CN110726592A - Self-cleaning sampling device and online spectrum detection method thereof - Google Patents
Self-cleaning sampling device and online spectrum detection method thereof Download PDFInfo
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/14—Suction devices, e.g. pumps; Ejector devices
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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
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
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- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/14—Suction devices, e.g. pumps; Ejector devices
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Abstract
The invention provides a self-cleaning sampling device, which is used for sample solution and comprises a filter head, a sample pool, a power pump and a sample collection channel, wherein the filter head, the sample pool and the power pump are sequentially connected through a conduit; still be equipped with a main entrance valve on the pipe, the front end of sample collection passageway is equipped with gathers the passageway valve, the power pump sets up to provide power for absorption and propelling movement of sample solution, can provide the power of forward and reverse motion. The invention also provides an online spectrum detection method thereof. The sampling point of the self-cleaning sampling device is also a sample reflux point, one period of sucking a sample and pushing the sample not only finishes the spectrum detection but also realizes the purpose of cleaning a channel, and the filtering and cleaning are carried out on the same device and are finished by the same sample fluid, so that the self-cleaning sampling device has the advantages of simpler and more compact structure, more flexible and convenient use and easy maintenance.
Description
Technical Field
The invention belongs to the field of sample pretreatment and online spectrum detection of analytical chemistry, and particularly relates to a self-cleaning sampling device and an online spectrum detection method thereof.
Background
Process Analysis Technology (PAT) is a technology for designing, analyzing and controlling production processes by timely measuring the key quality and performance characteristics of raw materials and materials in process. PAT is helpful to grasp the state, content and property of various materials in real time, deeply understand the working condition and essence of each procedure in the industrial process, and is more beneficial to the actual control of the production process. Therefore, the PAT plays an important role in reducing production time, improving product quality and improving automation degree. The online detection is an important content of PAT, and the spectroscopic technology, especially the near infrared spectroscopic technology, is one of the most important online detection technologies of PAT in the industry at present. The spectral analysis technology has simple operation, convenient use and quick measurement, can provide rich molecular information, and is an ideal on-line detection technology. In recent decades, spectral detection, mainly based on near infrared spectroscopy, has become more and more widely used in PAT, and representative application fields include pharmacy, petrochemical industry, basic organic chemical industry, food production and processing, wine brewing, and the like.
On-line detection techniques typically use optical fibers to connect the monitoring point to the spectrometer, thus avoiding many environmental concerns and limitations. For a clear solution sample, an optical fiber probe or a flow cell is arranged at a monitoring point, so that the on-line collection of the spectrum can be conveniently realized. However, in production links such as traditional Chinese medicine extraction, biological fermentation, chemical reaction caused by precipitation and the like, the object to be detected is a turbid liquid sample, and suspended particulate matters can seriously affect the measurement of the spectrum.
One simple way to solve this problem is to use a filter material at the front end of the spectrum detection point to remove the particulate matter, but the long-time on-line detection process can cause the filter material to be seriously clogged, which affects the smooth monitoring. Another solution, also the current mainstream method, is to use a bypass to lead the tested liquid sample out of the main line, and design a set or several sets of filtering devices on the bypass, and equip with a flushing device, the former is used to filter out particulate matter, the latter is a cleaning filter, therefore, after the solution sample is led out from the sample tank, it flows back to the sample tank from another point after a series of filtering, flushing processes, and spectrum collecting processes. Although the method better solves the problems of blockage, cleaning, spectral measurement and the like, the structure is often complex. The complicated equipment is not easy to maintain except that the cost is high, and the long-term use is easy to accumulate particulate matters to block the filter. The bypass sampling device in the existing on-line spectrum monitoring system has a complex structure and is difficult to maintain.
Therefore, there is a great need for developing an on-line spectrum detection device with simple structure, convenient use, easy maintenance and convenient spectrum measurement.
Disclosure of Invention
The invention aims to provide a self-cleaning sampling device with a simple structure and a self-cleaning function and an online spectrum detection method thereof, so as to realize online spectrum detection and self-cleaning of the device.
In order to achieve the above object, the present invention provides a self-cleaning sampling device for sample solution, comprising a filter head, a sample cell, a power pump, and a sample collection channel connected to a portion of a conduit at the front end or the rear end of the sample cell, which are connected in sequence by a conduit; still be equipped with a main channel valve on the pipe between filter head and sample cell, the front end of sample collection passageway is equipped with gathers the passageway valve, the power pump sets up to provide power for absorption and propelling movement of sample solution, can provide the power of forward and reverse motion.
And the two opposite sides of the sample cell are respectively provided with a light source and a detector which are connected with the sample cell, and the detector is connected with a computer.
The filter head is connected with a sample storage component, the sample storage component comprises a gear pump, an industrial feed liquid storage tank and a sample tank with a filter cartridge, the gear pump, the industrial feed liquid storage tank and the sample tank are sequentially connected through a stainless steel pipeline along the flow direction of a sample solution and form a loop, and the filter head is connected with the sample tank.
And a glass light screen is arranged between the filter head and the sample cell.
The power pump is a peristaltic pump with forward and reverse movement functions, or a syringe.
The collecting channel valve and the main channel valve are both electromagnetic valves, and the opening and closing of the collecting channel valve and the main channel valve are synchronous with the power direction of the power pump.
The filter head is made of a porous material, and the pore diameter of the filter head is in the range of 1-20 mu m; the sample cell is made of quartz glass or common optical glass and is in a regular square shape or a regular circular shape, and the optical path is 1mm-10 mm; the conduit is made of a corrosion-resistant plastic pipe, a metal pipe or a glass pipe; the total length of the entire conduit, together with the filter head, sample cell and power pump, is in the range 100mm-1000 mm.
In another aspect, the present invention provides a method for on-line spectral detection according to the self-cleaning sampling device described above, comprising:
s1: the power pump is started, and simultaneously, the main channel valve is opened, so that the power pump sucks the sample solution in the direction of the power pump, and the sample solution enters the sample pool and the sample collection channel through the filter head;
s2: carrying out rapid spectrum detection in a sample pool, collecting sample solution through a sample collection channel, sending the sample solution to a laboratory for detection and comparing results;
s3: the power of the power pump is reversed to push the sample solution through the filter head in a direction away from the power pump to clean the filter head, and then the main channel valve is closed until the next sample is taken.
The step S2 of collecting the sample solution through the sample collecting channel is synchronized with the step S1 of collecting the sample solution through the filter head into the sample cell and the sample collecting channel, or the step of collecting the sample solution through the sample collecting channel corresponds to a plurality of times of collecting the sample solution through the filter head into the sample cell and the sample collecting channel.
In the step S1, the total amount of the sample solution entering the sample cell is below 10mL, and the total time of the steps S1 and S2 is generally within 10 seconds.
The sampling point of the self-cleaning sampling device is also a sample reflux point, one period of sucking a sample and pushing the sample not only finishes the spectrum detection but also realizes the purpose of cleaning a channel, and the filtering and cleaning are carried out on the same device and are finished by the same sample fluid, so that the self-cleaning sampling device has the advantages of simpler and more compact structure, more flexible and convenient use and easy maintenance. The sampler has unique advantages for online spectrum detection in industrial production processes such as traditional Chinese medicine extraction, biological fermentation and other turbid liquid samples. In addition, because the sample amount needed by the sample spectrum measurement is generally small, the total amount of the sample sucked into the whole sampler is small, and the time for sucking the sample and measuring the spectrum is short, the delay caused by the sampling and measuring spectrum process is small, and the sucked sample returns to the sample tank, so the change of the sample component in the tank is small.
Drawings
FIG. 1 is a schematic diagram of a self-cleaning sampling apparatus according to one embodiment of the present invention.
FIG. 2 is a near infrared spectrum of the extraction process of gardenia jasminoides ellis by the on-line spectrum detection method of the self-cleaning sampling device of the present invention;
FIG. 3 is a visible spectrum diagram of the extraction process of gardenia jasminoides ellis by the on-line spectrum detection method of the self-cleaning sampling device of the present invention;
FIG. 4 is a graph of the ultraviolet spectrum of bisphenol A reaction process monitoring obtained by the on-line spectral detection method of the self-cleaning sampling apparatus of the present invention.
Detailed Description
The present invention will be further described with reference to the following specific examples. It should be understood that the following examples are illustrative only and are not intended to limit the scope of the present invention.
Referring to fig. 1, a self-cleaning sampling apparatus according to an embodiment of the present invention, which is adapted to sample solution, includes a filter head 1, a sample cell 2, a power pump 3, and a sample collection channel 5 connected to a portion of a conduit 4 at the front end or the rear end of the sample cell 2, which are connected in series via a conduit 4.
The other parts in fig. 1 belong to the matching parts, are not necessary for the invention, and can be increased, decreased and adjusted according to the production process conditions.
Wherein, a glass light screen 7 is arranged between the filter head 1 and the sample cell 2 and is used for shading the sample solution.
The filter head 1 is used for filtering micro particles in a sample solution, and is made of a porous material, wherein the material of the porous material is at least one of porous ceramic, a porous metal material (including a stainless steel screen) and a silicon dioxide material. The pore channels are required to be uniform and fine, are not easy to crack and can not pollute the sample. The porous material is selected to have a suitable pore size according to the particle size in the sample, and the pore size of the filter head is generally in the range of 1-20 μm.
The sample cell 2 is used for on-line spectrum measurement, is made of quartz glass or common optical glass, is in a regular square shape or a regular circular shape, has an optical path of 1mm-10mm, and has a specific value related to the absorption degree of a sample and required absorbance below 2. The light transmitting portion of the sample cell must be smooth, flat, and have a high light transmittance. The spectrum can be rapidly measured after the solution sample flows into the sample cell 2. The two opposite sides of the sample cell 2 are respectively provided with a light source 21 and a detector 22 connected with the sample cell 2, in this embodiment, the sample cell 2 is a cuboid, the light source 21 and the detector 22 are respectively connected with the bottom surface and the top surface of the sample cell 2 through silicone rubber tubes, and the detector 22 is connected with a computer 23.
The power pump 3 is set to provide power for the suction and the pushing of the sample solution, can provide power for forward and reverse movement, can select a reciprocating pump or a peristaltic pump with forward and reverse movement functions, and can also adopt a manual syringe to complete suction and pushing actions if the requirement is not high.
The conduit 4 is used for transmitting sample solution and is connected with the filter head 1, the sample pool 2, the power pump 4 and the sample collection channel 5. The conduit 4 can be made of corrosion-resistant plastic pipe, metal pipe or glass pipe, and the pipe diameter is matched with the size of the filter head and the sample cell. The pipe diameter should be as short as possible without affecting the operation, and the total length of the whole conduit 4, the filter head 1, the sample cell 2 and the power pump 3 is generally in the range of 100mm-1000 mm.
The sample collection channel 5 is used for taking out a sample solution from the device, sending the sample solution to a laboratory for detection, comparing a detection result with a spectrum detection result, and verifying whether the detection result is consistent. The front end of the sample collection channel 5 is provided with a collection channel valve 51. The collection channel valve 51 is opened to draw the sample solution and closed to stop the flow of the solution.
In addition, a main channel valve 41 is provided in the conduit 4 between the filter head 1 and the sample cell 2.
In this embodiment, the collection channel valve 51 and the main channel valve 41 are both solenoid valves, and the opening and closing of the collection channel valve 51 and the main channel valve 41 are synchronized with the power direction of the power pump 3, so as to automatically control the opening and closing of the collection channel valve and keep synchronization with the suction and pushing of the sample solution. The main channel valve 41 needs to be opened and closed every time the solution flows, whereas the collection channel valve 51 does not have to be opened every time and is opened only when the sample solution needs to be collected.
The filter head 1 is connected with a sample storage assembly 6, the sample storage assembly 6 comprises a gear pump 61, an industrial feed liquid storage tank 62 and a sample tank 63 with a filter cartridge, which are sequentially connected through a stainless steel pipeline along the flow direction of a sample solution and form a loop, and the filter head 1 is connected with the sample tank 63. Therefore, the liquid in the industrial liquid storage tank 62 can be conveyed to the sample tank 63 through the stainless steel pipeline by the gear pump 61, and then the liquid in the sample tank 63 is directed towards the west region of the power pump 3 under the action of the power pump 3, and the liquid passes through the filter head 1 connected with the screw thread and passes through the glass light screen 7 to be detected in the sample cell 2. The sample collection channel 5 can control the sample collection amount through the collection channel valve 51.
Based on the self-cleaning sampling device, the realized online spectrum detection method of the self-cleaning sampling device specifically comprises the following steps:
s1: the power pump 3 is started, and simultaneously the main channel valve 41 is opened, so that the power pump 3 sucks the sample solution from the sample storage assembly 6 towards the power pump 3, the sample solution passes through the filter head 1, turbid substances are filtered out by the filter head, and the clarified filtrate enters the sample cell, passes through the glass light screen 7 and enters the sample cell 2 and the sample collection channel 5;
the sample storage assembly 6 comprises a gear pump 61, an industrial feed liquid storage tank 62 and a sample tank 63 with a filter cartridge, which are sequentially connected through stainless steel pipelines and form a loop, wherein the sample solution conveys the liquid in the industrial feed liquid storage tank 62 to the sample tank 63 through the gear pump 61 and is sucked from the sample tank 63 towards the power pump 3.
S2: performing rapid spectrum detection in the sample cell 2, collecting partial sample solution through the sample collecting channel 5, and sending the sample solution to a laboratory for detection and result comparison;
wherein, the step S2 of collecting the sample solution through the sample collecting channel 5 is synchronized with the step S1 of collecting the sample solution through the filter head 1 into the sample cell 2 and the sample collecting channel 5, or the step of collecting the sample solution through the sample collecting channel 5 corresponds to a plurality of times of collecting the sample solution through the filter head 1 into the sample cell 2 and the sample collecting channel 5. In the step S1, the total amount of the sample solution entering the cuvette 2 is 10mL or less, and the total time of the steps S1 and S2 is generally within 10 seconds. The above-mentioned working process also requires the corresponding valves to work synchronously, i.e. when a part of the sample solution is collected through the sample collection channel 5, the collection channel valve 51 of the sample collection channel 5 is opened to collect the sample solution in the channel, and the collection channel valve 51 is closed after the sample solution is taken out.
The rapid spectrum detection of the invention can be used for the online detection of absorption spectra, including near infrared spectra, ultraviolet spectra, visible spectra and mid-infrared spectra, and also can be used for fluorescence spectra and Raman spectra. For the latter two spectra, the sample cell is adapted to the requirements of the two spectroscopic analysis techniques. Two or more spectra may also be measured simultaneously by adapting the sample cell.
S3: the power of the power pump 3 is reversed to push the sample solution back through the filter head 1 to the sample storage assembly 6 away from the power pump 3 to clean the filter head 1 and then close the main channel valve 41 until the next sample is taken.
Step S4: the steps S1-S3 are repeated after a period of time (the frequency can be adjusted according to actual production needs) so as to continuously detect the change of the sample solution in the whole process of the sample solution production in a time sequence.
In the above steps S1-S4, the whole sampler work flow needs to be set according to the requirement of on-line spectrum detection, and specific sample solution sucking, sample solution pushing and sample solution collecting time is specified. The sample solution is drawn in order to determine the spectrum, the sample solution is pushed in order to return the sample solution and clean the channel, and the sample solution is collected for subsequent laboratory testing of the sample solution for sampling.
Results of the experiment
Specific examples of the on-line spectral detection method of the self-cleaning sampling apparatus of the present invention are provided below. The examples are all on-line spectrum detection work carried out in a laboratory sampling small container, and the operation of the examples can be completely applied to larger-scale experiments or actual production on the premise of meeting production conditions.
Example 1 near infrared spectroscopy on-line monitoring of extraction process of active ingredient of gardenia jasminoides ellis
The online spectrum detection method of the self-cleaning sampling device is adopted to perform online monitoring of near infrared spectrum on the extraction process of the traditional Chinese medicine, and comprises the following steps:
s100: weighing 38g of traditional Chinese medicine gardenia, putting the traditional Chinese medicine gardenia into a 500mL round-bottom flask, adding 380mL of water into the round-bottom flask, and heating and boiling to extract active ingredients in the gardenia to obtain a sample solution.
S101: the filter head 1 of the self-cleaning sampling device of the present invention is placed in a round bottom flask and submerged in the solution. The other parts of the self-cleaning sampling device of the present invention are assembled as described above and connected to the near infrared spectrometer as detector 22.
S102: when the traditional Chinese medicine gardenia is completely wetted, heating and refluxing are started, and a peristaltic pump is used for pumping a solution to slowly flow through a sample cell for rapid spectrum detection; wherein, the heating is carried out by adopting an electric heating jacket for a laboratory, and the reflux is carried out by adopting a spherical condenser pipe. The heating power was around 300w to boil the aqueous solution and held for 4 hours. By the rapid spectrum detection, the near infrared spectrum can be analyzed, judged and extracted to obtain an end point or other information.
S103: after the assay was completed, the peristaltic pump was reversed to push the solution back into the flask.
The rotating speed of the pump is 20 r/min, so that the solution can flow stably and has moderate speed. The time for the solution to be drawn from the flask to the sample cell was about 5 seconds, and the spectroscopic detection time was about 10 seconds. After that, every 10 minutes is separated,
s104: the above procedure was repeated and the near infrared spectrum was recorded. Fig. 2 is a recorded near infrared spectrum.
Example 2 visible spectrum on-line monitoring of extraction process of active ingredient of fructus Gardeniae
The online spectrum detection method of the self-cleaning sampling device is adopted to carry out online monitoring on visible spectrum in the extraction process of the traditional Chinese medicine, and comprises the following steps:
s200: 38g of traditional Chinese medicine gardenia is weighed and placed into a 500mL round-bottom flask, 380mL of water is added into the round-bottom flask, and a sample solution is obtained. And the flask was equipped with a reflux cooling device, and a thermometer.
S201: the filter head 1 of the self-cleaning sampling device of the present invention is placed in a round bottom flask and submerged in the solution. The other parts of the self-cleaning sampling apparatus of the present invention are assembled and connected to a visible spectrometer as detector 22.
S202: when the traditional Chinese medicine gardenia is completely wetted, heating reflux is started, a peristaltic pump is used for pumping a solution to slowly flow through a sample cell for rapid spectrum detection, and the visible spectrum can be analyzed, judged and extracted to obtain an end point or other information through the rapid spectrum detection.
S203: after the assay was completed, the peristaltic pump was reversed to push the solution back into the flask.
The rotating speed of the pump is 20 r/min, so that the stable flowing and moderate speed of the solution are ensured. The time for the solution to be sucked from the flask to the sample cell was about 5 seconds, and the spectrum was detected for 8 seconds. After that, every 10 minutes is separated,
s204: the above procedure was repeated and the visible spectrum was recorded. Fig. 3 is a recorded visible spectrum.
Example 3 monitoring the progress of the bisphenol A Synthesis reaction in real time using ultraviolet spectroscopy
The online spectrum detection method of the self-cleaning sampling device is adopted to carry out online monitoring of ultraviolet spectrum on bisphenol A synthesis reaction, and comprises the following steps:
s200: in a 500ml three-necked flask, 1.0g of sodium thiosulfate pentahydrate was added, then the flask was heated to melt the sodium thiosulfate pentahydrate, 0.4g of chloroacetic acid was added and mixed well, and in a water bath, 10g of phenol and 160ml of chloroform, and 7.0ml of 80% sulfuric acid solution were added to the flask in this order. An electric stirrer is installed. Thus, a sample solution was obtained.
S201: the filter head 1 of the self-cleaning sampling device of the present invention is placed in a flask and submerged in the solution. The rest of the self-cleaning sampling device of the present invention is installed and connected to the uv spectrometer as detector 22, where the powered pump 3 employs a syringe to manually aspirate and push the sample.
S302: 4.0ml of acetone are added dropwise rapidly with stirring by motor, the temperature being required to be below 35 ℃. After the dropwise addition, stirring for 3 hours at the temperature of 35-40 ℃. During this period, one cycle of solution aspiration, rapid spectroscopic detection (S102, S202, supra) and solution push (S103, S203, supra) is completed every 6 minutes. By the rapid spectrum detection, the ultraviolet spectrum can be analyzed, the reaction endpoint can be judged in an auxiliary way, and meanwhile, the concentration change trend of reactants and products is researched by adopting a chemometric method.
FIG. 4 is a diagram of an ultraviolet spectrum, with a wavelength range of 238-348 nm.
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.
Claims (10)
1. A self-cleaning sampling device is used for sample solution and is characterized by comprising a filter head (1), a sample pool (2), a power pump (3) and a sample collection channel (5), wherein the filter head (1), the sample pool (2) and the power pump are sequentially connected through a conduit (4), and the sample collection channel is connected to the portion, at the front end or the rear end, of the sample pool (2) of the conduit (4); still be equipped with a main entrance valve door (41) on pipe (4), the front end of sample collection passageway (5) is equipped with gathers passageway valve door (51), power pump (3) set up to provide power for the absorption and the propelling movement of sample solution, can provide the power of forward and reverse motion.
2. A self-cleaning sampling device according to claim 1, wherein the sample cell (2) is provided with a light source (21) and a detector (22) associated with each of its opposite sides, and wherein the detector (22) is connected to a computer (23).
3. A self-cleaning sampling device according to claim 1, wherein the filter head (1) is connected to a sample storage module (6), the sample storage module (6) comprising a gear pump (61), an industrial feed liquid storage tank (62) and a sample tank with filter cartridge (63) connected in series and forming a circuit in the flow direction of the sample solution through stainless steel piping, the filter head (1) being connected to the sample tank (63).
4. A self-cleaning sampling device according to claim 1, wherein a glass baffle (7) is provided between the filter head (1) and the sample cell (2).
5. A self-cleaning sampling device according to claim 1, wherein the power pump (3) is a peristaltic pump with forward and reverse motion, or a syringe.
6. A self-cleaning sampling device according to claim 1, wherein the collection channel valve (51) and the main channel valve (41) are both solenoid valves, and the opening and closing of the collection channel valve (51) and the main channel valve (41) are synchronized with the power direction of the power pump (3).
7. A self-cleaning sampling device according to claim 1, characterized in that the filter head (1) is made of a porous material and has a pore size in the range of 1-20 μm; the sample cell (2) is made of quartz glass or common optical glass and is in a regular square or round shape, and the optical path is 1mm-10 mm; the guide pipe (4) is made of a corrosion-resistant plastic pipe, a metal pipe or a glass pipe; the total length of the whole conduit (4) together with the filter head (1), the sample cell (2) and the power pump (3) is in the range of 100mm-1000 mm.
8. An on-line spectral detection method of a self-cleaning sampling device according to any of claims 1-7, comprising the steps of:
s1: the power pump (3) is started, and meanwhile, the main channel valve (41) is opened, so that the power pump (3) sucks the sample solution towards the power pump (3), and the sample solution enters the sample pool (2) and the sample collection channel (5) through the filter head (1);
s2: carrying out rapid spectrum detection in the sample cell (2), collecting sample solution through the sample collecting channel (5), sending the sample solution to a laboratory for detection and comparing results;
s3: reversing the power of the power pump (3) to push the sample solution through the filter head (1) away from the power pump (3) to clean the filter head (1) and then closing the main channel valve (41) until the next sample.
9. The on-line spectrum detection method of a self-cleaning sampling device according to claim 8, wherein the step S2 of collecting the sample solution through the sample collection channel (5) is synchronized with the step S1 of collecting the sample solution through the filter head (1) into the sample cell (2) and the sample collection channel (5), or the step of collecting the sample solution through the sample collection channel (5) corresponds to a plurality of times of collecting the sample solution through the filter head (1) into the sample cell (2) and the sample collection channel (5).
10. The self-cleaning sampling device and its application in on-line spectrum detection of claim 8, wherein in step S1, the total amount of sample solution entering the sample cell (2) is below 10mL, and the total time of step S1 and step S2 is within 10 seconds.
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