CN116818749A - Soil total phosphorus detection method based on acid dissolution method - Google Patents

Soil total phosphorus detection method based on acid dissolution method Download PDF

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Publication number
CN116818749A
CN116818749A CN202310657150.9A CN202310657150A CN116818749A CN 116818749 A CN116818749 A CN 116818749A CN 202310657150 A CN202310657150 A CN 202310657150A CN 116818749 A CN116818749 A CN 116818749A
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soil
digestion
funnel
liquid
total phosphorus
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CN202310657150.9A
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张国芳
陈超
阚海明
庞卓
徐恒康
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Beijing Academy of Agriculture and Forestry Sciences
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Beijing Academy of Agriculture and Forestry Sciences
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems 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
    • G01N21/78Systems 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N2021/0106General arrangement of respective parts
    • G01N2021/0112Apparatus in one mechanical, optical or electronic block

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Plasma & Fusion (AREA)
  • Engineering & Computer Science (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention relates to the technical field of agricultural chemical detection, in particular to a soil total phosphorus detection method based on an acid dissolution method. According to the invention, the traditional digestion tube is replaced by the digestion tube with volume scales, so that the constant volume is directly digested, the experimental steps are obviously simplified, and the detection efficiency is improved; meanwhile, the step of transferring the soil digestion liquid is removed through the cooperation of the sealing cover, the funnel and the pipe body, so that loss of soil phosphorus in the detection process is avoided, and the accuracy of soil total phosphorus is improved.

Description

Soil total phosphorus detection method based on acid dissolution method
Technical Field
The invention relates to the technical field of agricultural chemical detection, in particular to a soil total phosphorus detection method based on an acid dissolution method.
Background
Phosphorus is an essential nutrient element for plant growth and development, and is involved in various ways in plant growth and various metabolic processes in a soil system, and is one of important indexes for evaluating soil quality. The total phosphorus content of the soil is the sum of various forms of phosphorus in the soil, and the determination of the total phosphorus content of the soil has important significance for knowing the phosphorus supply capacity of the soil, guiding the reasonable application of the phosphate fertilizer and researching plant nutrition.
In the determination of the phosphorus in the forest soil of the national forestry standard LY/T1232-2015, the total phosphorus in the soil can be determined by adopting an acid dissolution decomposition and molybdenum-antimony colorimetric method. According to the traditional method, soil samples and acid liquor are digested in a common digestion tube, and the digested soil samples and acid liquor are transferred to a specified volumetric flask and the digestion tube is required to be washed for multiple times.
Disclosure of Invention
The invention provides a soil total phosphorus detection method based on an acid dissolution method, which is characterized in that the volume is directly fixed in a digestion tube, so that the test steps are simplified; and removing the transferred soil digestion liquid, avoiding the loss of soil phosphorus in the detection process, and improving the accuracy of detecting the total phosphorus in the soil.
The present invention provides a digestion tube comprising: a pipe body with one end open, a sealing cover and a funnel;
the pipe body is provided with scales;
the sealing cover is matched with the opening end of the pipe body to form a closed space;
the conical outer side wall of the funnel is matched with the opening of the pipe body to form a liquid inlet channel. The digestion tube is applied to soil total phosphorus detection, and can be directly used for fixing the volume in the digestion tube, so that the test steps are simplified; and removing the transferred soil digestion liquid, avoiding the loss of soil phosphorus in the detection process, and improving the accuracy of soil total phosphorus.
According to the digestion tube of the invention, the funnel is a bent neck funnel.
According to the digestion tube, the tube body is made of glass.
Preferably, the digestion vessel is 50mL in size.
According to the digestion tube, the sealing cover comprises the plug-in end, and the plug-in end is matched with the opening end of the tube body to form a closed space;
the inner wall of the opening end of the pipe body and the outer wall of the inserting end are frosted.
According to the digestion tube, the tube body, the sealing cover and the funnel are independent from each other and have no connection relationship.
Preferably, the funnel is a small funnel.
The invention provides a soil total phosphorus detection method based on an acid dissolution method, which utilizes the digestion tube. The invention provides a soil total phosphorus detection method based on an acid dissolution method, which uses a digestion tube with volume scales to replace a common digestion tube to digest a soil sample, and the soil sample is directly fixed in volume after being cooled. The method does not need to wash out the acid-dissolved soil digestion liquid, simplifies the experimental steps of the traditional detection method, and is simple to operate, environment-friendly and efficient.
According to the soil total phosphorus detection method based on the acid dissolution method, the method comprises a soil acid dissolution pretreatment step and a to-be-detected liquid preparation step;
the soil acid-dissolution pretreatment comprises the following steps: weighing a soil sample in the digestion tube, adding sulfuric acid and perchloric acid, heating for digestion, sealing an upper funnel, digesting until the solution in the digestion tube turns white and transparent, maintaining, and cooling;
the preparation of the liquid to be tested comprises the following steps: and (3) cleaning the funnel with deionized water, collecting the funnel to a digestion tube, fixing the volume with deionized water, replacing the sealing cover, shaking the digestion liquid to be measured uniformly, and standing the digestion liquid until the digestion liquid is clear.
According to the soil total phosphorus detection method based on the acid dissolution method, in the soil acid dissolution pretreatment step, the soil is maintained for 20 minutes.
According to the method for detecting total phosphorus in soil based on the acid dissolution method, soil samples are air-dried, impurity-removed, ground and sieved and then subjected to acid dissolution.
According to the method for detecting total phosphorus in soil based on acid dissolution, disclosed by the invention, 2-10mL of blank and to-be-detected liquid are sucked into a 50mL volumetric flask, water is added to about 20mL, after the pH value is regulated, 5mL of molybdenum-antimony anti-chromogenic liquid is accurately added for color development, water is used for constant volume to scale, shaking is carried out, the mixture is placed at the room temperature higher than 20 ℃ for 30 minutes, meanwhile, 5mg/L of phosphorus standard solution is sucked to prepare standard series solution, and then the absorption values of the blank solution and the to-be-detected liquid are measured.
Preferably, the soil total phosphorus detection method of the invention comprises the following steps:
step one, soil sample treatment: the soil sample was air dried, purified, and ground to 0.149mm soil sieve.
Step two, soil acid dissolution pretreatment: weighing an air-dried soil sample 0.25 and xxg in a 50mL digestion tube with volume scales, adding a plurality of drops of water for wetting, adding 3.0mL of sulfuric acid and 10 drops of perchloric acid, shaking uniformly, adding a funnel for sealing, putting into a digestion instrument, slowly heating to 400 ℃, until the solution in the digestion tube turns white and transparent, maintaining for 20 minutes, and cooling.
Step three, preparing a liquid to be detected: the funnel was rinsed with a small amount of water and collected to the digestion tube, and the volume was fixed with water to scale marks. Adding a sealing cover into the digestion tube, fully shaking up the digestion liquid to be tested, standing for clarification, and testing.
Step four, preparing 5g/mL phosphorus standard solution: 10mL of 1000mg/L phosphorus standard solution is sucked into a 100mL volumetric flask, and water is used for volume fixing, wherein the volume fixing is 100mg/L phosphorus standard solution; 5mL of 100mg/L phosphorus standard solution is sucked up into a 100mL volumetric flask, and the volume is fixed by water, which is 5mg/L phosphorus standard solution.
Step five, colorimetric determination: absorbing blank and 2-10mL of liquid to be detected in a 50mL volumetric flask, adding water to about 20mL, adding 1 drop of dinitrophenol indicator, regulating pH solution to be slightly yellow by using sodium hydroxide and sulfuric acid solution, accurately adding 5mL of molybdenum-antimony anti-color developing agent, fixing the volume to a scale by using water, shaking uniformly, and standing for 30 minutes at room temperature higher than 20 ℃ for color development.
The standard series of 0.00mL,1.00mL,2.00mL,3.00mL,4.00mL,5.00mL and 50mL volumetric flasks were prepared by separately sucking 5mg/L of the phosphorus standard solution, and 0.10mg/L, 0.20mg/L, 0.30mg/L, 0.40mg/L and 0.50mg/L standard curves were prepared, and the same treatments were performed. And (3) colorimetry is carried out on a spectrophotometer by using 700nm wavelength, a standard solution of 0.00mg/L is used as a reference solution, zero setting is carried out, an absorbance standard curve is produced through the standard solution, then absorption values of a blank solution and a liquid to be detected are measured, and the concentration value is calculated through the standard curve.
Step six, calculating results:
the calculation of the total phosphorus content is shown in the formulas (1) - (3)
w P Total phosphorus content in grams per kilogram, g/kg;
the unit of the phosphorus concentration of the liquid to be measured is milligrams per liter and mg/L;
C 0 blank phosphorus concentration in milligrams per liter, mg/L;
v- -volume of color developing solution, 50mL;
t s -dividing and taking multiples;
k-converting the air-dried soil sample into a moisture conversion coefficient of the dried soil sample;
m h the mass of the dried soil sample is given in g;
m f air-dried soil sample mass in grams, g.
According to the invention, the traditional digestion tube is replaced by the digestion tube with volume scales, so that the constant volume is directly digested, the experimental steps are obviously simplified, and the detection efficiency is improved; meanwhile, the step of transferring the soil digestion liquid is removed, so that loss of soil phosphorus in the detection process is avoided, and the accuracy of soil total phosphorus is improved.
Drawings
In order to more clearly illustrate the invention or the technical solutions of the prior art, the following description will briefly introduce the drawings that are needed in the embodiments or the prior art description, and it is obvious that the drawings in the following description are some embodiments of the invention.
FIG. 1 is a graduated digestion tube provided in example 1 of the present invention.
Fig. 2 is a funnel provided in example 1 of the present invention.
Fig. 3 is a seal cap provided in example 1 of the present invention.
Wherein, 1 is the pipe shaft, 2 is the funnel, 3 is sealed lid, 4 is sealed dull polish layer of lid, 5 is the dull polish layer of pipe shaft.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The means in the examples are all means known in the art unless otherwise specified.
The main instrument equipment of the invention comprises: a digestion instrument (lebertaike EHD 36), a spectrophotometer (general analysis uv-vis spectrophotometer TU 1900); the main vessel is as follows: 50mL digestion tube with volume scale, funnel, sealing cap, 50mL volumetric flask. The reagents and water used in the test method refer to analytically pure reagents and tertiary water specified in GB/T6682 unless otherwise specified. The solutions, unless indicated as solvents, are aqueous solutions.
Reagent preparation
Dinitrophenol indicator: 0.2g of 2,4 dinitrophenol or 2,6 dinitrophenol is weighed out and dissolved in 100mL of water.
Sodium hydroxide solution: 80.0g of sodium hydroxide is weighed and dissolved in water, and after cooling, the volume is fixed to 1L.
Sulfuric acid solution: 28mL of concentrated sulfuric acid is measured and slowly added into a large beaker containing about 800mL of water, the mixture is continuously stirred, and after cooling, the mixture is subjected to constant volume to 1L by using water.
Antimony potassium tartrate solution: 0.50g of potassium antimonate tartrate is weighed and dissolved in 100mL of water;
molybdenum-antimony stock solution: 153mL of concentrated sulfuric acid was measured and slowly added to about 400mL of water, and the mixture was stirred and cooled. 10.0g of ammonium molybdate was additionally weighed and dissolved in 300mL of water at a temperature of about 60℃and cooled. The sulfuric acid solution was then slowly poured into the ammonium molybdate solution. Then 100mL of 0.5% antimony potassium tartrate solution is added, cooled, and then the volume is fixed to 1L by water, shaken well and stored in a brown reagent bottle.
Molybdenum-antimony color development resisting agent: 1.50g of ascorbic acid was weighed out and dissolved in 100mL of molybdenum-antimony stock solution, which was prepared as it is.
Phosphorus standard solution: 1000mg/L, from national institute of standards and substances, under the number GBW (E) 080431.
Example 1
The present embodiment provides a digestion tube, comprising: a pipe body 1 with one end open, a sealing cover 3 and a funnel 2;
the pipe body 1 is provided with scales;
the sealing cover 3 is matched with the opening end of the pipe body 1 to form a closed space;
the conical outer side wall of the funnel 2 is matched with the opening of the pipe body 1, so that a liquid inlet channel can be formed.
The frosted layer 4 of the sealing cover is matched with the frosted layer 5 of the pipe body, and a closed space is formed during plugging.
Example 2
The embodiment provides a soil total phosphorus detection method, which uses the digestion tube described in the embodiment 1, and comprises the following steps:
step one, soil sample treatment: the soil sample was air dried, purified, and ground to 0.149mm soil sieve.
Step two, soil acid dissolution pretreatment: weighing an air-dried soil sample 0.25 and xxg in a 50mL digestion tube with volume scales, adding a plurality of drops of water for wetting, adding 3.0mL of sulfuric acid and 10 drops of perchloric acid, shaking uniformly, adding a funnel for sealing, putting into a digestion instrument, slowly heating to 400 ℃, until the solution in the digestion tube turns white and transparent, maintaining for 20 minutes, and cooling.
Step three, preparing a liquid to be detected: the funnel was rinsed with a small amount of water and collected to the digestion tube, and the volume was fixed with water to scale marks. Adding a sealing cover into the digestion tube, fully shaking up the digestion liquid to be tested, standing for clarification, and testing.
Step four, colorimetric determination: absorbing blank and 5mL of liquid to be detected in a 50mL volumetric flask, adding water to about 20mL, adding 1 drop of dinitrophenol indicator, regulating pH solution to be slightly yellow by using sodium hydroxide and sulfuric acid solution, accurately adding 5mL of molybdenum-antimony color development inhibitor, fixing the volume to a scale by using water, shaking uniformly, and standing for 30 minutes at room temperature higher than 20 ℃ for color development.
The standard series of 0.00mL,1.00mL,2.00mL,3.00mL,4.00mL,5.00mL of the phosphorus standard solution is prepared by respectively sucking 5mg/L of the phosphorus standard solution, and the solution is processed as above. And (3) colorimetry is carried out on a spectrophotometer by using 700nm wavelength, a standard solution of 0.00mg/L is used as a reference solution, zero setting is carried out, an absorbance standard curve is produced through the standard solution, then absorption values of a blank solution and a liquid to be detected are measured, and the concentration value is calculated through the standard curve.
Step five, calculating results:
the calculation of the total phosphorus content is shown in the formulas (1) - (3)
w P Total phosphorus content in grams per kilogram, g/kg;
the phosphorus concentration of the liquid to be detected is expressed in milligrams per liter and mg/L;
C 0 blank phosphorus concentration in milligrams per liter, mg/L;
v- -volume of color developing solution, 50mL;
t s -dividing and taking multiples;
k-converting the air-dried soil sample into a moisture conversion coefficient of the dried soil sample;
m h the mass of the dried soil sample is given in g;
m f air-dried soil sample mass in grams, g.
Example 3
The national standard substances GBW07388, GBW07447 and GBW07385 with low, medium and high phosphorus content in the soil are selected, the total phosphorus content in the soil is detected according to the detection method of the example 2,6 repeats are measured for each sample, the total phosphorus content in the soil is measured, and the relative standard deviation of each sample is calculated, so that the results are shown in Table 1.
The detection results show that the relative standard deviation of the 3 national standard substances is less than 10%, and the measured average value is within the range of the reference value, thereby meeting the requirements of the standard method.
Table 1 determination of soil total phosphorus as a certified standard in the country
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. A digestion tube, comprising: a pipe body with one end open, a sealing cover and a funnel;
the pipe body is provided with scales;
the sealing cover is matched with the opening end of the pipe body to form a closed space;
the conical outer side wall of the funnel is matched with the opening of the pipe body to form a liquid inlet channel.
2. The digestion tube of claim 1, wherein the funnel is a necked funnel.
3. The digestion tube according to claim 1 or 2, wherein the tube body is made of glass;
preferably, the digestion vessel is 50mL in size.
4. A digestion tube according to any one of claims 1 to 3, wherein the sealing cover comprises a plug end which is matched with the open end of the tube body to form a closed space;
the inner wall of the opening end of the pipe body and the outer wall of the inserting end are frosted.
5. The digestion vessel according to any one of claims 1 to 4, wherein the vessel body, the sealing cap and the funnel are independent of each other and have no connection relationship.
6. A method for detecting total phosphorus in soil based on an acid dissolution method, which is characterized in that the digestion tube according to any one of claims 1 to 5 is utilized.
7. The method for detecting total phosphorus in soil based on the acid dissolution method according to claim 6, which is characterized by comprising a soil acid dissolution pretreatment step and a step for preparing a liquid to be detected;
the soil acid-dissolution pretreatment comprises the following steps: weighing a soil sample in the digestion tube, adding sulfuric acid and perchloric acid, heating for digestion, sealing an upper funnel, digesting until the solution in the digestion tube turns white and transparent, maintaining, and cooling;
the preparation of the liquid to be tested comprises the following steps: and (3) cleaning the funnel with deionized water, collecting the funnel to a digestion tube, fixing the volume with deionized water, replacing the sealing cover, shaking the digestion liquid to be measured uniformly, and standing the digestion liquid until the digestion liquid is clear.
8. The method for detecting total phosphorus in soil by acid dissolution method according to claim 7, wherein the soil is maintained for 20 minutes in the step of acid dissolution pretreatment.
9. The method for detecting total phosphorus in soil based on acid dissolution method according to any one of claims 7 to 8, wherein the soil sample is air-dried, decontaminated, ground and sieved and then acid-dissolved.
10. The method for detecting total phosphorus in soil based on acid dissolution method according to any one of claims 7 to 9, wherein 2 to 10mL of blank and to-be-detected liquid are sucked into a 50mL volumetric flask, water is added to about 20mL, after the pH value is adjusted, 5mL of molybdenum-antimony anti-chromogenic liquid is accurately added for color development, water is used for volume fixing to scale, shaking is carried out, the mixture is placed at room temperature higher than 20 ℃ for 30 minutes, meanwhile, 5mg/L of phosphorus standard solution is sucked to prepare standard series solution, and then the absorption values of the blank solution and to-be-detected liquid are measured.
CN202310657150.9A 2023-06-05 2023-06-05 Soil total phosphorus detection method based on acid dissolution method Pending CN116818749A (en)

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