CN113984754B - Device and method for continuously detecting nitrogen and phosphorus in organic fertilizer - Google Patents
Device and method for continuously detecting nitrogen and phosphorus in organic fertilizer Download PDFInfo
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- CN113984754B CN113984754B CN202111460424.2A CN202111460424A CN113984754B CN 113984754 B CN113984754 B CN 113984754B CN 202111460424 A CN202111460424 A CN 202111460424A CN 113984754 B CN113984754 B CN 113984754B
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000003895 organic fertilizer Substances 0.000 title claims abstract description 42
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 26
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 25
- 239000011574 phosphorus Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title description 5
- 230000029087 digestion Effects 0.000 claims abstract description 136
- 238000010438 heat treatment Methods 0.000 claims abstract description 47
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000001514 detection method Methods 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 23
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000007787 solid Substances 0.000 claims abstract description 10
- 238000005303 weighing Methods 0.000 claims abstract description 9
- 238000009736 wetting Methods 0.000 claims abstract description 9
- 238000004321 preservation Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 230000001079 digestive effect Effects 0.000 claims abstract description 4
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims abstract description 4
- 238000002133 sample digestion Methods 0.000 claims abstract description 4
- 239000000523 sample Substances 0.000 claims description 40
- 238000012360 testing method Methods 0.000 claims description 22
- 239000003638 chemical reducing agent Substances 0.000 claims description 11
- 230000035939 shock Effects 0.000 claims description 6
- 239000012496 blank sample Substances 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 5
- 230000006835 compression Effects 0.000 claims description 5
- 238000007906 compression Methods 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 claims 1
- 239000003337 fertilizer Substances 0.000 description 6
- 210000003608 fece Anatomy 0.000 description 5
- 239000010871 livestock manure Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 235000015097 nutrients Nutrition 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- GQWNECFJGBQMBO-UHFFFAOYSA-N Molindone hydrochloride Chemical compound Cl.O=C1C=2C(CC)=C(C)NC=2CCC1CN1CCOCC1 GQWNECFJGBQMBO-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002361 compost Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000035558 fertility Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000003303 reheating Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- 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
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N2021/786—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour with auxiliary heating for reaction
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a continuous detection method for nitrogen and phosphorus in an organic fertilizer, which comprises the following steps: a, preserving a sample: placing the prepared organic fertilizer sample in a shade and dry place for light-proof preservation; b, sample digestion: weighing a dry sample of the organic fertilizer in a digestion tube, adding water for wetting, adding sulfuric acid in the digestion tube, shaking up, carrying out cold digestion for one night, heating and digestion in a high-temperature digestion instrument to enable solids to disappear into a tan solution, taking down the digestion tube, cooling to room temperature, adding hydrogen peroxide, shaking up, heating at low temperature, then heating and digestion, then enabling the digestion tube to be removed from the high-temperature digestion instrument, facilitating cooling, adding hydrogen peroxide, shaking up, heating at low temperature, and then heating and digestion; c, sample constant volume, namely after cooling, transferring all the digestive juice into a volumetric flask by using water, and uniformly shaking the sample with constant volume; d, sample detection: and simultaneously measuring the contents of nitrogen and phosphorus by utilizing an online color development reaction of a double-channel continuous flow analyzer. Is convenient for continuously detecting nitrogen and phosphorus in the organic fertilizer.
Description
Technical Field
The invention relates to the technical field of detection, in particular to a device and a method for continuously detecting nitrogen and phosphorus in an organic fertilizer.
Background
Organic fertilizers are also known as "farmyard manure". Organic fertilizers are known as organic fertilizers using organic substances (compounds containing carbon elements) as fertilizers. Including human manure, compost, green manure, cake manure, biogas manure, and the like. Has the characteristics of multiple types, wide sources, longer fertilizer efficiency and the like. The organic fertilizer contains a plurality of nutrient elements in an organic state, so that crops are difficult to directly utilize, and the nutrient elements are slowly released under the action of microorganisms to continuously supply the nutrients to the crops. The organic fertilizer can improve the soil structure, effectively coordinate water, fertilizer, gas and heat in the soil, and improve the soil fertility and the land productivity.
When the organic fertilizer is prepared, continuous detection of nitrogen and phosphorus in the organic fertilizer is needed, a sample needs to be pretreated before detection, digestion is needed after pretreatment, and nitrogen and phosphorus detection is needed after digestion, so that the device and the method for continuous detection of nitrogen and phosphorus in the organic fertilizer are provided.
Disclosure of Invention
The invention aims to provide a continuous detection device for nitrogen and phosphorus in an organic fertilizer, which solves the problem that nitrogen and phosphorus in an organic fertilizer sample are not easy to continuously detect.
In order to solve the technical problems, the invention adopts the following technical scheme:
A continuous detection device for nitrogen and phosphorus in organic fertilizer comprises: a fixing frame;
a high-temperature digestion instrument is arranged on the fixing frame, and a placing groove is arranged on the high-temperature digestion instrument;
The fixing frame is provided with a first hydraulic rod, the first hydraulic rod is connected with a first hydraulic pump, the first hydraulic pump is connected with a first controller, the first hydraulic rod is connected with a placing frame, the placing frame is provided with a vibrating plate, the vibrating plate is connected with a first motor, holes are uniformly formed in the vibrating plate, and a fixing ring is arranged on the vibrating plate at the position of the holes;
the second hydraulic rod is arranged on the placing rack and connected with a second hydraulic pump, the second hydraulic pump is connected with a second controller, and the second hydraulic rod is connected with a fixed plate;
The fixing frame is provided with a fixing rod, the fixing rod is provided with a clamping groove hole, the clamping groove hole is provided with a clamping rod, clamping teeth are uniformly arranged on the clamping rod, and one end of the clamping rod is provided with a leaning ring.
Further; the fixing plate is uniformly provided with a convex plate, the convex plate is provided with a compression pad, and the convex plate is arranged above the opening of the vibrating plate;
the bottom of the fixing frame is provided with a shock pad;
the fixing frame is provided with a rotary connecting piece, and the rotary connecting piece is connected with a baffle.
Further; the rotary shaft is arranged on the fixing frame and connected with the rotating frame, the rotating shaft is connected with the speed reducer, the speed reducer is connected with the second motor, a fixed groove is formed in the rotating frame, a third hydraulic rod is arranged at one end of the rotating frame and connected with the third hydraulic pump, and the third hydraulic pump is connected with the third controller and provided with a clamping groove.
Further; and a double-channel continuous flow analyzer is arranged on one side of the fixing frame.
Further; the method comprises the following steps:
A, preserving a sample: drying the prepared organic fertilizer sample at 80 ℃ for 4 h, testing, and then placing the prepared organic fertilizer sample in a shade and dry place for light-proof preservation, wherein the preservation room temperature is less than 26 ℃ and the humidity is less than 60%;
B, sample digestion: weighing a dry sample of the organic fertilizer in a digestion tube, adding water for wetting, adding sulfuric acid in the digestion tube, shaking up, adding a cover, carrying out cold digestion for one night, placing in a high-temperature digestion instrument for heating and digestion to enable solids to disappear into a tan solution, enabling the digestion tube to be removed from the high-temperature digestion instrument, facilitating cooling to room temperature, adding hydrogen peroxide, shaking up, heating at low temperature, then heating and digestion, enabling the digestion tube to be removed from the high-temperature digestion instrument, facilitating cooling, adding hydrogen peroxide, shaking up, heating at low temperature, and then heating and digestion; repeating the steps until the solution is colorless or clear, and then continuing to decoct, wherein the decoct is finished;
c, sample constant volume, namely after cooling, transferring all the digestive juice into a volumetric flask by using water, and uniformly shaking the sample with constant volume;
D, sample detection: and the constant-volume sample and the blank sample simultaneously measure the contents of nitrogen and phosphorus by utilizing an online color development reaction of a double-channel continuous flow analyzer.
Further; in the step B, weighing a dry sample of an organic fertilizer sample 0.1-0.5 g in a 50mL digestion tube, adding 5-10 drops of water for wetting, adding 5mL sulfuric acid in the digestion tube, shaking up, adding a cover, cold digestion for one night, heating and digestion at 300 ℃ on a high-temperature digestion instrument to enable solids to disappear into a tan solution, enabling the digestion tube to be removed from the high-temperature digestion instrument, cooling to room temperature conveniently, adding 1 mL hydrogen peroxide, shaking up, heating at 110 ℃ at low temperature for 5 min, heating and digestion at 370 ℃ for 10-15 min, removing the digestion tube from the high-temperature digestion instrument, cooling conveniently, adding 10 drops of hydrogen peroxide, shaking up, heating at 110 ℃ for 5 min, and heating and digestion at 370 ℃ for 10-15 min; repeating the steps until the solution is colorless or clear, and then continuously boiling at 370 ℃ for 20-30 min.
Further; in the step C, the volumetric flask is placed in a fixed tank to be uniformly shaken to a constant volume.
Compared with the prior art, the invention has at least one of the following beneficial effects:
1. the continuous nitrogen and phosphorus detection device in the organic fertilizer is convenient for digestion, volume fixing and nitrogen and phosphorus detection, and is convenient for rapid determination in a test.
2. The continuous detection method for nitrogen and phosphorus in the organic fertilizer is convenient for continuous detection of nitrogen and phosphorus in the organic fertilizer by combining the device.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention.
Fig. 2 is a top view of the retaining ring of the present invention.
Fig. 3 is a side view of the structure of the present invention.
Fig. 4 is a top view of a fixing rod according to the present invention.
FIG. 5 is a schematic view showing the connection of the rotating frame in the present invention
In the figure: the high-temperature digestion instrument 2, the placing groove 3, the first hydraulic rod 4, the first hydraulic pump 5, the first controller 6, the placing rack 7, the vibrating plate 8, the first motor 9, the fixed ring 10, the second hydraulic rod 11, the second hydraulic pump 12, the second controller 13, the fixed plate 14, the fixed rod 15, the clamping groove hole 16, the clamping rod 17, the clamping teeth 18, the leaning ring 19, the convex plate 20, the compression pad 21, the shock pad 22, the rotating connecting piece 23, the baffle 24, the rotating rack 25, the rotating shaft 26, the speed reducer 27, the second motor 28, the fixed groove 29, the third hydraulic rod 30, the third hydraulic pump 31, the clamping groove 32, the dual-channel continuous flow analyzer 33 and the third controller 34.
Detailed Description
The present invention will be further described in detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent, as shown in fig. 1 to 5. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1:
A continuous detection device for nitrogen and phosphorus in organic fertilizer comprises: a fixing frame 1;
A high-temperature digestion instrument 2 is arranged on the fixing frame 1, and a placing groove 3 is arranged on the high-temperature digestion instrument 2;
The fixing frame 1 is provided with a first hydraulic rod 4, the first hydraulic rod 4 is connected with a first hydraulic pump 5, the first hydraulic pump 5 is connected with a first controller 6, the first hydraulic rod 4 is connected with a placing frame 7, the placing frame 7 is provided with a vibrating plate 8, the vibrating plate 8 is connected with a first motor 9, holes are uniformly formed in the vibrating plate 8, and a fixing ring 10 is arranged on the vibrating plate 8 at the position of each hole;
The placing frame 7 is provided with a second hydraulic rod 11, the second hydraulic rod 11 is connected with a second hydraulic pump 12, the second hydraulic pump 12 is connected with a second controller 13, and the second hydraulic rod 11 is connected with a fixed plate 14;
The fixing frame 1 is provided with a fixing rod 15, the fixing rod 15 is provided with a clamping groove hole 16, the clamping groove hole 16 is provided with a clamping rod 17, clamping teeth 18 are uniformly arranged on the clamping rod 17, and one end of the clamping rod 17 is provided with a leaning ring 19; the first hydraulic pump 5 that first hydraulic pump 5 on mount 1 is connected works, first hydraulic pump 5 drives the upward movement of first hydraulic stem 4, the upward movement of rack 7 that first hydraulic stem 4 is connected, the upward movement of vibrating plate 8 of rack 7, the trompil department of vibrating plate 8 has placed and has cleared up the test tube, clear up the test tube open end and establish the protrusion setting on the lateral wall, clear up the test tube and be common instrument, be convenient for place in the trompil department of vibrating plate 8, clear up sample and clear up the liquid and place in clearing up the test tube, solid fixed ring 10's setting, be convenient for clear up the better placing of test tube, according to needs, vibrating plate 8 moves, clear up the test tube on the vibrating plate 8 can vibrate, the second hydraulic pump 12 work of connection is connected to second controller 13, second hydraulic pump 12 drives the downward movement of second hydraulic stem 11, the fixed plate 14 motion that second hydraulic stem 11 is connected, clear up the cover of block up has been placed on the test tube, fixed plate 14 downward movement, be convenient for clear up the cover department of clearing up the test tube, again according to needs first hydraulic stem 4 downward movement, be convenient for clear up test tube on the vibrating plate 8 moves into high temperature instrument 2's place groove of clearing up, be convenient for clear up in. The fixed rod 15 of the fixed frame 1 is provided with the clamping groove hole 16, the clamping groove hole 16 is provided with two ends open, the clamping rod 17 penetrates through the clamping groove hole 16 to extend, the clamping teeth 18 of the clamping rod 17 move in the clamping groove hole 16, the leaning ring 19 of the clamping rod 17 moves, the leaning ring 19 is convenient to carry out the upper part of the hole of the vibrating plate 8, the worker can rely on the leaning ring 19 to add reagent according to the requirement, and the requirement is met.
Example 2:
on the basis of embodiment 1, the fixing plate 14 is uniformly provided with a convex plate 20, the convex plate 20 is provided with a compression pad 21, and the convex plate 20 is arranged above the opening of the vibration plate 8;
the bottom of the fixing frame 1 is provided with a shock pad 22;
The fixing frame 1 is provided with a rotary connecting piece 23, and the rotary connecting piece 23 is connected with a baffle 24; the convex plate 20 and the compression pad 21 are arranged so as to be convenient for fixing the cover for clearing the blockage of the test tube. The shock pad 22 is arranged to provide shock absorption. The baffle 24 is connected to the fixing frame 1 through the rotary connecting piece 23, and when the high-temperature digestion instrument 2 is not used, the baffle 24 rotates the placing groove 3 of the high-temperature digestion instrument 2 to block, so that dust and the like are reduced and enter the placing groove 3. The high-temperature digestion instrument 2 is common digestion equipment, and the high-temperature digestion instrument 2 is provided with corresponding temperature control.
Example 3:
On the basis of embodiment 1-2, the fixing frame 1 is provided with a rotating shaft 26, the rotating shaft 26 is connected with a rotating frame 25, the rotating shaft 26 is connected with a speed reducer 27, the speed reducer 27 is connected with a second motor 28, the rotating frame 25 is provided with a fixed groove 29, one end of the rotating frame 25 is provided with a third hydraulic rod 30, the third hydraulic rod 30 is connected with a third hydraulic pump 31, the third hydraulic pump 31 is connected with a third controller 34, and the third hydraulic rod 30 is provided with a clamping groove 32. The volumetric flask is placed in fixed slot 29, and the third hydraulic pump 31 work that third controller 34 is connected, and third hydraulic pump 31 drives third hydraulic stem 30 motion, and third hydraulic stem 30 drives draw-in groove 32 motion, and draw-in groove 32 sets up one end open-ended recess, and volumetric flask area lid one end is placed in assorted draw-in groove 32, and the speed reducer 27 motion that the second motor 28 is connected, speed reducer 27 drive pivot 26 motion, and pivot 26 drives the turret 25 motion, is convenient for shake and mixes.
Example 4:
on the basis of examples 1-3, a two-channel continuous flow analyzer 33 is placed on one side of the mount 1; the dual channel continuous flow analyzer 33 facilitates detection of nitrogen and phosphorous.
Example 5:
Based on examples 1-4, the following steps were followed:
a, preserving a sample: drying the prepared organic fertilizer sample at 80 ℃ for 4h, testing, and then placing the prepared organic fertilizer sample in a shade and dry place for light-proof preservation, wherein the preservation room temperature is less than 26 ℃ and the humidity is less than 60%; the organic fertilizer sample is convenient to dry and pretreat, and the sample is convenient to preserve after pretreat;
B, sample digestion: weighing a dry sample of the organic fertilizer in a digestion tube, adding water for wetting, adding sulfuric acid in the digestion tube, shaking up, adding a cover, performing cold digestion for one night, placing in a high-temperature digestion instrument 2 for heating and digestion to enable solids to disappear into a tan solution, enabling the digestion tube to be removed from the high-temperature digestion instrument, facilitating cooling to room temperature, adding hydrogen peroxide, shaking up, heating at low temperature, then heating and digestion, enabling the digestion tube to be removed from the high-temperature digestion instrument 2, facilitating cooling, adding hydrogen peroxide, shaking up, heating at low temperature again, and then heating and digestion; repeating the steps until the solution is colorless or clear, and then continuing to decoct, wherein the decoct is finished; the first hydraulic pump 5 connected with the first hydraulic pump 5 on the fixing frame 1 works, the first hydraulic pump 5 drives the first hydraulic rod 4 to move upwards, the placing frame 7 connected with the first hydraulic rod 4 moves upwards, the vibrating plate 8 of the placing frame 7 moves upwards, digestion test tubes are placed at the opening of the vibrating plate 8, digestion samples and digestion liquid (water and sulfuric acid) are placed in the digestion test tubes, the fixing ring 10 is arranged, so that the digestion test tubes can be placed well, the vibrating plate 8 moves according to requirements, the digestion test tubes on the vibrating plate 8 can vibrate, and the test tubes are capped and subjected to cold digestion for one night; the second hydraulic pump 12 connected and connected with the second controller 13 works, the second hydraulic pump 12 drives the second hydraulic rod 11 to move downwards, the fixed plate 14 connected with the second hydraulic rod 11 moves, a blocked cover is placed on a digestion test tube, the fixed plate 14 moves downwards, the blocked cover of the digestion test tube is convenient to fix, the first hydraulic rod 4 moves downwards as required, the digestion test tube on the vibration plate 8 is convenient to move into the placing groove 3 of the high-temperature digestion instrument 2, low-temperature heating digestion is firstly carried out, then the digestion is carried out, the first hydraulic rod 4 moves upwards again, the digestion tube is convenient to cool, shaking is added after cooling, then the low-temperature heating is carried out, the digestion is carried out after the reheating, and digestion are repeated until the solution is colorless or clear, and then the digestion is continued; the digestion is convenient; the fixed rod 15 of the fixed frame 1 is provided with the clamping groove hole 16, the clamping groove hole 16 is provided with two ends open, the clamping rod 17 penetrates through the clamping groove hole 16 to extend, the clamping teeth 18 of the clamping rod 17 move in the clamping groove hole 16, the leaning ring 19 of the clamping rod 17 moves, the leaning ring 19 is convenient to lean on the upper portion of the hole of the vibrating plate 8, workers can rely on the leaning ring 19 to add reagents according to requirements, and requirements are met.
C, sample constant volume, namely after cooling, transferring all the digestive juice into a volumetric flask by using water, and uniformly shaking the sample with constant volume; the cooled digestion liquid and water are fixed in a volumetric flask, the volumetric flask is placed in a fixed groove 29, a third hydraulic pump 31 connected with a third controller 34 works, the third hydraulic pump 31 drives a third hydraulic rod 30 to move, the third hydraulic rod 30 drives a clamping groove 32 to move, the clamping groove 32 is provided with a groove with one end open, one end of the volumetric flask is placed in the clamping groove 32 which is matched with the end cover, a speed reducer 27 connected with a second motor 28 moves, the speed reducer 27 drives a rotating shaft 26 to move, the rotating shaft 26 drives a rotating frame 25 to move, and shaking and volume fixing are facilitated.
D, sample detection: the constant volume sample and blank sample are subjected to online color development reaction by utilizing a double-channel continuous flow analyzer 33, and the contents of nitrogen and phosphorus are measured simultaneously; the sample water is a blank sample, and the sample and the blank sample with the constant volume are conveniently subjected to online color reaction by using the double-channel continuous flow analyzer 33, and the contents of nitrogen and phosphorus are simultaneously measured.
Example 6:
On the basis of examples 1-5, in the step B, weighing 0.1g of a dry sample of an organic fertilizer in a 50 mL digestion tube, adding 5 drops of water for wetting, adding 5mL of sulfuric acid in the digestion tube, shaking up, adding a cover, performing cold digestion for one night, heating and digestion at 300 ℃ on a high-temperature digestion instrument 2 to enable solids to disappear into a tan solution, enabling the digestion tube to be removed from the high-temperature digestion instrument, facilitating cooling to room temperature, adding 1 mL of hydrogen peroxide, shaking up, heating at 110 ℃ for 5 min at low temperature, heating and digestion at 370 ℃ for 10 min, enabling the digestion tube to be removed from the high-temperature digestion instrument 2, facilitating cooling, adding 10 drops of hydrogen peroxide, shaking up, heating at 110 ℃ for 5 min, and heating and digestion at 370 ℃ for 10 min; repeating the steps until the solution is colorless or clear, and then continuously boiling at 370 ℃ for 20 min; and the digestion of the organic fertilizer sample is facilitated.
Example 7:
On the basis of examples 1-6, in step B, weighing a dry sample of an organic fertilizer 0.5 g in a 50 mL digestion tube, adding 10 drops of water for wetting, adding 5 mL sulfuric acid in the digestion tube, shaking up, adding a cover, cold digestion for one night, heating and digestion at 300 ℃ on a high-temperature digestion instrument 2 to enable solids to disappear into a tan solution, enabling the digestion tube to be removed from the high-temperature digestion instrument, facilitating cooling to room temperature, adding 1 mL of hydrogen peroxide, shaking up, firstly heating at 110 ℃ for 5 min, then heating and digestion at 370 ℃ for 15 min, then enabling the digestion tube to be removed from the high-temperature digestion instrument 2, facilitating cooling, adding 10 drops of hydrogen peroxide, shaking up, then heating at 110 ℃ for 5 min, and then heating at 370 ℃ for 15 min; repeating the steps until the solution is colorless or clear, and continuously boiling at 370 ℃ for 30min; and the digestion of the organic fertilizer sample is facilitated.
Example 8:
On the basis of examples 1-7, in step B, weighing a dry sample of an organic fertilizer 0.25 g in a 50 mL digestion tube, adding 8 drops of water for wetting, adding 5 mL sulfuric acid in the digestion tube, shaking up, adding a cover, cold digestion for one night, heating and digestion at 300 ℃ on a high-temperature digestion instrument 2 to enable solids to disappear into a tan solution, enabling the digestion tube to be removed from the high-temperature digestion instrument, facilitating cooling to room temperature, adding 1 mL hydrogen peroxide, shaking up, heating at 110 ℃ for 5min at a low temperature, heating and digestion at 370 ℃ for 12.5 min, enabling the digestion tube to be removed from the high-temperature digestion instrument 2, facilitating cooling, adding 10 drops of hydrogen peroxide, shaking up, heating at 110 ℃ for 5min at a low temperature, and heating and digestion at 370 ℃ for 12.5 min; repeating the steps until the solution is colorless or clear, and continuously boiling at 370 ℃ for 25min; and the digestion of the organic fertilizer sample is facilitated.
Example 9:
based on examples 1-8, in step C, the volumetric flask is placed in a fixed tank 29 for constant volume shaking; is convenient for constant volume shaking.
Although the application has been described herein with reference to a number of illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the scope and spirit of the principles of this disclosure. More specifically, various variations and modifications may be made to the component parts and/or arrangements of the subject combination arrangement within the scope of the disclosure, drawings and claims. In addition to variations and modifications in the component parts and/or arrangements, other uses will be apparent to those skilled in the art.
Claims (4)
1. A continuous detection device of nitrogen phosphorus in organic fertilizer, its characterized in that: comprising the following steps: a fixing frame (1);
A high-temperature digestion instrument (2) is arranged on the fixing frame (1), and a placing groove (3) is arranged on the high-temperature digestion instrument (2);
The device comprises a fixing frame (1), a first hydraulic rod (4), a first hydraulic pump (5), a first controller (6), a first hydraulic rod (4), a first motor (9), a vibrating plate (8) and a digestion tube, wherein the first hydraulic rod (4) is arranged on the fixing frame (1), the first hydraulic rod (4) is connected with the first hydraulic pump (5), the first hydraulic pump (5) is connected with the first controller (6), the first hydraulic rod (4) is connected with the rack (7), the vibrating plate (8) is arranged on the rack (7), the vibrating plate (8) is connected with the first motor (9), the vibrating plate (8) is uniformly perforated, a fixing ring (10) is arranged on the vibrating plate (8) at the perforated position, the first hydraulic pump (5) drives the first hydraulic rod (4) to move upwards, the rack (7) connected with the first hydraulic rod (4) moves upwards, and the digestion tube is arranged at the perforated position of the vibrating plate (8);
The placing frame (7) is provided with a second hydraulic rod (11), the second hydraulic rod (11) is connected with a second hydraulic pump (12), the second hydraulic pump (12) is connected with a second controller (13), the second hydraulic rod (11) is connected with a fixed plate (14), the second hydraulic pump (12) drives the second hydraulic rod (11) to move downwards, the fixed plate (14) connected with the second hydraulic rod (11) moves, a blocked cover is placed on the digestion tube, the fixed plate (14) moves downwards, and the blocked cover of the digestion tube is convenient to fix;
The fixing frame (1) is provided with a fixing rod (15), the fixing rod (15) is provided with a clamping slot hole (16), the clamping slot hole (16) is provided with a clamping rod (17), clamping teeth (18) are uniformly arranged on the clamping rod (17), one end of the clamping rod (17) is provided with a leaning ring (19), the clamping teeth (18) of the clamping rod (17) move in the clamping slot hole (16), the leaning ring (19) of the clamping rod (17) moves, the leaning ring (19) can conveniently lean on the upper part of an opening of the vibrating plate (8), and reagent can be added at the leaning ring (19) in a leaning manner;
the fixing plate (14) is uniformly provided with a convex plate (20), the convex plate (20) is provided with a compression pad (21), and the convex plate (20) is arranged above the opening of the vibrating plate (8);
a shock pad (22) is arranged at the bottom of the fixing frame (1);
A rotary connecting piece (23) is arranged on the fixing frame (1), and the rotary connecting piece (23) is connected with a baffle (24);
the detection method adopting the continuous detection device for nitrogen and phosphorus in the organic fertilizer comprises the following steps:
A, preserving a sample: drying the prepared organic fertilizer sample at 80 ℃ for 4 h, testing, and then placing the prepared organic fertilizer sample in a shade and dry place for light-proof preservation, wherein the preservation room temperature is less than 26 ℃ and the humidity is less than 60%;
B, sample digestion: weighing a dry sample of the organic fertilizer in a digestion tube, adding water for wetting, adding sulfuric acid in the digestion tube, shaking uniformly, adding a cover, performing cold digestion, placing in a high-temperature digestion instrument (2), heating and digestion to enable solids to be digested into a tan solution, taking down the digestion tube, cooling to room temperature, adding hydrogen peroxide, shaking uniformly, heating at low temperature, then heating and digestion, removing the digestion tube from the high-temperature digestion instrument (2), facilitating cooling, adding hydrogen peroxide, shaking uniformly, heating at low temperature, and then heating and digestion; repeating the steps until the solution is colorless or clear, and then continuing to decoct, wherein the decoct is finished;
C, sample constant volume: transferring all the digestive juice into a volumetric flask with water after cooling, and shaking uniformly to constant volume;
D, sample detection: the constant volume sample and the blank sample are subjected to online color development reaction by utilizing a double-channel continuous flow analyzer (33) to simultaneously determine the contents of nitrogen and phosphorus;
In the step B, weighing a dry sample of an organic fertilizer sample 0.1-0.5 g in a 50 mL digestion tube, adding 5-10 drops of water for wetting, adding 5 mL sulfuric acid in the digestion tube, shaking up, adding a cover, performing cold digestion, heating and digestion at 300 ℃ on a high-temperature digestion instrument (2) to enable solids to be digested into a tan solution, taking down the digestion tube, cooling to room temperature, adding 1 mL hydrogen peroxide, shaking up, heating at 110 ℃ at first for 5min, heating and digestion at 370 ℃ for 10-15 min, removing the digestion tube from the high-temperature digestion instrument (2), facilitating cooling, adding 10 drops of hydrogen peroxide, shaking up, heating at 110 ℃ for 5min, and heating and digestion at 370 ℃ for 10-15 min; repeating the steps until the solution is colorless or clear, and then continuously boiling at 370 ℃ for 20-30 min.
2. The continuous detection device for nitrogen and phosphorus in organic fertilizer according to claim 1, wherein: be provided with pivot (26) on mount (1), pivot (26) are connected with rotating turret (25), and pivot (26) are connected with speed reducer (27), and speed reducer (27) are connected with second motor (28), are provided with fixed slot (29) on rotating turret (25), and rotating turret (25) one end is provided with third hydraulic stem (30), and third hydraulic stem (30) are connected with third hydraulic pump (31), and third hydraulic pump (31) are connected with third controller (34), are provided with draw-in groove (32) on third hydraulic stem (30).
3. The continuous detection device for nitrogen and phosphorus in organic fertilizer according to claim 1, wherein: a double-channel continuous flow analyzer (33) is arranged on one side of the fixing frame (1).
4. The continuous detection device for nitrogen and phosphorus in organic fertilizer according to claim 1, wherein: in the step C, the volumetric flask is placed in a fixed groove (29) for constant volume shaking.
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