CN111638290A - Heavy metal content detection method - Google Patents
Heavy metal content detection method Download PDFInfo
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- CN111638290A CN111638290A CN202010544569.XA CN202010544569A CN111638290A CN 111638290 A CN111638290 A CN 111638290A CN 202010544569 A CN202010544569 A CN 202010544569A CN 111638290 A CN111638290 A CN 111638290A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01—MEASURING; TESTING
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/36—Control of physical parameters of the fluid carrier in high pressure liquid systems
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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Abstract
The invention discloses a heavy metal content detection method, which comprises the steps of cleaning and filtering an article to be detected in cleaning equipment, drying the article to be detected, grinding the dried article to be detected to obtain powder of the article to be detected, treating the article to be detected in the early stage, effectively improving the detection accuracy of the article to be detected in the later stage, and detecting the heavy metal in the article to be detected in a high-efficiency and accurate manner by matching the article to be detected with equipment such as a crucible, a high-temperature furnace, an ultrasonic instrument, a heavy metal detector and the like, so that the defect that the detection result accuracy is low due to the fact that the heavy metal is easily influenced by pollutants during detection in the existing scheme is overcome; the problem of low cleanliness of a sample to be detected in the existing scheme is solved by the matching use of the box body, the base, the motor, the rotary column and the brush; the fixed column that sets up, the cooperation of first splint and second splint are used, have overcome cleaning equipment in the current scheme and have worked the not good problem of inside stability at the during operation.
Description
Technical Field
The invention relates to the technical field of heavy metal detection, in particular to a heavy metal content detection method, which is suitable for metal content detection in the fields of food and metal.
Background
The heavy metal is a metal with the density of more than 4.5g/cm3, including gold, silver, copper, iron, mercury, lead, cadmium and the like, and the heavy metal is accumulated in a human body to a certain degree to cause chronic poisoning. However, heavy metals in terms of environmental pollution mainly refer to mercury (mercury), cadmium, lead, chromium, metalloid arsenic and other heavy elements with remarkable biological toxicity, the heavy metals are very difficult to biodegrade, but can be enriched by thousands of times under the biological amplification effect of a food chain, and finally enter a human body, and the heavy metals can strongly interact with protein, enzyme and the like in the human body to lose activity, and can also be accumulated in certain organs of the human body to cause chronic poisoning; in addition, some metal products in the existing metal field have high requirements on metal elements and content, and the content of heavy metals in the metal products needs to be detected.
The existing heavy metal content detection method has certain defects: only articles in a single field can be detected, so that the detection range of heavy metals is limited; the sample to be tested can not be effectively processed before being detected, so that the sample to be tested is easily influenced by pollutants, and the test result is not accurate; and detecting the problem that the stability of the related equipment in the work is not good.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a heavy metal content detection method which comprises the following steps: according to the embodiment of the invention, on one hand, the to-be-detected article is cleaned and filtered in the cleaning equipment, dried and ground to obtain the to-be-detected article powder, the to-be-detected article is treated in the early stage, so that the detection accuracy of the to-be-detected article in the later stage can be effectively improved, the to-be-detected article is used in cooperation with equipment such as a crucible, a high-temperature furnace, an ultrasonic instrument, a heavy metal detector and the like, the detection of heavy metals in the to-be-detected article can be efficiently and accurately realized, and the defect that the detection result accuracy is low due to the fact that the heavy metals are easily influenced by pollutants during detection in the existing scheme is overcome; and can carry out heavy metal detection with metal product through handling back, can effectively improve heavy metal detection's efficiency and quality, improve the accuracy that heavy metal content detected.
On the other hand, through the matching use of the box body, the base, the motor, the rotary column and the brush, objects to be detected can be cleaned and filtered in the box body, the objects to be detected are conveyed into the box body through the inlet and the first guide pipe, the rotary column is driven to rotate anticlockwise in the box body through the motor, the brush is further driven to rotate anticlockwise in the box body, the objects to be detected in the box body are stirred and cleaned through the rotation of the brush, the objects to be detected in the box body can be prevented from being abraded through stirring and cleaning of the brushes, filtrate after stirring and cleaning is discharged through the outlet, the cleaned objects to be detected are received through the receiving port, the cleanliness of the objects to be detected can be improved through stirring and cleaning and filtering of the objects to be detected, and the problem that the cleanliness of samples to be detected in the existing scheme is not high is;
in other aspects disclosed by the embodiment of the invention, the stability of the brush in the box body can be effectively improved by the matching use of the fixed column, the first telescopic spring, the second telescopic spring and the first clamping plate and the second clamping plate, but also is convenient to install and disassemble, the fixed column penetrates into the rotating column to ensure that the fixed column rotates along with the rotating column, the first expansion spring and the second expansion spring can play a role of buffering the stirring of the brush, the fixed plate is fixed between the first clamping plate and the second clamping plate through a plurality of second fixed bolts, the rotary column is rotationally connected to the supporting underframe through a shaft collar, can effectively improve the stability of the rotating and stirring of the brush, avoid the resistance of the brush to the object to be measured in the stirring and cleaning process, make brush and rotary column separation, overcome cleaning equipment in the current scheme in the not good problem of stability of during operation inside.
The purpose of the invention can be realized by the following technical scheme:
a heavy metal content detection method comprises the following steps:
the method comprises the following steps: the method comprises the following steps of obtaining an article to be detected, conveying the article to be detected into a box body, conveying clear water into the box body through an inlet and a first guide pipe, driving a rotary column to rotate anticlockwise through a motor, driving a fixing plate and a hairbrush to rotate anticlockwise, stirring and cleaning the article to be detected in the box body through the hairbrush, and collecting the cleaned article to be detected through a third guide pipe and a containing port;
drying the cleaned object to be detected, and grinding the dried object to be detected to obtain powder of the object to be detected;
step two: adding 150-200 parts of to-be-detected object powder into a crucible according to parts by weight, adding 1-2 parts of nitric acid, heating to evaporate to dryness, adding 1-2 parts of concentrated sulfuric acid of a to-be-detected sample at a speed of 11-14 drops/min after no steam is generated, and heating the to-be-detected object powder in the crucible;
the operation of the heat treatment was: heating at a speed of 20 ℃/min in 0-10 min, heating at a speed of 15 ℃/min in 10-20 min, heating at a speed of 10 ℃/min in 20-25 min, heating at a speed of 5 ℃/min in 25-30 min, heating at a speed of 2 ℃/min in 30-35 min, and keeping constant temperature after 35min until the treatment is finished;
step three: adding the treated powder of the article to be detected into a high-temperature furnace for three times of ashing, wherein the first time of ashing is at 400-450 ℃ and is heated for 10-20 min, the second time of ashing is at 450-550 ℃ and is heated for 30-40 min, the third time of ashing is at 550-650 ℃ and is heated for 10-20 min, and after the three times of ashing, taking out the powder of the article to be detected and naturally cooling the powder to room temperature;
step four: adding hydrochloric acid with the same amount as the nitric acid in the step two into the sample subjected to ashing in the step three, soaking for 5-8 min in a sealed manner, adding 8-10 parts of methanol-water mixed solution of an article to be detected into the soaking solution, wherein the methanol-water mixed solution is a mixed melting solution of methanol and ultrapure water, and the weight ratio of the methanol to the ultrapure water is 1: 1, placing the mixture in an ultrasonic instrument for ultrasonic treatment for 20-25 min, adjusting the pH value to be neutral, transferring the mixture into a volumetric flask, and fixing the volume by using a methanol-water mixed solution;
step five: and detecting the treated object to be detected by adopting a heavy metal detector, filtering the object to be detected by using a permeable membrane of 0.2-0.3 mu m before detection, and obtaining the content of the heavy metal according to the display of the heavy metal detector.
As a further scheme of the invention: the cleaning equipment comprises a box body, a top cover is fixedly arranged at the upper end of the box body, a fixed seat is fixedly arranged at the upper end of the top cover, the upper end of the fixed seat is provided with a motor and a shaft seat, the motor is positioned at one side of the shaft seat, the inside of the shaft seat is connected with a rotating column, the rotary column penetrates through the fixed seat and the top cover to the interior of the box body, the lower end of the box body is fixedly provided with a base, a balance frame is fixedly arranged on the outer surface of the rotary column near the upper part, a plurality of fixed columns penetrate through the inner part of the rotary column, a first expansion spring and a second expansion spring are slidably mounted on the outer surface of the fixed column, the first expansion spring is positioned at one side of the second expansion spring, one end of the fixing column is fixedly connected with a first clamping plate and a second clamping plate, the first clamping plate is located in front of the second clamping plate, and a plurality of second fixing bolts are fixedly connected between the first clamping plate and the second clamping plate.
As a further scheme of the invention: fixedly connected with fixed plate between first splint and the second splint, one side fixed mounting that first splint were kept away from to the fixed plate has a plurality of brush, and a plurality of second gim peg runs through in the inside of fixed plate, the fixed plate passes through a plurality of second gim peg and first splint, second splint fixed connection, the upper end fixed mounting of fixed plate has the change.
As a further scheme of the invention: the outer surface of the rotary column is fixedly provided with a shaft collar at a position close to the lower part, the inner surface of the base is fixedly provided with a supporting bottom frame, the shaft collar is positioned in the supporting bottom frame at a position close to the middle, and the rotary column is rotatably connected with the supporting bottom frame through the shaft collar.
As a further scheme of the invention: the upper end of the top cover is fixedly provided with a plurality of first fixing bolts, the outer surface of the box body is fixedly provided with a first supporting leg, a second supporting leg and a third supporting leg at a position close to the lower part, and the shape formed by the first supporting leg, the second supporting leg and the third supporting leg in a surrounding mode is triangular.
As a further scheme of the invention: the outer surface of the box body is fixedly connected with a first guide pipe and a case close to the upper part, the first guide pipe is located on one side of the case, an inlet is formed in one end, far away from the case, of the first guide pipe, a first instrument and a second instrument are fixedly mounted on the outer surface of the case, and the first instrument is located on one side of the second instrument.
As a further scheme of the invention: the outer surface of the box body is fixedly connected with a second guide pipe at a position close to the lower part, and one end, far away from the box body, of the second guide pipe is provided with an outlet.
As a further scheme of the invention: the lower extreme of base is connected with the third pipe, the fixed surface of third pipe installs solid fixed ring, the fixed position that the surface of third pipe is close to the top installs the connecting seat, the upper end fixed mounting of connecting seat has the control valve, the one end that the base was kept away from to the third pipe is provided with the storage port.
The embodiment of the invention discloses the following beneficial effects:
(1) on one hand, the embodiment of the invention discloses that the heavy metal detection is carried out on the metal product through the heavy metal detector after the metal product is washed, dried and heated, so that the efficiency and the quality of the heavy metal detection can be effectively improved, the accuracy of the heavy metal content detection is improved, and the problem of low detection accuracy caused by the fact that the metal is easily influenced by pollutants in the existing scheme is solved; the heavy metal detection device has the advantages that articles to be detected can be cleaned and filtered in cleaning equipment, the articles to be detected are dried, the dried articles to be detected are ground to obtain powder of the articles to be detected, the articles to be detected are treated in an early stage, the detection accuracy of the articles to be detected in a later stage can be effectively improved, the articles to be detected can be used in cooperation with equipment such as a crucible, a high-temperature furnace, an ultrasonic instrument and a heavy metal detector, the heavy metal in the articles to be detected can be efficiently and accurately detected, the defect that the detection result accuracy is low due to the fact that the articles are easily affected by pollutants when being detected for detecting the heavy metal in the existing scheme is overcome, and the purpose that the heavy metal detection can be carried out in the fields of;
(2) according to the embodiment of the invention, on one hand, through the matched use of the box body, the base, the motor, the rotary column and the brush, an article to be detected can be cleaned and filtered in the box body, the article to be detected is conveyed into the box body through the inlet and the first guide pipe, the rotary column is driven to rotate anticlockwise in the box body through the motor, the brush is further driven to rotate anticlockwise in the box body, the article to be detected in the box body is stirred and cleaned through the rotation of the brush, the abrasion of the article to be detected can be avoided through the stirring and cleaning of the article to be detected by the brush, filtrate after the stirring and cleaning is discharged through the outlet, the cleaned article to be detected is accommodated through the accommodating port, and through the stirring, cleaning and filtering of the article to be detected, the cleanliness of;
(3) in other aspects disclosed by the embodiment of the invention, the fixing column, the first expansion spring, the second expansion spring and the matching use of the first clamping plate and the second clamping plate can effectively improve the stability of the brush in the box body and are convenient to install and disassemble, the fixing column penetrates into the rotating column to enable the fixing column to rotate along with the rotating column, the first expansion spring and the second expansion spring can play a role in buffering the stirring of the brush, the fixing plate is fixed between the first clamping plate and the second clamping plate through a plurality of second fixing bolts, and the rotating column is rotatably connected to the supporting underframe through a shaft collar, so that the rotating and stirring stability of the brush can be effectively improved, and the defect that the brush is separated from the rotating column due to the resistance of an object to be detected in the stirring and cleaning processes is avoided.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a schematic view of the structure of a cleaning apparatus of the present invention;
FIG. 2 is a schematic view showing the internal structure of the cleaning apparatus of the present invention;
FIG. 3 is a schematic diagram of the internal side view of the cleaning apparatus of the present invention;
FIG. 4 is a schematic view of the connection structure of the fixing post and the first clamping plate of the present invention;
fig. 5 is an enlarged schematic view of fig. 2 at a in the present invention.
In the figure: 1. a box body; 2. a base; 3. a top cover; 4. a fixed seat; 5. a motor; 6. a shaft seat; 7. a chassis; 8. a first meter; 9. a second meter; 10. a first conduit; 11. an inlet; 12. a second conduit; 13. an outlet; 14. a third conduit; 15. a fixing ring; 16. a connecting seat; 17. a receiving opening; 18. a first leg; 19. a second leg; 20. a third leg; 21. a first securing latch; 22. turning the column; 23. a balancing stand; 24. rotating the ring; 25. fixing a column; 26. a support chassis; 27. a collar; 28. a control valve; 29. a first extension spring; 30. a second extension spring; 31. a first splint; 32. a second splint; 33. a second securing latch; 34. a fixing plate; 35. and a brush.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1-5, the present embodiment is a method for detecting heavy metal content, including the following steps:
the method comprises the following steps: the method comprises the steps of obtaining an article to be detected, conveying the article to be detected into a box body 1, conveying clean water into the box body 1 through an inlet 11 and a first guide pipe 10, driving a rotary column 22 to rotate anticlockwise through a motor 5, driving a fixing plate 34 and a hairbrush 35 to rotate anticlockwise through the rotary column 22, stirring and cleaning the article to be detected in the box body 1 through the hairbrush 35, and collecting the cleaned article to be detected through a third guide pipe 14 and a containing port 17;
drying the cleaned object to be detected, and grinding the dried object to be detected to obtain powder of the object to be detected;
step two: adding 150-200 parts of to-be-detected object powder into a crucible according to parts by weight, adding 1-2 parts of nitric acid, heating to evaporate to dryness, adding 1-2 parts of concentrated sulfuric acid at a speed of 11-14 drops/min after no steam is generated, and heating the to-be-detected object powder in the crucible;
the operation of the heat treatment was: heating at a speed of 20 ℃/min in 0-10 min, heating at a speed of 15 ℃/min in 10-20 min, heating at a speed of 10 ℃/min in 20-25 min, heating at a speed of 5 ℃/min in 25-30 min, heating at a speed of 2 ℃/min in 30-35 min, and keeping constant temperature after 35min until the treatment is finished;
step three: adding the treated powder of the article to be detected into a high-temperature furnace for three times of ashing, wherein the first time of ashing is at 400-450 ℃ and is heated for 10-20 min, the second time of ashing is at 450-550 ℃ and is heated for 30-40 min, the third time of ashing is at 550-650 ℃ and is heated for 10-20 min, and after the three times of ashing, taking out the powder of the article to be detected and naturally cooling the powder to room temperature;
step four: adding hydrochloric acid with the same amount as the nitric acid in the step two into the sample subjected to ashing in the step three, sealing and soaking for 5-8 min, then adding 8-10 parts of methanol-water mixed solution into the soaking solution, wherein the methanol-water mixed solution is a mixed melt solution of methanol and ultrapure water, and the weight ratio of the methanol to the ultrapure water is 1: 1, placing the mixture in an ultrasonic instrument for ultrasonic treatment for 20-25 min, adjusting the pH value to be neutral, transferring the mixture into a volumetric flask, and fixing the volume by using a methanol-water mixed solution;
step five: and detecting the treated object to be detected by adopting a heavy metal detector, filtering the object to be detected by using a permeable membrane of 0.2-0.3 mu m before detection, and obtaining the content of the heavy metal according to the display of the heavy metal detector.
The cleaning equipment comprises a box body 1, a top cover 3 is fixedly installed at the upper end of the box body 1, a fixed seat 4 is fixedly installed at the upper end of the top cover 3, a motor 5 and a shaft seat 6 are installed at the upper end of the fixed seat 4, the motor 5 is positioned on one side of the shaft seat 6, a rotary column 22 is connected inside the shaft seat 6, the rotary column 22 penetrates through the fixed seat 4 and the top cover 3 to the inside of the box body 1, a base 2 is fixedly installed at the lower end of the box body 1, a balance frame 23 is fixedly installed at a position, close to the upper part, of the outer surface of the rotary column 22, a plurality of fixed columns 25 penetrate through the inside of the rotary column 22, a first telescopic spring 29 and a second telescopic spring 30 are installed on the outer surface of each fixed column 25 in a sliding mode, the first telescopic spring 29 is positioned on one side of the second telescopic spring 30, first splint 31 is located the place ahead of second splint 32, a plurality of second gim peg 33 of fixedly connected with between first splint 31 and the second splint 32, can play the effect of buffering to the stirring of brush 35 through first expanding spring 29 and second expanding spring 30, fixed plate 34 is fixed between first splint 31 and second splint 32 through a plurality of second gim peg 33, rotate the post 22 through the axle collar 27 and connect on supporting chassis 26, can effectively improve the stability that brush 35 rotated the stirring, avoid brush 35 because the resistance of the article that awaits measuring in the stirring cleaning process, make brush 35 and post 22 separate.
Fixedly connected with fixed plate 34 between first splint 31 and the second splint 32, one side fixed mounting that first splint 31 was kept away from to fixed plate 34 has a plurality of brush 35, and a plurality of second gim peg 33 runs through in the inside of fixed plate 34, fixed plate 34 can effectively improve the stability of fixed plate 34 through a plurality of second gim peg 33 and first splint 31, second splint 32 fixed connection, the upper end fixed mounting of fixed plate 34 has change 24, starter motor 5, and motor 5 drives the column 22 anticlockwise rotation, and column 22 drives fixed plate 34 and brush 35 and carries out anticlockwise rotation, and brush 35 rotates the in-process and stirs the washing to the article that awaits measuring in the box 1, and pollutant in the article that awaits measuring and the article separation that awaits measuring.
A collar 27 is fixedly arranged on the outer surface of the rotary column 22 close to the lower part, a supporting bottom frame 26 is fixedly arranged on the inner surface of the base 2, the collar 27 is arranged in the supporting bottom frame 26 close to the middle, and the rotary column 22 is rotatably connected with the supporting bottom frame 26 through the collar 27.
The upper end fixed mounting of top cap 3 has a plurality of first gim peg 21, the position fixed mounting that the surface of box 1 is close to the below has first stabilizer blade 18, second stabilizer blade 19 and third stabilizer blade 20, the shape that first stabilizer blade 18, second stabilizer blade 19 and third stabilizer blade 20 enclose is triangle-shaped, can effectively improve the stability of box 1.
A plurality of the surface of 1 of box is close to the position fixedly connected with first pipe 10 and quick-witted case 7 of top, first pipe 10 is located one side of quick-witted case 7, the one end that quick-witted case 7 was kept away from to first pipe 10 is provided with import 11, the fixed surface of quick-witted case 7 installs first instrument 8 and second instrument 9, first instrument 8 is located one side of second instrument 9, first instrument 8 and second instrument 9 are used for detecting the operating conditions of pressure and motor 5 in the box 1.
The outer surface of the box body 1 is fixedly connected with a second conduit 12 at a position close to the lower part, one end of the second conduit 12 far away from the box body 1 is provided with an outlet 13, and the outlet 13 is used for discharging filtrate.
The lower extreme of base 2 is connected with third pipe 14, the outer fixed surface of third pipe 14 installs solid fixed ring 15, the position fixed mounting that the surface of third pipe 14 is close to the top has connecting seat 16, the upper end fixed mounting of connecting seat 16 has control valve 28, and control valve 28 plays the collection of the article that awaits measuring after the control washing, the one end that base 2 was kept away from to third pipe 14 is provided with storage port 17, and the filtrating after will wasing is discharged through second pipe 12 and export 13, and the article that awaits measuring after will wasing is collected through third pipe 14 and storage port 17.
Example 2
The method comprises the following steps: obtain the article that awaits measuring, wherein, the article that awaits measuring can be the rice, places the article that awaits measuring and washs and filter in cleaning equipment, and concrete step includes: conveying an object to be detected into the box body 1, conveying clean water into the box body 1 through the inlet 11 and the first guide pipe 10, starting the motor 5 through the case 7, driving the rotary column 22 to rotate anticlockwise by the motor 5, driving the fixing plate 34 and the hairbrush 35 to rotate anticlockwise by the rotary column 22, stirring and cleaning the object to be detected in the box body 1 in the rotating process of the hairbrush 35, buffering the rotating stirring of the hairbrush 35 by the first expansion spring 29 and the second expansion spring 30, separating pollutants in the object to be detected from the object to be detected, discharging the cleaned filtrate through the second guide pipe 12 and the outlet 13, collecting the cleaned object to be detected through the third guide pipe 14 and the containing port 17, and controlling the control valve 28 to control the collection of the cleaned object to be detected;
drying the cleaned object to be detected, and grinding the dried object to be detected to obtain powder of the object to be detected;
step two: adding 200 parts of powder of an object to be detected into a crucible according to the parts by weight, adding 2 parts of nitric acid, heating to evaporate to dryness, adding 2 parts of concentrated sulfuric acid at the speed of 11 drops/min after no steam is generated, and heating the powder of the object to be detected in the crucible;
the operation of the heat treatment was: heating at 20 deg.C/min for 10min, at 15 deg.C/min for 20min, at 10 deg.C/min for 25min, at 5 deg.C/min for 30min, at 2 deg.C/min for 35min, and maintaining the constant temperature after 35min until the treatment is finished;
step three: adding the treated powder of the article to be detected into a high-temperature furnace for three times of ashing, wherein the first time of ashing is at 450 ℃ and heating for 20min, the second time of ashing is at 550 ℃ and heating for 40min, the third time of ashing is at 650 ℃ and heating for 20min, and after the three times of ashing is finished, taking out the powder of the article to be detected and naturally cooling the powder to room temperature;
step four: adding hydrochloric acid with the same amount as the nitric acid in the step two into the sample subjected to ashing in the step three, sealing and soaking for 8min, then adding 10 parts of methanol-water mixed solution into the soaking solution, wherein the methanol-water mixed solution is a mixed melting solution of methanol and ultrapure water, and the weight ratio of the methanol to the ultrapure water is 1: 1, placing the mixture in an ultrasonic instrument for ultrasonic treatment for 25min, adjusting the pH value to be neutral, transferring the mixture into a volumetric flask, and fixing the volume by using a methanol-water mixed solution;
step five: detecting the processed object to be detected by adopting a heavy metal detector, wherein the heavy metal detector can be an ultra-high performance liquid chromatograph, the type of the ultra-high performance liquid chromatograph can be LC600B, and the chromatographic conditions of the ultra-high performance liquid chromatograph are as follows: the chromatographic column is ACQUITYUPLC BEH C18, the specification of the chromatographic column is 1.7 μm and 2.1 × 50mm, the mobile phase is water-methanol gradient elution, the time is 0, 1, 2, 3, 4, 7, 8 and 11 minutes respectively, the mass percentages of water and methanol are respectively 100: 0,100: 0,99: 1,95: 5,85: 15, 88: 12, 91: 9,100: 0, detecting the wavelength of 254nm, the flow rate of 0.5m L/min and the sample volume of 5 mu L, filtering the object to be detected by using a permeable membrane with the thickness of 0.3 mu m before detection, and obtaining the heavy metal content according to the display of a heavy metal detector, wherein the heavy metal detector displays that the lead content is 0.0152mg/kg, the arsenic content is 0.006mg/kg and the cadmium content is 0.0248 mg/kg.
Several aspects disclosed in embodiments of the invention: when the article to be detected is a metal product, the metal product is cleaned and filtered in the cleaning equipment and dried, the metal product is treated in an early stage, so that the detection accuracy of the metal product in a later stage can be effectively improved, and the heavy metal detector can be a spectrum analyzer by matching with the heavy metal detector, so that the detection of the heavy metal in the metal product can be efficiently and accurately realized, and the defect that the detection result accuracy is low due to the fact that the metal product is easily influenced by pollutants when the heavy metal is detected in the existing scheme is overcome;
when an article to be detected is food, the article to be detected is cleaned and filtered in cleaning equipment and dried, the dried article to be detected is ground to obtain powder of the article to be detected, the accuracy of later-stage detection of the article to be detected can be effectively improved by processing the article to be detected in an earlier stage, the article to be detected is matched with equipment such as a crucible, a high-temperature furnace, an ultrasonic instrument, a heavy metal detector and the like for use, the heavy metal detector can be a spectrum analyzer or an ultra-high performance liquid chromatograph, the heavy metal in the article to be detected can be detected in a high-efficiency and accurate mode, and the defect that the accuracy of a detection result is low due to the fact that the heavy metal is easily influenced by pollutants when the heavy metal is detected by the food in the existing scheme;
through the matching use of the box body 1, the base 2, the motor 5, the rotary column 22 and the brush 35, the article to be tested can be cleaned and filtered in the box body 1, the article to be tested is conveyed into the box body 1 through the inlet 11 and the first guide pipe 10, the model of the motor 5 can be YE3-30KW, the rotating column 22 is driven by the motor 5 to rotate anticlockwise in the box body 1, thereby driving the brush 35 to rotate counterclockwise in the case 1, and by the rotation of the brush 35, the objects to be measured in the box body 1 are stirred and cleaned, the brush 35 can stir and clean the objects to be measured so as to avoid abrasion to the objects to be measured, filtrate after stirring and cleaning is discharged through the outlet 13, the cleaned objects to be measured are received through the receiving port 17, and through stirring, cleaning and filtering the objects to be measured, the cleanliness of the object to be detected can be improved, and the problem of low cleanliness of a sample to be detected in the existing scheme is solved;
the stability of the brush in the box body 1 can be effectively improved through the matching use of the fixed column 25, the first expansion spring 29, the second expansion spring 30, the first clamping plate 31 and the second clamping plate 32, and is convenient for installation and disassembly, the fixed column 25 penetrates into the rotating column 22, so that the fixed column 25 rotates along with the rotating column 22, the first and second extension springs 29 and 30 can buffer the stirring of the brush 35, the fixing plate 34 is fixed between the first and second clamping plates 31 and 32 by a plurality of second fixing bolts 33, the stability of the rotating and stirring of the brush 35 can be effectively improved, the rotating column 22 is rotatably connected on the supporting underframe 26 through the shaft collar 27, the problem that the brush 35 is not easy to rotate and stir due to the resistance of the object to be measured in the stirring and cleaning process is avoided, the brush 35 is separated from the rotary column 22, and the problem of poor stability of the cleaning equipment in the prior art during working is solved.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (8)
1. The heavy metal content detection method is characterized by comprising the following steps:
the method comprises the following steps: the method comprises the steps of obtaining an article to be detected, conveying the article to be detected to the inside of a box body (1), conveying clear water to the inside of the box body (1) through an inlet (11) and a first guide pipe (10), driving a rotary column (22) to rotate anticlockwise through a motor (5), driving a fixing plate (34) and a brush (35) to rotate anticlockwise through the rotary column (22), stirring and cleaning the article to be detected in the box body (1) through the brush (35), and collecting the cleaned article to be detected through a third guide pipe (14) and a containing port (17);
drying the cleaned object to be detected, and grinding the dried object to be detected to obtain powder of the object to be detected;
step two: adding 150-200 parts of to-be-detected object powder into a crucible according to parts by weight, adding 1-2 parts of nitric acid, heating to evaporate to dryness, adding 1-2 parts of concentrated sulfuric acid at a speed of 11-14 drops/min after no steam is generated, and heating the to-be-detected object powder in the crucible;
the operation of the heat treatment was: heating at a speed of 20 ℃/min in 0-10 min, heating at a speed of 15 ℃/min in 10-20 min, heating at a speed of 10 ℃/min in 20-25 min, heating at a speed of 5 ℃/min in 25-30 min, heating at a speed of 2 ℃/min in 30-35 min, and keeping constant temperature after 35min until the treatment is finished;
step three: adding the treated powder of the article to be detected into a high-temperature furnace for three times of ashing, wherein the first time of ashing is at 400-450 ℃ and is heated for 10-20 min, the second time of ashing is at 450-550 ℃ and is heated for 30-40 min, the third time of ashing is at 550-650 ℃ and is heated for 10-20 min, and after the three times of ashing, taking out the powder of the article to be detected and naturally cooling the powder to room temperature;
step four: adding hydrochloric acid with the same amount as the nitric acid in the step two into the sample subjected to ashing in the step three, sealing and soaking for 5-8 min, then adding 8-10 parts of methanol-water mixed solution into the soaking solution, wherein the methanol-water mixed solution is a mixed melt solution of methanol and ultrapure water, and the weight ratio of the methanol to the ultrapure water is 1: 1, placing the mixture in an ultrasonic instrument for ultrasonic treatment for 20-25 min, adjusting the pH value to be neutral, transferring the mixture into a volumetric flask, and fixing the volume by using a methanol-water mixed solution;
step five: and detecting the treated object to be detected by adopting a heavy metal detector, filtering the object to be detected by using a permeable membrane of 0.2-0.3 mu m before detection, and obtaining the content of the heavy metal according to the display of the heavy metal detector.
2. The heavy metal content detection method according to claim 1, wherein the cleaning equipment comprises a box body (1), a top cover (3) is fixedly mounted at the upper end of the box body (1), a fixed seat (4) is fixedly mounted at the upper end of the top cover (3), a motor (5) and a shaft seat (6) are mounted at the upper end of the fixed seat (4), the motor (5) is located on one side of the shaft seat (6), a rotating column (22) is connected to the inside of the shaft seat (6), the rotating column (22) penetrates through the fixed seat (4) and the top cover (3) to the inside of the box body (1), a base (2) is fixedly mounted at the lower end of the box body (1), a balance frame (23) is fixedly mounted at a position, close to the upper side, on the outer surface of the rotating column (22), a plurality of fixed columns (25) penetrate through the inside of the rotating column (22), and a first expansion spring (29) and a second expansion spring (25) are slidably mounted on 30) The first telescopic spring (29) is located on one side of the second telescopic spring (30), one end of the fixing column (25) is fixedly connected with a first clamping plate (31) and a second clamping plate (32), the first clamping plate (31) is located in front of the second clamping plate (32), and a plurality of second fixing bolts (33) are fixedly connected between the first clamping plate (31) and the second clamping plate (32).
3. The heavy metal content detection method according to claim 2, wherein a fixing plate (34) is fixedly connected between the first clamping plate (31) and the second clamping plate (32), a plurality of brushes (35) are fixedly installed on one side, away from the first clamping plate (31), of the fixing plate (34), a plurality of second fixing bolts (33) penetrate through the fixing plate (34), the fixing plate (34) is fixedly connected with the first clamping plate (31) and the second clamping plate (32) through the plurality of second fixing bolts (33), and a rotating ring (24) is fixedly installed at the upper end of the fixing plate (34).
4. The heavy metal content detection method according to claim 2, wherein a collar (27) is fixedly installed at a position, close to the lower part, of the outer surface of the rotary column (22), a supporting chassis (26) is fixedly installed at the inner surface of the base (2), the collar (27) is located at a position, close to the middle, inside the supporting chassis (26), and the rotary column (22) is rotatably connected with the supporting chassis (26) through the collar (27).
5. The method for detecting the content of the heavy metal according to claim 2, wherein a plurality of first fixing bolts (21) are fixedly installed at the upper end of the top cover (3), a first supporting leg (18), a second supporting leg (19) and a third supporting leg (20) are fixedly installed at positions, close to the lower part, of the outer surface of the box body (1), and the shape defined by the first supporting leg (18), the second supporting leg (19) and the third supporting leg (20) is triangular.
6. The heavy metal content detection method according to claim 2, wherein a first guide pipe (10) and a case (7) are fixedly connected to positions, close to the upper part, of the outer surfaces of the plurality of cases (1), the first guide pipe (10) is located on one side of the case (7), an inlet (11) is formed in one end, far away from the case (7), of the first guide pipe (10), a first instrument (8) and a second instrument (9) are fixedly installed on the outer surfaces of the case (7), and the first instrument (8) is located on one side of the second instrument (9).
7. The method for detecting the content of the heavy metal according to claim 2, wherein a second conduit (12) is fixedly connected to a position, close to the lower part, of the outer surface of the box body (1), and an outlet (13) is formed in one end, far away from the box body (1), of the second conduit (12).
8. The heavy metal content detection method according to claim 2, wherein a third guide pipe (14) is connected to the lower end of the base (2), a fixing ring (15) is fixedly mounted on the outer surface of the third guide pipe (14), a connecting seat (16) is fixedly mounted on the outer surface of the third guide pipe (14) at a position close to the upper side, a control valve (28) is fixedly mounted at the upper end of the connecting seat (16), and a containing opening (17) is formed in one end, far away from the base (2), of the third guide pipe (14).
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013064603A (en) * | 2011-09-15 | 2013-04-11 | Gunma Univ | Heavy metal analyzer and heavy metal analysis method |
| CN106970170A (en) * | 2017-06-10 | 2017-07-21 | 唐玉乐 | The detection method of heavy metal in a kind of ourishing rice flour |
| CN207528522U (en) * | 2017-10-17 | 2018-06-22 | 深圳市通量检测科技有限公司 | A kind of food inspection pomaceous fruits fruit sample pretreatment unit |
| CN207832779U (en) * | 2018-02-24 | 2018-09-07 | 上海谱实生态环境科技有限公司 | A kind of heavy-metal residual detection device |
| CN109959728A (en) * | 2017-12-26 | 2019-07-02 | 湖南泰华科技检测有限公司 | The detection method of the ion containing heavy metal copper in a kind of foodstuff samples |
| CN210474876U (en) * | 2019-03-18 | 2020-05-08 | 广东贝源检测技术股份有限公司 | Soil heavy metal monitor |
| CN210720279U (en) * | 2019-04-24 | 2020-06-09 | 王璐 | Device for measuring heavy metal content in food |
-
2020
- 2020-06-15 CN CN202010544569.XA patent/CN111638290A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013064603A (en) * | 2011-09-15 | 2013-04-11 | Gunma Univ | Heavy metal analyzer and heavy metal analysis method |
| CN106970170A (en) * | 2017-06-10 | 2017-07-21 | 唐玉乐 | The detection method of heavy metal in a kind of ourishing rice flour |
| CN207528522U (en) * | 2017-10-17 | 2018-06-22 | 深圳市通量检测科技有限公司 | A kind of food inspection pomaceous fruits fruit sample pretreatment unit |
| CN109959728A (en) * | 2017-12-26 | 2019-07-02 | 湖南泰华科技检测有限公司 | The detection method of the ion containing heavy metal copper in a kind of foodstuff samples |
| CN207832779U (en) * | 2018-02-24 | 2018-09-07 | 上海谱实生态环境科技有限公司 | A kind of heavy-metal residual detection device |
| CN210474876U (en) * | 2019-03-18 | 2020-05-08 | 广东贝源检测技术股份有限公司 | Soil heavy metal monitor |
| CN210720279U (en) * | 2019-04-24 | 2020-06-09 | 王璐 | Device for measuring heavy metal content in food |
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