CN103782154A - A flow cell for measuring electromagnetic radiation absorption spectra in a continuously flowing immiscible liquid(s) or liquids with entrained gas phases - Google Patents
A flow cell for measuring electromagnetic radiation absorption spectra in a continuously flowing immiscible liquid(s) or liquids with entrained gas phases Download PDFInfo
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- CN103782154A CN103782154A CN201280043363.2A CN201280043363A CN103782154A CN 103782154 A CN103782154 A CN 103782154A CN 201280043363 A CN201280043363 A CN 201280043363A CN 103782154 A CN103782154 A CN 103782154A
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- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N21/05—Flow-through cuvettes
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- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N2021/0346—Capillary cells; Microcells
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- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N21/05—Flow-through cuvettes
- G01N2021/054—Bubble trap; Debubbling
Abstract
An apparatus and method for spectral analysis of immiscible phases are disclosed. A flow cell for online absorption measurements of immiscible process phases can comprise: a body containing an inlet window and an outlet window in operable communication with a measurement instrument, and a series of partitions that divide the inside of the flow cell into three (3) or more vessels that have an inlet and an outlet, wherein the vessels are connected in series with one another. Optionally, the first vessel is equipped with a porous membrane to facilitate the separation of immiscible process phases.
Description
Technical field
The present invention relates to the field of in-situ measurement equipment and can flow for passing through absorption spectroanalysis Direct Analysis industrial process.
Background technology
It is known flowing (industrial stream) with online process analysis procedure analysis (the on-line process analysis) industry of the flow cell that comprises optical sensor (flow-through cell).Conventionally,, for industrial process is measured, after measuring, sample is flowed to return course pipeline (process line) to avoid product waste in the flow cell that comprises optical sensor.Before measuring, often need to anticipate process sample.
Conventionally, flow cell arranges two optical windows to allow electromagnetic radiation to pass first window, flow and pass Second Window out through industrial process.Generally be back to the long-range spectrometer that is positioned at for measuring with the light that optical fiber cable guides to input source radiation flow cell and also guides the part producing " to be absorbed ".
Simple flow pond by two parallel optical sheet structures is known.Distance between optical sheet is defined as optical path length.Process liquids stream is analyzed in the time of the spacing by between optical window.This flow cell is for on-line analysis biofluid, colloidal dispersion system and hydrocarbon.Being characterized as simple structure and can only not needing sample preparation or pre-service for sample analysis of these flow cells.Some analyses require careful temperature control, in these cases, flow cell can be placed in thermostatic control bath.This may be particularly useful to the temperature controlled reaction that wherein heat release need to be careful in flow cell.These measuring cells are limited to their structural strength and are not suitable for measuring under high pressure or high mechanical stress.
Flow measurement pond is used in high performance liquid chromatography (HPLC) analysis and Capillary Electrophoresis conventionally.The flow cell of this type is conventionally constructed, is had little volume and conventionally have short sample " path " by firm/durable material.Due to the mechanical stress by high pressure and the caused rising of high process flow rate, to application in industrial process, other requirement is proposed.Also these ponds must be designed to resist the Latent destruction effect of process medium, for example, can be angled to reduce the mechanical stress on optical window with optical path direction by entrance and exit channel arrangement.In the time using, can make pond supporter to extend the term of life in pond by inert plastic together with corrosivity process streams.
Some flow cells are used to the optical measurement under high pressure process.Other flow cells are designed to the optical absorption measurement of little liquid volume.By the nickel kapillary with polished inner surface for using the optical measurement of multiple radiation reflection.
The flow cell with multiple capillary analysis devices is designed for to biology capillary analysis.Use this class flow cell to allow minimizing of sample volume.Short path length flow cell is used in ultraviolet region, visible range or the middle infrared of electromagnetic radiation spectrum and obtains measurement result.But the relative absorbance of observing in the near-infrared region of electromagnetic radiation spectrum significantly reduces, thereby path that need to be longer is to minimize sample analysis error.
Liquid can also comprise the dissolved gases under the high pressure of can interference spectrum measuring.Can comprise the air separation being arranged on before measuring cell for the layout of analysis and Control metallurgical production.
As mentioned above, carried out optical measurement for various process condition.But prior art is not yet described for measuring the process streams that comprises one or more immiscible liquids phases or designing for the suitable pond that comprises process streams dissolving or a large amount of (bulk) gases.But aforesaid pond can be used for analyzing even sample is not suitable for measuring the process sample with immiscible phase.The process sample that comprises one or more immiscible phases causes in the obvious light scattering at each phase interface place (light dispersion) and causes unacceptable measuring error.
What need in the art is the flow cell that can measure immiscible liquids phase.
Summary of the invention
The application is provided for the flow cell of online absorptiometry unmixing process phase and uses its method.
In one embodiment, the flow cell of the unmixing process phase that comprises liquid phase and/or gas phase for online absorptiometry, can comprise: comprise the main body that can operate entrance window and the outlet window of communication with surveying instrument; With a series of dividing plates that by the internal separation of flow cell are three (3) or the containers with entrance and exit more, the wherein container connection that is one another in series.Alternatively, the first container is equipped with perforated membrane to promote the separation of unmixing process phase.
The method of the online absorptiometry of the immiscible phase that in one embodiment, comprises liquid phase and/or gas phase comprises: flow cell is associated with the process streams that comprises immiscible phase; And carry out the measurement of immiscible phase.Flow cell can comprise comprise with surveying instrument can operate communication entrance window and outlet window main body; Be a series of dividing plates of the three or more containers with entrance and exit by the internal separation of flow cell, the wherein container connection that is one another in series, and wherein the first container is equipped with perforated membrane.
The method of in another embodiment, carrying out the online absorptiometry of Immiscible fluid phase comprises: Immiscible fluid is introduced to flow cell; Separate Immiscible fluid phase with dividing plate at the inner perforated membrane that uses of flow cell; And measure the Immiscible fluid phase of above-mentioned separation.
These and other non-limiting features are below more specifically described.
Accompanying drawing explanation
With reference to exemplary, nonrestrictive accompanying drawing, and wherein identical element by identical numbering.
Fig. 1 illustrates according to the schematic diagram of the flow cell of an embodiment of the invention.
Fig. 2 is the curve map that uses the hydrogen phosphide cumene within 10 hours (cumene hydroperoxide, the CHP) concentration of common pond measurement.X-axis be take hour as time and the Y-axis of unit be CHP percent by weight (wt%) (from 19.7815 to 81.6681).
Fig. 3 is the curve map that uses the CHP concentration within 10 hours of the application's improved flow cell measurement.X-axis be take hour as time and the Y-axis of unit be CHP wt%(from 12.9 to 13.5).
Fig. 4 is the schematic diagram for measure the flow cell of hydrogen phosphide cumene concentration at cumene oxidation stream.
Embodiment
In order to address this problem, to design improved flow cell, and be configured to first separate each immiscible phase and then allow independent analysis (for example, spectrophotometric analysis (spectrophotometric analysis) etc.) each separates phase.In this improved flow cell, construct a series of connection containers and make to separate immiscible phase and guide to mutually different containers by what separate subsequently in the first container.Then, each absorption of electromagnetic radiation spectrum of the various phases of each phase be can obtain separately, detectability and the degree of accuracy improved produced.As required, by the application of specific process can to one or institute be separative measures mutually.
Definition:
The word of odd number can mean plural number, unless specifically described in addition.
" combination " comprises admixture, potpourri, alloy, reaction product etc.
Term " first ", " second " etc. do not represent any order, quantity or importance in this article, but for distinguishing between key element.
Unless separately have herein statement or with the obvious contradiction of context, otherwise term " one " and " " and " being somebody's turn to do " herein does not represent restricted number, but is interpreted as encompasses singular and plural number.
As used in this article suffix " (s) " be intended to the odd number of the term that comprises its modification and plural number both, thereby comprise one or more (for example, pond comprises one or more ponds) of this term.
Run through reference " a kind of embodiment ", " another kind of embodiment ", " embodiment " of instructions etc., (for example refer to described special key element relevant to embodiment, feature, structure and/or characteristic) be included at least one embodiment described herein, and can maybe cannot be present in other embodiments.In addition, should be appreciated that described key element can be combined in different embodiments in any suitable manner.
" gently " and " weight " liquid is relative terms is less than another kind of liquid density to identify respectively a kind of density of liquid.Those having ordinary skill in the art will appreciate that the implication of these terms in the context of present disclosure.
" subregion " can comprise baffle (baffle).
The stream that " fast loop " means to make a part to be analyzed around pond by pipeline or conduit flow rate is reduced to optimum value.Loop fast, that is, bypass, allows enough sample flow to approach with process in time to guarantee measured sample, thereby prevents the obvious delay in analysis.
As mentioned above, disclosure relates to and comprising for the flow cell of the device of on-line monitoring with for utilizing the method for electromagnetic radiation (it utilizes said apparatus) spectral measurement immiscible liquids and/or gas phase.
Below flow cell is the cable that bears its process streams condition standing in greater detail.Flow cell as fluid (liquid and/or gas) can Information Monitoring medium.Flow cell for example has, with the sensor (, spectrum sensor) of flow cell communication and makes to gather measurement result (for example, results of spectral measurements).Plumbing installation (plumbing), concerning the application's object, it comprises that electrical connection and the various component parts by device are placed as and the necessary conduit of flow cell communication, for example, optical sensor and process streams assembly, can be realized and without too much experiment by those of ordinary skill in the art.
A device
In one embodiment, device comprises: the main body that comprises one or more entrance windows and one or more outlet windows (for example, framework, housing, container etc.), wherein, depend on the requirement of surveying instrument, window can be optical window, with one or more surveying instruments (for example, Raman spectrometer, fluorescence spectrophotometer, refractive index measuring instrument, gas chromatograph, liquid chromatograph, mass spectrometer and comprise at least one the combination in above-mentioned) (be for example coupled to, can operate communication) a series of dividing plates, for example, baffle, it is three (3) or the container with one or more entrances and one or more outlets by the internal separation of flow cell more.The operate of the connection container that container connects based on being one another in series.The first container can be equipped with perforated membrane to promote to separate unmixing process phase, for example, and phase in the middle of phase and/or one or more liquid/gas in the middle of one or more liquid/liquid.
The flow cell that present disclosure embodies and process streams (for example, industrial process stream) are relevant.Those of ordinary skill in the art can be configured to the plumbing installation that flow cell is associated with process fluid.This can complete and not need too much experiment.
Select O-ring seal, accessory and main body that material for constructing flow cell makes pond to all the components of phase to be analyzed stable and, if adopt spectral measurement, enough rigidity do not change the optical path length in pond in the time being exposed to process measurement condition.Desirably, optical window is positioned to become about 85 to 105 degree (desirably becoming 90 degree) with process streams and can make source (the optics entrance in pond) and export (leaving the optical path in pond) and aims at so that light loss minimizes.
Can for example, by the transparent any material of the wavelength of analyzing for particular procedure (being enough to allow the transmission of the recently mass measurement of noise to expect) is formed to optical window.In various embodiments, measure according to ASTM D1003-07, rules A, for example, use from HAZE-GUARDDUAL, the use integrating sphere (0 °/diffusion geometric configuration) of BYK-Gardner measured, material can have and is more than or equal to 80%, is more than or equal to particularly 90% and be more specifically more than or equal to 95% transmission, wherein, spectrum sensitivity is consistent with International Commission on Illumination (CIE) standard spectrum value under standard lamp D65.
Some examples of possible material comprise there is the transmissivity of expectation and the synthetic sapphire compatible with process streams, quartz, glass (for example, Pyrex), plastics (for example, polycarbonate, the acrylic compounds etc. of optical grade) etc.
Physical parameter, includes but not limited to, dividing plate height, and its height ratio that can be regulated to realize expectation by those of ordinary skill in the art is to realize the necessary separation of one or more liquid and/or one or more gases.This can complete and not need excessive experiment.
Perforated membrane can be coalescent film (coalescing film).Coalescent film (porosint) should separate various discontinuous phases by particle or the drop in coalescent dispersion within reasonable time desirably.Generally speaking, expect each porosint mutually with significantly different angle of wettings to be separated.The suitable porosity of coalescing medium is also a factor.If hole is excessive, the drop that is not all dispersions all will contact with coalescing medium.Do not have coalescent any drop to suitable phase to cause higher measuring error.The existence of surfactant can make this be difficult to maybe can not occur.For constructing silicon/fluorinated material that some materials of coalescent film comprise fluorinated material, silicon materials or combination.These materials are wetting very poor by water, and therefore mainly make gentle out-of-date (reject) water that plays a part to reject that communicates of organic phase.
In liquid stream and/or air-flow, can carry out spectral measurement by the multiple technologies compatible with measurement.The method of spectral measurement includes but not limited to, ultraviolet electromagnetic radiation, both visible electromagnetic radiation and/or infrared electromagnetic radiation.
In one embodiment, spectral instrument utilizes Connectorized fiber optic cabling.
Flow cell, it is for the storage of for example fluid media (medium) of industrial process medium (, liquid and/or gas medium), must be able to measure by spectral analysis.
In one embodiment, pond is designed to utilize ultraviolet electromagnetic radiation, both visible electromagnetic radiation and/or infrared electromagnetic radiation to measure.Spectral measurement device can be connected to flow cell and without too much experiment.
Which kind of material the location of container in device measures in depending on system.
In one embodiment, flow cell has at least two for measuring the connection container of light phase of separation.
In another embodiment, there are at least four connection containers for measuring in two liquid phases and/or gas phase.
The schematic diagram of improved flow cell shown in Fig. 1.The absorption of electromagnetic radiation that this flow cell is designed in the industry stream that comprises one or more immiscible phases (wherein, in immiscible phase can be gas phase) is measured.
Flow cell can comprise main body 1 and built-in (built-in) dividing plate 2a, 2b and 2c and 2d alternatively.Pond is divided into container 3a, 3b, 3c, 3d by dividing plate.The height of dividing plate 2b is higher than the height of dividing plate 2a; The height of dividing plate 2c is less than the height of dividing plate 2a.The ratio of the dividing plate height of each dividing plate depends on the ratio of the density of phase.The height ratio of 2b/2c must exceed the density ratio of heavy-fluid/light liquid, and the height of 2a is approximately the mean value of the height of 2b and 2c.Meanwhile, the height of 2a/the go out density ratio that open height must be less than heavy-fluid/light liquid.
The process streams being made up of at least two immiscible phases enters container 3a, separates there.Promote the separation of immiscible phase by placing porous film in container 3a.Utilize character of surface to select barrier film to make barrier film improve the separation of the two-phase that enters pond.
Then, heavy phase enters container 3b by lower pipeline, and gently enters container 3b by upper pipe road.Two-phase enters container 3c from the lower part of container 3b.In container 3b, carry out absorbance measuring.In the design of above-mentioned pond, only light in upper pipe road and only heavy phase is under lower pipeline.By immiscible phase is separated first, be not subject to the impact of light scattering at the spectral measurement of interface, and greatly improved measuring accuracy.Heavy phase enters container 3d by lower pipeline from container 3c; And gently enter container 3d by upper pipe road.In container 3b, place accessory septa 2d to prevent gently entering container 3d by lower pipeline.In container 3d, carry out the measurement of heavy phase absorbance.Under upper pipe road, only find heavy phase.
The in the situation that of there is gas phase in process streams, gas phase enters output stream by the common gas space of whole container 3a, 3b, 3c and 3d.Can measure gas phase as required.
Outlet at container 3d goes out, reconsolidate separative phase and can be back to initial process streams and any variation does not occur.
Select to make each phase tool have sufficient time to be separated by the flow rate of flow cell.Those of ordinary skill in the art can regulate flow rate and without too much experiment.
The application's flow cell has been used to online spectral composition and has measured cumene oxidation product.In " wet type " oxidation of isopropyl benzene, oxidation product is the potpourri of water and organic phase and other gas phases.Utilize improved pond Separation of Water, organic (isopropyl benzene) layer and gas phase.In the near-infrared region of electromagnetic radiation spectrum, carry out spectral measurement.Measure hydrogen phosphide cumene (CHP) concentration.
Fig. 2 is the curve map that uses the CHP concentration within 10 hours of common pond measurement.Measured value be not reproducible and on reach to 100% relative measurement error be common.
Fig. 3 is the curve map that uses the CHP concentration within 10 hours of the application's improved flow cell measurement.Measuring error is no more than 0.2%.
Fig. 4 represents to use for the porous fluoropolymer plate of multilayer coalescent (layers coalescing) and is provided for fluid to push by the non-return valve of this dull and stereotyped pressure drop, in the scheme of the flow cell of cumene oxidation stream (air that it comprises water and dissolving) measurement hydrogen phosphide cumene concentration; In this case specialized designs container 3a hold (hold) it.All parts for stream by bottom pipe to optimize phase coalescence process.
In another embodiment, the various embodiments in dependent claims can be bonded to each other, and also can be incorporated in independent claims.
B monitoring method
As mentioned above, disclosure is also provided for the method for the online absorptiometry that carries out Immiscible fluid phase (for example, liquid phase and/or gas phase).
With reference to figure 1, head cavity will mix fractionation (split) mutually (for example, separation) for two or more separate phase, separate mutually and can will be used for analyzing by further separation subsequently.Can use and introduce the coalescer 2a flowing to into the position in pond and promote this separation.The size of chamber and coalescer depends on many factors: (a) relative density of immiscible phase (phase density is larger, and they are faster by what separate, thereby can use little chamber 2a, and on the contrary, little phase density difference will cause larger coalescer and chamber); (b) original dimension of the dispersion particle in inlet flow (drop) (particle or drop are less, longer for precipitating the time needing, and cause large 2a chamber); And the performance that (c) coalescent film (porosint) flows with respect to detailed process to be analyzed.If performance ideal, and can separate easily, can make so the minimized in size of chamber and coalescent film.Only by single phase in the situation that, can directly carry out optical measurement at coalescent film.(but in this case, conventionally only each in mutually one does not comprise other phases.) another factor is the amount that is present in the gas phase in inlet flow.The liquid surface that large air-flow can be upset flow cell inside causes fluctuation of service.In these cases, use more open surface area for chamber 2a.Consider these various factorss when pond in design, the mixing entering mutually can be separated or " fractionation " be continuous immiscible phase.For example, before, can in tail chamber, further separate these immiscible phases in analysis (, spectral luminosity is measured).
Tail chamber 2b, 2c, 2d play guiding various (now continuous) to for example, effect for analysis (, optical analysis) of disengagement chamber, wherein, can fill each chamber with the function of its phase density.Light liquid phase (minimum density) is passed through to chamber 2b.Heavy phase is passed through to chamber 2d.Chamber 2c is for gently providing mutually around the bypass of chamber 2d.Then, can, according to the needs of concrete process streams, in respective chamber, the phase (for example, the phase of pure separation) separating be measured.In the case of light mutually and the analysis of heavy phase not ideal, can distinguish binding cavity 2b and 2c or chamber 2c and 2d.This last situation shown in Figure 4.
Container device in location depend on system in material to be measured.
In one embodiment, pond has at least two for measuring the connection container of light phase of separation.
In another embodiment, there are at least four connection containers for measuring in two liquid phases and/or gas phase.
Can on the basis changing, complete spectral measurement.In one embodiment, on the basis basis of continuous basis, interruption or pre-programmed or that arrange, carry out spectral measurement.
Alternatively, can be to industrial process design of feedback loop, and carry out with the final goal that makes industrial process automation, for example, controller (for example, program logic controller) can be programmed to make transmission (relay) signal of expecting to be back to industrial system equipment to make necessary change aspect operating conditions.
Flow cell provides clean external phase for optical absorption measurement.Flow cell also can be for other optical measurement chaotic sensitivity of flow or in the time that the existence of multiple phases may disturb expectation to measure.The sample that analytical approach can be benefited from before analyzing as Raman spectroscopy, fluorescent spectrometry and refractometry is separated.In addition, this pond also can be used as " sample preparation " step of the on-line analysis (as vapor-phase chromatography, liquid chromatography, mass spectroscopy etc.) for other types.In these situations, the design class in pond seemingly; Optical window is optional.(however, they still can be used for installing or monitoring pool as the function of separation vessel.）
In one embodiment, the various embodiments in dependent claims can be bonded to each other, and also can be incorporated in independent claims.
In one embodiment, (be for example used for utilizing the online absorptiometry Immiscible fluid of electromagnetic radiation, liquid and/or gas phase) flow cell comprise: comprise and one or more entrance optical windows of one or more long-range spectral instrument communications and the housing of one or more outlet optical windows, be three (3) or a series of dividing plates with one or more entrances of the connection of being one another in series and the container of one or more outlets by the internal separation of flow cell, wherein the first container is equipped with perforated membrane to promote the separation of unmixing process phase more.
In another embodiment, the flow cell of the unmixing process phase that comprises liquid phase and/or gas phase for online absorptiometry, can comprise: comprise the main body that can operate entrance window and the outlet window of communication with surveying instrument; With a series of dividing plates that by the internal separation of flow cell are three (3) or the containers with entrance and exit more, the wherein container connection that is one another in series.The first container can be equipped with perforated membrane to promote the separation of unmixing process phase.
In one embodiment, utilize electromagnetic radiation to carry out the method for analyzing for process streams of the online absorptiometry of immiscible liquids (liquid and/or gas) phase, can comprise: the flow cell that comprises housing is provided, housing comprises one or more entrance optical windows and the one or more outlet optical window with one or more long-range spectral instrument communications, be a series of dividing plates of the container of three (3) or one or more entrance and exits with the connection of being one another in series by the internal separation of flow cell more, wherein the first container is equipped with perforated membrane to promote the separation of unmixing process phase, flow cell is associated with process fluid, and carry out one or more spectral measurements of described unmixing process phase.
In another embodiment, carry out the method for the online absorptiometry of Immiscible fluid (liquid and/or gas) phase, can comprise: Immiscible fluid is introduced to flow cell; Use perforated membrane and dividing plate in flow cell inside, Immiscible fluid to be separated; And carry out the measurement of the Immiscible fluid phase of above-mentioned separation.
In various embodiments, (i) perforated membrane can be fluorinated material and/or silicon materials; And/or (ii) can there be at least two for measuring the connection container of light phase of separation; And/or (iii) can there are at least four connection containers for for example measuring in two liquid phases and/or gas phase; (iv) flow cell can be designed to utilize ultraviolet electromagnetic radiation, both visible electromagnetic radiation and/or infrared electromagnetic radiation to measure; And/or (v) flow cell can comprise quick loop by-pass line; And/or (vi) one or more long-range spectral instruments can utilize Connectorized fiber optic cabling; And/or (vii) can on continuous basis, carry out spectral measurement; And/or (viii) can on the basis of being interrupted, carry out spectral measurement; And/or (ix) can on the basis of pre-programmed or setting, carry out spectral measurement; And/or (x) film can be arranged in the first container of flow cell; And/or (xi) measure select free spectroscopic methodology, refractometry, chromatography, chromatography, Spectrum Method and comprise the group that at least above-mentioned a kind of combination forms; And/or (xii) surveying instrument can select free Raman spectrometer, fluorescence spectrophotometer, refractive index measuring instrument, gas chromatograph, liquid chromatograph, mass spectrometer and comprise the group that at least above-mentioned a kind of combination forms; And/or (xiii) on continuous basis, measure; And/or (xiv) be interrupted basis on measure; And/or (xv) on the basis of pre-programmed or setting, measure; And/or (xvi) Immiscible fluid (for example, unmixing process phase) is the cumene oxidation stream that comprises hydrogen phosphide cumene.
The method of the online absorptiometry of the immiscible phase that in one embodiment, comprises liquid phase and/or gas phase comprises: any and process fluid that comprises immiscible phase in above-mentioned flow cell is associated; And carry out the measurement of immiscible phase.
The method of in another embodiment, carrying out the online absorptiometry of immiscible liquids phase comprises: immiscible liquids is introduced to any in above-mentioned flow cell; Separate Immiscible fluid phase with dividing plate at the inner perforated membrane that uses of flow cell; And carry out the measurement of the Immiscible fluid phase of above-mentioned separation.
All scopes disclosed herein comprise end points, and end points can combine (for example, the scope of " above reach to 25wt%, or, more specifically, 5wt% to 20wt% " comprises all intermediate values in the scope of end points and " 5wt% to 25wt% ") independently of one another." combination " comprises admixture, potpourri, alloy, reaction product etc.In addition, term " first ", " second " etc. herein do not represent any order, amount or importance, and for distinguishing between key element.Unless separately have herein statement or with the obvious contradiction of context, otherwise term herein " a kind of (a) " and " one (an) " and " this (the) " do not represent restricted number, but are interpreted as encompasses singular and plural number.As used in this article suffix " (s) " be intended to the odd number of the term that comprises its modification and plural number both, thereby comprise one or more (for example, film comprises one or more films) of this term.Run through reference " a kind of embodiment ", " another embodiment ", " embodiment " of instructions etc., (for example refer to described special key element relevant to embodiment, feature, structure and/or characteristic) be included at least one embodiment described herein, and can or can not be present in other embodiments.In addition, should be appreciated that described key element can be combined in any way in different embodiments.
Although described concrete embodiment, may occur that to the others skilled in the art in applicant or this area being may be maybe current unforeseen substitute, modification, variation, improvement and essence coordinator.Therefore, as the claim of enclosing of submitting to and they can be modified is intended to comprise all these substitutes, modification, variation, improvement and essence coordinator.
Claims (20)
1. a flow cell for the unmixing process phase that comprises liquid phase and/or gas phase for online absorptiometry, comprising:
Comprise the main body that can operate entrance window and the outlet window of communication with surveying instrument; And
Be a series of dividing plates of three (3) or the containers with entrance and exit by the internal separation of described flow cell more, wherein, the connection that is one another in series of described container, and wherein said the first container is equipped with perforated membrane to promote the separation of described unmixing process phase.
2. flow cell according to claim 1, wherein, described film is arranged in described first container of described flow cell, and wherein, described perforated membrane is fluorinated material and/or silicon materials.
3. according to the flow cell described in any one in claim 1-2, wherein, there are at least two for measuring the connection container of light phase of separation.
4. according to the flow cell described in any one in claim 1-2, wherein, there are at least four connection containers for measuring in two liquid phases and/or gas phase.
5. according to the flow cell described in any one in claim 1-4, wherein, described flow cell is designed to utilize ultraviolet electromagnetic radiation, both visible electromagnetic radiation and/or infrared electromagnetic radiation to measure.
6. according to the flow cell described in any one in claim 1-5, further comprise quick loop by-pass line.
7. according to the flow cell described in any one in claim 1-6, wherein, described surveying instrument is Raman spectrometer, fluorescence spectrophotometer, refractometry, gas chromatograph, liquid chromatograph, mass spectrometer and comprises at least one the combination in above-mentioned.
8. flow cell according to claim 7, wherein, described surveying instrument comprises long-range spectral instrument.
9. flow cell according to claim 8, wherein, described long-range spectral instrument utilizes Connectorized fiber optic cabling.
10. a method that comprises the online absorptiometry of the immiscible phase of liquid phase and/or gas phase, comprising:
Make to be associated with the process fluid that comprises described immiscible phase according to the flow cell described in any one in claim 1-9; And
Carry out the measurement of described immiscible phase.
11. 1 kinds are carried out the method for the online absorptiometry of Immiscible fluid phase, comprising:
Described Immiscible fluid is introduced according to the flow cell described in any one in claim 1-9;
Separate described Immiscible fluid phase with dividing plate at the inner perforated membrane that uses of described flow cell; And
Carry out the measurement of the Immiscible fluid phase of described separation.
The method of the online absorptiometry of 12. 1 kinds of immiscible phases that comprise liquid phase and/or gas phase, comprising:
Flow cell is associated with the process fluid that comprises described immiscible phase; And
Carry out the measurement of described immiscible phase;
Wherein, described flow cell comprise comprise with surveying instrument can operate communication entrance window and outlet window main body; Be a series of dividing plates of the three or more containers with entrance and exit by the internal separation of described flow cell, the wherein said container connection that is one another in series, and wherein the first container is equipped with perforated membrane.
13. 1 kinds are carried out the method for the online absorptiometry of Immiscible fluid phase, comprising:
Described Immiscible fluid is introduced into flow cell;
Separate described Immiscible fluid phase with dividing plate at the inner perforated membrane that uses of described flow cell; And
Carry out the measurement of the Immiscible fluid phase of described separation.
14. methods according to claim 12, wherein, described flow cell comprises
Comprise the main body that can operate entrance window and the outlet window of communication with surveying instrument; And
Be a series of dividing plates of the three or more containers with entrance and exit by the internal separation of described flow cell, wherein, the connection that is one another in series of described container; And
Wherein, described the first container is equipped with perforated membrane.
15. according to the method described in any one in claim 10-14, wherein, on the basis of continuous basis, interruption or the basis of pre-programmed or setting, carries out described measurement.
16. according to the method described in any one in claim 12-15, and wherein, described measurement is spectroscopic methodology, refractometry, chromatography, chromatography, Spectrum Method or comprises at least one the combination in above-mentioned.
17. according to the method described in any one in claim 10-16, wherein, carries out described measurement on continuous basis.
18. according to the method described in any one in claim 10-16, wherein, on the basis of being interrupted, carries out described measurement.
19. according to the method described in any one in claim 10-16, wherein, on the basis of pre-programmed or setting, measures.
20. according to the method described in any one in claim 10-19, and wherein, described Immiscible fluid is the cumene oxidation stream that comprises hydrogen phosphide cumene.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US13/231,276 | 2011-09-13 | ||
| US13/231,276 US8663562B2 (en) | 2011-09-13 | 2011-09-13 | Flow cell for measuring electromagnetic radiation absorption spectra in a continuously flowing immiscible liquid(s) or liquids with entrained gas phases |
| PCT/US2012/054426 WO2013039828A1 (en) | 2011-09-13 | 2012-09-10 | A flow cell for measuring electromagnetic radiation absorption spectra in a continuously flowing immiscible liquid(s) or liquids with entrained gas phases |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103782154A true CN103782154A (en) | 2014-05-07 |
| CN103782154B CN103782154B (en) | 2016-03-16 |
Family
ID=46981085
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201280043363.2A Expired - Fee Related CN103782154B (en) | 2011-09-13 | 2012-09-10 | For measure continuous print flowing immiscible liquids or have carry gas phase secretly liquid in the flow cell of absorption of electromagnetic radiation spectrum |
Country Status (4)
| Country | Link |
|---|---|
| EP (1) | EP2756284A1 (en) |
| KR (1) | KR20140058600A (en) |
| CN (1) | CN103782154B (en) |
| WO (1) | WO2013039828A1 (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3560099A (en) * | 1968-07-10 | 1971-02-02 | Inst Produktudvikling | Colorimeter flow cell including a baffle to remove gas bubbles |
| WO2006017141A2 (en) * | 2004-07-13 | 2006-02-16 | Newell Benjamin E | Refractive index sensor using internally reflective light beams |
| US20100072371A1 (en) * | 2005-10-05 | 2010-03-25 | Swan Analytische Instrument Ag | Photometric method and apparatus for measuring a liquid's turbidity, fluorescence, phosphorescence and/or absorption coefficient |
| WO2010059176A1 (en) * | 2008-11-24 | 2010-05-27 | Herbert Leckie Mitchell | Nephelometric turbidity sensor device |
| CN201539913U (en) * | 2009-12-08 | 2010-08-04 | 许庆华 | Flue gas cleaner of smoke exhaust ventilator |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3231091A (en) * | 1962-10-29 | 1966-01-25 | Pfaudler Permutit Inc | Separator |
| BRPI0417085A (en) * | 2003-12-03 | 2007-04-27 | Shell Int Research | method for separating organic acid from an organic hydroperoxide stream |
| JP4434041B2 (en) * | 2005-03-02 | 2010-03-17 | 住友化学株式会社 | Near-infrared spectroscopic sample pretreatment equipment, pretreatment method and analysis method |
-
2012
- 2012-09-10 KR KR1020147005892A patent/KR20140058600A/en not_active Application Discontinuation
- 2012-09-10 WO PCT/US2012/054426 patent/WO2013039828A1/en active Application Filing
- 2012-09-10 CN CN201280043363.2A patent/CN103782154B/en not_active Expired - Fee Related
- 2012-09-10 EP EP12769212.7A patent/EP2756284A1/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3560099A (en) * | 1968-07-10 | 1971-02-02 | Inst Produktudvikling | Colorimeter flow cell including a baffle to remove gas bubbles |
| WO2006017141A2 (en) * | 2004-07-13 | 2006-02-16 | Newell Benjamin E | Refractive index sensor using internally reflective light beams |
| WO2006017141A3 (en) * | 2004-07-13 | 2006-07-13 | Benjamin E Newell | Refractive index sensor using internally reflective light beams |
| US20100072371A1 (en) * | 2005-10-05 | 2010-03-25 | Swan Analytische Instrument Ag | Photometric method and apparatus for measuring a liquid's turbidity, fluorescence, phosphorescence and/or absorption coefficient |
| WO2010059176A1 (en) * | 2008-11-24 | 2010-05-27 | Herbert Leckie Mitchell | Nephelometric turbidity sensor device |
| CN201539913U (en) * | 2009-12-08 | 2010-08-04 | 许庆华 | Flue gas cleaner of smoke exhaust ventilator |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103782154B (en) | 2016-03-16 |
| KR20140058600A (en) | 2014-05-14 |
| EP2756284A1 (en) | 2014-07-23 |
| WO2013039828A1 (en) | 2013-03-21 |
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