CN111239080B - Quality control device and OCEC analysis system - Google Patents
Quality control device and OCEC analysis system Download PDFInfo
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- CN111239080B CN111239080B CN202010068568.2A CN202010068568A CN111239080B CN 111239080 B CN111239080 B CN 111239080B CN 202010068568 A CN202010068568 A CN 202010068568A CN 111239080 B CN111239080 B CN 111239080B
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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
- G01N21/55—Specular reflectivity
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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
- G01N21/59—Transmissivity
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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
- G01N21/55—Specular reflectivity
- G01N2021/558—Measuring reflectivity and transmission
Abstract
The application provides a quality control device and an OCEC analysis system, wherein the quality control device comprises a spray pipe which is used for extending into a sample furnace and extending to a filter membrane, a standard solution quantifying device which is communicated with the input end of the spray pipe and is used for providing quantitative standard solution, and a carrier gas device which is communicated with the input end of the standard solution quantifying device and is used for providing carrier gas so as to spray the quantitative standard solution in the standard solution quantifying device onto the filter membrane. When external standard is carried out, the carrier gas output by the carrier gas device is used for producing positive pressure, the quantitative standard solution in the standard solution quantifying device is sprayed onto the filter membrane for analysis through the spray pipe, and the impact effect formed by the positive pressure is beneficial to spraying the quantitative standard solution onto the filter membrane, and meanwhile, the pipeline residue is avoided. The quality control device is simple to operate, can reduce the man-made interference factors brought by manual operation, can reduce the maintenance amount, and realizes the automatic operation of the instrument.
Description
Technical Field
The application relates to the technical field of analysis of carbon components of air particulate matters, in particular to a quality control device. In addition, the application also relates to an OCEC analysis system comprising the quality control device.
Background
The carbonaceous component in the air particulate matter, which generally accounts for 10% -70% of the mass concentration of the air particulate matter, is an important constituent of the air particulate matter. The carbonaceous components can be divided into three main categories: organic Carbon (OC), elemental Carbon (EC), and Carbon Carbonate (CC). OC is mainly generated by emissions and biological emissions in the primary combustion process and products entering a particulate state after chemical reaction of volatile organic compounds in the air and oxidizing substances in the air. EC, also known as carbon Black (BC), is mainly derived from the incomplete combustion of carbonaceous fuels. CC is mainly present in soil and coal mine fly ash, and the mass concentration is much less than EC and OC, so the CC component in the air particulate matter is generally negligible.
The carbonaceous components of the air particulate matter can have an impact on three aspects of global climate, air visibility, and human health. The effect of particulate matter on global climate change has long been considered a cooling effect, but more and more reports now consider EC to be very significant on global warming. EC may absorb light in the full range from infrared to ultraviolet, thereby "heating" the earth. In addition, the EC can deepen the color of the particles, so that substances which are not or less absorbed by the radiation originally can absorb the light, the radiation force of the particles is increased, and the air visibility is reduced. OC can scatter light, greatly affecting regional air visibility, and is rich in carcinogens and genotoxic mutagens. Because the carbonaceous components of the air particles are mostly in the particles (0.1-2.5 mu m), the carbonaceous components can easily enter the lung of a human body through the respiration of the human body, damage and change the structure and function of the lung, cause chronic respiratory diseases and even change the structure of DNA. Thus, the carbonaceous component of air particulate matter is being investigated as a hotspot in the field of environmental monitoring today.
Currently, two main approaches are used for the study of the carbonaceous component (OC/EC) of air particulate matter: membrane sampling + off-line analysis and on-line OC/EC monitoring. However, the data obtained by the conventional membrane sampling and off-line analysis method has low time resolution, is difficult to reflect the information of the characteristic change of the air particulate matters in a short time, and is easy to introduce artificial interference, so that the on-line OC/EC analyzer is a trend of research.
In the prior art, aiming at the air samples which are continuously collected on line, an on-line analyzer for analyzing the carbonaceous components in the air particulate matters is provided, but the problems that the samples are not collected accurately and automatic full-flow blank test is not available exist are also solved. In a patent with the patent number of 201010249182.8 and the name of an online particulate matter carbonaceous component collection analyzer, an online aerosol carbonaceous component collection analyzer is provided, and comprises a carrier gas path system and a sampling-analysis gas path system; the carrier gas path system comprises a He gas path, a He-purge gas path, a He/Ox gas path and a He/CH4 gas path: the sampling-analyzing gas circuit system comprises a sampling gas circuit, an analyzing-oxidizing furnace and an analyzing gas circuit, and the following problems are also existed although the on-line analysis of the components of the air particulate matters is realized to a certain extent.
The use and maintenance of an organic carbon element carbon on-line analyzer (Hu Gang, chu Guodong) records that the calibration of the instrument requires that a quartz film is horizontally placed on the front section of a quartz liner tube of the instrument, the quartz liner tube is connected, impurities in the quartz film are removed completely, a precise sample injection needle is used for sucking sucrose solution with standard concentration, the solution is carefully dripped near the center of the quartz film which is horizontally placed, and the quartz liner tube is connected. Therefore, the existing organic carbon element carbon online analyzer needs to calibrate the instrument and calibrate a standard curve manually, and in the process of calibration or calibration, instrument components need to be assembled and disassembled repeatedly, so that the steps are very complicated, and the degree of automation is low.
The curve calibration and quality control processes of the online analyzer are both manual operations, and when standard solutions are adopted for external standard, the basic steps are approximately as follows: taking a clean filter membrane, burning the filter membrane, extracting a certain volume of standard solution with a certain concentration by using a sample injection needle, dripping the standard solution onto the filter membrane, and putting the filter membrane into a glass tube. The whole operation process is complex and complicated, the glass tube is required to be frequently disassembled and assembled, external interference is easy to bring in the operation process, each step is completed by manual operation, the requirement on operators is high, and the human interference factor is large.
Therefore, in order to obtain monitoring data more accurately and more rapidly, and reduce the interference factor brought by manual operation, there is a need for a quality control device capable of realizing automation, and an OCEC analysis system including the quality control device.
Disclosure of Invention
The application provides a quality control device and an OCEC analysis system, which are used for solving the problems of complicated operation and large human interference factor of the existing air particulate matter carbon component analysis system when external standard is carried out.
The technical scheme adopted by the application is as follows:
in one aspect, the application provides a quality control device comprising a spray pipe extending into a sample furnace and extending to a filter membrane, a standard solution quantifying device communicated with an input end of the spray pipe and used for providing quantitative standard solution, and a carrier gas device communicated with an input end of the standard solution quantifying device and used for providing carrier gas so as to spray the quantitative standard solution in the standard solution quantifying device onto the filter membrane.
Further, the standard solution quantifying device comprises a standard solution device for providing standard solution, a first control valve respectively communicated with the output end of the carrier gas device and the output end of the standard solution device, a quantifying device communicated with the output end of the first control valve, a second control valve respectively communicated with the output end of the quantifying device and the input end of the spray pipe, and an emptying pipeline communicated with the output end of the second control valve.
Further, the liquid labeling device comprises a liquid labeling bottle, a third control valve, an ultrapure water bottle and a fourth control valve, wherein the third control valve and the ultrapure water bottle are respectively communicated with the output end of the liquid labeling bottle and the input end of the first control valve; or the standard solution device comprises a plurality of standard solution bottles which are respectively communicated with the input ends of the first control valves and are used for storing standard solutions with different concentrations.
The application further provides an OCEC analysis system, which comprises a sampling pipeline, a sample furnace arranged on the sampling pipeline and a filter membrane arranged in the sample furnace and used for collecting particles in sample gas, wherein the input end of the sample furnace is respectively communicated with a carrier gas pipeline and a helium oxygen pipeline, a laser and a detection device are arranged outside the sample furnace, the output end of the sample furnace is communicated with an oxidation furnace, the output end of the oxidation furnace is communicated with a carbon dioxide sensor, and the OCEC analysis system further comprises the quality control device.
Further, a particle cutter for cutting and classifying particles in the sample gas, an erosion device communicated with the output end of the particle cutter and used for adsorbing gaseous organic matters in the sample gas, and a fifth control valve respectively communicated with the output end of the erosion device and the input end of the sample furnace are arranged on the sampling pipe.
Further, a sixth control valve is arranged between the output end of the particulate matter cutter and the input end of the corrosion device, and the input end of the sixth control valve is communicated with a particulate matter filter for filtering particulate matters in air to obtain blank sample gas.
Further, the output end of the carrier gas pipeline is communicated with the input end of the fifth control valve, and a first heating device is arranged outside the corrosion device and used for heating the corrosion device so as to release gaseous organic matters adsorbed by the corrosion device when the carrier gas in the carrier gas pipeline flows into the corrosion device through the fifth control valve.
Further, the sample furnace includes an outer tube, an inner tube disposed in the outer tube for fixing the filter membrane in the outer tube, and a second heating device disposed outside the outer tube for heating the filter membrane.
Further, the output end of the carrier gas pipeline is communicated with a purging pipeline which is communicated with a gap between the outer pipe and the inner pipe and is used for purging air in the gap by utilizing helium gas output by the carrier gas pipeline, and a seventh control valve is arranged on the purging pipeline.
Further, the input end of the carrier gas pipeline is communicated with a carrier gas bottle for providing carrier gas, the input end of the helium-oxygen pipeline is communicated with a helium-oxygen bottle for providing mixed gas of helium and oxygen, a valve group is arranged on the carrier gas pipeline, and the output end of the helium-oxygen pipeline is communicated with the input end of the valve group; the output end of the valve group is communicated with a flow controller for measuring the flow of carrier gas or mixed gas.
Further, a beam splitter is arranged on the output light path of the laser, and the detection device comprises a first detector for receiving the laser transmitted through the filter membrane and detecting the light intensity of the laser and a second detector for receiving the laser reflected by the filter membrane and the beam splitter and detecting the light intensity of the laser.
Further, a tenth control valve is provided between the output end of the oxidation furnace and the input end of the carbon dioxide sensor so as to check the air tightness of the OCEC analysis system by closing the tenth control valve and other valves.
The application has the following beneficial effects:
when the quality control device disclosed by the application is used for external standard, the carrier gas output by the carrier gas device is used for manufacturing positive pressure to spray the quantitative standard solution in the standard solution quantifying device onto the filter membrane for analysis through the spray pipe, and the impact effect formed by the positive pressure is beneficial to spraying the quantitative standard solution onto the filter membrane, so that the pipeline residue is avoided. The quality control device is simple to operate, can reduce the man-made interference factors brought by manual operation, can reduce the maintenance amount, and realizes the automatic operation of the instrument.
In addition to the objects, features and advantages described above, the present application has other objects, features and advantages. The application will be described in further detail with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the application. In the drawings:
FIG. 1 is a schematic diagram of a quality control device according to a preferred embodiment of the present application;
FIG. 2 is a schematic diagram of a quality control device according to a preferred embodiment of the present application;
FIG. 3 is a schematic view of a liquid labeling apparatus according to a first preferred embodiment of the present application;
FIG. 4 is a schematic view of a second preferred embodiment of the present application;
fig. 5 is a schematic diagram of an OCEC analysis system according to a preferred embodiment of the present application.
Reference numerals illustrate:
1. a filter membrane; 2. a spray pipe; 3. a standard liquid quantitative device; 4. a carrier gas device; 5. a liquid marking device; 6. a first control valve; 7. a dosing device; 8. a second control valve; 9. an evacuation line; 10. a label liquid bottle; 11. a third control valve; 12. ultrapure water bottles; 13. a fourth control valve; 14. a sampling pipeline; 15. a carrier gas line; 16. a helium oxygen line; 17. a laser; 18. an oxidation furnace; 19. a carbon dioxide sensor; 20. a particulate matter cutter; 21. an etcher; 22. a fifth control valve; 23. a sixth control valve; 24. a particulate filter; 25. a first heating device; 26. an outer tube; 27. an inner tube; 28. a second heating device; 29. purging the pipeline; 30. a seventh control valve; 31. a gas carrying cylinder; 32. a helium oxygen bottle; 33. a valve group; 34. a flow controller; 35. a light splitting sheet; 36. a first detector; 37. a second detector; 38. and an eighth control valve.
Detailed Description
It should be noted that, without conflict, the embodiments of the present application and features of the embodiments may be combined with each other. The application will be described in detail below with reference to the drawings in connection with embodiments.
FIG. 1 is a schematic diagram of a quality control device according to a preferred embodiment of the present application; FIG. 2 is a schematic diagram of a quality control device according to a preferred embodiment of the present application; FIG. 3 is a schematic view of a liquid labeling apparatus according to a first preferred embodiment of the present application; FIG. 4 is a schematic view of a second preferred embodiment of the present application; fig. 5 is a schematic diagram of an OCEC analysis system according to a preferred embodiment of the present application.
As shown in fig. 1 and 2, the quality control device of the present application includes a nozzle 2 for extending into the sample furnace and extending to the filter membrane 1, a standard solution quantifying device 3 communicating with an input end of the nozzle 2 for providing a quantified standard solution, and a carrier gas device 4 communicating with an input end of the standard solution quantifying device 3 for providing a carrier gas to spray the quantified standard solution in the standard solution quantifying device 3 onto the filter membrane 1.
When the quality control device is used for external standard, the carrier gas output by the carrier gas device 4 is used for manufacturing positive pressure to spray the quantitative standard solution in the standard solution quantifying device 3 onto the filter membrane 1 through the spray pipe 2 for analysis, and the impact effect formed by the positive pressure is beneficial to spraying the quantitative standard solution onto the filter membrane 1, and meanwhile, the pipeline residue is avoided. The quality control device is simple to operate, can reduce the man-made interference factors brought by manual operation, can reduce the maintenance amount, and realizes the automatic operation of the instrument. Alternatively, the nozzle 2 is a quartz capillary tube. Alternatively, the standard solution is a sucrose solution. Alternatively, the carrier gas device 4 may output a carrier gas such as helium, nitrogen, or argon as needed.
As shown in fig. 2, in the present embodiment, the standard solution dosing device 3 includes a standard solution device 5 for supplying a standard solution, a first control valve 6 in communication with the output end of the carrier gas device 4 and the output end of the standard solution device 5, a dosing device 7 in communication with the output end of the first control valve 6, a second control valve 8 in communication with the output end of the dosing device 7 and the input end of the spout 2, respectively, and an evacuation line 9 in communication with the output end of the second control valve 8. The standard solution output by the standard solution device 5 flows into the quantifying device 7 by controlling the first control valve 6 and the second control valve 8 to communicate the standard solution device 5, the quantifying device 7 and the emptying pipeline 9, and the quantifying device 7 collects the quantified standard solution. Then, the carrier gas device 4, the quantifying device 7 and the spray pipe 2 are communicated by controlling the first control valve 6 and the second control valve 8, and the standard solution quantified in the quantifying device 7 is sprayed onto the filter membrane 1 through the spray pipe 2 by using the carrier gas output by the carrier gas device 4 to produce a positive pressure. Alternatively, the dosing device 7 employs a dosing ring.
As shown in fig. 3 and 4, in the present embodiment, the labeling apparatus 5 includes a labeling bottle 10, a third control valve 11, an ultrapure water bottle 12, and a fourth control valve 13, which are respectively communicated with the output end of the labeling bottle 10 and the input end of the first control valve 6, and which are respectively communicated with the output end of the ultrapure water bottle 12 and the input end of the first control valve 6. The flow ratio of the standard solution to the ultrapure water is controlled by the third control valve 11 and the fourth control valve 13, so that the purpose of preparing the standard solutions with different concentrations for quantification is achieved. Optionally, the labeling device 5 comprises a plurality of labeling bottles 10 respectively communicated with the input ends of the first control valves 6 and used for storing the standard solutions with different concentrations. The flow path is switched to a standard solution bottle 10 for storing standard solutions of different concentrations by a first control valve 6, and the standard solution of a specific concentration is quantified. When external standard is carried out, standard solutions with different concentrations are switched through the standard solution device 5, after standard solutions with certain concentrations are selected and quantified, peak areas of the standard solutions with corresponding concentrations are obtained through normal detection processes of the standard solutions, standard curves are obtained through normal detection processes of the quantified standard solutions with different concentrations, and detection accuracy of organic carbon and elemental carbon can be guaranteed.
As shown in fig. 5, the preferred embodiment of the present application further provides an OCEC analysis system, which includes a sampling pipeline 14, a sample furnace disposed on the sampling pipeline 14, and a filter membrane 1 disposed in the sample furnace and used for collecting particles in a sample gas, wherein an input end of the sample furnace is respectively communicated with a carrier gas pipeline 15 and a helium oxygen pipeline 16, a laser 17 and a detection device are disposed outside the sample furnace, an output end of the sample furnace is communicated with an oxidation furnace 18, an output end of the oxidation furnace 18 is communicated with a carbon dioxide sensor 19, and the OCEC analysis system further includes the quality control device.
In the OCEC analysis system of the present application, after the sample gas in the air flows into the sample furnace through the sampling pipe 14, the particulate matter in the sample gas is collected through the filter membrane 1. Then helium is input into the sample furnace through a carrier gas pipeline 15 to purge the sample furnace so as to form an anaerobic environment in the sample furnace, and the filter membrane 1 is heated through the sample furnace so as to convert organic carbon in particulate matters on the filter membrane 1 into gas. Elemental carbon in the particulate matter on the filter membrane 1 is not converted to gas due to the oxygen-free environment formed in the sample furnace. And then, the helium and oxygen mixed gas is input into the sample furnace through a helium-oxygen pipeline 16 to form an oxygen environment in the sample furnace, and the filter membrane 1 is heated through the sample furnace to convert elemental carbon in particulate matters on the filter membrane 1 into gas. In the process of converting organic carbon and elemental carbon into gas, laser light is continuously emitted by the laser 17 and irradiated on the filter membrane 1, and the laser light is received by the detection device and the light intensity of the laser light is detected. In the process of converting organic carbon into gas, part of the organic carbon is carbonized into elemental carbon, and the light intensity of the laser received by the detection device is gradually weakened. In the process of converting the elemental carbon into the gas, the light intensity of the laser light received by the detection device is gradually increased. When the light intensity of the laser light received by the detection device is restored to the original light intensity, the point of distinction between organic carbon and elemental carbon is regarded as being converted from organic carbon to gas before and from elemental carbon to gas after. Finally, the gas is oxidized into carbon dioxide through an oxidation furnace 18, the amount of the carbon dioxide is detected through a carbon dioxide sensor 19, the amounts of organic carbon and elemental carbon in the particulate matters on the filter membrane 1 are converted according to the amount of the carbon dioxide, and the concentrations of the organic carbon and the elemental carbon in the air particulate matters are converted according to the amounts of the organic carbon and the elemental carbon in the particulate matters on the filter membrane 1 and the sampling volume. Alternatively, the carrier gas line 15 may output a carrier gas such as helium, nitrogen, or argon as needed.
As shown in fig. 5, in the present embodiment, the sampling pipe 14 is provided with a particulate matter cutter 20 for cutting and classifying particulate matters in the sample gas, an erosion 21 which is communicated with an output end of the particulate matter cutter 20 and is used for adsorbing gaseous organic matters in the sample gas, and a fifth control valve 22 which is respectively communicated with an output end of the erosion 21 and an input end of the sample furnace. The sample gas enters the sampling pipeline 14 through the particle cutter 20, and the particle cutter 20 can cut and classify the particles in the sample gas to obtain the particles with the required particle size range. The gaseous organic matters in the sample gas are adsorbed by the corrosion device 21, so that the gaseous organic matters in the sample gas can be removed, and the interference of the gaseous organic matters on the detection of organic carbon in the particulate matters is avoided. After the sampling is completed, the fifth control valve 22 is closed, so that air can be prevented from entering the sample furnace, and interference to detection of organic carbon and elemental carbon in the particulate matters is avoided.
As shown in fig. 5, in the present embodiment, a sixth control valve 23 is disposed between the output end of the particulate matter cutter 20 and the input end of the erosion device 21, and the input end of the sixth control valve 23 is connected with a particulate matter filter 24 for filtering particulate matters in the air to obtain blank sample gas. The sixth control valve 23 is controlled so that the input end of the etcher 21 is communicated with the output end of the particulate filter 24, particulate matter in the air is filtered by the particulate filter 24 to obtain a blank sample gas, and the subsequent detection process is consistent with the normal detection process, thereby performing a full-flow blank to check the reliability of the operation of the OCEC analysis system.
As shown in fig. 5, in the present embodiment, the output end of the carrier gas line 15 communicates with the input end of the fifth control valve 22, and a first heating device 25 for heating the etcher 21 is provided outside the etcher 21 to release the gaseous organic substances adsorbed by the etcher 21 when the carrier gas in the carrier gas line 15 flows into the etcher 21 through the fifth control valve 22. The efficiency of the corrosion device 21 is reduced after a period of use, and the corrosion device 21 is of an active carbon structure and adopts physical adsorption. When the first heating device 25 is installed outside the corrosion device 21 and regeneration of the corrosion device 21 is required, the fifth control valve 22 is controlled to enable the output end of the carrier gas pipeline 15 to be communicated with the corrosion device 21, carrier gas flows into the corrosion device 21 through the carrier gas pipeline 15, reverse purging is carried out on the corrosion device 21, the corrosion device 21 is heated through the first heating device 25, the temperature of the first heating device 25 is controlled to be a proper temperature (such as 260 ℃), and gaseous organic matters adsorbed in the corrosion device 21 are released from the corrosion device 21, so that regeneration of the corrosion device 21 is achieved without disassembling the corrosion device 21, and adsorption efficiency of the corrosion device 21 is guaranteed. Alternatively, the first heating device 25 employs a heater wire or a PTC heater.
As shown in fig. 5, in the present embodiment, the sample furnace includes an outer tube 26, an inner tube 27 provided in the outer tube 26 for fixing the filter membrane 1 in the outer tube 26, and a second heating device 28 provided outside the outer tube 26 for heating the filter membrane 1. The inner tube 27 compresses and fixes the filter membrane 1 at the step in the outer tube 26, and the sample gas, the carrier gas and other gases flow into the inner tube 27 and then pass through the filter membrane 1, and the second heating device 28 can heat the filter membrane 1. Optionally, the second heating device 28 employs a heating wire. Optionally, a fan is provided outside the second heating device 28 to dissipate heat from the second heating device 28.
As shown in fig. 5, in this embodiment, the output end of the carrier gas line 15 is connected to a purge line 29 which is connected to the gap between the outer tube 26 and the inner tube 27 and is used for purging the air in the gap with helium gas output from the carrier gas line 15, and a seventh control valve 30 is provided on the purge line 29. There is a gap between the outer tube 26 and the inner tube 27 where air cannot be purged through the carrier gas line 15, creating a purge dead volume. Once the air in the gap flows into the inner tube 27, it affects the detection of organic carbon and elemental carbon. The seventh control valve 30 controls the helium gas output by the carrier gas pipeline 15 to purge the air in the gap through the purging pipeline 29, so as to achieve the purpose of removing residual oxygen.
As shown in fig. 5, in this embodiment, the input end of the carrier gas pipeline 15 is connected to a carrier gas bottle 31 for providing carrier gas, the input end of the heliox pipeline 16 is connected to a heliox bottle 32 for providing a mixed gas of helium and oxygen, a valve group 33 is provided on the carrier gas pipeline 15, and the output end of the heliox pipeline 16 is connected to the input end of the valve group 33. After the mixed gas of helium and oxygen outputted from the helium oxygen bottle 32 flows into the helium oxygen pipeline 16, the mixed gas is communicated with the input end of the sample furnace through the valve group 33 and the carrier gas pipeline 15, so that the flow path design can be simplified. Optionally, the output of the valve block 33 is connected to a flow controller 34 for measuring the flow of carrier gas or mixed gas. The flow rate of the carrier gas or the mixed gas is measured by the flow rate controller 34 so as to control the flow rate of the carrier gas or the mixed gas outputted.
As shown in fig. 5, in the present embodiment, a beam splitter 35 is provided on the output optical path of the laser 17, and the detecting means includes a first detector 36 for receiving the laser light transmitted through the filter membrane 1 and detecting the intensity of the laser light, and a second detector 37 for receiving the laser light reflected by the filter membrane 1 and the beam splitter 35 and detecting the intensity of the laser light. The laser 17 emits laser light, the laser light irradiates the filter membrane 1 through the light-transmitting sheet 35, one part of the laser light is received by the first detector 36 and detected by the light intensity of the laser light after penetrating the filter membrane 1, and the other part of the laser light is received by the second detector 37 and detected by the light intensity of the laser light after being reflected by the filter membrane 1 and the light-dividing sheet 35. The distinguishing point of the organic carbon and the element carbon is judged through the transmitted light intensity and the reflected light intensity, and the distinguishing point is more accurate to judge.
As shown in fig. 5, in the present embodiment, an eighth control valve 38 is provided between the output end of the oxidation furnace 18 and the input end of the carbon dioxide sensor 19 so as to check the air tightness of the OCEC analysis system by closing the eighth control valve 38 and other valves. If the OCEC analysis system is not airtight, ambient air flowing into the sample furnace will affect the detection of organic and elemental carbon. By closing the eighth control valve 38 and other valves (for example, the sixth control valve 23, the valve group 33, etc.), the entire flow path of the OCEC analysis system is sealed, and the pressure change in the flow path is observed by the reading of the pressure sensor in the flow path after pressurizing the flow path, thereby realizing the air tightness check of the entire flow path.
The above description is only of the preferred embodiments of the present application and is not intended to limit the present application, but various modifications and variations can be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (11)
1. An OCEC analysis system, characterized in that,
comprises a sampling pipeline (14), a sample furnace arranged on the sampling pipeline (14) and a filter membrane (1) arranged in the sample furnace and used for collecting particles in sample gas,
the input end of the sample furnace is respectively communicated with a carrier gas pipeline (15) and a helium oxygen pipeline (16), a laser (17) and a detection device are arranged outside the sample furnace, the output end of the sample furnace is communicated with an oxidation furnace (18), the output end of the oxidation furnace (18) is communicated with a carbon dioxide sensor (19),
the OCEC analysis system further comprises a quality control device,
the quality control device comprises a spray pipe (2) which is used for extending into the sample furnace and extends to the filter membrane (1), a standard solution quantifying device (3) which is communicated with the input end of the spray pipe (2) and is used for providing quantitative standard solution, and a carrier gas device (4) which is communicated with the input end of the standard solution quantifying device (3) and is used for providing carrier gas so as to spray the quantitative standard solution in the standard solution quantifying device (3) onto the filter membrane (1).
2. The OCEC analysis system of claim 1, wherein,
the standard solution quantifying device (3) comprises a standard solution device (5) for providing standard solution, a first control valve (6) which is respectively communicated with the output end of the carrier gas device (4) and the output end of the standard solution device (5), a quantifying device (7) which is communicated with the output end of the first control valve (6), a second control valve (8) which is respectively communicated with the output end of the quantifying device (7) and the input end of the spray pipe (2), and an emptying pipeline (9) which is communicated with the output end of the second control valve (8).
3. The OCEC analysis system of claim 2, wherein,
the liquid labeling device (5) comprises a liquid labeling bottle (10), a third control valve (11) which is respectively communicated with the output end of the liquid labeling bottle (10) and the input end of the first control valve (6), an ultrapure water bottle (12) and a fourth control valve (13) which is respectively communicated with the output end of the ultrapure water bottle (12) and the input end of the first control valve (6); or alternatively
The standard solution device (5) comprises a plurality of standard solution bottles (10) which are respectively communicated with the input ends of the first control valves (6) and are used for storing standard solutions with different concentrations.
4. The OCEC analysis system according to any one of claim 1 to 3, wherein,
the sampling pipeline (14) is provided with a particulate matter cutter (20) for cutting and classifying particulate matters in the sample gas, an erosion device (21) which is communicated with the output end of the particulate matter cutter (20) and is used for adsorbing gaseous organic matters in the sample gas, and a fifth control valve (22) which is respectively communicated with the output end of the erosion device (21) and the input end of the sample furnace.
5. The OCEC analysis system of claim 4, wherein,
a sixth control valve (23) is arranged between the output end of the particulate matter cutter (20) and the input end of the corrosion device (21), and the input end of the sixth control valve (23) is communicated with a particulate matter filter (24) for filtering particulate matters in air to obtain blank sample gas.
6. The OCEC analysis system of claim 4, wherein,
the output end of the carrier gas pipeline (15) is communicated with the input end of the fifth control valve (22), and a first heating device (25) is arranged outside the corrosion device (21) and used for heating the corrosion device (21) so as to release gaseous organic matters adsorbed by the corrosion device (21) when the carrier gas in the carrier gas pipeline (15) flows into the corrosion device (21) through the fifth control valve (22).
7. The OCEC analysis system according to any one of claim 1 to 3, wherein,
the sample furnace comprises an outer tube (26), an inner tube (27) arranged in the outer tube (26) and used for fixing the filter membrane (1) in the outer tube (26), and a second heating device (28) arranged outside the outer tube (26) and used for heating the filter membrane (1).
8. The OCEC analysis system of claim 7, wherein,
the output end of the carrier gas pipeline (15) is communicated with a purging pipeline (29) which is communicated with a gap between the outer pipe (26) and the inner pipe (27) and is used for purging air in the gap by utilizing helium gas output by the carrier gas pipeline (15), and a seventh control valve (30) is arranged on the purging pipeline (29).
9. The OCEC analysis system according to any one of claim 1 to 3, wherein,
the input end of the carrier gas pipeline (15) is communicated with a carrier gas bottle (31) for providing carrier gas, the input end of the heliox pipeline (16) is communicated with a heliox bottle (32) for providing mixed gas of helium and oxygen, a valve group (33) is arranged on the carrier gas pipeline (15), and the output end of the heliox pipeline (16) is communicated with the input end of the valve group (33);
the output end of the valve group (33) is communicated with a flow controller (34) for measuring the flow of carrier gas or mixed gas.
10. The OCEC analysis system according to any one of claim 1 to 3, wherein,
the output light path of the laser (17) is provided with a light splitting sheet (35), and the detection device comprises a first detector (36) for receiving laser light transmitted through the filter membrane (1) and detecting the light intensity of the laser light and a second detector (37) for receiving the laser light reflected by the filter membrane (1) and the light splitting sheet (35) and detecting the light intensity of the laser light.
11. The OCEC analysis system according to any one of claim 1 to 3, wherein,
an eighth control valve (38) is provided between the output end of the oxidation furnace (18) and the input end of the carbon dioxide sensor (19) so as to check the air tightness of the OCEC analysis system by closing the eighth control valve (38) and other valves.
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