CN217443264U - Device for analyzing adsorption capacity of adsorption material on volatile mixture - Google Patents
Device for analyzing adsorption capacity of adsorption material on volatile mixture Download PDFInfo
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- CN217443264U CN217443264U CN202220321422.9U CN202220321422U CN217443264U CN 217443264 U CN217443264 U CN 217443264U CN 202220321422 U CN202220321422 U CN 202220321422U CN 217443264 U CN217443264 U CN 217443264U
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Abstract
The utility model relates to a chemical analysis field provides a device of analysis adsorption material to volatile mixture's adsorption efficiency, including sampling device, sample injector, quantitative sampling device, reference chromatographic column, test chromatographic column, detector and auto-change over device. During the test, the reference chromatographic column and the tested chromatographic column are respectively communicated with the sample injector and the detector through the switching device so as to obtain a reference spectrogram and a tested spectrogram. And repeating the comparison tests for multiple times to obtain multiple groups of reference spectrograms and tested spectrograms until the reference spectrograms are the same as the tested spectrograms. And finally, processing each group of reference spectrogram and tested spectrogram to obtain the adsorption capacity of the adsorption material to be detected on the volatile mixture generated in the complex real scene. Therefore, rapid analysis can be performed through a contrast test, the analysis time is shortened, and the test efficiency is improved. And the reference chromatographic column and the tested chromatographic column are integrated together, and share one set of sampling device and detector, so that the manufacturing cost is greatly reduced.
Description
Technical Field
The utility model relates to a chemical analysis technical field especially relates to an analysis and adsorption materials is to volatile mixture's adsorption efficiency's device.
Background
The solid material with certain adsorption capacity has important application in the fields of industrial and agricultural production, environmental protection, medical treatment, chemical research and the like. Therefore, how to analyze and test the adsorption performance of the solid material becomes a problem to be solved by an analytical instrument.
Adsorption of materials can be generally divided into physical adsorption and chemical adsorption. The adsorption material and the adsorbate firstly physically adsorb, and the adsorption material has no selectivity to the adsorbate, and the adsorption strength of the adsorbate on the surface of the adsorption material is weak. Along with the adsorption, chemical adsorption can take place between adsorbate and adsorption material, and compare with physical adsorption, adsorption material is selective to adsorbate, and the effort between the two is stronger.
For the characterization of the adsorption capacity of a material, the most common method is N based on the physical adsorption model (BET equation) 2 Adsorption method. The method is simple and reliable, and can obtain information such as specific surface area, pore volume, pore diameter and the like of the material. Based on this method, a physisorption apparatus was produced.
However, in actual production and application, one is concerned not only with the physical adsorption properties of the material, but also with the chemical adsorption properties of the material. In view of this, chemisorption instruments were produced. The chemical adsorption apparatus is developed based on a Temperature programming technology, and can perform experiments such as Temperature Programmed Reduction (TPR), Temperature Programmed Desorption (TPD), Temperature Programmed Oxidation (TPO), Temperature Programmed Surface Reaction (TPSR), and pulse titration, and is generally used for research on adsorption and Desorption properties of a material, and has various optional experimental conditions such as vacuum, pressurization, low Temperature, and the like. However, these high-precision instruments are only suitable for analyzing the adsorption capacity of the adsorption material to a specific gas or a specific mixture of gases, and have limited application scenarios and high manufacturing costs. In addition, physical adsorption instruments and chemical adsorption instruments require a long time for analyzing a sample, and require a pretreatment of the sample.
In some practical production fields, such as the field of food flavor, the field of perfume and spice production and the like, the volatilized mixture needs to be quickly adsorbed and sealed in a complex real scene, and the adsorbing material needs to have certain physical adsorption capacity and chemical adsorption capacity for some complex mixtures. However, the existing physical adsorption apparatus and chemical adsorption apparatus cannot analyze the adsorption capacity of the adsorption material to the complex mixture, and cannot meet the requirement of testing and characterizing the adsorption capacity of the adsorption material to the volatile mixture generated under the complex real scene.
Therefore, how to solve the problems that the physical adsorption instrument and the chemical adsorption instrument in the prior art can not analyze and test the adsorption capacity of the adsorption material to the volatile mixture in a complex real scene, the manufacturing cost is high, the analysis time is long, and the like becomes an important technical problem to be solved by technical personnel in the field.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide an analysis adsorption material is to volatile mixture's adsorption efficiency's device for physical adsorption appearance and the chemisorption appearance of solving among the prior art can not the analysis test adsorption material to the adsorption efficiency of volatile mixture under the complicated true scene, and the cost is high, the long scheduling problem of analysis time.
The utility model provides a device of adsorption efficiency of analysis and adsorption material to volatile mixture, include:
the sampling device is used for collecting samples to be detected and comprises at least two sample containers for storing the samples to be detected;
the sample injector is used for receiving the sample to be detected;
the quantitative sampling device is used for quantitatively extracting the sample to be detected from the sample container and injecting the sample to the sampler;
the device comprises a sample injector, a reference chromatographic column and a tested chromatographic column, wherein the reference chromatographic column and the tested chromatographic column are both connected with the sample injector, solid particles which are inert and have small specific surface area are arranged in the reference chromatographic column, the solid particles are used as reference, and an adsorbing material to be tested for adsorbing the sample to be tested is arranged in the tested chromatographic column;
the detector is respectively connected with the reference chromatographic column and the tested chromatographic column, and is used for detecting chromatograms of the reference chromatographic column and the tested chromatographic column so as to obtain the adsorption capacity of the adsorption material to be detected on the sample to be detected through comparison by a user;
a switching device having a first operating state and a second operating state and being capable of switching between the first operating state and the second operating state; in the first working state, the switching device is used for communicating the sample injector and the reference chromatographic column with the detector; and in the second working state, the switching device is used for communicating the sample injector, the tested chromatographic column and the detector.
According to the utility model provides an analysis adsorption material is to volatile mixture's adsorption efficiency's device, sampling device sets up to the headspace sample injector, the sample container sets up to the headspace bottle, the headspace sample injector is including heating temperature control dish, each the headspace bottle with the sample injector is arranged in the heating temperature control dish.
According to the utility model provides an analysis adsorption material is to volatile mixture's adsorption efficiency's device, quantitative sampling device sets up to airtight needle.
According to the utility model provides an analysis adsorbing material is to volatile mixture's adsorption efficiency's device, the detector sets up to flame ionization detector.
The device for analyzing the adsorption capacity of the adsorption material to the volatile mixture, provided by the utility model, also comprises an inert gas source, wherein the inert gas source is used for evacuating the impurity gas adsorbed in the reference chromatographic column or the tested chromatographic column,
in the first working state, the switching device is also used for communicating the inert gas source with the tested chromatographic column; in the second operating state, the switching device is further configured to communicate the inert gas source with the reference chromatography column.
According to the utility model provides a device of analysis adsorption material to volatile mixture's adsorption efficiency, switching device sets up to ten logical valves, the sample injector, the inert gas source, the reference chromatographic column, the chromatographic column under test and the detector all are connected with ten logical valves through the pipeline, ten logical valves are equipped with first route and second route, and ten logical valves can be in first operating condition with the second operating condition switch over;
in the first working state, the first passage is used for communicating the sample injector and the reference chromatographic column with the detector, and the second passage is used for communicating the inert gas source with the chromatographic column to be tested;
in the second working state, the first passage is used for communicating the sample injector, the chromatographic column to be tested and the detector, and the second passage is used for communicating the inert gas source and the reference chromatographic column.
According to the utility model provides an analysis adsorption material still includes temperature adjustable's insulation can to volatile mixture's device, the reference chromatographic column with the chromatographic column under test is arranged in the insulation can.
According to the utility model provides an analysis adsorption material is to volatile mixture's adsorption efficiency's device, the material of pipeline is polytetrafluoroethylene or quartz glass.
According to the utility model provides an analysis adsorption material is to volatile mixture's adsorption efficiency's device, the reference chromatographic column with the chromatographic column under test is the packed column, just the reference chromatographic column with the internal diameter and the length homogeneous phase of chromatographic column under test.
According to the utility model provides an analysis adsorption material is to volatile mixture's adsorption efficiency's device, solid particulate matter with the mesh number and the filling volume homogeneous phase of the adsorption material that awaits measuring.
The utility model provides a device of analysis adsorption material to volatile mixture's adsorption efficiency, include: the sampling device is used for collecting samples to be detected and comprises at least two sample containers for storing the samples to be detected; the sample injector is used for receiving a sample to be detected; the quantitative sampling device is used for quantitatively extracting a sample to be detected from the sample container and transferring the sample to the sample injector; the device comprises a reference chromatographic column and a tested chromatographic column, wherein the reference chromatographic column and the tested chromatographic column are both connected with a sample injector, solid particles which are inert and have small specific surface area are arranged in the reference chromatographic column and used as reference, and an adsorbing material to be tested for adsorbing a sample to be tested is arranged in the tested chromatographic column; the detector is respectively connected with the reference chromatographic column and the tested chromatographic column and is used for detecting chromatograms of the reference chromatographic column and the tested chromatographic column so that a user can obtain the adsorption capacity of the adsorption material to be detected on the sample to be detected through comparison; a switching device having a first operating state and a second operating state and being capable of switching between the first operating state and the second operating state; in a first working state, the switching device is used for communicating the sample injector and the reference chromatographic column with the detector; and in the second working state, the switching device is used for communicating the sample injector, the tested chromatographic column and the detector.
During the test, firstly, the sample injector and the reference chromatographic column are communicated with the detector through the switching device, and the quantitative sampling device quantitatively extracts the sample to be detected from the sample container and injects the sample into the sample injector, and then transmits the sample to the subsequent pipeline to obtain the reference spectrogram. And then communicating the sample injector, the tested chromatographic column and the detector through a switching device, and after the quantitative sampling device extracts the sample to be tested with the same volume from the next sample container and injects the sample into the sample injector, transmitting the sample to a subsequent pipeline to obtain a tested spectrogram. Repeating the above steps for multiple times until the reference spectrum is the same as the tested spectrum. And finally, making a difference spectrum for each group of the reference spectrogram and the tested spectrogram, and integrating the peak areas of the difference spectrum to obtain the adsorption capacity of the adsorption material to be tested on the volatile mixed gas generated in the complex real scene.
So set up, the device can rapid analysis await measuring the adsorption efficiency of adsorption material to the volatile mixture in certain complicated real scene through the contrast test, shortens analysis time, improves efficiency of software testing. And the reference chromatographic column and the tested chromatographic column are integrated together, and share one set of sampling device and detector, so that the manufacturing cost is greatly reduced. Therefore, the problems that a physical adsorption instrument and a chemical adsorption instrument in the prior art cannot analyze and test the adsorption capacity of the adsorption material on the volatile mixture in a complex real scene, the manufacturing cost is high, the analysis time is long and the like are solved.
Drawings
In order to more clearly illustrate the technical solutions of the present invention or the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a schematic structural diagram of an apparatus for analyzing the adsorption capacity of an adsorption material for a volatile mixture provided by the present invention;
fig. 2 is a second schematic structural diagram of an apparatus for analyzing the adsorption capacity of an adsorbing material for a volatile mixture provided by the present invention;
FIG. 3 is a partial schematic view of the sample injector provided by the present invention;
reference numerals are as follows:
1: a sample container; 2: a sample injector; 3: a quantitative sampling device; 4: a reference chromatography column; 5: a test chromatographic column; 6: a detector; 7: a switching device; 8: heating the temperature control disc; 9: an inert gas source; 10: a first path; 11: a second path; 12: and (4) an incubator.
Detailed Description
To make the objects, technical solutions and advantages of the present invention clearer, the drawings of the present invention are combined to clearly and completely describe the technical solutions of the present invention, and obviously, the described embodiments are some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
The device for analyzing the adsorption capacity of the adsorption material for volatile compounds according to the present invention is described below with reference to fig. 1 to 3.
As shown in fig. 1, the embodiment of the present invention provides an apparatus for analyzing the adsorption capacity of an adsorption material to a volatile mixture, which includes a sampling device, a sample injector 2, a quantitative sampling device 3, a reference chromatographic column 4, a tested chromatographic column 5, a detector 6, and a switching device 7. Particularly, the application scene of the analysis device is mostly a complex real scene in life, the sampling device is used for collecting samples to be detected, and the samples to be detected are volatile mixtures generated under the complex real scene. As shown in fig. 3, the sampling device comprises at least two sample containers 1 for storing samples to be tested, wherein the number of sample containers 1 can be determined according to the actual test requirements. The sample injector 2 is used for receiving a sample to be tested, and the quantitative sampling device 3 is used for quantitatively extracting the sample to be tested from the sample container 1 and injecting the sample into the sample injector 2. In order to facilitate the transfer of the samples to be tested, as shown in fig. 3, the sample containers 1 can be uniformly distributed around the sample injector 2 at intervals in the circumferential direction, and the device is reasonable in layout and convenient and rapid to operate.
The reference chromatographic column 4 and the tested chromatographic column 5 are both connected with the sample injector 2, and the detector 6 is respectively connected with the reference chromatographic column 4 and the tested chromatographic column 5. The detector is used for detecting chromatograms of the reference chromatographic column 4 and the tested chromatographic column 5 so that a user can obtain the adsorption capacity of the adsorption material to be detected on the sample to be detected through comparison. Wherein, the reference chromatographic column 4 and the tested chromatographic column 5 can be made of glass. The reference chromatographic column 4 is internally provided with inert solid particles with small specific surface area, and concretely, the solid particles can be selected from common quartz sand roasted at high temperature. Since the quartz sand has no micropore structure, the specific surface area is very small and inert, and the quartz sand can not adsorb odor, thereby being used as a reference column. The tested chromatographic column 5 is internally provided with an adsorbing material to be tested for adsorbing a sample to be tested, thereby being used as a tested column.
The switching device 7 has a first operating state and a second operating state and is capable of switching between the first operating state and the second operating state to form different passage states, so that a comparative test can be performed. In a first operating state, as shown in fig. 1, the switching device 7 is used to connect the sample injector 2 and the reference column 4 to the detector 6, so that the sample to be measured enters the reference column 4, thereby obtaining a reference spectrum. In the second working state, as shown in fig. 2, the switching device 7 is used to connect the sample injector 2, the chromatographic column under test 5 and the detector 6, so that the sample to be tested enters the chromatographic column under test 5, thereby obtaining the spectrogram under test.
Specifically, during the test, as shown in fig. 1, the sample injector 2 and the reference chromatographic column 4 are firstly communicated with the detector 6 through the switching device 7, and the quantitative sampling device 3 quantitatively extracts the sample to be measured from the sample container 1 and injects the sample into the sample injector 2, and then transmits the sample to the subsequent pipeline, so as to obtain the reference spectrogram. As shown in fig. 2, the sample injector 2 and the chromatographic column under test 5 are then communicated with the detector 6 through the switching device 7, and the quantitative sampling device 3 extracts an equal amount of sample to be tested from the next sample container 1, injects the sample into the sample injector 2, and then transmits the sample to a subsequent pipeline to obtain a spectrogram under test. Repeating the above steps for multiple times until the reference spectrogram is the same as the tested spectrogram, and the sample amount to be tested adsorbed by the tested chromatographic column 5 reaches a saturation state. And finally, making a difference spectrum for each group of the reference spectrogram and the tested spectrogram, and integrating the peak areas of the difference spectrum to obtain the adsorption capacity of the adsorption material to be tested on the volatile mixed gas generated in the complex real scene.
Because the amount of the sample to be detected injected each time is constant and the amount of the sample to be detected injected each time is in proportional relation with the area of the spectrum peak in the reference spectrogram each time, the area of the spectrum peak of the difference spectrum can quantitatively reflect the adsorption capacity of the adsorption material to be detected. Therefore, the analyzer can perform both qualitative analysis and quantitative analysis. In addition, the types of the adsorbing materials to be detected in the tested chromatographic column 5 are changed, and the filling volumes of the adsorbing materials to be detected in different types are ensured to be the same, so that the adsorbing capacities of different adsorbing materials on volatile mixtures generated in the same complex real environment can be quantitatively compared. In addition, the type of the sample to be detected in the sample container 1 can be changed, so that the adsorption capacity of the same adsorption material on volatile mixtures generated under different complex real scenes can be qualitatively compared.
So set up, the device can rapid analysis await measuring the adsorption efficiency of the adsorption material to the volatile mixture that produces in certain kind of complicated real scene through contrast test, need not to each component separation of complicated mixture, carry out sample pretreatment, has shortened analysis time, has improved efficiency of software testing. And the reference chromatographic column 4 and the tested chromatographic column 5 are integrated together and share one set of sampling device and detection instrument, so that the manufacturing cost is greatly reduced. Therefore, the problems that a physical adsorption instrument and a chemical adsorption instrument in the prior art can not analyze and test the adsorption capacity of the adsorption material on the volatile mixture in a complex real scene, the manufacturing cost is high, the analysis time is long and the like are solved.
The embodiment of the utility model provides an in, sampling device sets up to full-automatic headspace sample injector, and sample container 1 sets up to the headspace bottle, and the headspace sample injector is including heating temperature control dish 8, and each headspace bottle and sample injector 2 are arranged in heating temperature control dish 8. The headspace sampler is an existing mature product, and therefore the specific structure thereof is not described herein again. Wherein, heating temperature control dish 8 can set up suitable thermal desorption temperature according to the actual test demand. In the test, as shown in fig. 3, equal mass of sample matrix is put into each headspace bottle with the same volume, the sample matrix can be solid, liquid or gas, and then the headspace bottle is sealed. Wherein, the size of headspace bottle can be changed according to the experiment needs. Then, each headspace bottle is placed in a heating temperature control disc 8, a proper thermal desorption temperature is set, and volatile components are volatilized from the sample matrix in a heating temperature rise mode. And (3) keeping the headspace bottle at the thermal desorption temperature for a certain time to ensure that all components of the volatile mixture of the sample matrix in the bottle reach thermal balance, thereby collecting the sample to be detected. Then, the quantitative sampling device 3 will automatically and quantitatively extract the top gas, i.e. the sample to be tested, from the headspace bottle, and move to the sample injector 2 in the heating temperature control plate 8 after extraction, and inject the quantitatively extracted gas into the sample injector 2 for subsequent test operation. In addition, the headspace bottle and the sample injector 2 are both placed in the heating temperature-controlled plate 8, and can be kept at the same temperature for transporting the sample gas.
In an alternative embodiment of the present invention, the quantitative sampling device 3 is configured as a hermetic needle. During the experiment, airtight needle can prick sample container 1 automatically and draw a certain amount of gas that awaits measuring, then moves to injector 2 position department to gas that awaits measuring that will quantitatively draw pours into injector 2 into, thereby transmit to auto-change over device 7, guarantees that gas that awaits measuring does not receive external disturbance in the transfer process. The sample introduction amount and the sample introduction speed of the gas to be detected can be determined according to actual test requirements.
The reference chromatographic column 4 and the tested chromatographic column 5 are both packed columns, and the reference chromatographic column 4 and the tested chromatographic column 5 have the same inner diameter and the same length. In particular, the column has an internal diameter of 4 mm to 10 mm, for example 4 mm, suitably sized to ensure stability during the test.
Meanwhile, in the filling process, the quartz sand and the adsorbing material to be detected have the same mesh number and the same filling volume. The filling amount of the quartz sand and the adsorbing material to be detected can be determined according to the actual test requirements. Therefore, the comparison group and the test group have comparability, the reference spectrogram and the tested spectrogram are ensured to be obtained under the same test condition, and the reliability of the test result is ensured.
In an embodiment of the utility model, detector 6 sets up to flame ionization detector. The flame ionization detector is a mature product, and therefore the detailed structure thereof is not described herein. The Flame Ionization Detector (FID) is a high-sensitivity universal Detector, and as most of application scenes of the analysis device are complex real scenes in life, gas to be detected is a mixture and the components of the gas are organic matters, and the FID almost responds to all organic matters, and has no response or very small response to inorganic matters, inert gases or undissociated substances in Flame and the like, the FID is selected as the Detector in the embodiment, and the detection result is more accurate and reliable.
In the embodiment of the present invention, the device for analyzing the adsorption capacity of the adsorption material to the volatile mixture further includes an inert gas source 9, and the inert gas source 9 is used for evacuating the impurity gas adsorbed in the reference chromatographic column 4 or the tested chromatographic column 5. And in the first operating condition the switching device 7 is also used to connect the inert gas source 9 to the chromatographic column under test 5. In the second operating state, the switching device 7 is also used to place an inert gas source 9 in communication with the reference column 4. Specifically, the inert gas can be high-purity nitrogen with low cost, and is pumped into the device through a gas pump. Set up like this, when carrying out every group contrast test, can clear away the adsorbed gaseous impurity of chromatographic column, eliminate the influence of gaseous impurity to the test result, guarantee that the test result is more accurate.
In an alternative embodiment of the present invention, the switching device 7 is configured as a ten-way valve, as shown in fig. 1 and 2, and the sample injector 2, the inert gas source 9, the reference chromatographic column 4, the tested chromatographic column 5 and the detector 6 are all connected to each interface of the ten-way valve through pipelines. The ten-way valve is provided with a first passage 10 and a second passage 11, and is switchable between a first operating state and a second operating state. In the first operating state, the first passage 10 is used to connect the sample injector 2 and the reference column 4 to the detector 6, and the second passage 11 is used to connect the inert gas source 9 to the chromatographic column under test 5. In the second operating state, the first passage 10 is used to connect the sample injector 2, the chromatographic column under test 5 and the detector 6, and the second passage 11 is used to connect the inert gas source 9 and the reference chromatographic column 4.
Specifically, an electromagnetic ten-way valve is adopted, the position of the ten-way valve is changed through electromagnetic driving force, and a pipeline passage is switched, so that a comparison test is carried out. First, the ten-way valve is in the first operating state. As shown in fig. 1, the outlet of the sample injector 2, the reference chromatographic column 4 and the detector 6 are connected through a first passage 10 of a ten-way valve, and the volatile mixture gas quantitatively extracted by the gas-tight needle enters the sample injector 2 and is transmitted to a subsequent pipeline to obtain a reference spectrum. Meanwhile, the inert gas source 9 is communicated with the tested chromatographic column 5 through the second passage 11 of the ten-way valve, and purges the filled adsorbing material to be tested, and exhausts the adsorbed impurity gas.
And then, the ten-way valve is driven to rotate through electromagnetic force, and the communication interface of the ten-way valve is changed, so that the ten-way valve is in a second working state. As shown in fig. 2, the outlet of the sample injector 2, the chromatographic column under test 5 and the detector 6 are connected through the first path 10 of the ten-way valve, the airtight needle is inserted into the next headspace bottle, and the same volume of volatile mixture gas is re-extracted and injected into the sample injector 2, thereby obtaining the test spectrum. Meanwhile, the inert gas source 9 is communicated with the reference chromatographic column 4 through the second passage 11 of the ten-way valve, and purges the filled quartz sand to empty the impurity gas adsorbed by the quartz sand. Repeating the steps for multiple times to obtain multiple groups of comparison spectrograms until the reference spectrogram is the same as the tested spectrogram.
The material of the pipeline is polytetrafluoroethylene or quartz glass, and the diameter of the pipeline is 4 mm to 10 mm, for example, 4 mm. Among them, polytetrafluoroethylene has strong corrosion resistance, has the characteristics of acid and alkali resistance and resistance to various organic solvents, and is almost insoluble in all solvents. Meanwhile, the polytetrafluoroethylene has high temperature resistance, wear resistance, extremely low friction coefficient and extremely strong non-adhesion property. The quartz glass has high temperature resistance, acid and alkali resistance, good chemical stability and mechanical property, and can be made into instruments and products with various shapes. Therefore, each connecting pipeline is made of polytetrafluoroethylene or quartz glass, the service life is long, odor can not be adsorbed or adhered almost, and the test is prevented from being influenced.
In the embodiment of the present invention, the device for analyzing the adsorption capacity of the adsorption material to the volatile mixture further includes a temperature-adjustable thermal insulation box 12, and the reference chromatographic column 4 and the tested chromatographic column 5 are disposed in the thermal insulation box 12. Set up like this, can make reference chromatographic column 4 and test chromatographic column 5 be in same heat preservation system, through adjusting the temperature in insulation can 12, can test the adsorption efficiency of adsorption material to volatile mixture under different temperatures moreover, application range is wider, uses more nimble changeable. In addition, a controller can be arranged and is electrically connected with the sampling device, the quantitative sampling device 3, the detector 6, the switching device 7 and the like, so that the intelligent control of the test process is realized. The controller is a conventional mature technology, so the specific structure and the electrical connection relationship between the controller and each actuator are not described herein again.
Combine above-mentioned each embodiment, the utility model discloses to current chemical analysis technique can not study the adsorption efficiency of adsorption material to volatile mixture under the complicated real scene, can not carry out qualitative and quantitative research simultaneously, and the cost is high, the long scheduling problem of analysis time, provide a neotype can be used to the device of the adsorption efficiency of analysis adsorption material to the volatile mixture that produces under the complicated real scene, including sampling device, sample injector 2, quantitative sampling device 3, reference chromatographic column 4, subject chromatographic column 5, detector 6, switching device 7, inert gas source 9, insulation can 12 to and controller etc.. Specifically, the sampling device selects a full-automatic headspace sampler, the quantitative sampling device 3 selects a gas-tight needle, the reference chromatographic column 4 is internally provided with quartz sand used as a reference, the tested chromatographic column 5 is internally provided with an adsorbing material to be tested, the detector 6 selects an FID, the switching device 7 selects an electromagnetic ten-way valve, and the inert gas source 9 selects high-purity nitrogen. The controller can be electrically connected with the headspace sample injector, the air-tight needle, the FID, the ten-way valve and the like so as to automatically control according to the test requirement.
During testing, equal mass sample matrixes are placed into headspace bottles with the same volume, and the headspace bottles are sealed. Each headspace bottle is heated by the heating temperature control disc 8 to carry out thermal desorption, so that the volatile mixture in the matrix is fully volatilized. Then, the airtight needle can be automatically inserted into the headspace bottle to quantitatively extract the headspace gas, and the sample gas is injected into the sample injector 2 after being extracted and is transmitted to the ten-way valve.
The ten-way valve is switchable between a first operating state and a second operating state so that the first passage 10 and the second passage 11 connect different test passages. In the first operating state, the first channel 10 connects the sample injector 2 outlet, the reference column 4 and the FID. The airtight needle is inserted into the headspace bottle to quantitatively extract the sample gas and is injected into the sample injector 2, and the sample injector 2 is communicated with the reference chromatographic column 4 and the FID through a ten-way valve, so that a reference spectrogram is obtained. Meanwhile, the high-purity nitrogen is communicated with the tested chromatographic column 5 through the second passage 11 of the ten-way valve, and is used for purging the filled adsorbing material to be tested and evacuating the impurity gas adsorbed by the adsorbing material.
Then, the ten-way valve is switched to the second working state. The airtight needle is inserted into the next headspace vial and the same volume of sample gas is re-withdrawn and injected into the injector 2. The sample injector 2 communicates with the chromatographic column under test 5 and the FID through the first passage 10 of the ten-way valve, thereby obtaining a spectrum under test. Meanwhile, the high-purity nitrogen is communicated with the reference chromatographic column 4 through a second passage 11 of the ten-way valve, and is used for purging the filled quartz sand and evacuating the impurity gas adsorbed by the quartz sand.
And repeating the steps for multiple times according to the operation steps to obtain multiple groups of reference spectrograms and tested spectrograms until the reference spectrograms are the same as the tested spectrograms. And finally, making a difference spectrum for each group of the reference spectrogram and the tested spectrogram, and integrating the peak areas of the difference spectrum to obtain the adsorption capacity of the adsorption material to be tested on the volatile mixed gas generated in the complex real scene.
To sum up, the utility model discloses a contrast test can rapid analysis adsorption material to the adsorption efficiency of the smell in certain kind of complicated true scene, still can adjust the gaseous sample injection volume of sample and the filling volume in sample introduction speed and reference chromatographic column 4 and the test chromatographic column 5 according to the test demand to synthesize and advance kind condition and spectrogram result and can carry out qualitative and quantitative analysis simultaneously. Furthermore, the utility model discloses utilize electromagnetism ten logical valve with two sets of chromatogram packing column integrations in one set of insulation can system, one set of headspace sample injector and FID of sharing to manufacturing cost has been reduced. And simultaneously, the utility model discloses degree of automation is higher, has reduced the test system error that manual operation leads to.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention in its corresponding aspects.
Claims (10)
1. An apparatus for analyzing the adsorption capacity of an adsorbent material for a volatile mixture, comprising:
the sampling device is used for collecting samples to be detected and comprises at least two sample containers for storing the samples to be detected;
the sample injector is used for receiving the sample to be detected;
the quantitative sampling device is used for quantitatively extracting the sample to be detected from the sample container and injecting the sample to the sampler;
the device comprises a sample injector, a reference chromatographic column and a tested chromatographic column, wherein the reference chromatographic column and the tested chromatographic column are both connected with the sample injector, solid particles which are inert and have small specific surface area are arranged in the reference chromatographic column, the solid particles are used as reference, and an adsorbing material to be tested for adsorbing the sample to be tested is arranged in the tested chromatographic column;
the detector is respectively connected with the reference chromatographic column and the tested chromatographic column, and is used for detecting chromatograms of the reference chromatographic column and the tested chromatographic column so as to obtain the adsorption capacity of the adsorption material to be detected on the sample to be detected through comparison by a user;
a switching device having a first operating state and a second operating state and being capable of switching between the first operating state and the second operating state; in the first working state, the switching device is used for communicating the sample injector and the reference chromatographic column with the detector; and in the second working state, the switching device is used for communicating the sample injector, the tested chromatographic column and the detector.
2. The apparatus for analyzing an adsorbent material for a volatile compound according to claim 1, wherein the sampling device is configured as a headspace sampler, the sample container is configured as a headspace vial, the headspace sampler comprises a heated temperature controlled plate, and each of the headspace vial and the sampler is disposed within the heated temperature controlled plate.
3. The device for analyzing the adsorption capacity of an adsorption material for a volatile mixture according to claim 1, wherein the quantitative sampling device is configured as a gas-tight needle.
4. The apparatus for analyzing an adsorbent capacity of an adsorbent material for a volatile compound of claim 1, wherein the detector is configured as a flame ionization detector.
5. The apparatus according to claim 1, further comprising an inert gas source for evacuating impurity gases adsorbed in the reference or test chromatographic column,
in the first working state, the switching device is also used for communicating the inert gas source with the tested chromatographic column; in the second operating state, the switching device is further configured to communicate the inert gas source with the reference chromatography column.
6. The apparatus for analyzing an adsorption capacity of an adsorbent material for a volatile mixture according to claim 5, wherein the switching means is provided as a ten-way valve, the sample injector, the inert gas source, the reference chromatography column, the chromatography column under test and the detector are all connected to the ten-way valve through a pipeline, the ten-way valve is provided with a first passage and a second passage, and the ten-way valve is switchable between the first operating state and the second operating state;
in the first working state, the first passage is used for communicating the sample injector and the reference chromatographic column with the detector, and the second passage is used for communicating the inert gas source with the chromatographic column to be tested;
in the second operating state, the first passage is used for communicating the sample injector, the chromatographic column to be tested and the detector, and the second passage is used for communicating the inert gas source and the reference chromatographic column.
7. The apparatus according to claim 1, further comprising a temperature-adjustable incubator, wherein the reference column and the test column are disposed in the incubator.
8. The device for analyzing the adsorption capacity of an adsorption material on a volatile mixture according to claim 6, wherein the material of the pipeline is polytetrafluoroethylene or quartz glass.
9. The apparatus for analyzing the adsorption capacity of an adsorbent material for a volatile mixture according to claim 1, wherein the reference chromatography column and the test chromatography column are both packed columns, and the reference chromatography column and the test chromatography column have the same inner diameter and length.
10. The apparatus for analyzing the adsorptive capacity of an adsorbent material for a volatile mixture according to claim 1, wherein the mesh size and the packing volume of the solid particulate material and the adsorbent material to be tested are the same.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117686638A (en) * | 2024-02-04 | 2024-03-12 | 中国科学院合肥物质科学研究院 | Detection device and detection method for residual solvent in solid medicine |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117686638A (en) * | 2024-02-04 | 2024-03-12 | 中国科学院合肥物质科学研究院 | Detection device and detection method for residual solvent in solid medicine |
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