US3618767A - Process and apparatus for continuous liquid sampling - Google Patents

Process and apparatus for continuous liquid sampling Download PDF

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Publication number
US3618767A
US3618767A US872482A US3618767DA US3618767A US 3618767 A US3618767 A US 3618767A US 872482 A US872482 A US 872482A US 3618767D A US3618767D A US 3618767DA US 3618767 A US3618767 A US 3618767A
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US
United States
Prior art keywords
stream
filter disk
liquid
sectors
afflux
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
US872482A
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English (en)
Inventor
Gottfried Thummel
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.)
Roche Diagnostics GmbH
Original Assignee
Boehringer Mannheim 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 Boehringer Mannheim GmbH filed Critical Boehringer Mannheim GmbH
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Publication of US3618767A publication Critical patent/US3618767A/en
Anticipated expiration legal-status Critical
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D33/00—Filters with filtering elements which move during the filtering operation
    • B01D33/15—Filters with filtering elements which move during the filtering operation with rotary plane filtering surfaces
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D33/00—Filters with filtering elements which move during the filtering operation
    • B01D33/44—Regenerating the filter material in the filter
    • B01D33/48—Regenerating the filter material in the filter by flushing, e.g. counter-current air-bumps
    • B01D33/50—Regenerating the filter material in the filter by flushing, e.g. counter-current air-bumps with backwash arms, shoes or nozzles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D33/00—Filters with filtering elements which move during the filtering operation
    • B01D33/80—Accessories
    • B01D33/82—Means for pressure distribution
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2201/00—Details relating to filtering apparatus
    • B01D2201/28—Position of the filtering element
    • B01D2201/287—Filtering elements with a vertical or inclined rotation or symmetry axis
    • 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
    • G01N1/18—Devices for withdrawing samples in the liquid or fluent state with provision for splitting samples into portions
    • 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
    • G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
    • 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
    • G01N2001/1006—Dispersed solids
    • G01N2001/1012—Suspensions
    • G01N2001/1025—Liquid suspensions; Slurries; Mud; Sludge
    • 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)

Definitions

  • PATENTEDNUV 9 ml SHEET 1 [IF 5 PATENTED 9 SHEET 3 [IF 5 FIG. 3
  • INVIZNTOR ow-FRIED Tn nn 51.
  • the present invention is concerned with a method and an apparatus for the continuous taking of clear samples of fluids
  • liquids such samples being used, e.g., for the analytical monitoring and control of chemical and physical processes.
  • FIG. 1 is a cross section through the simplest form of the apparatus according to the invention.
  • FIG. 2 is a cross section of a preferred embodiment.
  • FIGS. 3 and 4 are plane views of two difierent embodiments of the filter disk with separators, which can be incorporated in the apparatus of FIGS. 1 and 2.
  • FIG. 5 is a plane view of the masking plate 31 shown in FIG.
  • FIG. 6 is a plane view of the intermediate ring 24 shown in FIG. 2.
  • FIGS. 7 and 8 are cross-sectional views of preferred embodiments of the filter assemblies usable in apparatus according to FIGs. 2 (fixedly joined unit composed of filter disk and masking plate.)
  • FIG. 9 is a diagrammatic representation of a typical measuring system incorporating the invention which can be used to control processes.
  • the simplest embodiment of the apparatus of the invention shown in FIG. 1 consists of a housing I, an afi'lux line 2 and an efflux line 3, a seal 5 affixed to the housing 1 and provided with apertures 4 for the inflow and outflow, respectively, of the liquid specimens, and a cylindrical filter disk 6 which is rotatable about its central drive shaft 9.
  • the filter disk 6 is divided by impermeable separators 7 into a plurality of sectors 8 consisting of liquid porous material. It lies against the seal 5 in such a manner that each individual sector 8 is connected successively during each rotation both to the afilux line 2 and to the efi'lux line 3.
  • the housing 1 consists of a steel tube (inside diameter 5 cm.
  • the tube is closed at both ends by steel plates which are provided with apertures for the afflux line 2 and the efi'lux line 3 and for the central drive shaft 9.
  • the more or less elastic seal 5 which abuts on housing 1, consists of a conventional sealing material, and is preferably equipped with tapered apertures 4 so as to increase the effective filtering area.
  • the filter disk 6 consists of a sintered metal or other appropriate filter material, e.g., porcelain, and is divided by a plurality (six, in the case illustrated in FIGS. 3 and 4) of impermeable dividers 7 and 29 into the sectors 8 and 30.
  • the filter disk 6 is mounted on and actuated by square drive means 13 extending from shaft 9 and is fastened thereon by nut 38.
  • the filter disk 6 is pressed against the seal 5 in such a manner that, on the one hand, an adequate seal is assured, and, on the other hand, the friction therebetween does not become excessive.
  • the shaft cavity in the housing 1 is additionally provided with a sealing ring 12 to keep the liquid out of the housing cavity 11.
  • the filter assembly 27 consists of a porous filter disk 28 and a masking plate 31 affixed thereto, plane views of these two parts being given in FIGS. 4 and 5.
  • the filter disk is divided by the impermeable steel dividers 29 into sectors 30 of equal size.
  • the masking plate 31 is joined to the filter disk 28 by a matching annular sea 32 equipped with radial spokes in such a manner as to form separate shallow chambers 33.
  • an elastic gasket 22 is used, fitted therebelow with an intermediate ring 24 of polytetrafiuoroethylene that is only 0.5 to l mm. thick and which is shown separately in a plane view in FIG. 6.
  • This intermediate ring 24 serves particularly to reduce the frictional resistance of the gasket 22, and it is provided with arcuate slots 25.
  • lateral lugs 26 are provided on the intermediate ring 24 and are locked into the housing I by means of bolts.
  • the gasket 22 has cylindrical apertures 23 whose diameter is approximately the same as that of the afi'lux line 2 and the efflux line 3.
  • Apertures 37 of the same size in the masking plate 31 lead down into the individual shallow chambers 33.
  • the arcuate slots 25 in the intermediate ring 24 are of such a length that one or two apertures 37 are constantly in operative conduit alignment with affiux line 2, and one or two apertures are always in operative conduit alignment with efflux line 3.
  • the apparatus of this invention should be so immersed in said liquid that the moving stream of liquid impinges first on the aiflux line 2 of the apparatus to ensure continuous provision of fresh liquid thereto and to prevent aspiration of analyzed liquid from the efilux line 3 into afflux line 2.
  • FIGS. 7 and 8 Two additional embodiments of the filter assembly 27 are shown in FIGS. 7 and 8, and are designated as 27 and 27", respectively.
  • the annular seal 32 is eliminated, since the filter disk 28 or 28" and the masking plate 31' or 31" are joined directly together with one another.
  • the decision as to which type of filter assembly is to be given preference depends largely on the nature of the porous material and the dimensions of the entire filter assembly.
  • FIG. 9 illustrates the installation of the apparatus according to the invention designated by the overall reference numeral 14, in a typical monitoring and control system.
  • Pump 21 pumps clear liquid separated from the mash 15 through the rotating filter assembly 27 driven by motor 16 and the affiux line 2 into a thermostat l7, and from there to the onstream test cell 18 of monitoring and control apparatus 19.
  • the temperature of the thermostat somewhat higher than the temperature in the reaction vessel, because this prevents the formation of crystals in the test cell and in the lines running therefrom.
  • the liquid emerging from the test cell can be additionally heated in a heating coil such as 20, so as to assure that the filter disk segments will be washed out thoroughly by the liquid entering them from the efilux line 3.
  • the process according to the invention and the apparatus according to FIG. 2 are ideally suited for service in the racemate separation of a chloramphenicol intermediate. Utilizing the process and means according to the present invention, it is possible to take clear samples of liquid from suspensions of solids, especially crystal mashes, by using the filter apparatus according to the invention which avoids clogging of the filter disk by solid materials.
  • inorganic and organic liquids such as water, inorganic acids and bases, liquid ammonia or sulfur dioxide, aromatic or aliphatic hydrocarbons, halogenated hydrocarbons or organic acids or anhydrides such as for example, acetic acid or acetic anhydride, or organic bases such as for example, triethylamine or pyridine.
  • solid material formation may be caused by precipitation effects due to the addition of reagents or merely by temperature control used to recrystallize dissolved compounds, which may merely have been added to the solvent or which may have originated during a chemical process taking place.
  • the process and apparatus according to the present invention are especially useful in controlling catalyzed reactions in which solid catalysts are applied, as for instance, in hydrogenation, e.g. fluidized bed reactions using raney-nickel, raney-cobalt, noble metals as platinum or palladium or silver with or without inert carriers such as calcium carbonate, charcoal or alumina.
  • solid catalysts such as for example ionexchange resins with specific acidic or basic properties is also within the scope of the present invention.
  • Process for taking a clear fluid sample stream from a suspension of filterable material in such fluid comprises filtering a fluid afflux stream withdrawn from said suspension through a rotating filter disk comprising at least two sectors consisting of material porous to said fluid which sectors are separated from each other by radial spokes of impermeable material and wherein said sectors during each rotation of said filter disk are successively moved into operative conduit alignment with said afflux stream and an efflux stream, respectively, said efflux stream comprising the afflux stream after it has passed through a substantially closed-cycle loop and passing through a sector in a flow direction opposite to the flow direction of the afflux stream passing through that section.
  • Process for monitoring chemical processes occuring in a suspension comprising a solid suspended in a liquid which process comprises filtering a liquid afi'lux stream withdrawn from said suspension through a rotating filter disk comprising at least two sectors consisting of material porous to said liquid which sectors are separated from each other by radial spokes of impermeable material and wherein said sectors during each rotation of each filter disk are successively moved into operative conduit alignment with said afflux stream and an efflux stream, respectively, leading the resulting clear liquid sample stream to a measuring device, taking measurements of said clear liquid sample stream and returning said clear liquid sample stream as the efilux stream to said filter disk, wherein the efilux stream passes through a section of said filter disk in a flow direction opposite to the flow direction of the afflux stream passing through that section.
  • Apparatus for taking a clear fluid sample stream from a suspension of filterable material in such fluid which apparatus comprises a housing, an afflux line through which said sample stream is withdrawn from said suspension, an efflux line through which said sample stream is returned to said suspension, said afi'lux and efflux lines being disposed within said housing, a rotatable filter disk comprising at least two sectors consisting of material porous to said fluid which sectors are separated from each other by radial spokes of impermeable material, said filter disk being so disposed in said housing that said sectors, during each rotation of the filter disk about its axis, are successively moved into operative conduit alignment with the said afflux stream and efflux stream, respectively, so that the efflux stream passes through a section in a flow direction opposite to the flow direction of the afflux stream passing through that section, and means for rotating said filter disk about its axis.
  • each of said shallow chambers opens to an orifice in said masking plate forming a conduit for removing and returning said clear fluid sample stream, said filter disk assembly having means for being rotated continuously about its axis.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Hydrology & Water Resources (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
US872482A 1968-11-06 1969-10-31 Process and apparatus for continuous liquid sampling Expired - Lifetime US3618767A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19681807230 DE1807230A1 (de) 1968-11-06 1968-11-06 Verfahren und Vorrichtung zur kontinuierlichen Entnahme von klaren Fluessigkeitsproben

Publications (1)

Publication Number Publication Date
US3618767A true US3618767A (en) 1971-11-09

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US872482A Expired - Lifetime US3618767A (en) 1968-11-06 1969-10-31 Process and apparatus for continuous liquid sampling

Country Status (10)

Country Link
US (1) US3618767A (enrdf_load_stackoverflow)
JP (1) JPS4834195B1 (enrdf_load_stackoverflow)
AT (1) AT284515B (enrdf_load_stackoverflow)
CA (1) CA918448A (enrdf_load_stackoverflow)
CH (1) CH502116A (enrdf_load_stackoverflow)
DE (1) DE1807230A1 (enrdf_load_stackoverflow)
FR (1) FR2022710A1 (enrdf_load_stackoverflow)
GB (1) GB1228284A (enrdf_load_stackoverflow)
NL (1) NL6916719A (enrdf_load_stackoverflow)
SE (1) SE346381B (enrdf_load_stackoverflow)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3926804A (en) * 1972-06-13 1975-12-16 Pro Tech Inc Fluid filtration and sampling
US3997447A (en) * 1974-06-07 1976-12-14 Composite Sciences, Inc. Fluid processing apparatus
US4436633A (en) 1981-08-14 1984-03-13 Robinsky Eli I Filtration thickening method and apparatus
US4839046A (en) * 1987-08-20 1989-06-13 The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration Bio-reactor chamber
EP0724145A3 (en) * 1995-01-26 1998-02-25 Koei Industry Co., Ltd. Process and apparatus for filtrate measurement
WO2007135226A1 (en) * 2006-05-24 2007-11-29 Valtion Teknillinen Tutkimuskeskus A method for taking a liquid sample

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2154317B (en) * 1984-01-17 1987-08-12 English Clays Lovering Pochin Measurement of physical properties of the solid component of a slurry
DE3520489C1 (de) * 1985-06-07 1986-05-22 B. Braun Melsungen Ag, 3508 Melsungen Probeentnahmegeraet

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2066479A (en) * 1931-06-08 1937-01-05 Vernon W Macisaac Fluid straining method and apparatus
US2246877A (en) * 1937-06-08 1941-06-24 Aiken C Cunningham Rotary filter
US2446364A (en) * 1945-10-11 1948-08-03 Demarest Daniel Douglas Filtering device
US2823242A (en) * 1953-09-08 1958-02-11 Phillips Petroleum Co Process and apparatus for crystal purification and separation
US2989037A (en) * 1959-06-30 1961-06-20 Filippino Samuel Robert Automatic gravity feed water system and control
US3241675A (en) * 1962-06-04 1966-03-22 Ajem Lab Inc Rotary filter and method
US3490879A (en) * 1964-03-23 1970-01-20 Universal Oil Prod Co Fluid-solid contacting apparatus utilizing plural rotor members containing contact masses

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2066479A (en) * 1931-06-08 1937-01-05 Vernon W Macisaac Fluid straining method and apparatus
US2246877A (en) * 1937-06-08 1941-06-24 Aiken C Cunningham Rotary filter
US2446364A (en) * 1945-10-11 1948-08-03 Demarest Daniel Douglas Filtering device
US2823242A (en) * 1953-09-08 1958-02-11 Phillips Petroleum Co Process and apparatus for crystal purification and separation
US2989037A (en) * 1959-06-30 1961-06-20 Filippino Samuel Robert Automatic gravity feed water system and control
US3241675A (en) * 1962-06-04 1966-03-22 Ajem Lab Inc Rotary filter and method
US3490879A (en) * 1964-03-23 1970-01-20 Universal Oil Prod Co Fluid-solid contacting apparatus utilizing plural rotor members containing contact masses

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3926804A (en) * 1972-06-13 1975-12-16 Pro Tech Inc Fluid filtration and sampling
US3997447A (en) * 1974-06-07 1976-12-14 Composite Sciences, Inc. Fluid processing apparatus
US4436633A (en) 1981-08-14 1984-03-13 Robinsky Eli I Filtration thickening method and apparatus
US4839046A (en) * 1987-08-20 1989-06-13 The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration Bio-reactor chamber
EP0724145A3 (en) * 1995-01-26 1998-02-25 Koei Industry Co., Ltd. Process and apparatus for filtrate measurement
WO2007135226A1 (en) * 2006-05-24 2007-11-29 Valtion Teknillinen Tutkimuskeskus A method for taking a liquid sample

Also Published As

Publication number Publication date
AT284515B (de) 1970-09-25
CA918448A (en) 1973-01-09
CH502116A (de) 1971-01-31
FR2022710A1 (enrdf_load_stackoverflow) 1970-08-07
JPS4834195B1 (enrdf_load_stackoverflow) 1973-10-19
NL6916719A (enrdf_load_stackoverflow) 1970-05-11
SE346381B (enrdf_load_stackoverflow) 1972-07-03
GB1228284A (enrdf_load_stackoverflow) 1971-04-15
DE1807230A1 (de) 1970-05-27

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