CN111721753B - Device and method for directly sampling oil - Google Patents

Device and method for directly sampling oil Download PDF

Info

Publication number
CN111721753B
CN111721753B CN202010413720.6A CN202010413720A CN111721753B CN 111721753 B CN111721753 B CN 111721753B CN 202010413720 A CN202010413720 A CN 202010413720A CN 111721753 B CN111721753 B CN 111721753B
Authority
CN
China
Prior art keywords
cavity
temperature control
reaction
oil
aerosol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202010413720.6A
Other languages
Chinese (zh)
Other versions
CN111721753A (en
Inventor
陈瑶瑶
李丹
邓维
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanghai Institute of Technology
Original Assignee
Shanghai Institute of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanghai Institute of Technology filed Critical Shanghai Institute of Technology
Priority to CN202010413720.6A priority Critical patent/CN111721753B/en
Publication of CN111721753A publication Critical patent/CN111721753A/en
Application granted granted Critical
Publication of CN111721753B publication Critical patent/CN111721753B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/02Preparation of oxygen
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/626Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/36Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Pathology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Inorganic Chemistry (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention relates to a device for directly injecting 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 aerosol from oil products; 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, wherein a refrigerating reactant is filled in the interlayer cavity, the temperature of the aerosol is controlled through heat exchange between the temperature control reaction cavity and the temperature control cavity, the environment temperature of the aerosol generated by an 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 can be used for preprocessing for analyzing the contents of various metal elements, can reduce or simplify complex sample pretreatment processes through temperature control and oxygen doping amount control, can realize rapid analysis and detection of trace elements in the oil, and ensures the stability and accuracy of analysis results.

Description

Device and method for directly sampling oil
Technical Field
The invention relates to the field of oil product detection, in particular to a device and a method for directly sampling oil products.
Background
With the rapid development of petrochemical industry, the demand of oil products is increasing. The contents of impurity elements and additive elements contained in the oil product are key to the quality control of the oil product. The common pretreatment methods of the oil products, such as a wet method digestion method, a dry method ashing method and the like, have the characteristics of complex operation, high reagent consumption, large environmental pollution and the like, and influence the rapid and accurate analysis of metal elements in the oil products to a certain extent. Therefore, the establishment of the direct sample injection analysis device and method for the impurity elements and the additive elements in the oil product has important practical significance.
At present, the analysis methods commonly used for impurity elements and additive elements in oil products are an inductively coupled plasma atomic emission spectrometry (ICP-OES) and an inductively coupled plasma mass spectrometry (ICP-MS), and if the methods are directly used for oil product direct analysis, carbon deposition of a torch tube is easily caused, the power consumption load of plasma is increased, and the stability and the accuracy of analysis results are affected.
CN205786632U discloses a sample injection device of changeable multiple oil, connects in an oil analysis instrument, is equipped with a plurality of oil passageway that the structure is the same, a first solenoid valve, an oil analysis instrument, a second solenoid valve, takes the exhaust hole to retrieve jar, and a plurality of oil passageways are passed through first solenoid valve merges the back and gets into oil analysis instrument, the exit end of oil analysis instrument with the entrance point intercommunication of second solenoid valve, the exit end of second solenoid valve with a plurality of oil passageways, take the exhaust hole to retrieve jar and be connected, wherein first solenoid valve is the many solenoid valve that advances one, the second solenoid valve is the one and advances many solenoid valves, the entrance point number of first solenoid valve with oil passageway number is the same, the exit end number of second solenoid valve is greater than oil passageway number. The device for directly injecting oil products in the technical scheme does not solve the problem of carbon deposition of a torch tube.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a device and a sample injection method for directly injecting the oil, wherein a temperature control and oxygenation combustion device is added in the process of directly analyzing metal elements in the oil by ICP-OES or ICP-MS, so that the direct sample injection analysis of the metal elements in the oil can be better realized, the complex sample pretreatment process can be reduced or simplified through temperature control and oxygen doping control, the rapid analysis and detection of trace elements in the oil can be realized, and the stability and accuracy of analysis results are ensured.
The aim of the invention can be achieved by the following technical scheme:
the invention relates to a device for directly injecting 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 device comprises the following components:
forming aerosol by the 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, wherein a refrigerating reactant is filled in the interlayer cavity, the temperature of the aerosol is controlled through heat exchange between the temperature control reaction cavity and the temperature control cavity, the environment temperature of the aerosol generated by an 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 generating component, 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-controlled reaction chamber comprises a first reaction chamber and a second reaction chamber, wherein:
the first reaction cavity is an interlayer cavity arranged on the outer wall of the temperature control cavity, and is filled with a refrigerant;
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 communication opening between the first reaction cavity and the second reaction cavity is adjustable.
Further, a movable isolation plate is arranged between the first reaction cavity and the second reaction cavity at intervals, and the communication opening between the first reaction cavity and the second reaction cavity is adjusted by the isolation plate through horizontal or vertical movement.
Further, the first reaction cavity and the second reaction cavity are respectively connected with a refrigerant feeder arranged outside and an ice-water mixture feeder arranged outside.
Further, the refrigerant is ammonium chloride or ammonium nitrate.
Further, the oxygen generating assembly comprises a third reaction chamber in which a chemical oxygen generating reaction occurs and the generated oxygen is mixed with the aerosol through a three-way valve.
Further, the third reaction chamber is provided with a transfusion tube which is connected with an external hydrogen peroxide pump;
the output port of the third reaction cavity is provided with a flow control valve, and the flow control valve 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 MnO 2 Or Al 2 O 3
Further, 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.
Further, the temperature is detected in real time by arranging the temperature sensor in the temperature control cavity, 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 real-time control of the feeding amount is realized, and the real-time adjustment of the temperature inside the temperature control cavity is realized through the real-time control.
Further, an oxygen sensor is arranged at the output port of the third reaction cavity, and the oxygen sensor is electrically connected with the ARM processor and is electrically connected with the hydrogen peroxide pump, so that the control of the oxygen output rate is formed, and the oxygen concentration in the aerosol is controlled.
The invention relates to a direct sample injection method for oil products, which comprises the following steps:
forming aerosol from the oil 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 through the refrigerating capacity generated by chemical reaction in the refrigerating interlayer;
and connecting the aerosol passing through the temperature control cavity with an output port of the oxygen generating assembly, regulating the oxygen content in the aerosol to 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 products can be used for preprocessing the content of various metal elements, can reduce or simplify complex pretreatment processes of the samples through temperature control and oxygen doping control, can realize rapid analysis and detection of trace elements in the oil products, ensures stability and accuracy of analysis results, and has the characteristics of simplicity in operation, rapidness in measurement, easiness in 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 the oil aerosol, thereby improving the stability of the analysis result of the oil element.
3) The invention adopts hydrogen peroxide to continuously supply oxygen for oil analysis, so that the oil can be burnt more fully in plasma, thereby avoiding plasma flameout caused by carbon deposition of a torch tube.
Drawings
FIG. 1 is a schematic diagram of a device for direct oil injection in the present invention;
in the figure: 1. the device comprises an atomizer, 2, a first reaction cavity, 3, a second reaction cavity, 4, a temperature control cavity, 5, a separation plate, 6, a first air duct, 7, a transfusion tube, 8, a catalyst, 9, a third reaction cavity, 10, a waste liquid tube, 11, an electromagnetic valve, 12, a flow control valve, 13, a second air duct, 14, a three-way valve, 15 and a third air duct.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples.
Example 1
The device for directly injecting oil in this embodiment includes an atomizer 1, a temperature control chamber 4, a temperature control reaction chamber, an oxygen generating component and a three-way valve 14, see fig. 1.
The atomizer 1 forms an aerosol from the 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, wherein a refrigerating reactant is filled in the interlayer cavity, the temperature of the aerosol is controlled through heat exchange with the temperature control cavity 4, the environmental temperature of the aerosol generated by an oil product is controlled, and the volatility of the oil product 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 between the first reaction chamber 2 and the second reaction chamber 3 is adjustable. A movable separation plate 5 is arranged between the first reaction cavity 2 and the second reaction cavity 3 at intervals, and the separation plate 5 adjusts the communication opening between the first reaction cavity 2 and the second reaction cavity 3 through horizontal or vertical movement. The first reaction cavity 2 and the second reaction cavity 3 are respectively connected with a peripheral refrigerant feeder and a peripheral ice-water mixture feeder. In a specific selection, the refrigerant is ammonium chloride or ammonium nitrate. Real-time detection of temperature is realized by arranging a temperature sensor in the temperature control cavity 4, the temperature sensor is connected with an ARM processor, and meanwhile, the ARM processor is electrically connected with a peripheral refrigerant feeder and a peripheral ice-water mixture feeder, so that real-time control of feeding quantity is realized, and 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 the first air duct 6, the second interface of the three-way valve is connected with the output port of the oxygen generating component through the second air duct 13, and the third interface of the three-way valve is connected with the sample inlet of the inductively coupled plasma atomic emission spectrometer through the third air duct 15.
The oxygen generating assembly comprises a third reaction chamber 9 in which a chemical oxygen generating reaction takes place and the generated oxygen is mixed with the aerosol via a three-way valve 14. The third reaction cavity 9 is provided with an infusion tube 7, and the infusion tube 7 is connected with an external hydrogen peroxide pump. The output port of the third reaction chamber 9 is provided with a flow control valve 12, the flow control valve 12 is connected with the second port 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 decomposing catalyst is free transition metal ion compound or catalase MnO 2 Or Al 2 O 3 . Three reactionsThe bottom of the cavity 9 is provided with a waste liquid pipe 10, and the waste liquid pipe 10 is provided with an electromagnetic valve 11. An oxygen sensor is arranged at the output port of the third reaction cavity 9, and is electrically connected with the ARM processor and the hydrogen peroxide pump, so that the control of the oxygen output rate is formed, and the oxygen concentration in the aerosol is controlled.
The sample injection device provided by the invention is used for analyzing the content of metal elements in a gasoline sample. The specific procedure is as in example 1.
(1) Drawing a standard curve: gradient standard solutions containing the metal elements to be tested are respectively prepared, and the gradients of the prepared solutions are shown in table 1. The standard solution is prepared by diluting standard oil (Conostan S-21, 1000 mg/Kg) with white oil or aviation kerosene as diluent.
(2) Test conditions for atomic emission spectrometer: power 1350w; cooling gas argon 15L/min; auxiliary gas argon is 0.8L/min; the flushing time is 60s; flushing pump speed: 20 revolutions per minute; analyzing the pump speed: 20 revolutions per minute; short wave analysis time: 60s; the flow rate of the atomized gas argon is 0.55L/min; a horizontal observation mode; analysis wavelength: see table 2.
(3) Analysis and detection of various metal elements in a gasoline sample: during specific operation, standard solutions with different concentration gradients are adopted for sample injection, the spectrum intensities of the standard solutions with different concentrations at the analysis wavelengths corresponding to the elements are recorded through an atomic emission spectrometer, and a standard curve between the spectrum intensities and the analysis concentrations is established.
Then adopting the device to sample and analyze the gasoline sample, forming aerosol from the oil 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 through the refrigerating capacity generated by chemical reaction in the refrigerating interlayer; and connecting the aerosol passing through the temperature control cavity with an output port of the oxygen generating assembly, regulating the oxygen content in the aerosol to 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 element in the gasoline sample, and the specific detection results are shown in table 2.
TABLE 1
Figure BDA0002494260430000051
Figure BDA0002494260430000061
TABLE 2
Figure BDA0002494260430000062
Example 2
The direct oil sample injection device provided by the invention is used for analyzing and detecting the content of metal elements in a diesel oil sample. The specific procedure is as in example 2.
(1) Drawing a standard curve: gradient standard solutions containing the metal elements to be tested are respectively prepared, and the gradients of the prepared solutions are shown in table 3. The standard solution is prepared by diluting standard oil (Conostan S-21, 1000 mg/Kg) with white oil or aviation kerosene as diluent.
(2) Test conditions for atomic emission spectrometer: power 1350w; cooling gas argon 15L/min; auxiliary gas argon is 0.8L/min; the flushing time is 60s; flushing pump speed: 20 revolutions per minute; analyzing the pump speed: 20 revolutions per minute; short wave analysis time: 60s; the flow rate of the atomized gas argon is 0.55L/min; a horizontal observation mode; analysis wavelength: see table 4.
(3) Analysis and detection of metal elements in diesel oil: during specific operation, standard solutions with different concentration gradients are adopted for sample injection, the spectrum intensities of the standard solutions with different concentrations at the analysis wavelengths corresponding to the elements are recorded through an atomic emission spectrometer, and a standard curve between the spectrum intensities and the analysis concentrations is established.
Then adopting the device to sample and analyze the gasoline sample, forming aerosol from the oil 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 through the refrigerating capacity generated by chemical reaction in the refrigerating interlayer; and connecting the aerosol passing through the temperature control cavity with an output port of the oxygen generating assembly, regulating the oxygen content in the aerosol to 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 element in the gasoline sample, and the specific detection results are shown in table 4.
TABLE 3 Table 3
Figure BDA0002494260430000071
TABLE 4 Table 4
Figure BDA0002494260430000072
Figure BDA0002494260430000081
Example 3
The multi-element analysis sample injection device provided by the invention is used for analyzing and detecting the content of metal elements in edible oil. The specific procedure is as in example 3.
(1) Drawing a standard curve: gradient standard solutions containing the metal elements to be tested were prepared separately, and the gradients of the prepared solutions are shown in table 5. The standard solution is prepared by diluting standard oil (Conostan S-21, 1000 mg/Kg) with white oil or aviation kerosene as diluent.
(2) Test conditions for atomic emission spectrometer: power 1350w; cooling gas argon 15L/min; auxiliary gas argon is 0.8L/min; the flushing time is 60s; flushing pump speed: 20 revolutions per minute; analyzing the pump speed: 20 revolutions per minute; short wave analysis time: 60s; the flow rate of the atomized gas argon is 0.55L/min; a horizontal observation mode; analysis wavelength: see table 6.
(3) Analysis and detection of metal elements in edible oil: during specific operation, standard solutions with different concentration gradients are adopted for sample injection, the spectrum intensities of the standard solutions with different concentrations at the analysis wavelengths corresponding to the elements are recorded through an atomic emission spectrometer, and a standard curve between the spectrum intensities and the analysis concentrations is established.
Then adopting the device to sample and analyze the gasoline sample, forming aerosol from the oil 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 through the refrigerating capacity generated by chemical reaction in the refrigerating interlayer; and connecting the aerosol passing through the temperature control cavity with an output port of the oxygen generating assembly, regulating the oxygen content in the aerosol to 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 element in the gasoline sample, and the specific detection results are shown in table 6.
TABLE 5
Figure BDA0002494260430000082
TABLE 6
Figure BDA0002494260430000091
It can be seen from examples 1 to 3 that the direct sample injection device for sampling oil products in the invention can be used for analyzing pretreatment of contents of various metal elements, and not only can reduce or simplify complex pretreatment processes of samples, but also can realize rapid analysis and detection of trace elements in the oil products by temperature control and oxygen doping control.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments 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-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.

Claims (6)

1. A device for oil direct sampling, which is characterized in that the device comprises:
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 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), is filled with a refrigeration reactant, and controls the temperature of the aerosol through heat exchange with the temperature control cavity (4);
an oxygen generating assembly;
the first interface of the three-way valve (14) 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 generating component, and the third interface of the three-way valve is connected with the sample inlet of the inductively coupled plasma atomic emission spectrometer;
the temperature-controlled reaction chamber includes:
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 between the first reaction cavity (2) and the second reaction cavity (3) can be adjusted;
a movable isolation plate (5) is arranged between the first reaction cavity (2) and the second reaction cavity (3) at intervals, and the isolation plate (5) adjusts the communication opening between the first reaction cavity (2) and the second reaction cavity (3) through horizontal or vertical movement;
the first reaction cavity (2) and the second reaction cavity (3) are respectively connected with a peripheral refrigerant feeder and a peripheral ice-water mixture feeder.
2. The device for direct oil sample injection according to claim 1, wherein the refrigerant is ammonium chloride or ammonium nitrate.
3. The device for direct oil sample injection according to claim 1, wherein the oxygen generating assembly comprises a third reaction chamber (9), wherein a chemical oxygen generating reaction occurs in the third reaction chamber (9), and the generated oxygen is mixed with the aerosol through a three-way valve (14).
4. A device for direct oil sample injection according to claim 3, characterized in that the third reaction chamber (9) is provided with a transfusion tube (7), and the transfusion tube (7) is connected with an external hydrogen peroxide pump;
the output port of the third reaction cavity (9) is provided with a flow control valve (12), and the flow control valve (12) is connected with a second interface of the three-way valve (14) through a pipeline;
the third reaction chamber (9) is filled with a hydrogen peroxide decomposition catalyst.
5. The device for direct oil sample injection according to claim 4, wherein the hydrogen peroxide decomposition catalyst is free transition metal ion compound, catalase or MnO 2 Or Al 2 O 3
6. The device for direct oil sample injection according to claim 4, wherein a waste liquid pipe (10) is arranged at the bottom of the third reaction chamber (9), and an electromagnetic valve (11) is arranged on the waste liquid pipe (10).
CN202010413720.6A 2020-05-15 2020-05-15 Device and method for directly sampling oil Active CN111721753B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010413720.6A CN111721753B (en) 2020-05-15 2020-05-15 Device and method for directly sampling oil

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010413720.6A CN111721753B (en) 2020-05-15 2020-05-15 Device and method for directly sampling oil

Publications (2)

Publication Number Publication Date
CN111721753A CN111721753A (en) 2020-09-29
CN111721753B true CN111721753B (en) 2023-06-30

Family

ID=72564572

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010413720.6A Active CN111721753B (en) 2020-05-15 2020-05-15 Device and method for directly sampling oil

Country Status (1)

Country Link
CN (1) CN111721753B (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009192475A (en) * 2008-02-18 2009-08-27 Shimadzu Corp Icp analyzer
CN101726482A (en) * 2009-12-24 2010-06-09 江苏天瑞仪器股份有限公司 Method for detecting content of elements in oil with inductively coupled plasma (ICP) spectrometer
CN104897621A (en) * 2015-05-14 2015-09-09 上海应用技术学院 Sampling device for multi-element analysis of environmental water and method for measuring concentration of metallic element
CN107976552A (en) * 2016-10-25 2018-05-01 中国石油化工股份有限公司 The universal sampling device and general sample injection method of gaseous hydrocarbon and liquefied petroleum gas

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009192475A (en) * 2008-02-18 2009-08-27 Shimadzu Corp Icp analyzer
CN101726482A (en) * 2009-12-24 2010-06-09 江苏天瑞仪器股份有限公司 Method for detecting content of elements in oil with inductively coupled plasma (ICP) spectrometer
CN104897621A (en) * 2015-05-14 2015-09-09 上海应用技术学院 Sampling device for multi-element analysis of environmental water and method for measuring concentration of metallic element
CN107976552A (en) * 2016-10-25 2018-05-01 中国石油化工股份有限公司 The universal sampling device and general sample injection method of gaseous hydrocarbon and liquefied petroleum gas

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
"甲苯溶解直接进样-电感耦合等离子体原子发射光谱法测定柴油抗磨剂中11种微量元素";李鹰 等;《理化检验(化学分册)》;20180518;第54卷(第05期);第516-519页 *
"电感耦合等离子体原子发射光谱法测定汽油中的铁、锰、铅和硅";马放钧 等;《理化检验(化学分册)》;20160918;第52卷(第09期);第1076-1079页 *
"电感耦合等离子体原子发射光谱法测定汽油中硫";刘林 等;《冶金分析》;20161231;第36卷(第08期);第60-64页 *

Also Published As

Publication number Publication date
CN111721753A (en) 2020-09-29

Similar Documents

Publication Publication Date Title
Edlund et al. Analysis of biodiesel by argon–oxygen mixed-gas inductively coupled plasma optical emission spectrometry
CN103926236B (en) The method of impurity element and matrix element content of niobium in simultaneous determination ferrocolumbium
US6987565B2 (en) Organometallic compound vaporizing/feeding system
CN111103271B (en) Atomic fluorescence analysis method for outer tube sample injection
US11435301B2 (en) Reaction control and mass spectrometry workstation for coupling an X-ray spectroscopic characterization instrument with an in-situ reaction cell
Hutton et al. Investigations into the direct analysis of semiconductor grade gases by inductively coupled plasma mass spectrometry
US20040056368A1 (en) Liquid organometallic compound vaporizing/feeding system
CN111721753B (en) Device and method for directly sampling oil
CN218725612U (en) Constant-temperature sample introduction analysis system
CN215066132U (en) Analysis appearance based on CAPS surveys nitrogen oxide
CN102331416B (en) Micro pulse sample introduction device and method for determining content of trace iron in nickel matrix solution
CN114813901A (en) Method for simultaneously detecting 12 elements in plant sample
JP3804798B2 (en) Evaporation supply device for liquid organometallic compounds
EP3040801B1 (en) Automatic ph adjustment device
Ek et al. Sequential injection analysis system for the determination of hydride-forming elements by direct current plasma atomic emission spectrometry
CN211402266U (en) Gas phase sample introduction device capable of diluting and testing greenhouse gas
CN211905089U (en) Lithium ion battery thermal runaway gas production analysis system containing hydrofluoric acid
CN205958458U (en) A hydride generation device for atomic fluorescence spectrometer
CN112858263A (en) Method for measuring content of metal elements in organic solution
CN219328769U (en) On-line detection device for detecting PH3 content in recovered hydrogen
US11896991B1 (en) Systems and methods for automatic adjustment of mixed gas flow for an injector coordinated with the acquistion of particular groups of chemical elements for analysis
CN116699046B (en) Sampling pressurized dilution sampling system and application method thereof
CN211697491U (en) Device for measuring carbon-oxygen isotope of carbonate rock in field
Lobo et al. Comparison of metallic and ceramic tubes as atomization cells for tin determination by TS-FF-AAS
CN216560387U (en) Device for external standard quantification of time-of-flight mass spectrum

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant