A rock particle fluorescence quantitative analysis pre-processing device and method

Abstract

The present invention discloses a pre-treatment device and method for fluorescence quantitative analysis of rock particles. The device includes a support system, a sample inlet and outlet system, and a reaction system. The treatment method includes: loading rock particle samples; adding dichloromethane for ultrasonic vibration and discharging, and then drying; adding hydrogen peroxide for ultrasonic vibration, discharging after standing, and then cleaning; adding hydrochloric acid for ultrasonic vibration and discharging, and then cleaning and drying; adding dichloromethane for ultrasonic vibration and testing; and air blowing to avoid residue. The present invention adopts a filling pipe connected in parallel with a peristaltic pump for filling multiple liquids, and through the selective operation of the peristaltic pump, the independent filling of the filling liquid is realized, the liquid can be discharged through the liquid discharge pump, and the sample is ultrasonically and dried through the built-in heater and ultrasonic vibration device. The pre-treatment method of the present invention adjusts the concentration of hydrocarbon substances to be detected in the sample to the detectable range while removing impurities, so that the subsequent rock fluorescence quantitative analysis can be carried out smoothly.

Description

Technical Field

[0001] The invention belongs to the technical field of petroleum exploration, and in particular relates to a rock particle fluorescence quantitative analysis pre-processing device and method. Background Art

[0002] At present, the methods of quantitative fluorescence analysis of reservoirs in domestic oil fields, scientific research and teaching units all adopt manual operation methods. There are the following problems in the manual operation process: First, laboratory personnel need to contact toxic and harmful reagents such as dichloromethane, hydrochloric acid, hydrogen peroxide, etc. to carry out a series of reactions, cleaning, water changes, etc. Volatile hydrochloric acid, hydrogen peroxide and dichloromethane are very easy to choke the operator's mouth and nose; acid addition, ultrasonic oscillation, and acid discharge are all manual operations, which poses a safety hazard to employee health. Second, the reservoir fluorescence analysis experiment is an accurate quantitative data test. Manual operation has errors in quantitative liquid addition and manual instability is easy to cause sample loss, which will increase the risk of large errors in experimental data. Third, in the rock particle pretreatment process specified in the existing standards, the equipment used is easily corroded by reagents; for example: ultrasonic waves, fume hoods and other equipment are very easy to be corroded by hydrochloric acid, and the hardware facilities of the laboratory are required to be high. Question 4: The implementation cycle of reservoir quantitative fluorescence analysis technology is long. It takes about 4 days to manually process a batch of samples, such as 12 pieces. However, the drilling site requires timeliness of experimental data within 2 days. The existing manual processing is likely to fail to meet the site requirements. Summary of the invention

[0003] The purpose of the present invention is to overcome the deficiencies of the prior art and to provide a device and method for pre-processing rock particle fluorescence quantitative analysis.

[0004] The present invention is achieved through the following technical solutions:

[0005] A rock particle fluorescence quantitative analysis pre-processing device comprises a support system, a sample inlet and outlet system and a reaction system;

[0006] The support system includes a chassis, a cover plate, a hood, and a lifting device. The upper surface of the chassis is provided with a cover plate, and a number of circular holes are formed on the surface of the cover plate. The circular holes are used to place the reaction tanks. The hood is arranged above the chassis;

[0007] The sample inlet and outlet system includes a sample injection device, a reaction tank, a sample cup, a waste liquid barrel, a purge device and a liquid pipeline; the sample injection device includes a container containing distilled water, hydrochloric acid, hydrogen peroxide and dichloromethane, and four peristaltic pumps respectively connected to the above containers; the reaction tank is installed in the circular hole of the cover plate, and four sample injection holes are formed on the tank body of the reaction tank, and the sample injection holes are respectively connected to the four peristaltic pumps through fluid pipelines, and a sample outlet hole is formed at the bottom of the reaction tank, and the sample outlet hole is connected to the waste liquid barrel through the fluid pipeline; a sample cup is arranged in the reaction tank, and the sample cup includes a barrel, an upper cover, a lower cover and a handle, the lower half of the barrel is composed of a filter screen (for the reaction liquid to pass through), and a penetrating air hole is formed in the handle; the purge device includes a gas nozzle, an air pump and a gas pipeline, the gas nozzle is arranged above the reaction tank, and is connected to the air pump through a gas pipeline, and the gas nozzle is connected to the air hole of the handle through a gas pipeline;

[0008] The reaction system comprises a heating device and an ultrasonic vibration device, wherein the heating device is arranged in a chassis, and the ultrasonic vibration device is arranged at the bottom of the reaction tank.

[0009] In the above technical solution, the hood is connected to a cylinder arranged in the chassis through a lifting rod, and the lifting rod can be driven by the cylinder to open and close the hood.

[0010] In the above technical solution, a raised ring is formed on the body of the reaction tank, and the outer diameter of the raised ring is larger than the outer diameter of the circular hole, so that the reaction tank is clamped on the cover plate. The injection hole is arranged on the raised ring and is arranged around the body of the reaction tank. The four injection holes are adjacent to each other and distributed at 90 degrees.

[0011] In the above technical solution, the cylinder body is connected to the upper cover and the lower cover through threads, and the upper cover is connected to the handle through threads.

[0012] In the above technical solution, a drainage pump is arranged in the chassis, and the waste liquid in the reaction tank is discharged into the waste liquid barrel through the drainage pump.

[0013] In the above technical solution, the heating device can realize the heating function in the following two forms: 1. The heating device is a PTC heating element arranged on the side wall of the reaction tank; 2. The heating device is a PTC air heater, which heats the enclosed area in the chassis.

[0014] In the above technical solution, the ultrasonic vibration device includes an ultrasonic transducer, a horn and a tool head.

[0015] A method for pre-processing rock particle fluorescence quantitative analysis comprises the following steps:

[0016] Step 1: Loading rock particle samples

[0017] Put the sieved rock particle sample into the sample cup and put it into the reaction tank;

[0018] Step 2: Add dichloromethane, vibrate ultrasonically and discharge, then dry

[0019] Add redistilled dichloromethane through a peristaltic pump for filling dichloromethane, perform ultrasound on the reaction tank, discharge the dichloromethane into a waste liquid barrel through a drainage pump, and start a heating device for drying;

[0020] Step 3: Add hydrogen peroxide, ultrasonically vibrate, let stand, drain, and then clean

[0021] Add hydrogen peroxide solution to the reaction tank through a peristaltic pump filled with hydrogen peroxide, sonicate, let stand, and sonicate again, discharge the hydrogen peroxide into a waste liquid bucket through a drainage pump, wash with tap water through a peristaltic pump filled with tap water, and then drain, and wash repeatedly to ensure that no sample is lost;

[0022] Step 4: Add hydrochloric acid, ultrasonically vibrate and discharge, then clean and dry

[0023] Add hydrochloric acid through a peristaltic pump and perform ultrasound, then discharge the hydrochloric acid into a waste liquid bucket through a drainage pump, add tap water through a peristaltic pump to wash and drain, wash repeatedly, add distilled water twice to wash and drain, ensure that no sample is lost, and then dry;

[0024] Step 5: Add dichloromethane and ultrasonically vibrate and test

[0025] Redistilled dichloromethane was added to the reaction tank through a peristaltic pump filled with dichloromethane. After ultrasonication, the sample was taken out for testing on the machine.

[0026] Step 6: Blow to avoid residue

[0027] When adding the latter liquid, the former liquid cannot remain in the pipeline. Use air pump-air nozzle-air pipe to empty the remaining liquid to avoid affecting the accurate measurement of the liquid added this time.

[0028] In the above technical solution, in step 1, the particle size of the particle sample is 60-140 mesh and the mass is 1-3g.

[0029] In the above technical solution, in step 2, the volume of dichloromethane is 15-25 ml, the ultrasonic time is 5-15 min, and the drying condition is performed at a temperature below 60° C. for 1-1.5 hours.

[0030] In the above technical solution, in step three, the volume of the hydrogen peroxide solution is 35-45 ml, the ultrasonic time is 8-12 min, the standing time is 35-45 min, the ultrasonic time is 8-12 min, the volume of tap water is 45-55 ml, and the number of repeated washings is 5-6 times.

[0031] In the above technical scheme, in step four, the volume of hydrochloric acid added is 35-45 ml, the ultrasonic time is 8-12 min, the volume of tap water added is 45-55 ml, the number of repeated washings is 5-6 times, the volume of distilled water is 45-55 ml, the drying temperature is 55-65°C, and the drying time is 8-9 hours.

[0032] In the above technical solution, in step 5, the volume of dichloromethane is 18-22 ml, and the ultrasonic time is 5-15 min. The advantages and beneficial effects of the present invention are:

[0033] The present invention adopts a filling pipe connected in parallel with a peristaltic pump for filling multiple liquids, and realizes independent filling of the filling liquid by selectively working the peristaltic pump, and can realize the discharge of the liquid by the liquid discharge pump. At the same time, the ultrasonic and drying of the sample are realized by the built-in PTC heater and ultrasonic vibration device. The residual liquid is purged by the air nozzle, and the upper cover can be opened and closed by the air cylinder and the lifting rod, so as to facilitate the observation and taking and placing of the sample cup.

[0034] The present invention effectively solves the problem of operators being exposed to chemical reagents, which is time-consuming, labor-intensive and harmful, and greatly improves the analysis efficiency. A large number of experiments have shown that the device is easy to operate and has a low failure rate, and subsequent experiments have achieved good analysis parameters. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 It is a schematic diagram of the overall structure of the present invention.

[0036] Figure 2 It is a front view structural schematic diagram of the present invention.

[0037] Figure 3 Schematic diagram of pipeline connection of the present invention.

[0038] Figure 4 This is a schematic diagram of the local structure of the reaction tank.

[0039] Figure 5 1406.5m - artificial test QGF-E - data.

[0040] Figure 6 QGF-E-data for the 1406.5m-instrument test.

[0041] Figure 7It is 1434m-artificial test QGF-E-data.

[0042] Figure 8 QGF-E-data for 1434m-instrument test.

[0043] Fig. 9 1582m-artificial test QGF-E-data.

[0044] Fig.10 QGF-E-data for 1582m-instrument test.

[0045] Among them: 1 is a computer, 2 is a sample injection device, 3 is a reaction tank, 3-1 is a raised ring, 3-2 is a sample addition hole, 3-3 is a sample outlet hole, 4 is an ultrasonic vibration device, 5 is a machine cover, 6 is a purge device, 7 is a lifting rod, 8 is a cover plate, 9 is a cylinder, 10 is a frame, 11 is a heating device, 12 is a waste liquid barrel, 13 is a chassis, 14 is a sample cup, 14-1 is a blowing hole, 14-2 is an upper cover, 14-3 is a cylinder, 14-4 is a lower cover, 14-5 is a handle, and 14-6 is a filter.

[0046] For ordinary technicians in this field, other relevant drawings can be obtained based on the above drawings without any creative work. DETAILED DESCRIPTION

[0047] In order to enable those skilled in the art to better understand the technical solution of the present invention, the technical solution of the present invention is further described below in conjunction with specific embodiments.

[0048] Example 1

[0049] like Figures 1 to 4 As shown, a rock particle fluorescence quantitative analysis pretreatment device comprises a chassis 13, wherein the upper end opening of the chassis 13 is provided with a cover plate 8, wherein a plurality of assembly holes are formed in the cover plate 8, wherein a reaction tank 3 is embedded in the assembly hole, wherein a sample cup is provided in the reaction tank 3, wherein a filling hole and a drainage hole are formed on the tank wall of the reaction tank, wherein an air blowing hole is formed on the sample cup, wherein the filling hole is connected with the filling device 2 via a filling pipe, wherein an air pipe connected with the air purge device 6 is provided in the air blowing hole, and wherein a drainage pipe connected with the drainage pump is provided in the drainage hole.

[0050] An ultrasonic vibration device 4 is disposed at the lower end of the reaction tank 3 .

[0051] The upper end of the chassis 13 is also provided with a hood 5 that can be buckled on the cover plate 8 .

[0052] A mounting plate is disposed in the hood 5 , a lifting rod 7 is disposed at the lower end of the mounting plate, and the lifting rod 7 passes through a cover plate 8 .

[0053] The chassis 13 includes a frame 10 and a box plate arranged outside the frame 10 . A cylinder 9 is arranged in the frame 10 , and a telescopic rod of the cylinder 9 is connected to the lifting rod 7 .

[0054] The filling device 2 is a peristaltic pump, and the filling pipe is connected in parallel with a peristaltic pump for filling tap water, a peristaltic pump for filling distilled water, a peristaltic pump for filling hydrochloric acid, a peristaltic pump for filling hydrogen peroxide, and a peristaltic pump for filling dichloromethane.

[0055] The cabinet 13 is also provided with a heating device 11 for heating and drying the sample cup. The heating device can realize the heating function in the following two forms: 1. The heating device is a PTC heating element arranged on the side wall of the reaction tank; 2. The heating device is a PTC air heater, which heats the enclosed area in the cabinet.

[0056] The air blowing device 6 is an air nozzle arranged in the mounting plate, and the air nozzle is connected to the air pump.

[0057] The liquid discharge pump is disposed in the chassis 13 , and a liquid outlet end of the liquid discharge pump is communicated with the waste liquid barrel 12 .

[0058] The peristaltic pump filled with tap water, the peristaltic pump filled with distilled water, the peristaltic pump filled with hydrochloric acid, the peristaltic pump filled with hydrogen peroxide, and the peristaltic pump filled with dichloromethane selectively work, that is, at most only one of them works at a time, or the peristaltic pump filled with tap water, the peristaltic pump filled with distilled water, the peristaltic pump filled with hydrochloric acid, the peristaltic pump filled with hydrogen peroxide, and the peristaltic pump filled with dichloromethane do not work.

[0059] The peristaltic pump for filling tap water, the peristaltic pump for filling distilled water, the peristaltic pump for filling hydrochloric acid, the peristaltic pump for filling hydrogen peroxide, and the peristaltic pump for filling dichloromethane are all controlled by the computer 1, so that the filling speeds thereof can be controlled.

[0060] There are at least two lifting rods 7, and there are also two cylinders 9 in the corresponding chassis 13.

[0061] The cylinder 9 can open or close the upper cover 5 through the lifting rod 7 connected thereto. When the upper cover 5 is opened, the operator can observe the cover plate 8 and the reaction tank 3 installed on the cover plate.

[0062] The chassis 13, the cover plate 8 and the reaction tank 3 enclose a closed chamber, and the heating device 11 can heat the chamber, so that the temperature of the reaction tank 3 is increased to achieve the effect of drying the reaction tank.

[0063] The heating device 11 is a 20V corrugated heating element PTC air heater, which has an over-temperature alarm and a temperature adjustment range from room temperature to 90°C.

[0064] The peristaltic pump model of the filling device 2 can be but is not limited to BT300 / R-12 multi-head peristaltic pump.

[0065] The ultrasonic vibration device 4 can be, but is not limited to, a 40KHZ50W ultrasonic vibrator. The ultrasonic vibration device 4 is used for the vibration of the reaction cup.

[0066] The reaction tank 3 is made of polytetrafluoroethylene, and a sample cup is placed inside it, so that organic solvent reaction and acid reaction can be carried out.

[0067] The filling pipe is connected in parallel with the peristaltic pump for filling multiple liquids, and the independent filling of the filling liquid is realized by the peristaltic pump's selective operation. The liquid can be discharged through the liquid discharge pump. At the same time, the ultrasonic and drying of the sample are realized through the built-in PTC heater and ultrasonic vibration device. The residual liquid is purged through the air nozzle, and the upper cover can be opened and closed through the air cylinder and lifting rod, so as to facilitate observation and taking and placing of the sample cup.

[0068] Example 2

[0069] A method for pre-processing rock particle fluorescence quantitative analysis is carried out according to the following steps:

[0070] Step i. About 2 g of the sieved rock particle sample (60-140 mesh size sample) is placed in a sample cup and placed in the reaction tank 3.

[0071] Step ⅱ. Add 20 ml of redistilled dichloromethane by a peristaltic pump filled with dichloromethane, the reaction tank 3, ultrasonic 10min, the dichloromethane is discharged into the waste liquid barrel 12 through the drainage pump, start the heating device 11, and dry at a temperature below 60 ℃ for 1 hour.

[0072] The purpose of this step is to remove excess soluble hydrocarbons and accompanying impurities in the sample to prevent fluorescence quenching caused by excessive hydrocarbon concentration.

[0073] Step iii. Add 40 ml of hydrogen peroxide solution to the reaction tank 3 through a peristaltic pump filled with hydrogen peroxide, ultrasonicate for 10 min, let stand for 40 min, and then ultrasonicate for 10 min. Drain the hydrogen peroxide into the waste liquid barrel 12 through a drainage pump, add 50 ml of tap water through a peristaltic pump filled with tap water, and then drain. Repeat the washing 5 times to ensure that there is no loss of the sample.

[0074] The purpose of this step is to remove active organic compounds in the sample and clay materials adhering to the particle surface.

[0075] Step iv. Add 40 ml of hydrochloric acid through a peristaltic pump and ultrasonicate for 10 minutes, then drain the hydrochloric acid into the waste liquid bucket 12 through a drainage pump, add 50 ml of tap water through a peristaltic pump, wash and drain, repeat the washing 5 times, add 50 ml of distilled water twice, wash and drain, ensure that the sample is not lost, and then dry at 60°C for 8 hours.

[0076] Remove carbonate minerals, metal oxides and covering materials that can produce mineral fluorescence from the sample.

[0077] Step ⅴ. Add 20 ml of redistilled dichloromethane to the reaction tank 3, and after ultrasonication for 10 minutes, take out the sample for testing on the machine. The instrument used is a fluorescence spectrophotometer with a specification model of Cary Eclipse, produced by Agilent, and the factory number is MY13400004.

[0078] The purpose is to test the fluorescence intensity of hydrocarbons adsorbed on the particle surface.

[0079] Step ⅵ. When adding the latter liquid, the former liquid cannot remain in the pipeline. Use the air pump-air nozzle-air pipe to empty the remaining liquid to avoid affecting the accurate measurement of the liquid added this time.

[0080] The peristaltic pump can realize automatic liquid addition (tap water, distilled water, hydrochloric acid, hydrogen peroxide, dichloromethane), and can realize flow rate and flow control for liquid addition, with a flow rate range of (0.5ml-100ml / min) and a flow control accuracy of ±1ml.

[0081] Analysis

[0082] When a certain room temperature substance is irradiated by incident light of a certain wavelength (usually ultraviolet rays or X-rays), it absorbs light energy and enters an excited state, and immediately de-excites and emits light with a wavelength longer than that of the incident light (usually a wavelength in the visible light band). The process is that when the molecules of the substance are in the ground state, they can transition to the excited state after absorbing light, and the excited state molecules collide with each other and return to the lowest vibration energy level of the first excited state in the form of no radiation energy loss. The light emitted by the molecules of this vibration energy level when returning to the ground state is called fluorescence.

[0083] Aromatic hydrocarbons and other hydrocarbon substances in petroleum have a fluorescence effect. The detection of hydrocarbon content in rocks is of great significance for the study of oil reserves in rock formations. Rock samples collected from rock formations often contain soluble hydrocarbons, active organic compounds, carbonate minerals, metal oxides, covering materials that can produce mineral fluorescence, and other incidental impurities. Through the pre-treatment of rock particle fluorescence quantitative analysis, it can be achieved: first, remove excessive soluble hydrocarbons and incidental impurities in the sample to prevent fluorescence quenching caused by excessive hydrocarbon concentration; second, remove active organic compounds in the sample and clay substances adhering to the surface of particles; third, remove carbonate minerals, metal oxides, and covering materials that can produce mineral fluorescence in the sample. While removing impurities, the concentration of the hydrocarbon substance to be detected in the sample is adjusted to the detectable range, so that the subsequent rock fluorescence quantitative analysis can be carried out smoothly.

[0084] Example 3

[0085] Parallel sample test: After the instrument is precisely debugged, three groups of downhole rock samples collected from the Bohai Oil Well KL6-5-3 at 1406.5m, 1434m and 1582m are selected as samples to be tested, numbered 1, 2, and 3 respectively; the above samples are weighed after grinding and sieving, and the weighed samples are pre-processed and tested by manual testing and instrument testing. Among them, the instrument test adopts the steps described in the above embodiment, and the pre-processing steps, test methods, and test environment of the manual test are the same as those of the instrument test.

[0086] As shown in the figure, Figure 5 It is 1406.5m-artificial test QGF-E-data; Figure 6 QGF-E-data for 1406.5m-instrument test; Figure 7 1434m-manual test QGF-E-data; Figure 8 QGF-E-data for 1434m-instrument testing; Fig. 9 1582m-manual test QGF-E-data; Fig.10 QGF-E-data for 1582m-instrument test.

[0087] The parameter calculation values ​​after the three samples were tested are shown in Table 1. The QGF-E intensity of each sample extract quantitative fluorescence test is a one-time test, and the particle samples of the particle quantitative fluorescence test can be tested repeatedly. To avoid possible errors and individual abnormal points, each sample QGF index is tested at more than 16 points according to the standard, and the average value is obtained by testing three times for comparison. index , QGF LamMax , QGF-E are commonly used parameters in reservoir quantitative fluorescence analysis. According to the data in Table 2, the relative deviations of the above three parameters are calculated.

[0088] Table 1 Parallel sample analysis parameter data table

[0089]

[0090] Table 2 Parallel Sample QGF index , QGF Lam Max, QGF-E relative deviation comparison table

[0091]

[0092] It can be seen from Table 2 that the parallel sample QGF index With QGF LamMax The relative deviation of the parameters is small, less than 4%, which meets the requirements (relative deviation less than 10% is sufficient). The above embodiments show that the rock particle fluorescence quantitative analysis pretreatment method implemented by the device of the present invention has a similar accuracy rate to the manual method, and can be applied to laboratory testing. However, compared with the manual method, the device effectively solves the problem of operators contacting chemical reagents, consuming time and effort, and causing great harm, and can greatly improve the analysis efficiency.

[0093] The present invention is described above by way of example. It should be noted that, without departing from the core of the present invention, any simple deformation, modification or other equivalent replacement that can be made by those skilled in the art without inventive effort falls within the protection scope of the present invention.

Claims

1. A rock particle fluorescence quantitative analysis pre-processing device, characterized by: Including support system, sample inlet and outlet system and reaction system; The support system includes a chassis, a cover plate, a hood, and a lifting device. The upper surface of the chassis is provided with a cover plate, and a number of circular holes are formed on the surface of the cover plate. The circular holes are used to place the reaction tanks. The hood is arranged above the chassis; The sample inlet and outlet system includes a sample injection device, a reaction tank, a sample cup, a waste liquid barrel, a purge device and a liquid pipeline; the sample injection device includes a container containing distilled water, hydrochloric acid, hydrogen peroxide and dichloromethane, and four peristaltic pumps respectively connected to the above containers; the reaction tank is installed in the circular hole of the cover plate, and four sample injection holes are formed on the tank body of the reaction tank, and the sample injection holes are respectively connected to the four peristaltic pumps through fluid pipelines, and a sample outlet hole is formed at the bottom of the reaction tank, and the sample outlet hole is connected to the waste liquid barrel through the fluid pipeline; a sample cup is arranged in the reaction tank, and the sample cup includes a barrel, an upper cover, a lower cover and a handle, the lower half of the barrel is composed of a filter screen, and a penetrating air hole is formed in the handle; the purge device includes an air nozzle, an air pump and a gas pipeline, the air nozzle is arranged above the reaction tank, and is connected to the air pump through a gas pipeline, and the air nozzle is connected to the air hole of the handle through a gas pipeline; The reaction system comprises a heating device and an ultrasonic vibration device, wherein the heating device is arranged in a chassis, and the ultrasonic vibration device is arranged at the bottom of the reaction tank.

2. A rock particle fluorescence quantitative analysis pre-processing device according to claim 1, characterized in that: The hood is connected to a cylinder arranged in the chassis through a lifting rod, and the lifting rod can be driven by the cylinder to realize opening and closing of the hood.

3. The rock particle fluorescence quantitative analysis pre-processing device according to claim 1 is characterized by: A raised ring is formed on the body of the reaction tank, and the outer diameter of the raised ring is larger than the outer diameter of the circular hole, so that the reaction tank is clamped on the cover plate. The injection hole is arranged on the raised ring and surrounds the body of the reaction tank. The four injection holes are adjacent to each other and distributed at 90 degrees.

4. The rock particle fluorescence quantitative analysis pre-processing device according to claim 1 is characterized by: The cylinder body is connected to the upper cover and the lower cover through threads, and the upper cover is connected to the handle through threads.

5. The rock particle fluorescence quantitative analysis pre-processing device according to claim 1 is characterized by: A drainage pump is arranged in the chassis, and waste liquid in the reaction tank is discharged into a waste liquid barrel through the drainage pump.

6. The rock particle fluorescence quantitative analysis pre-processing device according to claim 1 is characterized by: The ultrasonic vibration device comprises an ultrasonic transducer, a horn and a tool head.

7. A method for pre-processing rock particles for fluorescence quantitative analysis based on the rock particles fluorescence quantitative analysis pre-processing device according to any one of claims 1 to 6, characterized in that: The following steps are involved: Step 1: Loading rock particle samples Put the sieved rock particle sample into the sample cup and put it into the reaction tank; Step 2: Add dichloromethane, vibrate ultrasonically and discharge, then dry Add redistilled dichloromethane through a peristaltic pump for filling dichloromethane, perform ultrasound on the reaction tank, discharge the dichloromethane into a waste liquid barrel through a drainage pump, and start a heating device for drying; Step 3: Add hydrogen peroxide, ultrasonically vibrate, let stand, drain, and then clean Add hydrogen peroxide solution to the reaction tank through a peristaltic pump filled with hydrogen peroxide, sonicate, let stand, and sonicate again, discharge the hydrogen peroxide into a waste liquid bucket through a drainage pump, wash with tap water through a peristaltic pump filled with tap water, and then drain, and wash repeatedly to ensure that no sample is lost; Step 4: Add hydrochloric acid, ultrasonically vibrate and discharge, then clean and dry Add hydrochloric acid through a peristaltic pump and perform ultrasound, then discharge the hydrochloric acid into a waste liquid bucket through a drainage pump, add tap water through a peristaltic pump to wash and drain, wash repeatedly, add distilled water twice to wash and drain, ensure that no sample is lost, and then dry; Step 5: Add dichloromethane and ultrasonically vibrate and test Redistilled dichloromethane is added to the reaction tank through a peristaltic pump for filling dichloromethane, and after ultrasonication, the sample is taken out for testing on the machine; Step 6: Blow to avoid residue When adding the latter liquid, the former liquid cannot remain in the pipeline. Use air pump-air nozzle-air pipe to empty the remaining liquid to avoid affecting the accurate measurement of the liquid added this time.

8. A method for pre-processing rock particles for fluorescence quantitative analysis according to claim 7, characterized in that: In step 1, the particle size of the particle sample is 60-140 mesh and the mass is 1-3 g; In step 2, the volume of dichloromethane is 15-25 mL, the ultrasonic time is 5-15 min, and the drying condition is performed at a temperature below 60° C. for 1-1.5 hours; In step 3, the volume of the hydrogen peroxide solution is 35-45 mL, the ultrasonic time is 8-12 min, the standing time is 35-45 min, the ultrasonic time is 8-12 min, the volume of tap water is 45-55 mL, and the number of repeated washings is 5-6 times; In step 4, the volume of hydrochloric acid added is 35-45 mL, the ultrasonic time is 8-12 min, the volume of tap water added is 45-55 mL, the number of repeated washings is 5-6 times, the volume of distilled water is 45-55 mL, the drying temperature is 55-65° C., and the drying time is 8-9 hours; In step 5, the volume of dichloromethane is 18-22 mL, and the ultrasonic time is 5-15 min.

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