CN111076997A - Rock particle fluorescence quantitative analysis pretreatment device and method - Google Patents
Rock particle fluorescence quantitative analysis pretreatment device and method Download PDFInfo
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- CN111076997A CN111076997A CN201911381852.9A CN201911381852A CN111076997A CN 111076997 A CN111076997 A CN 111076997A CN 201911381852 A CN201911381852 A CN 201911381852A CN 111076997 A CN111076997 A CN 111076997A
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- G01N1/34—Purifying; Cleaning
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention discloses a pretreatment device and a pretreatment method for rock particle fluorescence quantitative analysis, wherein the device comprises a support system, a sample inlet and outlet system and a reaction system, and the treatment method comprises the following steps: loading a rock particle sample; adding dichloromethane, ultrasonically vibrating, discharging, and drying; adding hydrogen peroxide, ultrasonically vibrating, standing, discharging, and cleaning; adding hydrochloric acid, ultrasonically vibrating, discharging, cleaning and drying; adding dichloromethane for ultrasonic vibration and testing; air blowing is carried out to avoid residue. The filling pipe is communicated with the peristaltic pump for filling various liquids in parallel, independent filling of the filled liquids is realized through one operation of the peristaltic pump, liquid discharge can be realized through the liquid discharge pump, and ultrasonic treatment and drying of a sample are realized through the built-in heater and the ultrasonic vibration device. The pretreatment method provided by the invention can be used for adjusting the concentration of the hydrocarbon substances to be detected in the sample to a detectable range while removing impurities, so that the subsequent rock fluorescence quantitative analysis can be smoothly carried out.
Description
Technical Field
The invention belongs to the technical field of petroleum exploration, and particularly relates to a rock particle fluorescence quantitative analysis pretreatment device and method.
Background
At present, all domestic methods for analyzing reservoir quantitative fluorescence by units such as oil fields, scientific research, teaching and the like adopt manual operation methods. The following problems exist in the manual operation process: firstly, laboratory personnel need to contact toxic and harmful reagents such as dichloromethane, hydrochloric acid, hydrogen peroxide and the like to carry out a series of operations such as reaction, cleaning, water changing and the like, and volatile hydrochloric acid, hydrogen peroxide and dichloromethane are easy to choke to the mouth and nose of the operation personnel; the acid addition, the ultrasonic oscillation and the acid discharge are all performed manually, and potential safety hazards exist to the health of staff. Secondly, the reservoir fluorescence analysis experiment is an accurate quantitative data test, errors exist in quantitative liquid adding through manual operation, manual instability easily causes sample loss, and the risk of larger experimental data errors is increased. Thirdly, in the rock particle pretreatment process specified by the existing standard, the used equipment is easily corroded by the reagent; such as: ultrasonic wave, fume hood and other equipment are extremely easy to be corroded by hydrochloric acid, and have higher requirements on hardware facilities in an experimental room. And fourthly, the real period of the reservoir quantitative fluorescence analysis technology is long, about 4 days are needed for manually processing a batch of samples such as 12 samples, the timeliness of experimental data in a drilling site is required to be within 2 days, and the field requirement can not be easily met by the existing manual processing.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a pretreatment device and a pretreatment method for fluorescence quantitative analysis of rock particles.
The invention is realized by the following technical scheme:
a rock particle fluorescence quantitative analysis pretreatment device comprises a supporting system, a sample inlet and outlet system and a reaction system;
the supporting system comprises a case, a cover plate, a hood and a lifting device, wherein the cover plate is arranged on the upper surface of the case, a plurality of round holes are formed in the surface of the cover plate and used for placing reaction tanks, and the hood is arranged above the case;
the sample inlet and outlet system comprises a sample feeding device, a reaction tank, a sample cup, a waste liquid barrel, a purging device and a liquid pipeline; the sample feeding device comprises a container containing distilled water, hydrochloric acid, hydrogen peroxide and dichloromethane, and 4 peristaltic pumps respectively communicated with the container; the reaction tank is arranged in the round hole of the cover plate, 4 sample inlet holes are formed in the body of the reaction tank, the sample inlet holes are respectively connected with 4 peristaltic pumps through fluid pipelines, sample outlet holes are formed in the bottom of the reaction tank, and the sample outlet holes are connected with the waste liquid barrel through fluid pipelines; a sample cup is arranged in the reaction tank, the sample cup comprises a cylinder body, an upper cover, a lower cover and a handle, the lower half part of the cylinder body is formed by a filter screen (through which reaction liquid can pass), and a through air blowing hole is formed in the handle; the blowing device comprises an air faucet, an air pump and an air pipeline, wherein the air faucet is arranged above the reaction tank and is connected with the air pump through the air pipeline, and the air faucet is connected with an air blowing hole of the handle through the air pipeline;
the reaction system comprises a heating device and an ultrasonic vibration device, wherein the heating device is arranged in the case, and the ultrasonic vibration device is arranged at the bottom of the reaction tank.
In the technical scheme, the hood is connected with the cylinder arranged in the case through the lifting rod, and the hood can be opened and closed by driving the lifting rod through the cylinder.
In the above technical scheme, be formed with protruding ring on the body of retort, the external diameter of protruding ring is greater than the external diameter of round hole makes the retort card on the apron, the sample inlet sets up on protruding ring, encircles the body setting of retort, and 4 sample inlet are adjacent to be 90 degrees distributions.
In the technical scheme, the barrel is connected with the upper cover and the lower cover through threads, and the upper cover is connected with the handle through threads.
In the technical scheme, a liquid discharge pump is arranged in the case, and waste liquid in the reaction tank is discharged into the waste liquid barrel through the liquid discharge pump.
In the above technical solution, the heating device can realize the heating function through the following 2 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 closed area in the case.
In the above technical solution, the ultrasonic vibration device includes an ultrasonic transducer, an amplitude transformer and a tool bit.
A pretreatment method for fluorescence quantitative analysis of rock particles comprises the following steps:
step one, filling a rock particle sample
Putting a particle sample obtained after the rock is sieved into a sample cup and putting the sample cup into a reaction tank;
step two, adding dichloromethane, ultrasonically vibrating, discharging, and drying
Adding the redistilled dichloromethane through a peristaltic pump for adding dichloromethane, carrying out ultrasound on the reaction tank, discharging the dichloromethane into a waste liquid barrel through a liquid discharge pump, and starting a heating device for drying;
thirdly, adding hydrogen peroxide, ultrasonically vibrating, standing, discharging, and cleaning
Adding hydrogen peroxide solution into a reaction tank through a peristaltic pump for injecting hydrogen peroxide, performing ultrasonic treatment, standing, performing ultrasonic treatment again, discharging hydrogen peroxide into a waste liquid barrel through a liquid discharge pump, and discharging liquid after cleaning through a peristaltic pump for injecting tap water and then repeatedly cleaning, so as to ensure that a sample is not lost;
step four, adding hydrochloric acid for ultrasonic vibration and discharging, and then cleaning and drying
Adding hydrochloric acid by a peristaltic pump for adding hydrochloric acid, performing ultrasonic treatment, discharging the hydrochloric acid into a waste liquid barrel by a liquid discharge pump, adding tap water by the peristaltic pump for adding tap water, cleaning, repeatedly cleaning, adding 2 times of distilled water, cleaning, discharging liquid to ensure that a sample is not lost, and drying;
step five, adding dichloromethane for ultrasonic vibration and testing
Adding the redistilled dichloromethane into the reaction tank through a peristaltic pump for injecting dichloromethane, and taking out the sample after ultrasonic treatment for on-machine test.
Step six, air blowing is carried out to avoid residues
When the latter liquid is filled, the former liquid cannot be remained in the pipeline, and the air pump, the air tap and the air pipe are adopted to empty the remained liquid, so that the accurate metering of the filled liquid is not influenced.
In the technical scheme, in the step one, the particle size of the particle sample is 60-140 meshes, and the mass is 1-3 g.
In the technical scheme, in the second step, the volume of the dichloromethane is 15-25ml, the ultrasonic time is 5-15min, and the drying is carried out at the temperature lower than 60 ℃ for 1-1.5 hours.
In the technical scheme, in the third step, the volume of the hydrogen peroxide solution is 35-45ml, the ultrasonic time is 8-12min, the standing time is 35-45min, the ultrasonic time is 8-12min, the volume of tap water is 45-55ml, and the repeated cleaning times are 5-6 times.
In the technical scheme, in the fourth step, the added volume of the hydrochloric acid is 35-45ml, the ultrasonic time is 8-12min, the added volume of the tap water is 45-55ml, the repeated cleaning times are 5-6 times, the volume of the distilled water is 45-55ml, the drying temperature is 55-65 ℃, and the drying time is 8-9 hours.
In the technical scheme, in the step five, the volume of the dichloromethane is 18-22ml, and the ultrasonic time is 5-15min, and the method has the advantages and beneficial effects that:
the filling pipe is communicated with the peristaltic pump for filling various liquids in parallel, independent filling of the filled liquids is realized through one operation of the peristaltic pump, liquid discharge can be realized through the liquid discharge pump, and meanwhile, ultrasonic treatment and drying of the sample are realized through the built-in PTC heater and the ultrasonic vibration device. Sweep remaining liquid through the air cock, can realize opening and the lock of upper cover through cylinder, lifter to be convenient for observe and get and put the sample cup.
The invention effectively solves the problems of large time consumption and labor consumption damage caused by the contact of operators with chemical reagents, greatly improves the analysis efficiency, and has the advantages of easy operation, low fault and good analysis parameters obtained in subsequent experiments.
Drawings
Fig. 1 is a schematic view of the overall structure of the present invention.
FIG. 2 is a schematic front view of the present invention.
FIG. 3 is a schematic view of the piping connection of the present invention.
FIG. 4 is a schematic view of a partial structure of a reaction tank.
FIG. 5 is 1406.5 m-Manual test QGF-E-data.
FIG. 6 is 1406.5 m-Instrument test QGF-E-data.
FIG. 7 shows 1434 m-manual test QGF-E-data.
FIG. 8 shows the 1434 m-instrument test QGF-E-data.
FIG. 9 shows 1582 m-manual test QGF-E-data.
FIG. 10 shows the 1582 m-instrument test QGF-E-data.
Wherein: the device comprises a computer 1, a sample feeding device 2, a reaction tank 3, a raised ring 3-1, a sample feeding hole 3-2, a sample discharging hole 3-3, an ultrasonic vibration device 4, a hood 5, a purging device 6, a lifting rod 7, a cover plate 8, a cylinder 9, a frame 10, a heating device 11, a waste liquid barrel 12, a case 13, a sample cup 14, a gas blowing hole 14-1, an upper cover 14-2, a cylinder 14-3, a lower cover 14-4, a handle 14-5 and a filter screen 14-6.
For a person skilled in the art, other relevant figures can be obtained from the above figures without inventive effort.
Detailed Description
In order to make the technical solution of the present invention better understood, the technical solution of the present invention is further described below with reference to specific examples.
Example 1
As shown in fig. 1 to 4, a pretreatment device for fluorescence quantitative analysis of rock particles comprises a case 13, wherein a cover plate 8 is arranged at an open position at the upper end of the case 13, a plurality of assembly holes are formed in the cover plate 8, a reaction tank 3 is embedded in the assembly holes, a sample cup is arranged in the reaction tank 3, a filling hole and a liquid discharge hole are formed in the tank wall of the reaction tank, an air blowing hole is formed in the sample cup, the filling hole is communicated with a filling device 2 through a filling pipe, an air pipe communicated with an air blowing device 6 is arranged in the air blowing hole, and a liquid discharge pipe communicated with a liquid discharge pump is arranged in the liquid discharge hole.
The lower end of the reaction tank 3 is provided with an ultrasonic vibration device 4.
The upper end of the case 13 is also provided with a hood 5 which can be buckled on the cover plate 8.
The mounting plate is arranged in the hood 5, the lifting rod 7 is arranged at the lower end of the mounting plate, and the lifting rod 7 penetrates through the cover plate 8.
The case 13 comprises a frame 10 and a case plate arranged on the outer side of the frame 10, wherein a cylinder 9 is arranged in the frame 10, and an expansion rod of the cylinder 9 is connected with the lifting rod 7.
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.
And a heating device 11 for heating and drying the sample cup is also arranged in the case 13. The heating device can realize the heating function through the following 2 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 closed area in the case.
The air blowing device 6 is an air nozzle arranged in the mounting plate, and the air nozzle is communicated with the air pump.
The liquid discharge pump is arranged in the case 13, and the liquid outlet end of the liquid discharge pump is communicated with the waste liquid barrel 12.
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 selected to work, namely at most one peristaltic pump works at a certain moment, or 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 do not work.
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 speed of the peristaltic pump can be controlled.
The number of the lifting rods 7 is at least two, and the number of the cylinders 9 in the corresponding machine box 13 is also two.
The cylinder 9 can open or lock the upper cover 5 through the lifting rod 7 connected with the cylinder, and an operator can observe the cover plate 8 and the reaction tank 3 arranged on the cover plate when the upper cover 5 is in an open state.
The case 13, the cover plate 8 and the reaction tank 3 are enclosed to form a closed cavity, and the heating device 11 can heat the cavity, so that the temperature of the reaction tank 3 is increased, and the reaction tank is dried.
The heating device 11 is a 20V corrugated heating element PTC air heater which is provided with an overtemperature alarm, and the temperature adjusting range is from room temperature to 90 ℃.
The peristaltic pump model of the filling device 2 can be but is not limited to a BT300/R-12 multi-head peristaltic pump.
The ultrasonic vibration device 4 may be, but is not limited to, a 40KHZ50W ultrasonic transducer. The ultrasonic vibration device 4 is used for vibrating the reaction cup.
The reaction tank 3 is made of polytetrafluoroethylene, and a sample cup is placed in the reaction tank for organic solvent reaction and acid reaction.
The filling pipe is communicated with a peristaltic pump for filling various liquids in parallel, independent filling of the filled liquids is achieved through one operation of the peristaltic pump, liquid can be discharged through a liquid discharge pump, and meanwhile, ultrasonic treatment and drying of a sample are achieved through a built-in PTC heater and an ultrasonic vibration device. Sweep remaining liquid through the air cock, can realize opening and the lock of upper cover through cylinder, lifter to be convenient for observe and get and put the sample cup.
Example 2
A pretreatment method for fluorescence quantitative analysis of rock particles comprises the following steps:
and step i, putting about 2g of a particle sample (60-140 mesh particle size sample) obtained after the rock is sieved into a sample cup, and putting the sample cup into a reaction tank 3.
And step ii, adding 20ml of redistilled dichloromethane through a peristaltic pump for adding dichloromethane, carrying out ultrasonic treatment on the reaction tank 3 for 10min, discharging the dichloromethane into a waste liquid barrel 12 through a liquid discharge pump, starting a heating device 11, and drying for 1 hour at the temperature lower than 60 ℃.
The purpose of this step is to remove excess soluble hydrocarbons and incidental impurities from the sample and to prevent fluorescence quenching phenomena from occurring due to too high a concentration of hydrocarbons.
And iii, adding 40ml of hydrogen peroxide solution through a peristaltic pump for adding hydrogen peroxide, carrying out ultrasonic treatment for 10min in a reaction tank for 3 min, standing for 40min, carrying out ultrasonic treatment for 10min again, discharging hydrogen peroxide into a waste liquid barrel 12 through a liquid discharge pump, cleaning through adding 50ml of tap water through the peristaltic pump for adding tap water, discharging liquid, and repeatedly cleaning for 5 times to ensure that the sample is not lost.
The purpose of this step is to remove the reactive organic compounds and clay materials adhering to the surface of the particles in the sample.
Step iv, adding 40ml of hydrochloric acid through a peristaltic pump for adding hydrochloric acid, performing ultrasonic treatment for 10min, discharging the hydrochloric acid into a waste liquid barrel 12 through a liquid discharge pump, cleaning the hydrochloric acid through the peristaltic pump for adding tap water and 50ml of tap water, discharging the liquid, repeatedly cleaning the liquid for 5 times, and then cleaning the liquid through 2 times of 50ml of distilled water, so as to ensure that the sample is not lost. Then dried at 60 ℃ for 8 hours.
Removing carbonate minerals, metal oxides and covering substances capable of generating mineral fluorescence in the sample.
And v, adding 20ml of redistilled dichloromethane into the dichloromethane, carrying out ultrasonic treatment in a reaction tank for 3 min, taking out the sample, and carrying out on-machine test, wherein the adopted instrument is a fluorescence spectrophotometer, the specification model is Cary Eclipse, the production unit is Agilent company, and the delivery number is MY 13400004.
The aim was to test the fluorescence intensity of the hydrocarbon adsorbed on the particle surface.
And step vi, when the former liquid cannot be remained in the pipeline during the filling of the latter liquid, emptying the remained liquid by using an air pump-air nozzle-air pipe so as to avoid influencing the accurate metering of the filled liquid.
The peristaltic pump can realize automatic liquid adding (tap water, distilled water, hydrochloric acid, hydrogen peroxide and dichloromethane), flow rate and flow control of liquid adding can be realized, the flow rate range (0.5ml-100ml/min) and the flow control precision can reach +/-1 ml.
Description of the analysis
When a certain normal temperature substance is irradiated by incident light (usually ultraviolet rays or X-rays) with a certain wavelength, the substance enters an excited state after absorbing light energy, and immediately excites and emits emergent light (usually with a wavelength in a visible light band) with a wavelength longer than that of the incident light. The process is that when the molecules of the substance are in the ground state, after absorption of light, the molecules can transition to the excited state, and the molecules in the excited state collide with each other and return to the lowest vibration level of the first excited state in a form without radiation energy loss, and the light emitted by the molecules in the vibration level when returning to the ground state is called fluorescence.
The hydrocarbon substances such as aromatic hydrocarbon in the petroleum have a fluorescence effect, and the detection of the content of the hydrocarbon substances in the rock has important significance for the research of the petroleum reserves in the rock stratum. Rock samples collected from rock formations often contain soluble hydrocarbons, active organic compounds, carbonate minerals, metal oxides, covering substances capable of generating mineral fluorescence, other incidental impurities and the like, and pretreatment of rock particle fluorescence quantitative analysis can realize that: firstly, removing excessive soluble hydrocarbons and incidental impurities in a sample, and preventing the phenomenon of fluorescence quenching caused by overhigh hydrocarbon concentration; secondly, removing the active organic compound and clay substances adhered to the surfaces of the particles in the sample; and thirdly, removing carbonate minerals, metal oxides and covering substances capable of generating mineral fluorescence in the sample. And (3) while removing impurities, adjusting the concentration of the hydrocarbon substance to be detected in the sample to a detectable range, so that the subsequent rock fluorescence quantitative analysis can be smoothly carried out.
Example 3
And (3) parallel sample testing: after the instrument is accurately debugged, 3 groups of underground rock samples which are 1406.5m, 1434m and 1582m respectively and are collected from the Bohai sea petroleum well section with the number of KL6-5-3 are selected as samples to be detected and are numbered as 1, 2 and 3 respectively; the samples are respectively ground and sieved and then weighed, and the weighed samples are respectively subjected to pretreatment testing in two modes of manual testing and instrument testing. The instrument test adopts the steps of the embodiment, and the manual test adopts the pretreatment step, the test method and the test environment which are the same as those of the instrument test.
As shown, FIG. 5 is 1406.5 m-Manual test QGF-E-data; FIG. 6 is 1406.5 m-Instrument test QGF-E-data; FIG. 7 is 1434 m-manual test QGF-E-data; FIG. 8 shows 1434 m-instrument test QGF-E-data; FIG. 9 is 1582 m-manual test QGF-E-data; FIG. 10 shows the 1582 m-instrument test QGF-E-data.
The calculated parameters after the testing of the 3 samples are shown in table 1. The QGF-E intensity of the quantitative fluorescence test for each sample extract is a one-time testThe particle samples of the particle quantitative fluorescence test can be tested repeatedly, in order to avoid possible errors and respective abnormal points, each sample QGF index is tested for more than 16 points according to the standard, and the average value is obtained by testing for 3 times for comparison. QGFindex、QGFLamMaxQGF-E are parameters commonly used in quantitative fluorescence analysis of reservoirs, and relative deviation calculations of the three parameters were performed based on the data in Table 2.
Table 1 table of analysis parameter data of parallel samples
Table 2 replicates QGFindexQGF Lam Max, QGF-E relative deviation comparison table
As can be seen from Table 2, parallel QGFindexAnd QGFLamMaxThe relative deviation of the parameters is small and is less than 4%, and the requirements are met (the relative deviation is less than 10%). The embodiment shows that the rock particle fluorescence quantitative analysis pretreatment method implemented by the device has similar accuracy rate compared with the manual method, and is suitable for laboratory test, but compared with the manual method, the device effectively solves the problems that operators contact chemical reagents, and the time and the labor are consumed and the damage is large, and can greatly improve the analysis efficiency.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (8)
1. A rock particle fluorescence quantitative analysis pretreatment device is characterized in that: comprises a supporting system, a sample inlet and outlet system and a reaction system;
the supporting system comprises a case, a cover plate, a hood and a lifting device, wherein the cover plate is arranged on the upper surface of the case, a plurality of round holes are formed in the surface of the cover plate and used for placing reaction tanks, and the hood is arranged above the case;
the sample inlet and outlet system comprises a sample feeding device, a reaction tank, a sample cup, a waste liquid barrel, a purging device and a liquid pipeline; the sample feeding device comprises a container containing distilled water, hydrochloric acid, hydrogen peroxide and dichloromethane, and 4 peristaltic pumps respectively communicated with the container; the reaction tank is arranged in the round hole of the cover plate, 4 sample inlet holes are formed in the body of the reaction tank, the sample inlet holes are respectively connected with 4 peristaltic pumps through fluid pipelines, sample outlet holes are formed in the bottom of the reaction tank, and the sample outlet holes are connected with the waste liquid barrel through fluid pipelines; a sample cup is arranged in the reaction tank and comprises a cylinder body, an upper cover, a lower cover and a handle, wherein the lower half part of the cylinder body is formed by a filter screen, and a through air blowing hole is formed in the handle; the blowing device comprises an air faucet, an air pump and an air pipeline, wherein the air faucet is arranged above the reaction tank and is connected with the air pump through the air pipeline, and the air faucet is connected with an air blowing hole of the handle through the air pipeline;
the reaction system comprises a heating device and an ultrasonic vibration device, wherein the heating device is arranged in the case, and the ultrasonic vibration device is arranged at the bottom of the reaction tank.
2. The pretreatment device for fluorescent quantitative analysis of rock particles according to claim 1, wherein: the hood is connected with the cylinder arranged in the case through the lifting rod, and the hood can be opened and closed by driving the lifting rod through the cylinder.
3. The pretreatment device for fluorescent quantitative analysis of rock particles according to claim 1, wherein: be formed with protruding ring on the body of retort, the external diameter of protruding ring is greater than the external diameter of round hole makes the retort card on the apron, the sample inlet sets up on protruding ring, encircles the body setting of retort, and 4 sample inlet are adjacent to be 90 degrees distributions.
4. The pretreatment device for fluorescent quantitative analysis of rock particles according to claim 1, wherein: the barrel is connected with the upper cover and the lower cover through threads, and the upper cover is connected with the handle through threads.
5. The pretreatment device for fluorescent quantitative analysis of rock particles according to claim 1, wherein: a liquid discharge pump is arranged in the case, and waste liquid in the reaction tank is discharged into a waste liquid barrel through the liquid discharge pump.
6. The pretreatment device for fluorescent quantitative analysis of rock particles according to claim 1, wherein: the ultrasonic vibration device comprises an ultrasonic transducer, an amplitude transformer and a tool head.
7. The pretreatment method for the fluorescent quantitative analysis of the rock particles is characterized by comprising the following steps of:
step one, filling a rock particle sample
Putting a particle sample obtained after the rock is sieved into a sample cup and putting the sample cup into a reaction tank;
step two, adding dichloromethane, ultrasonically vibrating, discharging, and drying
Adding the redistilled dichloromethane through a peristaltic pump for adding dichloromethane, carrying out ultrasound on the reaction tank, discharging the dichloromethane into a waste liquid barrel through a liquid discharge pump, and starting a heating device for drying;
thirdly, adding hydrogen peroxide, ultrasonically vibrating, standing, discharging, and cleaning
Adding hydrogen peroxide solution into a reaction tank through a peristaltic pump for injecting hydrogen peroxide, performing ultrasonic treatment, standing, performing ultrasonic treatment again, discharging hydrogen peroxide into a waste liquid barrel through a liquid discharge pump, and discharging liquid after cleaning through a peristaltic pump for injecting tap water and then repeatedly cleaning, so as to ensure that a sample is not lost;
step four, adding hydrochloric acid for ultrasonic vibration and discharging, and then cleaning and drying
Adding hydrochloric acid by a peristaltic pump for adding hydrochloric acid, performing ultrasonic treatment, discharging the hydrochloric acid into a waste liquid barrel by a liquid discharge pump, adding tap water by the peristaltic pump for adding tap water, cleaning, repeatedly cleaning, adding 2 times of distilled water, cleaning, discharging liquid to ensure that a sample is not lost, and drying;
step five, adding dichloromethane for ultrasonic vibration and testing
Adding the redistilled dichloromethane into the reaction tank through a peristaltic pump for injecting dichloromethane, and taking out the sample after ultrasonic treatment for on-machine test.
Step six, air blowing is carried out to avoid residues
When the latter liquid is filled, the former liquid cannot be remained in the pipeline, and the air pump, the air tap and the air pipe are adopted to empty the remained liquid, so that the accurate metering of the filled liquid is not influenced.
8. The pretreatment method for fluorescent quantitative analysis of rock particles according to claim 7, wherein the pretreatment method comprises the following steps:
in the first step, the particle size of the particle sample is 60-140 meshes, and the mass is 1-3 g;
in the second step, the volume of the dichloromethane is 15-25ml, the ultrasonic time is 5-15min, and the drying condition is that the temperature is lower than 60 ℃ for 1-1.5 hours;
in the third step, the volume of the hydrogen peroxide solution is 35-45ml, the ultrasonic time is 8-12min, the standing time is 35-45min, the ultrasonic time is 8-12min, the volume of tap water is 45-55ml, and the number of repeated cleaning is 5-6;
in the fourth step, the added volume of the hydrochloric acid is 35-45ml, the ultrasonic time is 8-12min, the added volume of the tap water is 45-55ml, the repeated cleaning times are 5-6 times, the volume of the distilled water is 45-55ml, the drying temperature is 55-65 ℃, and the drying time is 8-9 hours;
in the fifth step, the volume of the dichloromethane is 18-22ml, and the ultrasonic time is 5-15 min.
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| CN111426651A (en) * | 2020-05-18 | 2020-07-17 | 河北中烟工业有限责任公司 | Near-infrared analyzer liquid sample sampling detection device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111426651A (en) * | 2020-05-18 | 2020-07-17 | 河北中烟工业有限责任公司 | Near-infrared analyzer liquid sample sampling detection device |
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