter à travers le tuyau d'échantillonnage (15) et la remettre à nouveau en circulation. La troisième entrée de la première vanne (13) est en communication avec une source (18) de gaz comprimé et la troisième entrée de la deuxième vanne (14) est en communication avec un conduit de prélèvement (19). Lorsque l'on commute les vannes (13, 14) de sorte que la pompe (10) ne puisse plus refouler la matière à prélever à travers le tuyau d'échantillonnage, le volume contenu dans le tuyau d'échantillonnage (15) reçoit directement le gaz comprimé et est conduit jusqu'à un dispositif d'analyse (23).
PCT/EP1991/000442 1990-03-20 1991-03-08 Dispositif de prelevement d'echantillons WO1991014932A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DEP4008915.0 1990-03-20
DE4008915 1990-03-20

Publications (1)

Publication Number Publication Date
WO1991014932A1 true WO1991014932A1 (fr) 1991-10-03

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Application Number Title Priority Date Filing Date
PCT/EP1991/000442 WO1991014932A1 (fr) 1990-03-20 1991-03-08 Dispositif de prelevement d'echantillons

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FI (2) FI911329A (fr)
WO (1) WO1991014932A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999000656A1 (fr) * 1997-06-17 1999-01-07 Neste Oy Systeme automatique d'echantillonnage et de traitement
DE19932050A1 (de) * 1999-03-12 2001-01-18 Hermann Reingruber Abrollbare Kugel am Ende des Ventilschafftes
EP1508791A1 (fr) * 2003-08-22 2005-02-23 Ismatec SA, Laboratoriumstechnik Dispositif de prélèvement automatique d'échantillons d'un bioréacteur
DE102004039378A1 (de) * 2004-08-13 2006-02-23 Hte Ag The High Throughput Experimentation Company Vorrichtung zur kontrollierten Entnahme von Fluidproben aus Druckbehältern

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2076797A5 (fr) * 1970-01-28 1971-10-15 Girolami Antoine
US3974681A (en) * 1973-10-23 1976-08-17 Jerry Namery Ultrasonic bubble detector
FR2308098A1 (fr) * 1975-04-18 1976-11-12 British Petroleum Co Dispositif d'echantillonnage pour liquides
US4361041A (en) * 1980-09-24 1982-11-30 The United States Of America As Represented By The United States Department Of Energy Non-intrusive ultrasonic liquid-in-line detector for small diameter tubes

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2076797A5 (fr) * 1970-01-28 1971-10-15 Girolami Antoine
US3974681A (en) * 1973-10-23 1976-08-17 Jerry Namery Ultrasonic bubble detector
FR2308098A1 (fr) * 1975-04-18 1976-11-12 British Petroleum Co Dispositif d'echantillonnage pour liquides
US4361041A (en) * 1980-09-24 1982-11-30 The United States Of America As Represented By The United States Department Of Energy Non-intrusive ultrasonic liquid-in-line detector for small diameter tubes

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999000656A1 (fr) * 1997-06-17 1999-01-07 Neste Oy Systeme automatique d'echantillonnage et de traitement
DE19932050A1 (de) * 1999-03-12 2001-01-18 Hermann Reingruber Abrollbare Kugel am Ende des Ventilschafftes
EP1508791A1 (fr) * 2003-08-22 2005-02-23 Ismatec SA, Laboratoriumstechnik Dispositif de prélèvement automatique d'échantillons d'un bioréacteur
WO2005019805A1 (fr) * 2003-08-22 2005-03-03 Ismatec Sa, Laboratoriumstechnik Dispositif d'echantillonnage de bioreacteur automatise
DE102004039378A1 (de) * 2004-08-13 2006-02-23 Hte Ag The High Throughput Experimentation Company Vorrichtung zur kontrollierten Entnahme von Fluidproben aus Druckbehältern
WO2006018247A1 (fr) * 2004-08-13 2006-02-23 Hte Aktiengesellschaft The High Throughput Experimentation Company Dispositif pour le prelevement controle d'echantillons de fluide dans des contenants sous pression

Also Published As

Publication number Publication date
FI911328A (fi) 1991-09-21
FI911329A (fi) 1991-09-21
FI911329A0 (fi) 1991-03-19
FI911328A0 (fi) 1991-03-19

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