US3109713A - Liquid analysis apparatus with closed flow cell - Google Patents

Liquid analysis apparatus with closed flow cell Download PDF

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Publication number
US3109713A
US3109713A US42258A US4225860A US3109713A US 3109713 A US3109713 A US 3109713A US 42258 A US42258 A US 42258A US 4225860 A US4225860 A US 4225860A US 3109713 A US3109713 A US 3109713A
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United States
Prior art keywords
liquid
stream
segments
flow cell
inlet
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
US42258A
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English (en)
Inventor
Ferrari Andres
Isreeli Jack
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.)
Bayer Corp
Original Assignee
Technicon Instruments Corp
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
Priority to BE593146D priority Critical patent/BE593146A/xx
Priority claimed from US828810A external-priority patent/US3109714A/en
Priority to GB24081/60A priority patent/GB923285A/en
Application filed by Technicon Instruments Corp filed Critical Technicon Instruments Corp
Priority to US42258A priority patent/US3109713A/en
Priority to FR833032A priority patent/FR1262910A/fr
Priority to CH832760A priority patent/CH394127A/de
Priority to GB18131/61A priority patent/GB919759A/en
Priority to FR864744A priority patent/FR1292062A/fr
Priority to CH806661A priority patent/CH431462A/de
Priority to BE605995A priority patent/BE605995A/fr
Publication of US3109713A publication Critical patent/US3109713A/en
Application granted granted Critical
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D19/00—Degasification of liquids
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/72—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using flame burners
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/08—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a stream of discrete samples flowing along a tube system, e.g. flow injection analysis

Definitions

  • the present invention relates to automatic analysis apparatus and, more particularly, -to such apparatus which includes a closed flow cell of a colorimeter for the colorimetric analysis of a liquid stream to quantitatively determine a constituent thereof.
  • the apparatus may be used for analyzing a series of individual samples or may be used ⁇ for monotoring a system continuously, for example, a steam power plant on a ship.
  • the invention is especially useful 4in its application to automatic continuous analysis apparatus of the type described, for example, in United States Patent No. 2,797,- 149, of the assignee of the present application, wherein streams of fluid .are transmitted through small tubular passages which are provided in such apparatus.
  • air is introduced into the liquid streams lto divide them into a series of successive small segments separated from each other by intervening air segments or bubbles which serve to cleanse the internal walls of the passages.
  • air is also introduced between successive samples of the liquids to separate the samples from each other and to provide a cleansing action of the passages between successive samples in order to prevent contamination of one sample by another, which might otherwise occur due to the fact that the samples are introduced into the passages in series one after the other in a tlowing stream.
  • the apparatus is being employed to monitor, for example, the chlorine content in the boiler feed water of a steam power plant which is installed aboard a ship, it is necessary that the apparatus be in a closed system so that the pitching, rolling and yawing of the ship does not cause any spilling of the liquids in the system and, therefore, the flow cell of the colorimeter must be of the closed or non-vented type.
  • the air or other inert separable tluid introdu-ced into the liquid stream is removed prior to its introduction into the llow cell of the colorimeter.
  • a blender is provided in the path of llow of the liquid segments so that they are consolidated into a continuous liquid stream for flow through the tlow cell for proper operation of the colorimeter and a colorimeter controlled recorder.
  • FIG. l is a more or less diagrammatic view illustrating the apparatus according to the present invention.
  • FIG. 2 is a view of part of the apparatus of FIG. l, on a larger scale, partly in section and partly in perspective.
  • the apparatus comprises a proportioning pump 12 which has pro- 3,109,713 Patented Nov. 5, 1963 ice vision for pumping a plurality of fluids for the continuous treatment of a liquid stream for colorimetric analysis.
  • the treated stream is colorimetrically analyzed in the colorimeter 14 which operates a recorder 16, in a well known manner, to record the results of the colorimetric analysis.
  • the ow of cell 18 of the colorimeter is in the form of a hollow cylinder and has transparent end walls 20 and 22 which are therefore permeable to light and through which a beam of light 24 passes for the colorimetric examination of the liquid in the ow cell.
  • :light beam Z4 comes from a suitable light source (not shown) and is absorbed in accordance with the light transmittance qualities of the liquid. The degree of absorption of the light by the liquid is measured by a photoelectric device (not shown) which is placed in the path of the light beam which passes through end wall 22 of the llow cell.
  • the ow cell includes the tubular members or nipples 26 and 28 which provide a liquid inlet and a liquid outlet, respectively, for the flow of liquid into and out of the ilow cell. Except for the liquid inlet and liquid outlet, the How cell is completely closed and does not include any vent openings. Accordingly, such a ow cell may be placed an any of a plurality of positions without any spilling occurring of the liquid through an opening in the ow cel-l. This is especially advantageous when the flow cell is used in an analysis apparatus or system which may be aboard a ship or other moving vehicle and the pitching, rolling and yawing of the vehicle will not cause any spilling of the liquid in the liow cell.
  • the fluid stream as it flows through a tube or conduit 30 from the pump 12 is composed of segments of liquid L and intervening segments G of air, which is introduced into the stream of the liquid under analysis at iitting 32 where ythe stream of liquid flowing in tube or conduit 34 joins the stream of air flowing in conduit or tube 36.
  • the liquid under analysis Y is introduced into the system by way of pump tube 38 and the air is introduced into the system by way of pump tube 40.
  • any other suitable inert separable fluid may be used to divide the liquid stream into alternate segments of liquid separated from each other by intervening segments of fluid.
  • the segmented stream flows from the outlet of the fitting 32 through a Itube or conduit 42 where it joins a stream of processing liquid or color reagent tlowing in conduit 44.
  • the processing liquids are introduced into the system by way of pump tubes 46 and 48 and flow through conduits or tubes 50 and 52, respectively, to fitting 54 where they join each other and are mixed together in helical mixing coil 56.
  • the segmented stream consisting of liquid segments containing sample and processing liquid or reagent separated by intervening segments of air is transmitted by the action of the pump through conduit or tube 58 to a helical mixing coil 60, where the liquids in each of the liquid segments L are mixed with each other.
  • the outlet end of mixing coil 60 is connected to conduit 30 which transmits the segemented stream to a tting or separating device 62 which is positioned at a point upstream of the inlet to the flow cell and removes and separates lthe air segments of the stream from lthe liquid segments.
  • the itting 62 comprises tubular inlet part 64, tubular outlet part 66 and tubular oitake par-t 68 which is intermediate the inlet land outlet par-ts of the iitting and is connected by a conduit 70 to lthe pump tube72.
  • the air segments or bubbles G are separated from the segmented stream by the aspirating action of the pump an-d ow through opening 74 in fitting 62 into ofltake part 68 and conduit 70, along with small quantities of the liquid segments,
  • a blender device 76 Disposed between fitting 62 and the flow cell is a blender device 76, preferably made of glass, which assists in the blending of the individual liquid segments into a continuous consolidated stream of liquid.
  • the blender device is a tubular member consisting of a series of spherical hollow parts 78 separated from each other lengthwise of the path of flow of the stream by a series of intervening tubular connecting parts 80.
  • the liquid segments alternately and continuously change their velocities as they flow successively Ithrough the spherical parts and tubular parts, which results in a thorough blending of adjacent liquid segments with each other, so that a consolidated liquid stream flows to the inlet 26 of the flow cell, which is connected to the outlet end of the blender 76.
  • other lblender means for the liquid segment for example the helical mixing coil shown in U.S. Patent No. 2,933,293 which is owned -by the assignee of the present invention.
  • outlet 28 of the flow cell preferably extends to a discharge position remote from the colori-meter 14.
  • Outlet 28 is preferably so arranged that a part thereof (not shown) extends higher than the flow cell so that the flow cell is completely filled with liquid at all times.
  • Pump 12 may be of any suitable type. As here shown it is la proportioning pump of the type described in U.S. Patent No. 2,893,324. Briefly described, this type of pump comprises a platen 82 and the flexible pump tubes 38, 40, 46, 48 and 72 which are resiliently compressible and are all simultaneously compressed progressively along their lengths against platen 82 by transverse pressure rollers 84 carried by conveyor sprocket chains 86 which are driven by a shaft 88 actuated by a motor (not shown). Said chains 86 are carried by a frame 90 which is pivoted at 92 so that said pressure rollers can be moved to a retracted position out of engagement with the pump tubes for access to the latter when desired.
  • the apparatus may be employed for the continuous analysis of a flowing stream of a series of samples or for the analysis of a continuous liquid stream and is especially useful where the apparatus must be installed in a vehicle which may move in a plurality of directions.
  • the apparatus is particularly useful for determining, for example, the chloride content in the boiler feed water of a steam power plant aboard a ship.
  • the boiler feed water is continuously supplied as a stream to pump tube 38 and air or other suitable inert and separable fluid is supplied to pump tube 40.
  • a 6% solution of ferrie alum FeNH4(SO4) %N HNO3 is supplied to pump tube 46 and a saturated solution of mercuric thiocyanate Hg(CNS)2 is supplied to pump tube 48.
  • the streams of ferrie alum and mercuric thiocyanate are mixed in helical mixing coil 56 and join the segmented liquid stream of boiler feed water flowing in conduit 42.
  • the mixed reagent joins each of the liquid segments in the segmented stream and is mixed with the boiler feed water in each liquid segment in helical mixing coil 60.
  • the air segments in the segmented stream are removed in fitting 62 and the liquid segments are blended together in blender 76 and are transmitted, as a consolidated stream, to the flow cell 18 where ⁇ the color of the stream is measured to indicate the quantity of the chlorine present in the boiler feed water.
  • the results of this measurement are recorded on the recorder 16 which is operated under the control of the colorimeter 14 in a well known manner.
  • a system of liquid treatment and analysis in which the liquid is transmitted in the form of a stream and is treated while in transit for analysis, said system including tubular means through which said stream flows, means for .introducing an inert separable fluid int-o said liquid stream in said tubular means to divide said liquid stream into a segmented stream comprised of a series of liquid segments separated by intervening segments of said inert fluid; a flow cell comprising a closed tubular chamber having a peripheral wall provided with a liquid inlet to receive liquid from said tubular means and with a liquid outlet and otherwise closed to the passage of fluid, said outlet being spaced from said inlet as measured along the longitudinal axis of said chamber, said chamber comprising a hollow cylinder having opposite end walls permeable to the passage of light therethrough for the transmission of light Ithrough the liquid in said cell to colorimetrically examine the liquid in said chamber of said flow cell, said opposite end walls closing said cylinder except for said inlet and outlet, means in communication with said tubular means at a point upstream of said
  • a flow cell comprising a closed tubular chamber having a peripheral wall provided with a liquid inlet and with -a liquid outlet and otherwise closed to the passa-ge of fluid, said outlet being spaced from said inlet as measured yalong the longitudinal ⁇ axis of said chamber, said chamber comprising a hollow cylinder having end walls permeable to the passage of light therethrough for the transmission of light through the liquid in said cell to colorimetrically examine the liquid in said chamber of said flow cell, said opposite end walls closing said cylinder except for said inlet and outlet, a tubular passage for the flow of liquid to said flow cell, means for removing said inert fluid segments from said segmented stream during the flow thereof in said passage
  • said chamber comprising a hollow cylinder having end walls permeable to the passage of light therethrough for the transmission of light through the liquid in said cell to colorimetrically examine the liquid in said chamber of said llow cell, a tubular passage which is in communication with said inlet of the flow cell, means for removing said inert fluid segments from said segmented stream during lthe oW thereof and prior to the introduction of said liquid into said flow cell, said tubular passage having an opening therein upstream of said inlet of the flow cell, suction means connected to said opening for aspirating said inert fluid segments from said segmented stream for said removal of the segments as said stream flows through said passage to said flow cell, and liquid blender means inserted between said tubular passage and said
  • a system of liquid treatment and analysis in which the liquid is transmitted in the form of a stream and is treated while in transit for analysis, said system including means for introducing an inert separable iluid into said liquid stream to divide said liquid stream into a segmented stream comprised of a series of liquid segments separated by intervening segments of said inert iluid; a ow cell comprising a closed tubular chamber having a peripheral wall provided with a liquid inlet and with a liquid outlet and otherwise closed to the passage of uid, said outlet being spaced from said inlet as measured along the 1ongitudinal axis of said chamber, said chamber comprising a hollow cylinder having end walls permeable to the passage of light therethrough for the transmission of light through the liquid in said cell to colorimetrically examine the liquid in said chamber of said ow cell, said opposite end walls closingsaid cylinder except for said inlet and outlet, a tubular passage in communication with said inlet of the flow cell, means for removing said inert uid segments
  • liquid blender means in said tubular passage between said opening and said ilow cell for blending said liquid segments together after the removal of said fluid segments to form a consolidated liquid stream
  • said liquid blender means comprising a tubular member having a series of hollow spherical portions connected to each other by a series of intervening tubes, said spherical port-ions having a different cross sectional area transversely of the direction of ow of said liquid segments than said tubes to vary ythe velocity of tlow of said liquid segments through said liquid blender means.
  • a system of liquid treatment and analysis in which i the liquidis transmitted in the form of a stream and is treated while in transit for analysis, said system including means for introducing ⁇ an inert separable uid into said liquid stream to divide said liquid stream into a segmented stream comprised of a series of liquid segments separated by intervening segments of said inert lluid; a ow cell comprising a closed tubular chamber having la peripheral wall provided with a liquid inlet and with a liquid outlet and otherwise closed to the passage of fluid, said outlet being spaced from saidl inlet as measured along its longitudinal axis of said chamber, said chamber comprising a hollow cylinder having end walls permeable to the passage of light therethrough for the transmission of light through the liquid in said cell to colorirnetrically examine the liquid in said chamber of said ilow cell, said opposite end walls closing said cylinder except for said inlet and outlet, a tubular passage connected to the inlet of said ilow cell, means fo-r removing said inert fluid segments

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Optical Measuring Cells (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Automatic Analysis And Handling Materials Therefor (AREA)
US42258A 1959-07-22 1960-07-12 Liquid analysis apparatus with closed flow cell Expired - Lifetime US3109713A (en)

Priority Applications (9)

Application Number Priority Date Filing Date Title
BE593146D BE593146A (en)) 1959-07-22
GB24081/60A GB923285A (en) 1959-07-22 1960-07-11 Separating fluids from each other during analysis
US42258A US3109713A (en) 1959-07-22 1960-07-12 Liquid analysis apparatus with closed flow cell
FR833032A FR1262910A (fr) 1959-07-22 1960-07-15 Appareil pour la séparation de deux fluides
CH832760A CH394127A (de) 1959-07-22 1960-07-20 Verfahren und Vorrichtung zur automatischen, kontinuierlichen Behandlung von Flüssigkeiten für Analysen oder andere Zwecke
GB18131/61A GB919759A (en) 1959-07-22 1961-05-18 Liquid analysis apparatus with closed flow cell
FR864744A FR1292062A (fr) 1959-07-22 1961-06-13 Appareil automatique d'analyse au colorimètre
CH806661A CH431462A (de) 1959-07-22 1961-07-10 Verfahren und Vorrichtung zum automatischen, kontinuierlichen und kolorimetrischen Analysieren von Stoffen
BE605995A BE605995A (fr) 1960-07-12 1961-07-11 Appareil automatique d'analyse au colorimètre

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US828810A US3109714A (en) 1959-07-22 1959-07-22 Means for separating fluids from each other
US42258A US3109713A (en) 1959-07-22 1960-07-12 Liquid analysis apparatus with closed flow cell

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US3109713A true US3109713A (en) 1963-11-05

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US42258A Expired - Lifetime US3109713A (en) 1959-07-22 1960-07-12 Liquid analysis apparatus with closed flow cell

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US (1) US3109713A (en))
BE (1) BE593146A (en))
CH (2) CH394127A (en))
FR (1) FR1262910A (en))
GB (2) GB923285A (en))

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3236602A (en) * 1962-05-03 1966-02-22 Technicon Instr Colorimeter flow cell and holder therefor
US3332748A (en) * 1964-07-20 1967-07-25 Courtaulds Ltd Extraction of hop bitters from beer with iso-octane using synchronized pulses in a helical coil
US3404962A (en) * 1964-10-22 1968-10-08 Honeywell Inc Apparatus for detecting a constituent in a mixture
US3435684A (en) * 1967-10-02 1969-04-01 Technicon Corp Method and apparatus for the dilution and division of a stream of samples for continuous analysis
US3512936A (en) * 1967-09-06 1970-05-19 Technicon Corp Liquid analysis method and apparatus therefor
US4212845A (en) * 1977-07-06 1980-07-15 The Rank Organisation Limited Analytical apparatus
EP0200235A2 (en) 1982-11-15 1986-11-05 TECHNICON INSTRUMENTS CORPORATION(a Delaware corporation) Continuous flow method
DE3931971A1 (de) * 1989-09-25 1991-04-04 Knapp Guenter Univ Prof Dipl I Vorrichtung zur aufbereitung von fluessigen analysenproben
EP2033699A2 (en) 2007-09-10 2009-03-11 Samsung Electronics Co., Ltd. 3-dimensional air bubble trapping apparatus and method thereof
WO2014191022A1 (en) * 2013-05-28 2014-12-04 Ibis Technologies B.V. Measuring system, such as an interaction measuring system and a measuring method

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3518010A (en) * 1967-03-03 1970-06-30 Technicon Corp Colorimeter
US4804519A (en) * 1987-03-06 1989-02-14 Thermo Jarrell Ash Corporation Sample analysis apparatus
FR2673382B1 (fr) * 1991-03-01 1994-04-08 Hospal Industrie Dispositif pour eliminer les bulles de gaz d'un liquide en circulation.
DE20113127U1 (de) * 2001-08-14 2001-10-18 Berger, Bruno, Braunau Schrägrohrreaktor

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1658950A (en) * 1927-04-15 1928-02-14 Stein Berthold Apparatus for determining the alcohol in a liquid
US2462995A (en) * 1947-04-11 1949-03-01 Gulf Oil Corp Process control system
US2797149A (en) * 1953-01-08 1957-06-25 Technicon International Ltd Methods of and apparatus for analyzing liquids containing crystalloid and non-crystalloid constituents
US2899280A (en) * 1957-03-06 1959-08-11 Method of fluid analysis
US2967764A (en) * 1958-04-24 1961-01-10 Technicon Instr Apparatus for analysis and other processing of fluids
US2999673A (en) * 1959-08-05 1961-09-12 Technicon Instr Liquid mixing means
US3010800A (en) * 1956-10-09 1961-11-28 Technicon Chromatography Corp Analysis and recording apparatus
US3047367A (en) * 1959-12-01 1962-07-31 Technicon Instr Automatic analysis with fluid segmentation

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1658950A (en) * 1927-04-15 1928-02-14 Stein Berthold Apparatus for determining the alcohol in a liquid
US2462995A (en) * 1947-04-11 1949-03-01 Gulf Oil Corp Process control system
US2797149A (en) * 1953-01-08 1957-06-25 Technicon International Ltd Methods of and apparatus for analyzing liquids containing crystalloid and non-crystalloid constituents
US3010800A (en) * 1956-10-09 1961-11-28 Technicon Chromatography Corp Analysis and recording apparatus
US2899280A (en) * 1957-03-06 1959-08-11 Method of fluid analysis
US2967764A (en) * 1958-04-24 1961-01-10 Technicon Instr Apparatus for analysis and other processing of fluids
US2999673A (en) * 1959-08-05 1961-09-12 Technicon Instr Liquid mixing means
US3047367A (en) * 1959-12-01 1962-07-31 Technicon Instr Automatic analysis with fluid segmentation

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3236602A (en) * 1962-05-03 1966-02-22 Technicon Instr Colorimeter flow cell and holder therefor
US3332748A (en) * 1964-07-20 1967-07-25 Courtaulds Ltd Extraction of hop bitters from beer with iso-octane using synchronized pulses in a helical coil
US3404962A (en) * 1964-10-22 1968-10-08 Honeywell Inc Apparatus for detecting a constituent in a mixture
US3512936A (en) * 1967-09-06 1970-05-19 Technicon Corp Liquid analysis method and apparatus therefor
US3435684A (en) * 1967-10-02 1969-04-01 Technicon Corp Method and apparatus for the dilution and division of a stream of samples for continuous analysis
US4212845A (en) * 1977-07-06 1980-07-15 The Rank Organisation Limited Analytical apparatus
EP0200235A2 (en) 1982-11-15 1986-11-05 TECHNICON INSTRUMENTS CORPORATION(a Delaware corporation) Continuous flow method
DE3931971A1 (de) * 1989-09-25 1991-04-04 Knapp Guenter Univ Prof Dipl I Vorrichtung zur aufbereitung von fluessigen analysenproben
EP2033699A2 (en) 2007-09-10 2009-03-11 Samsung Electronics Co., Ltd. 3-dimensional air bubble trapping apparatus and method thereof
EP2033699A3 (en) * 2007-09-10 2011-04-20 Samsung Electronics Co., Ltd. 3-dimensional air bubble trapping apparatus and method thereof
WO2014191022A1 (en) * 2013-05-28 2014-12-04 Ibis Technologies B.V. Measuring system, such as an interaction measuring system and a measuring method
US11442010B2 (en) 2013-05-28 2022-09-13 Ibis Technologies B.V. Measuring system, such as an interaction measuring system and a measuring method
EP3004897B1 (en) * 2013-05-28 2024-12-18 Ibis Technologies BV Measuring system, such as an interaction measuring system and a measuring method

Also Published As

Publication number Publication date
CH431462A (de) 1967-03-15
FR1262910A (fr) 1961-06-05
BE593146A (en))
GB923285A (en) 1963-04-10
GB919759A (en) 1963-02-27
CH394127A (de) 1965-06-30

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