CN111721753A - Device and method for directly feeding samples into oil product - Google Patents
Device and method for directly feeding samples into oil product Download PDFInfo
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Abstract
The invention relates to a device for directly feeding samples into oil products, which comprises an atomizer, a temperature control cavity, a temperature control reaction cavity, an oxygen generation assembly and a three-way valve, wherein the atomizer forms an aerosol from an oil product sample; the temperature control cavity is provided with a temperature control cavity inlet and a temperature control cavity outlet and is connected with the atomizer; the temperature control reaction cavity is an interlayer cavity arranged on the outer wall of the temperature control cavity, a refrigeration reactant is filled in the interlayer cavity, the temperature of the aerosol is controlled through heat exchange with the temperature control cavity, the ambient temperature of the aerosol generated by the oil product is controlled, and the volatility of the oil product is reduced. Compared with the prior art, the direct sampling device for the sampled oil product can be used for pretreatment of analysis of the content of various metal elements, and not only can the complicated sample pretreatment process be reduced or simplified, but also the rapid analysis and detection of trace elements in the oil product can be realized through the temperature control and the oxygen doping control, and the stability and the accuracy of an analysis result are ensured.
Description
Technical Field
The invention relates to the field of oil product detection, in particular to a device and a method for directly feeding samples to oil products.
Background
With the rapid development of petrochemical industry, the demand of oil products is increasing day by day. The content of impurity elements and additive elements in the oil product is the key for controlling the quality of the oil. Common pretreatment methods of oil products, such as a wet digestion method, a dry ashing method and the like, influence the rapid and accurate analysis of metal elements in the oil products to a certain extent due to the characteristics of complex operation, high reagent consumption, large environmental pollution and the like. Therefore, the device and the method for establishing the direct sample injection analysis of the impurity elements and the additive elements in the oil product have important practical significance.
At present, the commonly used analysis methods of impurity elements and additive elements in oil products are inductively coupled plasma atomic emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS), and if the methods are directly used for oil product analysis, carbon deposition of a torch tube is easily caused, the power consumption load of plasma is increased, and the stability and accuracy of an analysis result are influenced.
CN205786632U discloses a sampling device of changeable multiple oil connects in an oil analysis instrument, is equipped with the same oil route of a plurality of structures, a first solenoid valve, an oil analysis instrument, a second solenoid valve, takes the exhaust hole recovery tank, and a plurality of oil routes warp first solenoid valve joins the back and gets into oil analysis instrument, oil analysis instrument's exit end with the entrance point intercommunication of second solenoid valve, the exit end of second solenoid valve with a plurality of oil routes, take the exhaust hole recovery tank to connect, wherein first solenoid valve is the first solenoid valve that advances more, the second solenoid valve is one and advances many solenoid valves, the inlet end number of first solenoid valve with oil route number is the same, the outlet end number of second solenoid valve is greater than oil route number. The device for directly feeding the oil in the technical scheme does not solve the problem of carbon deposition of the torch tube.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a device and a sample injection method for directly injecting samples into oil products.
The purpose of the invention can be realized by the following technical scheme:
the invention relates to a device for directly feeding samples into oil products, which comprises an atomizer, a temperature control cavity, a temperature control reaction cavity, an oxygen generation assembly and a three-way valve, wherein the temperature control reaction cavity comprises the following specific parts:
forming an aerosol from an oil sample by an atomizer;
the temperature control cavity is provided with a temperature control cavity inlet and a temperature control cavity outlet and is connected with the atomizer;
the temperature control reaction cavity is an interlayer cavity arranged on the outer wall of the temperature control cavity, a refrigeration reactant is filled in the interlayer cavity, the temperature of the aerosol is controlled through heat exchange with the temperature control cavity, the ambient temperature of the aerosol generated by the oil product is controlled, and the volatility of the oil product is reduced.
The first interface of the three-way valve is connected with the outlet of the temperature control cavity, the second interface of the three-way valve is connected with the output port of the oxygen generation assembly, and the third interface of the three-way valve is connected with the sample inlet of the inductively coupled plasma atomic emission spectrometer.
Further, the temperature control reaction cavity comprises a first reaction cavity and a second reaction cavity, wherein:
the first reaction cavity is an interlayer cavity arranged on the outer wall of the temperature control cavity, and a refrigerant is filled in the interlayer cavity;
the second reaction cavity is an interlayer cavity arranged on the outer wall of the temperature control cavity, and is filled with an ice-water mixture;
the opening degree of the communication between the first reaction cavity and the second reaction cavity is adjustable.
Furthermore, a movable partition plate is arranged between the first reaction chamber and the second reaction chamber at intervals, and the communication opening degree between the first reaction chamber and the second reaction chamber is adjusted through horizontal or vertical movement of the partition plate.
Furthermore, the first reaction cavity and the second reaction cavity are respectively connected with an external refrigerant feeder and an external ice-water mixture feeder.
Further, the refrigerant is ammonium chloride or ammonium nitrate.
Further, the oxygen generation assembly comprises a third reaction chamber, wherein a chemical oxygen generation reaction is performed in the third reaction chamber, and generated oxygen is mixed with the aerosol through a three-way valve.
Furthermore, a liquid conveying pipe is arranged on the third reaction cavity and is connected with an external hydrogen peroxide pump;
a flow control valve is arranged on an output port of the third reaction chamber and is connected with a second interface of the three-way valve through a pipeline;
the third reaction chamber is filled with a hydrogen peroxide decomposition catalyst.
Further, the hydrogen peroxide decomposition catalyst is a free transition metal ion compound or catalase MnO2Or Al2O3。
Furthermore, a waste liquid pipe is arranged at the bottom of the third reaction cavity, and an electromagnetic valve is arranged on the waste liquid pipe.
Furthermore, a temperature sensor is arranged in the temperature control cavity to realize real-time detection of temperature, the ARM processor is connected with the temperature sensor, and meanwhile, the ARM processor is electrically connected with an external refrigerant feeder and an external ice-water mixture feeder, so that the real-time control of the feeding amount is realized, and the real-time regulation of the temperature inside the temperature control cavity is realized through the real-time control.
Further, an oxygen sensor is arranged at an output port of the third reaction chamber, and the oxygen sensor is electrically connected with the ARM processor and the hydrogen peroxide pump so as to control the output rate of oxygen and control the oxygen concentration in the aerosol.
The invention relates to a direct sample injection method for oil products, which comprises the following steps:
forming aerosol from an oil product sample and introducing the aerosol into a temperature control cavity with a refrigeration interlayer;
the refrigerating capacity and the refrigerating temperature are regulated and controlled by the refrigerating capacity generated by the chemical reaction in the refrigerating interlayer;
and connecting the aerosol passing through the temperature control cavity with an output port of the oxygen generation assembly, adjusting the oxygen content in the aerosol until reaching a target value, and finally introducing the mixed gas into an inductively coupled plasma atomic emission spectrometer for detection.
Compared with the prior art, the invention has the following advantages:
1) the direct sampling device for the sampled oil product can be used for analyzing the pretreatment of the content of various metal elements, and by temperature control and oxygen doping control of temperature determination, not only can the complicated sample pretreatment process be reduced or simplified, but also the rapid analysis and detection of trace elements in the oil product can be realized, the stability and the accuracy of an analysis result are ensured, and the method has the characteristics of simple operation, rapid determination, easy realization of automation and the like.
2) The invention realizes simple and effective temperature control environment by controlling the proportion of the refrigerant and the ice water mixture, and can effectively reduce the volatility of oil product aerosol, thereby improving the stability of oil product element analysis results.
3) The invention adopts hydrogen peroxide as the continuous oxygen supply for oil analysis, and can ensure that the oil burns more fully in the plasma, thereby avoiding plasma flameout caused by carbon deposition of the torch tube.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for direct sample injection of oil products according to the present invention;
in the figure: 1. atomizer, 2, first reaction chamber, 3, second reaction chamber, 4, accuse temperature chamber, 5, division board, 6, first air duct, 7, transfer line, 8, catalyst, 9, third reaction chamber, 10, waste liquid pipe, 11, solenoid valve, 12, flow control valve, 13, second air duct, 14, three-way valve, 15, third air duct.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
The device for oil direct sampling in this embodiment includes atomizer 1, temperature control chamber 4, temperature control reaction chamber, oxygen generation component and three-way valve 14, refer to fig. 1.
The atomizer 1 forms an aerosol from an oil sample.
The temperature control cavity 4 is provided with a temperature control cavity inlet and a temperature control cavity outlet, and the temperature control cavity is connected with the atomizer 1.
The temperature control reaction cavity is an interlayer cavity arranged on the outer wall of the temperature control cavity 4, wherein a refrigeration reactant is filled in the interlayer cavity, the temperature of the aerosol is controlled through heat exchange with the temperature control cavity 4, the ambient temperature of the aerosol generated by oil products is controlled, and the volatility of the oil products is reduced.
The temperature control reaction cavity comprises a first reaction cavity 2 and a second reaction cavity 3, wherein the first reaction cavity 2 is an interlayer cavity arranged on the outer wall of the temperature control cavity 4 and is filled with a refrigerant; the second reaction cavity 3 is an interlayer cavity arranged on the outer wall of the temperature control cavity 4, and is filled with an ice-water mixture; the communication opening degree between the first reaction chamber 2 and the second reaction chamber 3 can be adjusted. Establish the interval between first reaction chamber 2 and the second reaction chamber 3 and be equipped with mobilizable division board 5, division board 5 adjusts the intercommunication aperture between first reaction chamber 2 and the second reaction chamber 3 through horizontal or vertical migration. The first reaction cavity 2 and the second reaction cavity 3 are respectively connected with an external refrigerant feeder and an external ice-water mixture feeder. Specifically, the refrigerant is ammonium chloride or ammonium nitrate. The temperature sensor is arranged in the temperature control cavity 4 to realize real-time detection of temperature, the ARM processor is connected with the temperature sensor, and meanwhile, the ARM processor is electrically connected with the external refrigerant feeder and the external ice-water mixture feeder, so that the feeding amount is controlled in real time, and the real-time regulation of the temperature inside the temperature control cavity 4 is realized through the real-time control.
The first interface of the three-way valve 14 is connected with the outlet of the temperature control cavity through a first gas-guide tube 6, the second interface is connected with the output port of the oxygen generation assembly through a second gas-guide tube 13, and the third interface is connected with the sample inlet of the inductively coupled plasma atomic emission spectrometer through a third gas-guide tube 15.
The oxygen generation assembly comprises a third reaction chamber 9, the oxygen generation assemblyThe chemical oxygen production reaction takes place in the third reaction chamber 9 and the produced oxygen is mixed with the aerosol through the three-way valve 14. The third reaction chamber 9 is provided with a liquid conveying pipe 7, and the liquid conveying pipe 7 is connected with an external hydrogen peroxide pump. A flow control valve 12 is arranged on an output port of the third reaction chamber 9, the flow control valve 12 is connected with a second interface of the three-way valve 14 through a pipeline, and the third reaction chamber 9 is filled with a hydrogen peroxide decomposition catalyst. The hydrogen peroxide decomposition catalyst is free transition metal ion compound or catalase MnO2Or Al2O3. And a waste liquid pipe 10 is arranged at the bottom of the three reaction cavities 9, and an electromagnetic valve 11 is arranged on the waste liquid pipe 10. An oxygen sensor is arranged at the output port of the third reaction chamber 9, and the oxygen sensor is electrically connected with the ARM processor and the hydrogen peroxide pump so as to control the output rate of oxygen and control the oxygen concentration in the aerosol.
The sampling device provided by the invention is used for analyzing the content of metal elements in the gasoline sample. The specific procedure is as shown in example 1.
(1) Drawing a standard curve: respectively preparing gradient standard solutions containing the metal elements to be detected, wherein the gradients of the prepared solutions are shown in table 1. The standard solution is prepared by diluting standard oil (Conostan S-21, 1000mg/Kg), and the diluting solvent is white oil or aviation kerosene.
(2) Test conditions of the atomic emission spectrometer: power 1350 w; cooling gas argon gas 15L/min; the auxiliary gas argon is 0.8L/min; the rinsing time was 60 s; speed of the washing pump: 20 r/min; analyzing the pump speed: 20 r/min; short-wave analysis time: 60 s; the flow of the atomizing gas argon is 0.55L/min; a horizontal observation mode; analyzing the wavelength: see table 2.
(3) Analyzing and detecting various metal elements in a gasoline sample: during specific operation, standard solutions with different concentration gradients are firstly adopted for sample injection, the spectral intensity of the standard solutions with different concentrations at the corresponding element analysis wavelength positions is recorded through an atomic emission spectrometer, and a standard curve between the spectral intensity and the analysis concentration is established.
Then the device is adopted to sample and analyze the gasoline sample, and the oil sample is formed into aerosol and is introduced into a temperature control cavity with a refrigeration interlayer; the refrigerating capacity and the refrigerating temperature are regulated and controlled by the refrigerating capacity generated by the chemical reaction in the refrigerating interlayer; and connecting the aerosol passing through the temperature control cavity with an output port of the oxygen generation assembly, adjusting the oxygen content in the aerosol until reaching a target value, and finally introducing the mixed gas into an inductively coupled plasma atomic emission spectrometer for detection. And calculating the concentration of each element according to the spectral intensity of each element in the gasoline sample, thereby completing the rapid analysis and detection of the metal elements in the gasoline sample, wherein the specific detection result is shown in table 2.
TABLE 1
TABLE 2
Example 2
The device for directly feeding the oil product is used for analyzing and detecting the content of the metal elements in the diesel oil sample. The specific procedure is as shown in example 2.
(1) Drawing a standard curve: respectively preparing gradient standard solutions containing the metal elements to be detected, wherein the gradients of the prepared solutions are shown in table 3. The standard solution is prepared by diluting standard oil (Conostan S-21, 1000mg/Kg), and the diluting solvent is white oil or aviation kerosene.
(2) Test conditions of the atomic emission spectrometer: power 1350 w; cooling gas argon gas 15L/min; the auxiliary gas argon is 0.8L/min; the rinsing time was 60 s; speed of the washing pump: 20 r/min; analyzing the pump speed: 20 r/min; short-wave analysis time: 60 s; the flow of the atomizing gas argon is 0.55L/min; a horizontal observation mode; analyzing the wavelength: see table 4.
(3) Analyzing and detecting metal elements in diesel oil: during specific operation, standard solutions with different concentration gradients are firstly adopted for sample injection, the spectral intensity of the standard solutions with different concentrations at the corresponding element analysis wavelength positions is recorded through an atomic emission spectrometer, and a standard curve between the spectral intensity and the analysis concentration is established.
Then the device is adopted to sample and analyze the gasoline sample, and the oil sample is formed into aerosol and is introduced into a temperature control cavity with a refrigeration interlayer; the refrigerating capacity and the refrigerating temperature are regulated and controlled by the refrigerating capacity generated by the chemical reaction in the refrigerating interlayer; and connecting the aerosol passing through the temperature control cavity with an output port of the oxygen generation assembly, adjusting the oxygen content in the aerosol until reaching a target value, and finally introducing the mixed gas into an inductively coupled plasma atomic emission spectrometer for detection. And calculating the concentration of each element according to the spectral intensity of each element in the gasoline sample, thereby completing the rapid analysis and detection of the metal elements in the gasoline sample, wherein the specific detection result is shown in table 4.
TABLE 3
TABLE 4
Example 3
The multi-element analysis sample introduction device provided by the invention is used for analyzing and detecting the content of metal elements in the edible oil. The specific procedure is as shown in example 3.
(1) Drawing a standard curve: respectively preparing gradient standard solutions containing the metal elements to be detected, wherein the gradients of the prepared solutions are shown in Table 5. The standard solution is prepared by diluting standard oil (Conostan S-21, 1000mg/Kg), and the diluting solvent is white oil or aviation kerosene.
(2) Test conditions of the atomic emission spectrometer: power 1350 w; cooling gas argon gas 15L/min; the auxiliary gas argon is 0.8L/min; the rinsing time was 60 s; speed of the washing pump: 20 r/min; analyzing the pump speed: 20 r/min; short-wave analysis time: 60 s; the flow of the atomizing gas argon is 0.55L/min; a horizontal observation mode; analyzing the wavelength: see table 6.
(3) Analyzing and detecting metal elements in the edible oil: during specific operation, standard solutions with different concentration gradients are firstly adopted for sample injection, the spectral intensity of the standard solutions with different concentrations at the corresponding element analysis wavelength positions is recorded through an atomic emission spectrometer, and a standard curve between the spectral intensity and the analysis concentration is established.
Then the device is adopted to sample and analyze the gasoline sample, and the oil sample is formed into aerosol and is introduced into a temperature control cavity with a refrigeration interlayer; the refrigerating capacity and the refrigerating temperature are regulated and controlled by the refrigerating capacity generated by the chemical reaction in the refrigerating interlayer; and connecting the aerosol passing through the temperature control cavity with an output port of the oxygen generation assembly, adjusting the oxygen content in the aerosol until reaching a target value, and finally introducing the mixed gas into an inductively coupled plasma atomic emission spectrometer for detection. And calculating the concentration of each element according to the spectral intensity of each element in the gasoline sample, thereby completing the rapid analysis and detection of the metal elements in the gasoline sample, wherein the specific detection result is shown in table 6.
TABLE 5
TABLE 6
From the embodiments 1 to 3, it can be seen that the direct sampling device for the sampled oil product can be used for pretreatment of analysis of contents of various metal elements, and by means of temperature control and oxygen doping control of temperature setting, not only can the complicated sample pretreatment process be reduced or simplified, but also the rapid analysis and detection of trace elements in the oil product can be realized.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. The utility model provides a device for oil direct sampling which characterized in that includes:
an atomizer (1) for forming an aerosol from an oil sample;
the temperature control cavity (4) is provided with a temperature control cavity inlet and a temperature control cavity outlet and is connected with the atomizer (1);
the temperature control reaction cavity is an interlayer cavity arranged on the outer wall of the temperature control cavity (4), a refrigeration reactant is filled in the temperature control reaction cavity, and the temperature of the aerosol is controlled through heat exchange between the temperature control reaction cavity and the temperature control cavity (4);
an oxygen generating assembly;
and a first interface of the three-way valve (14) is connected with an outlet of the temperature control cavity, a second interface of the three-way valve is connected with an output port of the oxygen generation assembly, and a third interface of the three-way valve is connected with a sample inlet of the inductively coupled plasma atomic emission spectrometer.
2. The device for direct sample injection of oil products as claimed in claim 1, wherein the temperature-controlled reaction chamber comprises:
the first reaction cavity (2) is an interlayer cavity arranged on the outer wall of the temperature control cavity (4) and is filled with a refrigerant;
the second reaction cavity (3) is an interlayer cavity arranged on the outer wall of the temperature control cavity (4), and ice-water mixture is filled in the interlayer cavity;
the opening degree of the communication between the first reaction cavity (2) and the second reaction cavity (3) is adjustable.
3. The device for oil direct sampling according to claim 2, wherein a movable partition plate (5) is arranged between the first reaction chamber (2) and the second reaction chamber (3) at an interval, and the opening degree of the communication between the first reaction chamber (2) and the second reaction chamber (3) is adjusted by the partition plate (5) through horizontal or vertical movement.
4. The device for directly feeding the sample of the oil product as claimed in claim 2, wherein the first reaction chamber (2) and the second reaction chamber (3) are respectively connected with an external refrigerant feeder and an external ice-water mixture feeder.
5. The device for direct injection of oil products as claimed in claim 2, wherein the refrigerant is ammonium chloride or ammonium nitrate.
6. The device for direct injection of oil products as claimed in claim 1, wherein the oxygen generation assembly comprises a third reaction chamber (9), a chemical oxygen generation reaction occurs in the third reaction chamber (9), and the generated oxygen is mixed with the aerosol through a three-way valve (14).
7. The device for directly feeding the sample of the oil product as claimed in claim 1, wherein a liquid transport tube (7) is arranged on the third reaction chamber (9), and the liquid transport tube (7) is connected with an external hydrogen peroxide pump;
a flow control valve (12) is arranged on an output port of the third reaction chamber (9), and the flow control valve (12) is connected with a second interface of a three-way valve (14) through a pipeline;
the third reaction chamber (9) is filled with a hydrogen peroxide decomposition catalyst.
8. The device for direct injection of oil product as claimed in claim 7, wherein the hydrogen peroxide decomposition catalyst is a free transition metal ion compound or catalase MnO2Or Al2O3。
9. The device for direct sample injection of oil products as claimed in claim 7, wherein a waste liquid pipe (10) is disposed at the bottom of the third reaction chamber (9), and the waste liquid pipe (10) is provided with a solenoid valve (11).
10. A direct sample introduction method for oil products is characterized by comprising the following steps:
forming aerosol from an oil product sample and introducing the aerosol into a temperature control cavity with a refrigeration interlayer;
the refrigerating capacity and the refrigerating temperature are regulated and controlled by the refrigerating capacity generated by the chemical reaction in the refrigerating interlayer;
and connecting the aerosol passing through the temperature control cavity with an output port of the oxygen generation assembly, adjusting the oxygen content in the aerosol until reaching a target value, and finally introducing the mixed gas into an inductively coupled plasma atomic emission spectrometer for detection.
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| CN202010413720.6A CN111721753B (en) | 2020-05-15 | 2020-05-15 | Device and method for directly sampling oil |
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| CN202010413720.6A CN111721753B (en) | 2020-05-15 | 2020-05-15 | Device and method for directly sampling oil |
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