CN206420760U - A kind of sample cell for Dynamic Absorption spectra collection - Google Patents

Abstract

The utility model is used for the sample cell of Dynamic Absorption spectra collection, including：Gasket construction, the thickness with setting and with sample well；Paired thang-kng piece, is stacked in the both sides of gasket construction respectively, and respective inner surface defines the sample space of film-form with the sample well；Temperature control device, is arranged on close to sample space peripheral position on the outside of thang-kng piece, to control sample temperature in sample space；And clamping device, it is arranged on the outside of paired thang-kng piece, so that gasket construction is brought into close contact with thang-kng piece.Wherein, the gasket construction includes single pad or the multiple pads including being removably closely superimposed, there is the catalytic activity for promoting example reaction in sample space to constitute a series of contact surfaces with sample in the sample space for setting light path, and the pad and sample space.The utility model sample pool structure is compact, heat transfer is efficient, using flexible.

Description

A kind of sample cell for Dynamic Absorption spectra collection

Technical field

It is specially that one kind is used for continuous acquisition example reaction the present invention relates to the Optical devices applied to analytical chemistry field The sample cell of process dynamics absorption spectrum.

Background technology

Using sample absorbance spectrum signal, the chemical composition and chemistry knot information of sample can be obtained quick nondestructive.And incite somebody to action The course of reaction of sample combines with absorption spectromtry, reaches the on-line continuous monitoring of chemical reaction, so that it may obtain sample Dynamic Absorption spectrum in the chemical reaction environment, realizes hence for whole reaction process and accurately portrays, available for reacting Dynamics and the field such as thermodynamic study, qualitative material and concentration analysis, catalyst activity evaluation.Therefore, developing reaction-detection The spectra sample pool structure of integration has important academic research and engineering application value.

At present, the common spectra sample pool structure of existing several classes can realize above-mentioned functions to a certain extent：One is perseverance Warm sample cell, i.e., increase constant temperature jacket on conventional cuvette support, so that the sample in cuvette maintains required reaction At a temperature of, so as to start the reaction dynamic spectrum of specific reaction and collecting sample.The major defect of this sample pool structure exists It is small in heat transfer area, therefore rate of heat transfer and temperature homogeneity are relatively low；And without mass transfer enhancement mechanism, therefore its chemical composition is homogeneous Property is also poor.Secondly being flowing sample cell, i.e., the sample in external reactor is continually entered into cuvette simultaneously by pipeline and pump Flowing is kept, so as to gather dynamic spectrum.The subject matter of this sample cell is that structure is more complicated and it is high viscous to be difficult to processing There is certain hysteresis quality in property fluid, the spectroscopic acquisition of course of reaction.Thirdly being fibre-optical probe, reactor body can be inserted directly into Phase online acquisition dynamic spectrum.But it is with high costs and be difficult to light path regulation, and will be difficult to if occurring probe pollution clear Reason.This few class dynamic spectrum acquisition scheme also all needs larger sample volume in addition to drawbacks described above is respectively present, and causes temperature control spirit Sensitivity and precision are relatively low.What is more important, the light path of these structures is typically all not less than 1mm, therefore for high absorbance Sample standard deviation can not directly determine, and need first to mix the sample with solvent dilution.Thus bring three big limitations：(1) it must take into consideration Influence of the solvent to reaction and to spectrometric interference；(2) process for preparation of sample solution is must take into consideration in quantitative determination And its introduced error；(3) also need to consider the high pressure harm that solvent volatilization or its steam are produced for pyroreaction.

In summary, there is certain limitation in existing dynamic spectrum harvester.

The content of the invention

For the limitation of existing Dynamic Absorption spectra collection device, the present invention proposes that a kind of new Dynamic Absorption spectrum is adopted Collect sample cell, its compact conformation, heat transfer efficiently, use the dynamic spectrum sample of flexible and executable a variety of homogeneous and heterogeneous reaction Product pond.It not only may be directly applied to the desk-top ultraviolet, visible ray and infrared spectrometer of current main flow, it may also be used for miniature portable The absorption spectrum instrument of change, further expands the application of spectrum analysis.

The sample cell for Dynamic Absorption spectra collection of the present invention, including：Gasket construction, thickness and tool with setting There is sample well；Paired thang-kng piece, is stacked in the both sides of gasket construction respectively, and respective inner surface is defined with the sample well The sample space of film-form；Temperature control device, is arranged on close to sample space peripheral position on the outside of thang-kng piece, to control sample space Interior sample temperature；And clamping device, it is arranged on the outside of paired thang-kng piece, so that gasket construction is brought into close contact with thang-kng piece.Its In, the gasket construction includes single pad or the multiple pads including being removably closely superimposed, and a series of has to constitute The sample space of light path is set, and the contact surface of the pad and sample in sample space has sample in promotion sample space anti- The catalytic activity answered.

In the preferred embodiment for the present invention, each pad is sheet metal or potsherd with predetermined thickness, the sheet metal Constituted by can serve as the platinum of reaction system catalyst in sample space, rhodium, palladium, nickel, copper, iron, aluminium or its alloy, the potsherd Area load can serve as the solid catalyst of reaction system catalyst in sample space.

In the preferred embodiment for the present invention, the thickness of each pad is 0.01-0.5mm；And/or, the sample well A diameter of 6-20mm.

In the preferred embodiment for the present invention, a gasket surface of laminating thang-kng piece is provided with the overflow connected with sample well Groove.

In the preferred embodiment for the present invention, positioning hole is additionally provided with favor of in multiple pads on sample well periphery on the pad Alignment in the case of piece each other.

In the preferred embodiment for the present invention, the clamping device includes：Paired grip block, for being stacked in respectively in pairs Thang-kng piece outside；And retention mechanism, the paired grip block for clamping, so that thang-kng piece and pad between keeping grip block Fix and be brought into close contact in the position of piece.

In the preferred embodiment for the present invention, the temperature control device includes：It is arranged on inside a grip block or outer surface Heat piece and/or cooling piece, and be arranged on inside another grip block or inner surface temperature sensor, temperature sensor can be with Relay connect and controls to heat/keying of cooling piece.

In the preferred embodiment for the present invention, the retention mechanism is selected from screw threads for fastening, elastic fastening and magnetic clamp；And institute State 3 times of area not less than sample hole area thereon of pad, the surface area that the paired thang-kng piece is contacted with pad laminating Not less than 3 times of sample hole area, and the paired grip block fits the surface area contacted with thang-kng piece not less than sample well 3 times of area.

In the preferred embodiment for the present invention, the gasket construction includes the multiple pads being removably superimposed, and adjacent pads The sample well of piece it is of different sizes, to obtain the increase of liquid-solid contact interface area and adjustable sample space.

In the preferred embodiment for the present invention, the gasket construction includes the multiple pads being removably closely superimposed up and down, And at least one pad close to upside has the guiding gutter connected with sample well, to obtain the sample that solution-air contact interface is stable Product space, so as to be collected suitable for gas-liquid reaction dynamic spectrum.

The advantage of the invention is that：(1) spacing of quartz plate is adjusted using the pad of predetermined thickness, film-form sample can be achieved Product pond light path is precisely controlled；(2) because sample is in film space, therefore light path is easily set to the percent of conventional apparatus One even one thousandth, for the sample with high absorbance, without again with solvent dilution i.e. can directly observe；(3) Film-form cuvette volume is small but heat exchange area is big, therefore temperature control is sensitiveer and more accurate；(4) film-form sample cell can be corpusculum Product sample provides larger solid-liquid or solution-air contact interface, and higher mass transfer still can be obtained for heterogeneous reaction system Efficiency and reaction homogeneity；(5) pad with sample contacting surface there is catalytic activity to promote example reaction, without empty in sample Interior addition solid catalyst.

Brief description of the drawings

Fig. 1 is the schematic diagram of an embodiment in inventive samples pond, and wherein Fig. 1 (a) is the vertical view of pad in sample cell Plan, Fig. 1 (b) is the side view cutaway drawing of sample cell；

Fig. 2 be inventive samples pond can be used for solid-liquid reaction system when the second embodiment schematic diagram, wherein Fig. 2 (a) be pad in sample cell plan view from above, Fig. 2 (b) be sample cell side view cutaway drawing；And

Fig. 3 be inventive samples pond can be used for gas-liquid reaction system when the 3rd embodiment schematic diagram, wherein Fig. 3 (a) be pad in sample cell plan view from above, Fig. 3 (b) be sample cell side view cutaway drawing.

Embodiment

The essence of Dynamic Absorption spectrum, is to join material absorbing spectral signal and time correlation, so as to increase sample table Seek peace the dimension and precision portrayed, in Chemical Kinetics and thermodynamic study, material is qualitative and quantitative, catalyst activity is commented There is significant application value in terms of valency.

A kind of sample cell for Dynamic Absorption spectra collection of the present invention, including：Fine gasket, middle part is provided with sample Sample wells can load sample, and the contact surface of itself and sample can also have the catalytic activity for promoting sample to participate in chemical reaction；It is logical in pairs Mating plate, such as quartz plate, respectively positioned at the both sides of fine gasket, and are used as two light pass surfaces of sample cell, respective inner surface The sample space of film-form is defined with the sample well.Also include temperature control device, be arranged on empty close to sample on the outside of thang-kng piece Between peripheral position, to control sample temperature in sample space.Also include clamping device, be arranged on the outside of paired thang-kng piece, with Pad is set to be brought into close contact with thang-kng piece.

Accurate adjustment sample cell light path and seriation can be allowed to by the way of the superposition of single or multiple lift fine gasket, so that Make sample cell that there is extensive versatility and flexibility for all kinds of samples with different absorbance properties.Therefore, it is of the invention Be further characterized as, the fine gasket can single or multiple lift superposition use so that it is a series of to constitute to adjust quartz plate spacing Sample cell with setting light path.

Preferably, the thickness of each pad may be selected to be 0.01-0.5mm.

Preferably, sample well of the present invention is diameter 6-20mm circular port.

The material of fine gasket should generally have following characteristics：(1) it is easily achieved Precision Machining；(2) in temperature in use model There is high rigidity in enclosing；(3) there is preferable heat conductivility.Sheet metal or potsherd can for example be used.

When using sheet metal as fine gasket when, can use, the metal such as platinum, rhodium, palladium, nickel, copper, iron, aluminium or its Alloy etc..During for using potsherd as fine gasket, one layer of catalyst can be covered on potsherd surface.

Another preferred feature of fine gasket of the present invention is that it is fixed no less than 2 also to have around the sample well at middle part Position pore structure, plays a part of assembling positioning.Such as positioning hole is 2-6mm circular ports, and quantity is 4, using 4 positioning holes Sample well surrounding is evenly distributed on to be beneficial to ensure sealing surface uniform force and avoid sample from revealing.

In addition, some samples may produce excessive pressure because of expanded by heating to thang-kng piece under the high temperature conditions, and then lead Cause the failure of the sealing surface between thang-kng piece and fine gasket and sample is occurred leakage and be lost in, final destruction dynamic spectrum was gathered The stability of journey.Therefore, one of feature of the present invention is that an overflow launder and sample well can be set on the surface of fine gasket Connection.One width 1-2mm rectangle overflow launder is for example set, can be overflowed when sample expanded by heating from overflow launder, and it is remaining Sample can still be full of sample cell and keep the stabilization of course of reaction and spectra collection process.

Temperature control device may include to heat/cooling piece and temperature sensor, for by sample heating/cooling in sample cell and Thermometric, temperature sensor can be connected and control the keying of calandria with temperature relay.

Clamping device may include：Paired grip block, for remaining in quartz plate between grip block and fine gasket Fix and be brought into close contact in position；And fastener, the position for paired grip block is fixed and is allowed to keep chucking power.

In order to it is uniform and delicately in control sample cell sample temperature, it is necessary to assure enough thermal contact conductance areas with up to Into good heat-transfer effect.Therefore, one of feature of the present invention is also resided in, the area of the fine gasket is not less than sample thereon 3 times of hole area；The paired quartz plate is respectively at fine gasket both sides and fitted with fine gasket, and can be with fine gasket The surface area of laminating contact is not less than 3 times of sample hole area；The paired grip block respectively be located at quartz plate on the outside of and with Quartz plate is fitted, and the surface area contacted of being fitted with quartz plate is not less than 3 times of sample hole area.

It is described heat/one of cooling piece and paired grip block contact and as heating/refrigeration source, for example, heat piece and/or Cooling piece may be provided inside a grip block or outer surface.Temperature sensor may be provided inside same or another grip block or Inner surface.Temperature sensor can be connected with relay and controls to heat/keying of cooling piece.

Preferably, temperature sensor is then contacted and temperature-sensitive with opposite side grip block./ refrigeration source and TEMP will be heated Device is placed in the heteropleural rather than homonymy of sample cell, and its reason is when the two is in homonymy, heat/refrigeration source and temperature sensor Heat conduction path is shorter, measured temperature closer to heating/temperature of refrigeration source；And when the two is in heteropleural, TEMP The heat conduction path of device and sample cell is shorter, and measured temperature is closer to sample cell temperature.

Grip block is generally by having Thermal conductivity and the enough materials of intensity are made.Stainless steel, aluminium, copper can for example be used Or alloy.

In general, due to chemical reaction be required to more than could starting under certain temperature (more than activation energy) or Person has observable reaction rate, therefore use heats piece offer sample cell institute calorific requirement more.But when sample cell is for infrared During Dynamic Absorption spectra collection, because the continuous heating of infra-red radiation is acted on, the sample in sample cell may be caused to exceed setting Temperature；In addition when chemical reaction is exothermic reaction, the sample in sample cell may be caused to exceed design temperature, it is therefore desirable to adopt Waste heat is removed with cooling piece.Therefore, thermal source or low-temperature receiver of the selection direct current semiconductor heating/cooling piece as the sample cell, Sample cell can be heated or cooled by switching direct current supply both positive and negative polarity.

Thermal insulation layer can be also set on the outside of grip block, for reducing the heat loss of sample cell and avoiding spectrometer other parts Influenceed by high temperature.

Because sample cell of the present invention is made up of each component combination, therefore it is easy to loading in a disassembled state and includes All kinds of samples including high viscosity liquid, and then need to ensure each component contact face based on certain chucking power in the assembled state Be brought into close contact, so as to prevent sample from revealing and ensure heat-transfer effect.Therefore, sample cell of the present invention also has fastening dress Put, its form includes but is not limited to screw threads for fastening, elastic fastening and magnetic clamp.

Wherein screw threads for fastening and elastic fastening belong to mechanical fasteners mode, and magnetic clamp refers on sandwich plate Permanent magnetism or electromagnet are fixed respectively, and fastening is realized using high-intensity magnetic field sucking action when grip block is close to each other.It is tight using magnetic force Admittedly decomposition-combination operation of sample cell can be made relatively simple and make chucking power more equalization stable, therefore magnetic clamp is excellent Select fastening means.

In addition, when being superimposed using the fine gasket with different-diameter sample well, can be formed with annular solid-liquid contact The sample cell at interface.The annular contact interface can be located at the upper of the exposure on sample well periphery on the pad of small diameter sample well Surface and/or lower surface are formed, and such as Fig. 2 (b) shows the minor diameter sample well pad being clipped between two panels fine gasket 70, it is provided by two annular solid-liquid contact interfaces of exposed upper and lower delimited.But also can be by selecting diameter big Small difference and/or the increase and decrease pad superposition number of plies (preferably, the fine gasket with different-diameter sample well is alternately superimposed) come smart Really regulate and control the interfacial area.When fine gasket selects the material with catalytic activity, due to catalysis interfacial area and sample body The equal controllable of phase volume, therefore there is prominent practical value for the dynamics research of solid-liquid catalytic reaction.

The present invention can provide a kind of organization plan determined for liquid-solid reaction dynamic spectrum, i.e., more than two panels and have The fine gasket for having different sample bore dias is alternately superimposed constituted sample cell, with the controllable annular solid-liquid contact of area Interface.

On the other hand, can be using the fine gasket with guiding gutter and without guiding gutter when reaction system is solution-air system Fine gasket above and below overlaying structure.When loading fluid sample, if fluid sample liquid level exceedes lower floor and padded without guiding gutter precision The thickness of piece, then can be overflowed by the guiding gutter on the fine gasket of upper strata, so as to obtain the fluid sample thickness of setting.Work as sample When the closing of product pond fastens and keeps horizontality, there is the gas that certain volume will be kept in the sample well of guiding gutter fine gasket on upper strata There will be the stable and controllable interface of an area between phase, and upper strata gas phase and lower floor's liquid phase, (the big I in interface passes through choosing Select the realization of sample bore dia).Under this condition start course of reaction by can continuous acquisition gas-liquid reaction dynamic spectrum.

The present invention may also provide a kind of organization plan determined for gas-liquid reaction dynamic spectrum, i.e., by no less than a piece of It is controllable with area with guiding gutter and no less than a piece of fine gasket superposition without guiding gutter and the sample cell of horizontal positioned Solution-air contact interface.

The preferred embodiments of the invention are done by principle and advantage for a better understanding of the present invention below in conjunction with the accompanying drawings Describe in detail.

The schematic diagram of one embodiment in inventive samples pond shown in Figure 1, wherein Fig. 1 (a) is pad in sample cell Plan view from above, Fig. 1 (b) be sample cell side view cutaway drawing.In the sample cell of the present embodiment, one group of fine gasket 4 is folded It is added together, forms the sample well with controllable thickness (light path).A slabstone has been brought into close contact respectively in the both sides of fine gasket English piece 3, thus with the sample well on fine gasket constitute can loading liquid sample film space.The two of two panels quartz plate Individual outside, and a piece of grip block 1 of having fitted respectively.Heating/refrigerating piece 6 is mounted with the grip block of side, as thermal source/low-temperature receiver, Temperature-sensing probe 2 is mounted with opposite side grip block, for determining temperature and control heating/refrigerating piece being connected with temperature relay Open and close to constitute isoperibol.In order to keep above-mentioned fine gasket, quartz plate and grip block to be brought into close contact, at grip block two ends Also magnetic clamp mechanism 5.Visible from the top view of fine gasket 4, i.e. Fig. 1 (a), fine gasket 4, which is provided with, is no less than 2 Positioning hole 7, the positioning for fine gasket；In addition with a circular sample hole 8.If the device (exceedes for higher temperature 80 DEG C) the dynamic spectrum signal acquisition of reaction, can also be in the outside of grip block 1 laminating layer of insulation material.

The invention is not restricted to the particular number in the present embodiment and material, 3 pads are shown in figure, each pad has predetermined Thickness (such as 0.05mm).The sample well of each pad is aligned with each other, and diameter is 10mm.According to example reaction needs, gold can select Belong to piece or potsherd.For sheet metal, platinum, rhodium, palladium, nickel, copper, iron, aluminium or its alloy may be selected from.For potsherd, its surface Cover solid catalyst layer.Solid catalyst can serve as reaction system catalyst in sample space, for example solid acid catalytic or Person's solid basic catalyst.

The application method of present embodiment sample cell is described below.

The Dynamic Absorption spectral signal of fluid sample is gathered using following steps：(1) by fluid sample and reactant and Homogeneous catalyst (if desired) is mixed evenly；(2) level stacks side grip block, a piece of quartz plate and with setting from bottom to top Determine the fine gasket of thickness (light path), be added dropwise in fine gasket sample well and full of foregoing mixture；(3) full of mixture Sample well on successively stack another quartz plate and opposite side grip block, compress above-mentioned each part with magnetic clamp mechanism and make It is combined integrated；(4) sample cell combined is placed between the light source transmitting terminal of spectrometer and receiving terminal, and ensures quartz Piece window is vertical just to light path；(5) heating/refrigerating piece on dynamic spectrum sample cell is started to design temperature and constant temperature, simultaneously Utilize the serial dynamic spectrum signal of spectrometer continuous acquisition sample.

The advantage introduced below that sample dynamic spectrum signal is gathered using the device：(1) fine gasket or its superposition are utilized Combination can accurately regulate and control the light path of sample cell, and the sample with high absorbance can be directly observed without using solvent dilution；(2) With film-form sample space, sample volume is small but heat transfer area is big, therefore is easily achieved homogeneous and sensitive temperature control；(3) it is whole Device is easily-disassembled or combination, is easy to load high viscosity sample, easy cleaning is thoroughly to avoid the pollution between sample；(4) structure letter List is compact to can be universally used in all kinds of spectrometers, and reaction-measure integral collecting signal is without hysteresis quality.The embodiment is suitable for liquid State homogeneous reaction system, i.e., miscible each reactant and catalyst (if desired) are a phase.

Fig. 2 be inventive samples pond be used for solid-liquid reaction system when the second embodiment schematic diagram, wherein Fig. 2 (a) It is the plan view from above of pad in sample cell, Fig. 2 (b) is the side view cutaway drawing of sample cell.In sample cell, one group with not same Sample wells diameter and it is superimposed with the fine gasket 40 and 70 of catalytic activity, forms the sample with controllable thickness (light path) Hole.And because fine gasket sample bore dia is different, and substantially coaxial setting, and with the upper and lower surface exposed by pad The annular solid-liquid contact interface defined.Be brought into close contact a piece of quartz plate 30 respectively in the both sides of fine gasket, thus with essence Sample well on gasket piece constitute can loading liquid sample film space.In two outsides of two panels quartz plate, distinguish again Fit a piece of grip block 10.Have and heating/refrigerating piece 60 is mounted with the grip block of side, be used as thermal source/low-temperature receiver, opposite side clamping Temperature-sensing probe 20 is mounted with plate, controls the keying of calandria to constitute constant temperature for determining temperature and being connected with temperature relay Environment.In order to keep above-mentioned fine gasket, quartz plate and grip block to be brought into close contact, there is elastic fastening machine at grip block two ends Structure 50.From on top view Fig. 2 (a) of fine gasket, fine gasket is provided with no less than 2 positioning holes 80, for precision The positioning of pad；In addition with circular sample hole 90.If the device is used for the dynamic spectrum that higher temperature (more than 80 DEG C) reacts Signal acquisition, can also be in the outside of grip block 10 laminating layer of insulation material.

Wherein described fine gasket, which has been the metal material as previously described with catalytic action or area load, to be catalyzed The potsherd of agent.

The application method of present embodiment sample room is described below.

The Dynamic Absorption spectral signal of fluid sample is gathered using following steps：(1) fluid sample and reactant are mixed Uniformly；(2) level stacks side grip block, a piece of quartz plate and with setting thickness (light path) and annular solid from bottom to top The fine gasket at interface is catalyzed, is added dropwise in fine gasket sample well and full of foregoing mixture；(3) in the sample full of mixture Another quartz plate and opposite side grip block are successively stacked in sample wells, above-mentioned each part is compressed with elastic fastening mechanism and is allowed to group Unify body；(4) sample cell combined is placed between the light source transmitting terminal of spectrometer and receiving terminal, and ensures quartzy gate Mouth is vertical just to light path；(5) start the heating/refrigerating piece on dynamic spectrum sample cell to design temperature and constant temperature, utilize simultaneously The serial dynamic spectrum signal of spectrometer continuous acquisition sample.

The advantage introduced below that sample dynamic spectrum signal is gathered using the device：(1) use flexibly, can be straight by selection Footpath difference in size or the increase and decrease pad superposition number of plies (fine gasket with different-diameter sample well need to be alternately superimposed) are accurately adjusted Control solid catalysis interfacial area；(2) there is film-form sample space, sample is big with solid catalyst contact surface, is conducive to obtaining Homogeneous reaction effect.The embodiment is suitable for solid-liquid heterogeneous reaction system.

Fig. 3 be inventive samples pond be used for gas-liquid reaction system when the 3rd embodiment schematic diagram, wherein Fig. 3 (a) It is the plan view from above of pad in sample cell, Fig. 3 (b) is the side view cutaway drawing of sample cell.The sample cell of the present embodiment is by such as Lower construction：

By one group there is the fine gasket 700 of guiding gutter 900 and the fine gasket 400 without guiding gutter to be superimposed； The both sides of fine gasket have been brought into close contact a piece of quartz plate 300 respectively, so that being constituted with the sample well on fine gasket to fill Carry the film space of fluid sample.In two outsides of two panels quartz plate, and a piece of grip block 100 of having fitted respectively.Side is pressed from both sides Hold and heating/refrigerating piece 600 is mounted with plate, as thermal source/low-temperature receiver, temperature-sensing probe 200 is mounted with opposite side grip block, is used for Determine temperature and be connected the keying of control calandria with temperature relay to constitute isoperibol.In order to keep above-mentioned accurate pad Piece, quartz plate and grip block are brought into close contact, and also have screw threads for fastening mechanism 500 at grip block two ends.From the vertical view of fine gasket Visible in figure Fig. 3 (a), fine gasket is provided with no less than 2 positioning holes 800, the positioning for fine gasket；In addition with one Individual circular sample hole and the guiding gutter 900 with the sample well UNICOM.If the device reacts for higher temperature (more than 80 DEG C) Dynamic spectrum signal acquisition, can also be in the outside of grip block 1 laminating layer of insulation material.

The application method of present embodiment sample room is described below.

The Dynamic Absorption spectral signal of fluid sample is gathered using following steps：(1) level stacks side folder from bottom to top Holding plate, a piece of quartz plate and fine gasket combination, (wherein the fine gasket without guiding gutter is placed in the fine gasket of guiding gutter Lower section), fluid sample is added dropwise in fine gasket sample well in (2), will when fluid sample liquid level exceedes without guiding gutter sample well Overflowed from the guiding gutter on upper strata；(3) another quartz plate and opposite side folder are successively stacked on the sample well full of mixture Plate is held, above-mentioned each part is compressed with screw threads for fastening mechanism and is allowed to combined integrated；(4) the sample cell level combined is put Put, then the light source transmitting terminal and receiving terminal of spectrometer are respectively placed in both sides above and below sample cell, and ensure that quartz plate window is vertical Just to light path；(5) the heating/refrigerating piece on dynamic spectrum sample cell is started to design temperature and constant temperature, while utilizing spectrometer The serial dynamic spectrum signal of continuous acquisition sample.

The advantage introduced below that sample dynamic spectrum signal is gathered using the device：(1) solution-air can be implemented heterogeneous anti- The dynamic spectrum of process is answered to gather；(2) there is film-form sample space, sample is big with gas phase contact surface, is conducive to obtaining homogeneous Reaction effect.The embodiment is suitable for solution-air heterogeneous reaction system, but requires the light source transmitting terminal of spectrometer and connect Receiving end can be implemented to be arranged vertically.

In summary, the sample cell of Dynamic Absorption spectra collection proposed by the invention has advantages below：(1) using tool The pad for having predetermined thickness determines or adjusted the spacing of thang-kng piece, and being precisely controlled for film-form sample cell light path can be achieved；(2) by It is in sample in film space, therefore light path can realize 1 percent or even one thousandth of only conventional apparatus, for tool Have for the sample of high absorbance, can directly be observed without being diluted again with solvent；(3) film-form cuvette volume is small but changes Hot area is big, therefore temperature control is sensitiveer and more accurate；(4) film-form sample cell can be provided for corpusculum product sample larger solid-liquid or Solution-air contact interface, still can obtain higher mass-transfer efficiency and reaction homogeneity for heterogeneous reaction system；(5) It is easy to disassemble and combines, the measure and cleaning for high viscosity sample is more convenient.(6) it is simple and compact for structure, it can lead to extensively For existing all kinds of spectroscopy equipments, and reaction-measure integration can be realized.

Claims (10)

1. a kind of sample cell for Dynamic Absorption spectra collection, it is characterised in that including：

Gasket construction, the thickness with setting and with sample well；

Paired thang-kng piece, is stacked in the both sides of gasket construction respectively, and respective inner surface defines film with the sample well The sample space of shape；

Temperature control device, is arranged on close to sample space peripheral position on the outside of thang-kng piece, to control sample temperature in sample space；And

Clamping device, is arranged on the outside of paired thang-kng piece, so that gasket construction is brought into close contact with thang-kng piece,

Wherein, the gasket construction includes single pad or the multiple pads including being removably closely superimposed, and is to constitute one Contact surface of the row with sample in the sample space for setting light path, and the pad and sample space, which has, to be promoted in sample space The catalytic activity of example reaction.

2. sample cell according to claim 1, it is characterised in that each pad is sheet metal or ceramics with predetermined thickness Piece, the sheet metal is by can serve as the platinum of reaction system catalyst in sample space, rhodium, palladium, nickel, copper, iron, aluminium or its alloy structure The solid catalyst of reaction system catalyst in sample space is can serve as into, the potsherd area load.

3. sample cell according to claim 1, it is characterised in that the thickness of each pad is 0.01-0.5mm；And/or Person, a diameter of 6-20mm of the sample well.

4. sample cell according to claim 1 a, it is characterised in that gasket surface of laminating thang-kng piece is provided with and sample The overflow launder of hole connection, for sample, in expansion, overflow goes out sample space.

5. the sample cell according to claim any one of 1-4, it is characterised in that also set on sample well periphery on the pad There is positioning hole in favor of the alignment in the case of multiple pads each other.

6. the sample cell according to claim any one of 1-4, it is characterised in that the clamping device includes：Paired folder Plate is held, the outside of paired thang-kng piece for being stacked in respectively；And retention mechanism, the paired grip block for clamping, so as to protect Fix and be brought into close contact in the position for holding the thang-kng piece between grip block and pad.

7. the sample cell according to claim any one of 1-4, it is characterised in that the temperature control device includes：

Be arranged on inside a grip block or outer surface heat piece and/or cooling piece, and be arranged on inside another grip block or The temperature sensor of inner surface, temperature sensor can be connected with relay and controls to heat/keying of cooling piece.

8. sample cell according to claim 6, it is characterised in that the retention mechanism is selected from screw threads for fastening, elastic fastening And magnetic clamp；And

The area of the pad is not less than 3 times of sample hole area thereon, the table that the paired thang-kng piece is contacted with pad laminating Face area is not less than 3 times of sample hole area, and the paired grip block is not less than with the surface area that the laminating of thang-kng piece is contacted 3 times of sample hole area.

9. the sample cell according to claim any one of 1-4, it is characterised in that the gasket construction includes removably folding Plus multiple pads, and the sample well of adjacent pads is of different sizes, to obtain liquid-solid contact interface area increase and adjustable Sample space.

10. the sample cell according to claim any one of 1-4, it is characterised in that the gasket construction is included removably The multiple pads being closely superimposed up and down, and at least one pad of close upside has the guiding gutter connected with sample well, with To the sample space that solution-air contact interface is stable, so as to be collected suitable for gas-liquid reaction dynamic spectrum.