Method for detecting content of boron in soil and sediment

Abstract

The invention belongs to the technical field of chemical detection, and particularly relates to a method for detecting the content of boron in soil and sediment, which comprises the following detection methods: S1, weighing a sample and putting the sample into a digestion tank; s2, adding a digestion solution into the digestion tank; s3, after uniform stirring, putting the digestion tank into a microwave digestion instrument for microwave digestion; s4, after digestion is completed, closing the microwave digestion instrument, and after the digestion tank is cooled to the room temperature, filtering to remove precipitates; s5, transferring the digestion solution into a volumetric flask, and fixing the volume for subsequent analysis; and S6, analyzing the digestion solution by using ICP-OES / MS (Inductively Coupled Plasma-Optical Emission According to the method for detecting the boron content in the soil and the sediment, ammonium fluoride is used for replacing hydrofluoric acid in boron detection of the soil and the sediment, use of toxic reagents is reduced, mannitol is added, a stable complex is formed by mannitol and boron, and the recovery rate of boron is increased.

Description

Technical Field

[0001] The present invention relates to the technical field of chemical detection, and in particular to a method for detecting boron content in soil and sediment. Background Art

[0002] Currently, boron content in soil and sediment is typically detected using acid digestion to release boron from the sample matrix. Acid digestion involves decomposing the sample using various acids, such as aqua regia, hydrochloric acid, nitric acid, hydrofluoric acid, and perchloric acid. The digestion solution is selected based on the sample's properties; concentrated nitric acid, hydrofluoric acid, or a mixture of these acids is commonly used. This method can result in boron loss, particularly when hydrofluoric acid is used. Hydrofluoric acid is highly toxic and can cause severe burns upon skin contact. It is also volatile, leading to boron loss. Summary of the Invention

[0003] Based on the above-mentioned existing technical problems, the present invention proposes a method for detecting the boron content in soil and sediment.

[0004] The present invention proposes a method for detecting boron content in soil and sediment, comprising the following detection method: S1. Weigh the sample and place it into the digestion tank.

[0005] S2. Add digestion solution into the digestion tank.

[0006] S3. After stirring evenly, place the digestion tank into a microwave digester for microwave digestion.

[0007] S4. After digestion is completed, turn off the microwave digester, wait for the digestion tank to cool to room temperature, and then filter to remove the precipitate.

[0008] S5. Transfer the digestion solution to a volumetric flask and adjust the volume for subsequent analysis.

[0009] S6. Analyze the digestion solution using ICP-OES / MS.

[0010] It also includes a box body and a support frame arranged inside the box body. The digestion tank is inserted into the surface of the support frame. The inside of the box body is respectively provided with a material taking mechanism and a filtering mechanism.

[0011] Wherein, the material taking mechanism includes a grinding basin for grinding the collected samples and a sampling plate with a first filter screen provided on the upper surface.

[0012] Wherein, the filtering mechanism includes a second filter screen arranged inside the volumetric flask.

[0013] Preferably, the digestion solution is a mixture of concentrated nitric acid, ammonium fluoride and mannitol.

[0014] Preferably, the material-taking mechanism also includes support plates symmetrically installed on the upper surface of the support frame, and connecting rods are installed on the surface of the support plates through bearings. The free ends of two connecting rods are fixedly connected to the surface of the grinding basin, and a deflection motor is fixedly installed on the surface of one of the support plates, and one end of the output shaft of the deflection motor is fixedly sleeved with one end of one of the connecting rods through a coupling.

[0015] Preferably, the sampling plate is located on the upper surface of the support frame and is arranged on the lower side of the grinding basin. The upper surface of the first filter screen is installed with square clips distributed in a circular array, and the inner surface of the square clips is slidably connected to the surface of the sampling plate.

[0016] Preferably, a weight sensor is embedded in the upper surface of the support frame, and the sampling tray is located in the center above the weight sensor.

[0017] Preferably, a concentrated nitric acid bottle, an ammonium fluoride bottle and a mannitol bottle are placed in sequence on one side of the upper surface of the support frame, and the bottle mouths of the concentrated nitric acid bottle, the ammonium fluoride bottle and the mannitol bottle are all provided with droppers.

[0018] Preferably, two feed ports are provided on the upper surface of the digestion tank, and sealing covers are threadedly sleeved on the surfaces of the feed ports. A stirring motor is provided on the upper surface of the digestion tank, and a stirring rod is installed on the inner top wall of the digestion tank through a bearing. One end of the output shaft of the stirring motor passes through the digestion tank and is fixedly sleeved on the upper end of the stirring rod.

[0019] Preferably, the filtering mechanism also includes a slide groove opened on the surface of the volumetric flask, the surface of the second filter screen is slidably engaged with the inner wall of the slide groove, the surface of the second filter screen is fixedly connected to a handle, a rotating shaft is installed in the center of the upper surface of the second filter screen through a bearing, a brush is fixedly sleeved on the surface of the rotating shaft, the lower surface of the brush is in contact with the surface of the second filter screen, and a support plate is provided on the upper surface of the brush, and one side surface of the support plate is fixedly connected to one side surface of the handle.

[0020] Preferably, an L-shaped bracket is installed on the surface of the volumetric flask, a drive shaft is installed on the surface of the L-shaped bracket through a bearing, a drive motor is fixedly installed on the upper surface of the L-shaped bracket, and one end of the output shaft of the drive motor is fixedly sleeved with one end of the drive shaft.

[0021] Preferably, a telescopic rod is fixedly sleeved on the outer surface of the driving shaft, a servo motor is fixedly mounted on the upper surface of one end of the telescopic rod, one end of the output shaft of the servo motor passes through the telescopic rod and is fixedly sleeved on a driving gear, two pushing cylinders are installed on the upper surface of the support plate, one end of the piston rod of the pushing cylinder is fixedly connected to a tapered sleeve, a driven gear is fixedly sleeved on the surface of the rotating shaft, and the driven gear is meshed with the driving gear.

[0022] The beneficial effects of the present invention are: 1. By using ammonium fluoride instead of hydrofluoric acid in boron detection in soil and sediment, the use of toxic reagents can be reduced, and mannitol can be added to form a stable complex with boron, thereby improving the recovery rate of boron.

[0023] 2. By setting up a material taking mechanism, it is easy to control the amount of sample and digestion solution taken, thereby ensuring that the sample can be completely decomposed.

[0024] 3. By setting up a filtering mechanism, it is convenient to filter and fix the volume of the mixed and digested liquid, which is convenient for subsequent analysis and detection. At the same time, the servo motor is used to drive the brush to rotate, and the tapered sleeve is used to prevent the liquid from being retained on the brush and the driven gear. It not only does not hinder the filtering efficiency, but also can clean the surface of the second filter. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is a schematic diagram of a method for detecting boron content in soil and sediment proposed by the present invention; Figure 2 A three-dimensional diagram of the stirring motor structure of a method for detecting boron content in soil and sediment proposed by the present invention; Figure 3 A three-dimensional diagram of the grinding basin structure of a method for detecting boron content in soil and sediment proposed by the present invention; Figure 4 A three-dimensional diagram of the support structure of a method for detecting boron content in soil and sediment proposed by the present invention; Figure 5 A three-dimensional diagram of the digestion tank structure of a method for detecting boron content in soil and sediment proposed by the present invention; Figure 6 A three-dimensional diagram of the stirring rod structure of a method for detecting boron content in soil and sediment proposed by the present invention; Figure 7 A three-dimensional diagram of the weight sensor structure of a method for detecting boron content in soil and sediment proposed by the present invention; Figure 8 A three-dimensional diagram of the volumetric flask structure of a method for detecting boron content in soil and sediment proposed by the present invention; Figure 9A three-dimensional diagram of an L-shaped support structure for a method for detecting boron content in soil and sediments proposed by the present invention; Figure 10 This is a three-dimensional diagram of the driving cylinder structure of the method for detecting boron content in soil and sediment proposed by the present invention.

[0026] In the figure: 1. Digestion tank; 2. Volumetric flask; 3. Box; 4. Support frame; 5. Grinding basin; 51. Sampling plate; 52. First filter; 53. Support plate; 54. Connecting rod; 55. Deflection motor; 56. Square buckle; 57. Weight sensor; 58. Concentrated nitric acid bottle; 59. Ammonium fluoride bottle; 510. Mannitol bottle; 511. Dropper; 6. Second filter; 61. Slide; 62. Handle; 63. Rotating shaft; 64. Brush; 65. Support plate; 66. L-shaped bracket; 67. Drive shaft; 68. Drive motor; 69. Telescopic rod; 610. Servo motor; 611. Driving gear; 612. Push cylinder; 613. Conical sleeve; 614. Driven gear; 7. Feed inlet; 8. Sealing cover; 9. Stirring motor; 10. Stirring rod. DETAILED DESCRIPTION

[0027] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0028] Reference Figures 1-10 , a method for detecting boron content in soil and sediment, comprising the following detection methods: S1, weigh the sample and put it into digestion tank 1; S2, adding digestion solution into digestion tank 1; S3. After stirring evenly, place the digestion tank 1 into a microwave digestion apparatus for microwave digestion; S4. After the digestion is completed, turn off the microwave digester, wait for the digestion tank 1 to cool to room temperature, and then filter to remove the precipitate; S5. Transfer the digestion solution to volumetric flask 2 and adjust the volume for subsequent analysis; S6. Analyze the digestion solution using ICP-OES / MS.

[0029] In order to improve the recovery rate of boron, the digestion solution is a mixture of concentrated nitric acid, ammonium fluoride and mannitol, which replaces the traditional method of using a mixed acid of concentrated nitric acid and hydrofluoric acid, which easily causes boron to volatilize and lose. The use of ammonium fluoride instead of hydrofluoric acid not only reduces the use of toxic reagents, but also reduces the volatility of boron. Mannitol forms a stable complex with boron to prevent boron loss and improve the recovery rate of boron.

[0030] By using ammonium fluoride instead of hydrofluoric acid in boron detection in soil and sediment, the use of toxic reagents can be reduced, and mannitol is added to form a stable complex with boron, thereby improving the recovery rate of boron.

[0031] The present invention proposes a method for detecting the boron content in soil and sediment, which also includes a box body 3 and a support frame 4 arranged inside the box body 3. The digestion tank 1 is inserted through the surface of the support frame 4. The inside of the box body 3 is respectively provided with a material taking mechanism and a filtering mechanism.

[0032] Among them, in order to process the collected samples, the material collection mechanism includes a grinding basin 5 for grinding the collected samples and a sampling plate 51 with a first filter screen 52 on the upper surface. The sample in the grinding basin 5 is ground into uniform particles by a grinding rod, and is filtered through the first filter screen 52 and falls into the sampling plate 51 to ensure the uniformity of the sample.

[0033] In order to make the sample in the grinding basin 5 fall into the sampling tray 51, the material taking mechanism also includes a support plate 53 symmetrically installed on the upper surface of the support frame 4. The surface of the support plate 53 is equipped with a connecting rod 54 through a bearing. The free ends of the two connecting rods 54 are fixedly connected to the surface of the grinding basin 5. A deflection motor 55 is fixedly installed on the surface of one of the support plates 53. One end of the output shaft of the deflection motor 55 is fixedly connected to one end of one of the connecting rods 54 through a coupling. The rotation of the output shaft of the deflection motor 55 drives the connecting rod 54 connected to it to rotate. The rotation of the connecting rod 54 drives the grinding basin 5 connected to it to rotate, thereby driving the other connecting rod 54 connected to the grinding basin 5 to rotate.

[0034] In order to filter the sample in the grinding basin 5 before it falls into the sampling plate 51, the sampling plate 51 is located on the upper surface of the support frame 4 and is arranged on the lower side of the grinding basin 5. The upper surface of the first filter screen 52 is installed with square clips 56 distributed in a circular array. The inner surface of the square clip 56 is slidably connected to the surface of the sampling plate 51. Through the deflection of the grinding basin 5, the ground sample therein falls onto the first filter screen 52, and the sample filtered by the first filter screen 52 falls into the sampling plate 51. The design of the square clip 56 facilitates the removal of the first filter screen 52.

[0035] In order to weigh the sample, a weight sensor 57 is embedded in the upper surface of the support frame 4 , and the sampling tray 51 is located above the center of the weight sensor 57 . The sample in the sampling tray 51 is weighed by the weight sensor 57 .

[0036] In order to take the amount of the digestion solution, a concentrated nitric acid bottle 58, an ammonium fluoride bottle 59 and a mannitol bottle 510 are placed in sequence on one side of the upper surface of the support frame 4. The bottle mouths of the concentrated nitric acid bottle 58, the ammonium fluoride bottle 59 and the mannitol bottle 510 are all provided with a dropper 511. The dropper 511 is used to facilitate the placement of an appropriate amount of concentrated nitric acid, ammonium fluoride and mannitol into the digestion tank 1 as needed.

[0037] In order to mix the sample and digestion liquid in the digestion tank 1 together, two feed ports 7 are provided on the upper surface of the digestion tank 1. The surface of the feed port 7 is threadedly sleeved with a sealing cover 8. A stirring motor 9 is provided on the upper surface of the digestion tank 1. A stirring rod 10 is installed on the inner top wall of the digestion tank 1 through a bearing. One end of the output shaft of the stirring motor 9 passes through the digestion tank 1 and is fixedly sleeved with the upper end of the stirring rod 10. Concentrated nitric acid, ammonium fluoride, and mannitol enter the digestion tank 1 through one feed port 7, and the sample is poured into the digestion tank 1 through the other feed port 7. The rotation of the output shaft of the stirring motor 9 drives the stirring rod 10 connected thereto to rotate, and when microwave digestion is required, the feed port 7 is sealed with a sealing cover 8.

[0038] By setting up a material taking mechanism, it is easy to control the amount of sample and digestion solution taken, thereby ensuring that the sample can be completely decomposed.

[0039] In order to filter the mixed liquid in the digestion tank 1 , the filtering mechanism includes a second filter screen 6 arranged inside the volumetric flask 2 , and the second filter screen 6 is used for filtering.

[0040] In order to clean the second filter 6, the filtering mechanism also includes a slide groove 61 opened on the surface of the volumetric flask 2. The surface of the second filter 6 is slidably engaged with the inner wall of the slide groove 61. The surface of the second filter 6 is fixedly connected to a handle 62. A rotating shaft 63 is installed in the center of the upper surface of the second filter 6 through a bearing. A brush 64 is fixedly sleeved on the surface of the rotating shaft 63. The lower surface of the brush 64 contacts the surface of the second filter 6. A support plate 65 is provided on the upper surface of the brush 64. One side surface of the support plate 65 is fixedly connected to one side surface of the handle 62. The handle 62 is used to facilitate the removal of the second filter 6 from the slide groove 61, thereby facilitating the replacement of the second filter 6. The rotation of the brush 64 facilitates the cleaning of the filter holes on the second filter 6.

[0041] In order to drive the brush 64 to rotate, an L-shaped bracket 66 is installed on the surface of the volumetric flask 2, and a driving shaft 67 is installed on the surface of the L-shaped bracket 66 through a bearing. A driving motor 68 is fixedly installed on the upper surface of the L-shaped bracket 66, and one end of the output shaft of the driving motor 68 is fixedly sleeved with one end of the driving shaft 67. A telescopic rod 69 is fixedly sleeved on the outer surface of the driving shaft 67, and a servo motor 610 is fixedly installed on the upper surface of one end of the telescopic rod 69. One end of the output shaft of the servo motor 610 passes through the telescopic rod 69 and is fixedly sleeved with a driving gear 611. Two pushing cylinders 612 are installed on the upper surface of the support plate 65, and one end of the piston rod of the pushing cylinder 612 is fixedly connected to a tapered sleeve 6 13. A driven gear 614 is fixedly sleeved on the surface of the rotating shaft 63. The driven gear 614 is meshed with the driving gear 611. The rotation of the output shaft of the driving motor 68 drives the driving shaft 67 connected thereto to rotate. The rotation of the driving shaft 67 drives the telescopic rod 69 connected thereto to rotate, pushing the extension of the piston rod of the cylinder 612 to drive the tapered sleeve 613 connected thereto to move upward and away from the support plate 65. The rotation of the output shaft of the servo motor 610 drives the driving gear 611 connected thereto to rotate. The rotation of the driving gear 611 drives the driven gear 614 meshed therewith to rotate. The rotation of the driven gear 614 drives the rotating shaft 63 to rotate. The rotation of the rotating shaft 63 drives the brush 64 to rotate.

[0042] By setting up a filtering mechanism, it is convenient to filter and volume the mixed and digested liquid, which is convenient for subsequent analysis and detection. At the same time, the servo motor 610 is used to drive the brush 64 to rotate, and the conical sleeve 613 is used to prevent the liquid from being retained on the brush 64 and the driven gear 614. It not only does not hinder the filtering efficiency, but also can clean the surface of the second filter screen 6.

[0043] Working principle: When in use, the collected sample is placed in the grinding basin 5, and the sample in the grinding basin 5 is ground into uniform particles using a grinding rod. Then, the deflection motor 55 is started, and the rotation of the output shaft of the deflection motor 55 drives the connecting rod 54 connected thereto to rotate. The rotation of the connecting rod 54 drives the grinding basin 5 connected thereto to rotate, so that the ground sample in the grinding disc falls onto the first filter 52 on the sampling disc 51. The filtered sample falls into the sampling disc 51, and the weight sensor 57 weighs the sample in the sampling disc 51. When the weight reaches the set threshold, the output shaft of the deflection motor 55 rotates in the opposite direction to drive the grinding basin 5 to reset. Then, remove the first filter screen 52 through the square buckle 56, pour the sample in the sampling tray 51 into the digestion tank 1 through the feed port 7, and then use the dropper 511 on the concentrated nitric acid bottle 58, the ammonium fluoride bottle 59 and the mannitol bottle 510 to sequentially add appropriate amounts of concentrated nitric acid, ammonium fluoride and mannitol into the digestion tank 1 through another feed port 7 according to the ratio, and then seal the two feed ports 7 with the sealing cover 8; Start the stirring motor 9, and the stirring rod 10 connected to the stirring motor 9 rotates by rotating the output shaft thereof, so that the liquid in the digestion tank 1 is evenly mixed, and then the digestion tank 1 is placed in a microwave digestion apparatus for microwave digestion; After the digestion is completed, turn off the microwave digester, wait for the digestion tank 1 to cool to room temperature, put the digestion tank 1 back on the support frame 4, open the drain port at the bottom of the digestion tank 1, and allow the liquid to filter through the second filter 6 and fall into the volumetric flask 2; After the filtration is completed, the piston rod of the push cylinder 612 is extended to drive the conical sleeve 613 connected thereto to move upward and away from the support plate 65, so that the driven gear 614 is exposed, and then the telescopic rod 69 is extended to drive the driving gear 611 to engage with the driven gear 614, and the servo motor 610 is started. The rotation of the output shaft of the servo motor 610 drives the driving gear 611 connected thereto to rotate, and the rotation of the driving gear 611 drives the driven gear 614 engaged therewith to rotate, and the rotation of the driven gear 614 drives the rotating shaft 63 to rotate, and the rotation of the rotating shaft 63 drives the brush 64 to rotate, so that the brush 64 can clean the clogged filter holes on the second filter screen 6. After cleaning, the second filter screen 6 is taken out of the chute 61 using the handle 62 to clean the dirt on the second filter screen 6.

[0044] The above description is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with the technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solution and inventive concept of the present invention, should be covered by the scope of protection of the present invention.

Claims

1. A method for detecting boron content in soil and sediment, characterized in that: The following detection methods are included: S1. Weigh the sample and place it into the digestion tank (1); S2, adding digestion solution into the digestion tank (1); S3. After stirring evenly, place the digestion tank (1) into a microwave digestion apparatus for microwave digestion; S4. After the digestion is completed, the microwave digester is turned off, and the digestion tank (1) is cooled to room temperature, and then filtered to remove the precipitate; S5. Transfer the digestion solution to the volumetric flask (2) and adjust the volume for subsequent analysis; S6. Analyze the digestion solution using ICP-OES / MS; It also includes a box body (3) and a support frame (4) arranged inside the box body (3), the digestion tank (1) is inserted through the surface of the support frame (4), and a material taking mechanism and a filtering mechanism are respectively arranged inside the box body (3); The material taking mechanism comprises a grinding basin (5) for grinding the collected sample and a sampling plate (51) with a first filter screen (52) provided on the upper surface; Wherein, the filtering mechanism comprises a second filter screen (6) arranged inside the volumetric flask (2).

2. The method for detecting boron content in soil and sediment according to claim 1, wherein: The digestion solution is a mixture of concentrated nitric acid, ammonium fluoride and mannitol.

3. The method for detecting boron content in soil and sediment according to claim 1, wherein: The material taking mechanism further comprises support plates (53) symmetrically mounted on the upper surface of the support frame (4), the surface of the support plates (53) being mounted with connecting rods (54) via bearings, the free ends of the two connecting rods (54) being fixedly connected to the surface of the grinding basin (5), a deflection motor (55) being fixedly mounted on the surface of one of the support plates (53), and one end of the output shaft of the deflection motor (55) being fixedly sleeved with one end of one of the connecting rods (54) via a coupling.

4. The method for detecting boron content in soil and sediment according to claim 3, wherein: The sampling plate (51) is located on the upper surface of the support frame (4) and is arranged on the lower side of the grinding basin (5). The upper surface of the first filter screen (52) is provided with square buckles (56) distributed in a circular array. The inner surface of the square buckle (56) is slidably connected to the surface of the sampling plate (51).

5. The method for detecting boron content in soil and sediment according to claim 4, characterized in that: A weight sensor (57) is embedded in the upper surface of the support frame (4), and the sampling plate (51) is located in the center above the weight sensor (57).

6. The method for detecting boron content in soil and sediment according to claim 2, wherein: A concentrated nitric acid bottle (58), an ammonium fluoride bottle (59), and a mannitol bottle (510) are sequentially placed on one side of the upper surface of the support frame (4), and a dropper (511) is provided at the bottle mouths of the concentrated nitric acid bottle (58), the ammonium fluoride bottle (59), and the mannitol bottle (510).

7. The method for detecting boron content in soil and sediment according to claim 1, wherein: The upper surface of the digestion tank (1) is provided with two feed ports (7), and the surface of the feed port (7) is threadedly sleeved with a sealing cover (8). The upper surface of the digestion tank (1) is provided with a stirring motor (9), and the inner top wall of the digestion tank (1) is mounted with a stirring rod (10) through a bearing. One end of the output shaft of the stirring motor (9) passes through the digestion tank (1) and is fixedly sleeved with the upper end of the stirring rod (10).

8. The method for detecting boron content in soil and sediment according to claim 1, wherein: The filtering mechanism further comprises a slide groove (61) provided on the surface of the volumetric flask (2), the surface of the second filter screen (6) is slidably engaged with the inner wall of the slide groove (61), the surface of the second filter screen (6) is fixedly connected with a handle (62), a rotating shaft (63) is mounted on the center of the upper surface of the second filter screen (6) through a bearing, a brush (64) is fixedly sleeved on the surface of the rotating shaft (63), the lower surface of the brush (64) contacts the surface of the second filter screen (6), and a support plate (65) is provided on the upper surface of the brush (64), and one side surface of the support plate (65) is fixedly connected with one side surface of the handle (62).

9. The method for detecting boron content in soil and sediment according to claim 8, characterized in that: An L-shaped bracket (66) is mounted on the surface of the volumetric flask (2), a driving shaft (67) is mounted on the surface of the L-shaped bracket (66) via a bearing, a driving motor (68) is fixedly mounted on the upper surface of the L-shaped bracket (66), and one end of the output shaft of the driving motor (68) is fixedly sleeved with one end of the driving shaft (67).

10. The method for detecting boron content in soil and sediment according to claim 9, characterized in that: The outer surface of the driving shaft (67) is fixedly sleeved with a telescopic rod (69), and a servo motor (610) is fixedly mounted on the upper surface of one end of the telescopic rod (69). One end of the output shaft of the servo motor (610) passes through the telescopic rod (69) and is fixedly sleeved with a driving gear (611). Two pushing cylinders (612) are mounted on the upper surface of the support plate (65), and one end of the piston rod of the pushing cylinder (612) is fixedly connected with a tapered sleeve (613). A driven gear (614) is fixedly sleeved on the surface of the rotating shaft (63), and the driven gear (614) is meshed with the driving gear (611).

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