CN116046495A - Sample processing method and device for measuring metal elements in soil - Google Patents

Sample processing method and device for measuring metal elements in soil Download PDF

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Publication number
CN116046495A
CN116046495A CN202310032504.0A CN202310032504A CN116046495A CN 116046495 A CN116046495 A CN 116046495A CN 202310032504 A CN202310032504 A CN 202310032504A CN 116046495 A CN116046495 A CN 116046495A
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soil
fixedly connected
sample
test tube
carousel
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CN116046495B (en
Inventor
李谦
吴明
张学玲
蒋媛
李智
杨建兴
吴少涛
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Ningxia Hui Autonomous Region Food Inspection Research Institute
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Ningxia Hui Autonomous Region Food Inspection Research Institute
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B65CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65CLABELLING OR TAGGING MACHINES, APPARATUS, OR PROCESSES
    • B65C9/00Details of labelling machines or apparatus
    • B65C9/08Label feeding
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4044Concentrating samples by chemical techniques; Digestion; Chemical decomposition
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat
    • 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G01N2001/2866Grinding or homogeneising
    • 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
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A90/00Technologies having an indirect contribution to adaptation to climate change
    • Y02A90/30Assessment of water resources

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
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  • Electrochemistry (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention provides a sample processing method and device for measuring metal elements in soil, and relates to the technical field of soil detection. This a sample processing device for determining metallic element in soil, the on-line screen storage device comprises a base, the fixedly connected with of base rotates the motor, fixedly connected with carousel on the output shaft of rotating the motor to the carousel is located the top of base, the top of carousel is provided with a plurality of processing section of thick bamboo, and processing section of thick bamboo passes through support column and carousel fixed connection, the bottom of processing section of thick bamboo is provided with the unloading pipe, fixedly connected with dog on the periphery of support column, sliding connection has the slider on the periphery of support column. Through setting up rotation motor, carousel and a plurality of processing section of thick bamboo, conveniently separate the processing to the sample soil of different positions, in avoiding last remaining sample soil to get into the sample soil of processing next time, be favorable to improving the accuracy that sample soil detected.

Description

Sample processing method and device for measuring metal elements in soil
Technical Field
The invention relates to the technical field of soil detection, in particular to a sample processing method and device for determining metal elements in soil.
Background
Soil refers to a loose layer of substances on the surface of the earth, and consists of various granular mineral substances, organic substances, moisture, air, microorganisms and the like, plants can grow, and the soil is seriously over-standard due to the massive application of pesticides, fertilizers and auxins and the pollution of industrial three wastes, so that the heavy metal content of the soil needs to be detected regularly.
The applicant has found that, when applying for the present invention, the chinese patent discloses a sample treatment method and apparatus for measuring metal elements in soil, the application number of which is CN202010978009.5, the patent mainly uses a drying apparatus, a crushing and screening apparatus and a sample adding apparatus to dry, crush and screen the sampled soil, and finally adds the treated soil into a test tube to digest, but when the patent needs to treat sample soil at different positions, the sample soil treated in the previous time will partially remain in the sample treatment apparatus, so that when the sample soil is treated in the next time, the sample soil remained in the previous time will enter the sample soil treated in the next time, and the detection data will be inaccurate.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a sample treatment method and a sample treatment device for measuring metal elements in soil, which solve the problems that when sample soil at different positions is treated, part of sample soil treated before is remained in the sample treatment device, so that when the next sample soil treatment is carried out, the sample soil remained before can enter the sample soil treated next time, and the detection data is inaccurate.
(II) technical scheme
In order to achieve the above purpose, the invention is realized by the following technical scheme: the utility model provides a sample processing device for determining metallic element in soil, includes the base, the fixedly connected with rotation motor of base, fixedly connected with carousel on rotation motor's the output shaft to the carousel is located the top of base, the top of carousel is provided with a plurality of processing section of thick bamboo, and processing section of thick bamboo passes through support column and carousel fixed connection, the bottom of processing section of thick bamboo is provided with the unloading pipe, fixedly connected with dog on the periphery of support column, sliding connection has the slider on the periphery of support column, and the slider is located the top of dog, fixedly connected with connecting rod on the lateral wall of slider, the one end fixedly connected with spacing ring that the slider was kept away from to the connecting rod, the cover is equipped with the spring on the periphery of connecting rod, and the spring is located the top of slider, the top fixedly connected with of carousel is placed the seat, and place the seat is located the below of unloading pipe, place the inside of seat and place the test tube.
The inside of the treatment cylinder is provided with a screen plate, the side wall of the screen plate is fixedly connected with a clamping rod, the inner wall of the treatment cylinder is provided with a clamping groove, the clamping rod is positioned in the clamping groove, the clamping rod is fixedly connected with a positioning bracket, the inside of the positioning bracket is rotationally connected with a rotating shaft, the top of the rotating shaft is fixedly connected with a gear, and the circumferential surface of the rotating shaft is fixedly connected with a crushing blade;
the top fixedly connected with of base handles the cover, the top fixedly connected with electronic jar of handling the cover, the expansion end fixedly connected with fixed plate of electronic jar, the bottom fixedly connected with of fixed plate smashes the motor, fixedly connected with fixture block on smashing the output shaft of motor to the fixture block is located the inside of handling the cover, the bottom of fixture block is provided with the tooth hole, the interior top of handling the cover is provided with the heating lamp.
Preferably, the bottom of carousel fixedly connected with a plurality of wheels to the wheel corresponds the setting with the processing section of thick bamboo.
Preferably, two support columns are arranged at the bottom of each treatment cylinder and symmetrically arranged at two sides of the blanking pipe.
Preferably, the limiting ring is positioned below the blanking pipe, the limiting ring is matched with the test tube for use, and the limiting ring is made of polytetrafluoroethylene.
Preferably, four clamping grooves and four clamping rods are formed in each processing cylinder, a positioning support is arranged in each processing cylinder, and the prone surface of the positioning support is cross-shaped.
Preferably, the number of the electric cylinders is two, the electric cylinders are symmetrically arranged on the left side and the right side of the crushing motor, and the gears are matched with the tooth holes for use.
A sample processing method for measuring metal elements in soil comprises the following specific steps: s1, firstly, selecting and dividing a rectangular stable soil area in a region where soil needs to be detected, selecting a plurality of sampling points in the rectangular stable soil area by adopting a diagonal sampling method, placing the sampled soil into a sample container, simultaneously removing branches, leaves and stones in a soil sample, and labeling;
s2, before soil samples are processed, firstly supporting a limiting ring by hand, then placing a test tube into a placing seat, loosening the limiting ring after the test tube is placed, positioning the test tube under the action of a spring at the moment, sequentially pouring the collected soil samples into a plurality of processing cylinders, after the soil samples are placed, rotating a motor control turntable, transferring a first processing cylinder into a processing cover, drying the soil samples in the processing cylinders by a heating lamp, after the drying is completed, controlling a crushing motor to move downwards by an electric cylinder, clamping a gear into a tooth hole, controlling a crushing motor to rotate, crushing the soil samples, screening the crushed soil samples by a screen plate, falling the crushed soil samples into the test tube from a blanking pipe, after the soil samples in the first processing cylinder are processed, controlling the crushing motor to move upwards, enabling a gear to move out of a tooth hole, rotating a motor control turntable, repeating the steps to process the residual soil samples, and finally attaching a label again after the taking out;
s3, adding nitric acid, hydrochloric acid and hydrofluoric acid into the test tube, sealing, putting the test tube into a super microwave digestion instrument for primary digestion, taking out the test tube after cooling, adding boric acid solution, and putting the test tube into the super microwave digestion instrument again for secondary digestion;
s4, after digestion is completed, constant volume and film coating are carried out, the measurement is carried out by an inductively coupled plasma mass spectrometer, the quality is determined by using the specific mass number of the element, and the quantitative analysis is carried out by adopting an external standard method and the intensity ratio of the mass spectrum signal of the element to be measured and the mass spectrum signal of the internal standard element is in direct proportion to the concentration of the element to be measured.
Preferably, the heating time of the heating lamp in the step S2 is 10-20min, the temperature of the first digestion in the step S3 is 90-150 ℃, the constant temperature time is 5min, the temperature of the second digestion is 180-220 ℃, the constant temperature time is 5min, the power of the super microwave digestion instrument is 1200W, and the step S3 is measured by firstly using a balance when adding nitric acid, hydrochloric acid and hydrofluoric acid, and 1.2m l nitric acid, 0.4m l hydrochloric acid, 0.4m l hydrofluoric acid and 5.0m l boric acid solution are added to each 0.05g soil sample.
(III) beneficial effects
The invention provides a sample processing method and device for measuring metal elements in soil. The beneficial effects are as follows:
1. according to the invention, through arranging the rotating motor, the rotating disc and the plurality of treatment cylinders, the sample soil at different positions is conveniently treated separately, so that the sample soil left in the previous time is prevented from entering the sample soil treated next time, and the accuracy of sample soil detection is improved.
2. According to the invention, through arranging the stop block, the sliding block, the spring, the connecting rod, the limiting ring and the placing seat, the test tube is convenient to take and place, and the operation is simple.
Drawings
FIG. 1 is a front view of a sample processing device for measuring metallic elements in soil according to the present invention;
FIG. 2 is a schematic view of the structure A in FIG. 1;
FIG. 3 is a schematic view of a processing cylinder of a sample processing device for measuring metallic elements in soil according to the present invention;
FIG. 4 is a top view of a turntable of a sample processing device for measuring metallic elements in soil according to the present invention;
FIG. 5 is a front cross-sectional view of a treatment cartridge of a sample treatment apparatus for measuring metallic elements in soil according to the present invention;
FIG. 6 is a top view of a gear of a sample processing device for measuring metallic elements in soil according to the present invention;
FIG. 7 is a side view of a treatment housing of a sample treatment apparatus for measuring metallic elements in soil according to the present invention;
FIG. 8 is a front cross-sectional view of a treatment housing of a sample treatment apparatus for measuring metallic elements in soil according to the present invention;
FIG. 9 is a schematic view showing the bottom structure of a fixture block of a sample processing device for measuring metallic elements in soil according to the present invention;
fig. 10 is a top view of a treatment hood of a sample treatment apparatus for measuring metallic elements in soil according to the present invention.
1, a base; 2. a rotating motor; 3. a turntable; 4. a treatment cylinder; 5. a support column; 6. a stop block; 7. a slide block; 8. a spring; 9. a connecting rod; 10. a limiting ring; 11. a test tube; 12. a placement seat; 13. discharging pipes; 14. a clamping groove; 15. a sieve plate; 16. a clamping rod; 17. a positioning bracket; 18. a rotating shaft; 19. a crushing blade; 20. a gear; 21. a treatment cover; 22. an electric cylinder; 23. a fixing plate; 24. a crushing motor; 25. a clamping block; 26. a heating lamp; 27. and (5) tooth holes.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Examples:
as shown in fig. 1-10, the embodiment of the invention provides a sample processing device for measuring metal elements in soil, which comprises a base 1, a rotating motor 2 is fixedly connected to the base 1, the rotating motor 2 is mainly used for controlling a turntable 3 to rotate, thereby converting a plurality of processing cylinders 4, the rotating motor 2 rotates at the same angle each time and just transfers the processing cylinders 4 into a processing cover 21, a turntable 3 is fixedly connected to an output shaft of the rotating motor 2, the turntable 3 is positioned above the base 1, a plurality of processing cylinders 4 are arranged above the turntable 3, the processing cylinders 4 are fixedly connected with the turntable 3 through a supporting column 5, the processing cylinders 4 are mainly used for crushing and screening of soil samples, a blanking pipe 13 is arranged at the bottom of the processing cylinders 4, a stop block 6 is fixedly connected to the circumferential surface of the supporting column 5, the stop block 6 is mainly used for limiting the sliding block 7, a sliding block 7 is connected to the circumferential surface of the supporting column 5, the sliding block 7 is positioned above the stop block 6, a connecting rod 9 is fixedly connected to the side wall of the sliding block 7, a limiting ring 10 is fixedly connected to one end of the connecting rod 9, which is far from the sliding block 7, the limiting ring 11 is mainly used for limiting the test tube 11, a spring seat 12 is arranged above the test tube 11 and is always placed above the spring seat 12, and is positioned above the spring seat 12 and is fixedly placed below the test tube 8, and is placed above the spring seat 12;
the inside of the treatment cylinder 4 is provided with a screen plate 15, the screen plate 15 is mainly used for screening soil, the screen plate 15 is 100 meshes, the side wall of the screen plate 15 is fixedly connected with a clamping rod 16, the inner wall of the treatment cylinder 4 is provided with a clamping groove 14, the clamping rod 16 is positioned in the clamping groove 14, the positioning support 17 and the screen plate 15 are mainly positioned through the clamping rod 16 and the clamping groove 14, the positioning support 17 is fixedly connected to the clamping rod 16, the positioning support 17 is mainly used for positioning a rotating shaft 18, the inside of the positioning support 17 is rotationally connected with the rotating shaft 18, the top of the rotating shaft 18 is fixedly connected with a gear 20, a clamping block 25 and a tooth hole 27 are arranged, so that a crushing motor 24 is convenient to control the rotating shaft 18 to drive a crushing blade 19 to rotate, and the crushing blade 19 is fixedly connected to the circumferential surface of the rotating shaft 18;
the top fixedly connected with of base 1 handles cover 21, the top fixedly connected with electronic jar 22 of handle cover 21, electronic jar 22 mainly used control crushing motor 24 reciprocates, the loose end fixedly connected with fixed plate 23 of electronic jar 22, the bottom fixedly connected with crushing motor 24 of fixed plate 23, fixedly connected with fixture block 25 on crushing motor 24's the output shaft, and fixture block 25 is located the inside of handle cover 21, the bottom of fixture block 25 is provided with tooth hole 27, the interior top of handle cover 21 is provided with heating lamp 26, heating lamp 26 mainly carries out drying treatment to the soil sample.
The bottom fixedly connected with wheel of carousel 3 to the wheel corresponds the setting with handling section of thick bamboo 4, and the bottom of every handling section of thick bamboo 4 all is provided with two support columns 5, and the symmetry sets up in the both sides of unloading pipe 13, stop collar 10 is located the below of unloading pipe 13, stop collar 10 and test tube 11 supporting use, test tube 11 adopts polytetrafluoroethylene to make, the inside of every handling section of thick bamboo 4 all is provided with four draw-in grooves 14 and four clamping bars 16, the inside of every handling section of thick bamboo 4 all is provided with a locating support 17, and the plane shape of depression of locating support 17 is the cross, the quantity of electronic jar 22 is provided with two, and the symmetry sets up the left and right sides at crushing motor 24, gear 20 and tooth aperture 27 cooperation use.
A sample processing method for measuring metal elements in soil comprises the following specific steps: s1, firstly, selecting and dividing a rectangular stable soil area in a region where soil needs to be detected, selecting a plurality of sampling points in the rectangular stable soil area by adopting a diagonal sampling method, placing the sampled soil into a sample container, simultaneously removing branches, leaves and stones in a soil sample, and labeling;
s2, before soil samples are processed, firstly supporting the limiting ring 10 by hand, then placing the test tube 11 into the placing seat 12, loosening the limiting ring 10 after the test tube 11 is placed, positioning the test tube 11 by the limiting ring 10 under the action of the springs 8, then pouring the collected soil samples into the plurality of processing cylinders 4 in sequence, after the soil samples are placed, controlling the turntable 3 to rotate by the rotating motor 2, transferring the first processing cylinder 4 into the processing cover 21, then drying the soil samples in the processing cylinders 4 by the heating lamp 26, after the drying is finished, controlling the smashing motor 24 to move downwards by the electric cylinder 22, clamping the gear 20 into the tooth holes 27, controlling the smashing blade 19 to rotate by the smashing motor 24, smashing the soil samples, screening the smashed soil samples from the blanking pipe 13 by the screen plate 15, after the soil samples in the first processing cylinder 4 are processed, moving upwards by the electric cylinder 22 to enable the gear 20 to move out of the tooth holes 27, then controlling the turntable 3 to rotate by the rotating motor 2, repeating the steps, finally taking out the rest soil samples from the tooth holes 27, and sticking the test tubes 11 again;
s3, adding nitric acid, hydrochloric acid and hydrofluoric acid into the test tube 11, sealing, putting the test tube 11 into a super microwave digestion instrument for primary digestion, taking out the test tube 11 after cooling, adding boric acid solution, and putting the test tube into the super microwave digestion instrument again for secondary digestion;
s4, after digestion is completed, constant volume and film coating are carried out, the measurement is carried out by an inductively coupled plasma mass spectrometer, the quality is determined by using the specific mass number of the element, and the quantitative analysis is carried out by adopting an external standard method and the intensity ratio of the mass spectrum signal of the element to be measured and the mass spectrum signal of the internal standard element is in direct proportion to the concentration of the element to be measured.
The heating time of the heating lamp 26 in S2 is 10-20min, the temperature of the first digestion in S3 is 90-150 ℃, the constant temperature time is 5min, the temperature of the second digestion is 180-220 ℃, the constant temperature time is 5min, the power of the super microwave digestion instrument is 1200W, and when nitric acid, hydrochloric acid and hydrofluoric acid are added, S3 is measured by using a balance, 1.2m l nitric acid, 0.4m l hydrochloric acid, 0.4m l hydrofluoric acid and 5.0m l boric acid solution are added to each 0.05g soil sample.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (8)

1. Sample processing device for determining metallic elements in soil, comprising a base (1), characterized in that: fixedly connected with rotation motor (2) of base (1), fixedly connected with carousel (3) on the output shaft of rotation motor (2) to carousel (3) are located the top of base (1), the top of carousel (3) is provided with a plurality of processing section of thick bamboo (4), and processing section of thick bamboo (4) are through support column (5) and carousel (3) fixed connection, the bottom of processing section of thick bamboo (4) is provided with unloading pipe (13), fixedly connected with dog (6) on the periphery of support column (5), sliding connection has slider (7) on the periphery of support column (5) to slider (7) are located the top of dog (6), fixedly connected with connecting rod (9) on the lateral wall of slider (7), one end fixedly connected with spacing ring (10) of slider (7) are kept away from to connecting rod (9), the cover is equipped with spring (8) on the periphery of connecting rod (9) to spring (8) is located the top of slider (7), the top fixedly connected with of carousel (3) places seat (12), and places seat (12) below placing tube (12) and place inside seat (11) below placing;
the inside of a treatment cylinder (4) is provided with a screen plate (15), the side wall of the screen plate (15) is fixedly connected with a clamping rod (16), the inner wall of the treatment cylinder (4) is provided with a clamping groove (14), the clamping rod (16) is positioned in the clamping groove (14), the clamping rod (16) is fixedly connected with a positioning bracket (17), the inside of the positioning bracket (17) is rotationally connected with a rotating shaft (18), the top of the rotating shaft (18) is fixedly connected with a gear (20), and the circumferential surface of the rotating shaft (18) is fixedly connected with a crushing blade (19);
the utility model discloses a base, including base (1), base, fixed plate, clamping block (25) are fixed on the top fixedly connected with of base (1), the top fixedly connected with of treating cover (21) is electronic jar (22), the expansion end fixedly connected with fixed plate (23) of electronic jar (22), the bottom fixedly connected with of fixed plate (23) smashes motor (24), fixedly connected with fixture block (25) on the output shaft of smashing motor (24) to fixture block (25) are located the inside of treating cover (21), the bottom of fixture block (25) is provided with tooth hole (27), the interior top of treating cover (21) is provided with heating lamp (26).
2. A sample processing device for determining metallic elements in soil according to claim 1, wherein: the bottom of carousel (3) fixedly connected with a plurality of wheels to the wheel corresponds setting with handling section of thick bamboo (4).
3. A sample processing device for determining metallic elements in soil according to claim 1, wherein: the bottom of each treatment cylinder (4) is provided with two support columns (5) which are symmetrically arranged on two sides of the blanking pipe (13).
4. A sample processing device for determining metallic elements in soil according to claim 1, wherein: the limiting ring (10) is located below the blanking pipe (13), the limiting ring (10) is matched with the test tube (11) for use, and the test tube (11) is made of polytetrafluoroethylene.
5. A sample processing device for determining metallic elements in soil according to claim 1, wherein: four clamping grooves (14) and four clamping rods (16) are formed in each processing cylinder (4), a positioning support (17) is arranged in each processing cylinder (4), and the shape of the depression surface of the positioning support (17) is cross-shaped.
6. A sample processing device for determining metallic elements in soil according to claim 1, wherein: the number of the electric cylinders (22) is two, the electric cylinders are symmetrically arranged on the left side and the right side of the crushing motor (24), and the gears (20) are matched with the tooth holes (27).
7. A sample processing method for measuring metallic elements in soil, based on the sample processing device for measuring metallic elements in soil according to claim 1, characterized in that: the method comprises the following specific steps:
s1, firstly, selecting and dividing a rectangular stable soil area in a region where soil needs to be detected, selecting a plurality of sampling points in the rectangular stable soil area by adopting a diagonal sampling method, placing the sampled soil into a sample container, simultaneously removing branches, leaves and stones in a soil sample, and labeling;
s2, before soil samples are processed, firstly, a limiting ring (10) is supported by hands, then a test tube (11) is placed in a placing seat (12), after the test tube (11) is placed, the limiting ring (10) is loosened, at this time, the limiting ring (10) positions the test tube (11) under the action of a spring (8), then the collected soil samples are sequentially poured into a plurality of processing drums (4), after the soil samples are placed, a rotating motor (2) controls a turntable (3) to rotate, the first processing drum (4) is shifted into a processing cover (21), then a heating lamp (26) dries the soil samples in the processing drum (4), after the drying is completed, an electric cylinder (22) controls a crushing motor (24) to move downwards, a gear (20) is clamped into a tooth hole (27), the crushing motor (24) controls a crushing blade (19) to rotate, the crushed soil samples are screened from a blanking tube (13), the soil samples in the first processing drum (4) are subjected to crushing treatment, after the electric motor (24) controls the electric motor to move the gear (24) to complete the soil samples in the processing drum (4), the rest soil samples are repeatedly moved from the tooth hole (27), and then the soil samples are repeatedly processed by rotating the rotating drum (20), finally, taking out the test tube (11) and labeling again;
s3, adding nitric acid, hydrochloric acid and hydrofluoric acid into the test tube (11) and sealing the test tube, then placing the test tube (11) into a super microwave digestion instrument for primary digestion, taking out the test tube (11) after cooling, adding boric acid solution, and placing the test tube into the super microwave digestion instrument again for secondary digestion;
s4, after digestion is completed, constant volume and film coating are carried out, the measurement is carried out by an inductively coupled plasma mass spectrometer, the quality is determined by using the specific mass number of the element, and the quantitative analysis is carried out by adopting an external standard method and the intensity ratio of the mass spectrum signal of the element to be measured and the mass spectrum signal of the internal standard element is in direct proportion to the concentration of the element to be measured.
8. A sample processing method for measuring metallic elements in soil according to claim 7, wherein: the heating time of the heating lamp (26) in the step S2 is 10-20min, the temperature of the first digestion in the step S3 is 90-150 ℃, the constant temperature time is 5min, the temperature of the second digestion is 180-220 ℃, the constant temperature time is 5min, the power of the super microwave digestion instrument is 1200W, and when nitric acid, hydrochloric acid and hydrofluoric acid are added, the step S3 is measured by firstly using a balance, and 1.2ml of nitric acid, 0.4ml of hydrochloric acid, 0.4ml of hydrofluoric acid and 5.0ml of boric acid solution are added to each 0.05g of soil sample.
CN202310032504.0A 2023-01-10 2023-01-10 Sample processing method and device for measuring metal elements in soil Active CN116046495B (en)

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CN202310032504.0A CN116046495B (en) 2023-01-10 2023-01-10 Sample processing method and device for measuring metal elements in soil

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