CN114993805A - Application of heating ashing method in determination of phosphorus and potassium in organic fertilizer - Google Patents

Application of heating ashing method in determination of phosphorus and potassium in organic fertilizer Download PDF

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CN114993805A
CN114993805A CN202210634735.4A CN202210634735A CN114993805A CN 114993805 A CN114993805 A CN 114993805A CN 202210634735 A CN202210634735 A CN 202210634735A CN 114993805 A CN114993805 A CN 114993805A
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heating
potassium
phosphorus
hydrogen peroxide
determination
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雒连春
李聪
姚萌奇
汪天胜
张琪玮
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Gansu Product Quality Supervision And Inspection Institute
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • 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
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/3103—Atomic absorption analysis
    • 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
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    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
    • Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
    • Y02A40/20—Fertilizers of biological origin, e.g. guano or fertilizers made from animal corpses

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  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Fertilizers (AREA)

Abstract

The invention relates to a heating ashing method for determining phosphorus and potassium in organic fertilizers, which is characterized by comprising the following steps: placing 1.0g of the air-dried organic fertilizer sample with the accuracy of 0.0001g in a ceramic crucible, placing the ceramic crucible in a muffle furnace for burning, cooling, and transferring the ashed sample into a 100mL beaker; adding 5mL of sulfuric acid solution and 1mL of hydrogen peroxide for heating treatment, placing on an electric heating plate for heating until white smoke appears, cooling, adding a plurality of drops of cold water and hydrogen peroxide, shaking, then adding 20mL of hot water, and continuing heating until the temperature is close to boiling; and finally, completely transferring the content of the beaker into a 100mL volumetric flask by using water, adding water to a constant volume, and filtering to obtain the product for measuring phosphorus and potassium. The invention can improve the pretreatment efficiency.

Description

Application of heating ashing method in determination of phosphorus and potassium in organic fertilizer
Technical Field
The invention relates to the technical field of fertilizer determination, in particular to application of a heating and ashing method in determination of phosphorus and potassium in organic fertilizers.
Background
With the development of social economy, the requirements of people on the quality of agricultural products are higher and higher, organic fertilizers are used as green and efficient fertilizers, production raw materials mainly come from plants and animals and are carbon-containing organic materials which are fermented and decomposed, the functions of the organic fertilizers are to improve soil fertility, provide plant nutrition and improve crop quality, industrial wastes are recycled, agricultural economy can be better developed, and sustainable development is assisted.
At present, according to the requirements of national industry standard NY/T525-plus 2021 organic fertilizer, phosphorus is measured by a phosphorus-vanadium-molybdenum yellow spectrophotometry, potassium is measured by a flame photometry, a sample is digested by concentrated sulfuric acid-hydrogen peroxide in an electric furnace, organic matters are carbonized by sulfuric acid, the hydrogen peroxide belongs to a strong oxidant and has good digestion effect on the organic fertilizer, and the obtained test solution can be simultaneously used for measuring nitrogen, phosphorus and potassium. However, according to the requirements of NY/T525-2021, during sample pretreatment, after adding sulfuric acid-hydrogen peroxide, the sample needs to be kept stand overnight, and acid required for digestion needs to be continuously supplemented during wet digestion, so that the reagent consumption is large; meanwhile, because the organic fertilizer contains a large amount of organic matters, the organic fertilizer is digested more violently and is easy to generate a large amount of foam, the gushed foam is attached to the wall of the flask and is not easy to be digested completely, and the result is low, so that the digestion is carried out carefully, and a large amount of time is consumed.
Disclosure of Invention
The invention aims to solve the technical problem of providing the application of a heating ashing method for improving the pretreatment efficiency in the determination of phosphorus and potassium in organic fertilizers.
In order to solve the problems, the heating ashing method is applied to the determination of phosphorus and potassium in organic fertilizers, and is characterized in that: placing 1.0g of the air-dried organic fertilizer sample with the accuracy of 0.0001g in a ceramic crucible, placing the ceramic crucible in a muffle furnace for burning, cooling, and transferring the ashed sample into a 100mL beaker; adding 5mL of sulfuric acid solution and 1mL of hydrogen peroxide for heating treatment, placing on an electric heating plate for heating until white smoke appears, cooling, adding a plurality of drops of cold water and hydrogen peroxide, shaking, then adding 20mL of hot water, and continuing heating until the temperature is close to boiling; and finally, completely transferring the content of the beaker into a 100mL volumetric flask by using water, adding water to a constant volume, and filtering to obtain the product for measuring phosphorus and potassium.
The volume concentration of the sulfuric acid solution is 1: 1.
the volume concentration of the hydrogen peroxide is 30%.
The ashing heating condition is that the temperature is 850 ℃ and the time is more than or equal to 20 min.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, organic matters in the organic fertilizer are heated and incinerated by the muffle furnace, the incinerated sample is acidified by a small amount of acid and an oxidant, and the sample is heated and acidified by the electric heating plate, so that batch treatment can be realized, the reagent consumption is reduced, the sample pretreatment time is shortened, and the sample pretreatment efficiency is improved.
2. Tests show that the method compares the organic fertilizer samples subjected to batch treatment by adopting a heating and ashing method with the NY/T525-2021 analysis results, so that the content of phosphorus and potassium in the organic fertilizer is measured without large deviation on experimental data, and the accuracy and the repeatability meet the measurement requirements.
3. Compared with the concentrated sulfuric acid-hydrogen peroxide wet digestion treatment of a standard method, the method improves the inspection efficiency, is safe and convenient to operate, and provides reference for quickly measuring the content of phosphorus and potassium in the organic fertilizer.
Detailed Description
The heating ashing method is applied to the determination of phosphorus and potassium in organic fertilizers:
placing 1.0g of the air-dried organic fertilizer sample with the accuracy of 0.0001g in a ceramic crucible, placing the ceramic crucible in a muffle furnace for burning, cooling, and transferring the ashed sample into a 100mL beaker; adding 5mL of sulfuric acid solution (1:1) and 1mL of hydrogen peroxide with volume concentration of 30%, heating on an electric heating plate at 850 deg.C for 20min or more. Cooling until white smoke appears, adding a plurality of drops of cold water and hydrogen peroxide with the volume concentration of 30%, shaking, then adding 20mL of hot water, and continuing heating until the temperature is close to boiling; and finally, completely transferring the content of the beaker into a 100mL volumetric flask by using water, adding water to a constant volume, and filtering to obtain the product for measuring phosphorus and potassium.
Examples
The method comprises the following main instruments:
TLE204E electronic balance, mettler-toledo; L9/12/P330 muffle furnace, Nabo fever, Germany; EG37C electric hot plate, lebettaceae; cary300 uv-vis spectrophotometer, agilent, usa; PinAAcle 900H atomic absorption spectrometer (equipped with flame atomization emission spectrum), usa PE.
The test sample and the main reagent:
organic fertilizer samples, enterprise submission.
Premium grade pure concentrated sulfuric acid, rho (H) 2 SO 4 ) 1.84 g/mL; analytically pure nitric acid, rho (HNO) 3 ) 1.65 g/mL; hydrogen peroxide, omega (H) 2 O 2 ) 30 percent; sodium hydroxide, 2, 4-dinitrophenol, ammonium molybdate and ammonium metavanadate are all analytically pure; phosphorus standard solution, 1000. mu.g/mL, 50. mu.g/mL; potassium standard solution, 8mg/mL, 100. mu.g/mL.
Treating the sample:
the 5 organic fertilizers are respectively treated by a concentrated sulfuric acid-hydrogen peroxide wet digestion method and a heating ashing method in NY/T525-2021 standard so as to determine phosphorus and potassium (phosphorus pentoxide and potassium oxide) in the organic fertilizers.
Wet digestion sample treatment:
the treatment process of the concentrated sulfuric acid-hydrogen peroxide wet digestion method comprises the following steps: according to the requirement of standard NY/T525-2021, 1.0g (accurate to 0.0001 g) of the air-dried sample is transferred to a 100mL volumetric flask through digestion treatment, and water is added for volume determination and filtration for measuring phosphorus and potassium.
Processing the sample by a heating ashing method:
the phosphorus content color development principle is that under a certain acidity, phosphate ions in a liquid to be detected react with metavanadate and molybdic acid to form yellow ternary heteropoly acid, so that a sample is heated and incinerated and then needs to be treated by adding a proper amount of acid solution and oxidant to ionize potassium and convert phosphorus in the sample into orthophosphate, so that the potassium phosphate is released and exists in the solution in an ionic state. The sulfuric acid solution can dissolve potassium salt and has oxidizability, while the hydrogen peroxide belongs to a strong oxidizer, so that potassium in the sample is completely dissolved, phosphorus in the sample is completely converted into phosphate ions, and the ashed sample is heated by the sulfuric acid solution and the hydrogen peroxide with higher concentration and excessive concentration so as to improve the experimental efficiency.
The sample treatment process by the heating ashing method comprises the following steps: air-drying 1.0g (accurate to 0.0001 g) of the sample in a ceramic crucible, putting the ceramic crucible in a muffle furnace for burning, transferring the ashed sample into a 100mL beaker after cooling, adding 5mL of sulfuric acid solution (1:1) and 1mL of hydrogen peroxide for heating treatment, putting the beaker on an electric hot plate for heating until white smoke appears, cooling, adding a plurality of drops of cold water and hydrogen peroxide and shaking, then adding 20mL of hot water, and continuing to heat until the sample is nearly boiled. The content of the beaker is completely transferred to a 100mL volumetric flask by water, and water is added for constant volume and filtration for measuring phosphorus and potassium.
Determination of phosphorus and potassium:
drawing a phosphorus standard curve: transferring 0, 1.0, 2.0, 5.0, 8.0, 10.0mL and 15.0mL of phosphorus standard solution of 50 mu g/mL into a 50mL volumetric flask, adding water to about 30mL, adding 2 drops of 2, 4-dinitrophenol indicator, adjusting to be just yellowish by using sulfuric acid solution and sodium hydroxide solution, adding 10.0mL of ammonium vanadomolybdate reagent, shaking up, and fixing the volume. After standing at room temperature for 20min, the cells were subjected to colorimetry using a 1cm cuvette at 450 nm. 5.0mL of organic fertilizer filtrate is taken and is subjected to color comparison with standard yeast under the same condition.
Drawing a potassium standard curve: preparing 0.00, 0.50, 1.00, 2.00, 3.00 and 5.00 mu g/mL standard series, taking 2.0mL organic fertilizer filtrate for measuring potassium under the atomic absorption spectrometer luminous intensity emission method, adjusting the zero point of an instrument by using a blank solution, and drawing a standard curve according to the potassium concentration and the indication value of the instrument.
Fifthly, result and discussion:
selection of ashing temperature and time:
as the organic fertilizer has wide raw material sources, such as planting industry, breeding industry, kitchen waste and the like, and has high organic matter content, the ashing temperature and time are selected after a plurality of tests in order to completely ash organic carbon. Experimental results show that the organic carbon can be completely burned by ashing and heating at 850 ℃ for 20 min. If ashing is incomplete due to sample variation, the heating time can be prolonged.
② comparison of the measurement results of two pretreatment methods:
5 organic fertilizer samples are respectively treated by a thermal ashing method and a concentrated sulfuric acid-hydrogen peroxide wet digestion method in NY/T525-plus 2021 standard, the measurement is repeated for 6 times, the phosphorus and the potassium in the organic fertilizer are measured, and the measurement result of the average mass fraction is shown in Table 1. As can be seen from the table 1, the results of phosphorus and potassium of the organic fertilizer by the thermal ashing method and the NY/T525-2021 wet digestion method are basically consistent, and the experimental error is in a required range. The relative standard deviation of phosphorus detected by the two methods is 1.32-2.45%, and the relative standard deviation of potassium detected by the two methods is 1.37-2.35%. Experiments show that the method for detecting the content of phosphorus and potassium by treating the organic fertilizer by a heating and ashing method can be used for replacing the national specified NY/T525-2021 wet digestion method organic fertilizer pretreatment method.
TABLE 1 comparison of results of thermal ashing method and NY/T525-2021 analysis (n = 6)
Figure 538902DEST_PATH_IMAGE001
Analysis of recovery rate of added standard:
taking the principle that the addition amount of a standard solution is close to the content of a substance to be detected, the linear range of a standard curve and the fluctuation factor of an instrument signal into comprehensive consideration, weighing 1 # of organic fertilizer samples, 2 # of organic fertilizer samples and 1.0000g of organic fertilizer samples, 3 # of organic fertilizer samples, 2.0mL of 1000 microgram/mL of phosphorus standard solution, 1.0mL of 8mg/mL potassium standard solution, treating the samples by a heating and ashing method, transferring 5.0mL of liquid to be detected, determining phosphorus by a spectrophotometry method, and transferring 2.0mL of liquid to be detected, and determining potassium by a flare photometry method. The results of 6 determinations were shown in Table 2. As can be seen from Table 2, the recovery rate of the organic fertilizer treated by the heating and ashing method is 96.1-102.4%, and the specified requirements are met.
Table 2 results of the thermal ashing method in the recovery of phosphorus and potassium from organic fertilizers (n = 6)
Figure 318639DEST_PATH_IMAGE002
In summary, in view of the high content of organic matters in the organic fertilizer, the organic fertilizer can be heated, ashed, burned and eliminated, and the organic fertilizer sample is heated, ashed and then acidified by a small amount of acid and oxidant to dissolve phosphorus and potassium therein. The muffle furnace is used for heating the sample, and the electric heating plate is used for heating and acidifying, so that not only can batch treatment be realized, but also the sample pretreatment time is shortened, and the sample pretreatment efficiency is improved. Compared with a standard method, the experimental data obtained by treating the sample by the heating ashing method has no great difference in result, good reproducibility, high recovery rate and safe and convenient experimental process, and provides reference for improving the working efficiency of inspectors and realizing the batched and accurate determination of the content of phosphorus and potassium in the organic fertilizer.

Claims (4)

1. The application of the heating ashing method in the determination of phosphorus and potassium in organic fertilizers is characterized in that: placing 1.0g of the air-dried organic fertilizer sample with the accuracy of 0.0001g in a ceramic crucible, placing the ceramic crucible in a muffle furnace for burning, cooling, and transferring the ashed sample into a 100mL beaker; adding 5mL of sulfuric acid solution and 1mL of hydrogen peroxide for heating treatment, placing on an electric heating plate for heating until white smoke appears, cooling, adding a plurality of drops of cold water and hydrogen peroxide, shaking, then adding 20mL of hot water, and continuing heating until the temperature is close to boiling; and finally, completely transferring the content of the beaker into a 100mL volumetric flask by using water, adding water to a constant volume, and filtering to obtain the product for measuring phosphorus and potassium.
2. The application of the heating ashing method as claimed in claim 1 in the determination of phosphorus and potassium in organic fertilizers, wherein: the volume concentration of the sulfuric acid solution is 1: 1.
3. the application of the heating ashing method as claimed in claim 1 in the determination of phosphorus and potassium in organic fertilizers, wherein: the volume concentration of the hydrogen peroxide is 30%.
4. The application of the heating ashing method as claimed in claim 1 in the determination of phosphorus and potassium in organic fertilizers, wherein: the ashing heating condition is that the temperature is 850 ℃ and the time is more than or equal to 20 min.
CN202210634735.4A 2022-06-07 2022-06-07 Application of heating ashing method in determination of phosphorus and potassium in organic fertilizer Pending CN114993805A (en)

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