CN114755081B - Method for reducing influence of grinding instrument on analysis accuracy of soil sample preparation components - Google Patents

Method for reducing influence of grinding instrument on analysis accuracy of soil sample preparation components Download PDF

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CN114755081B
CN114755081B CN202210309237.2A CN202210309237A CN114755081B CN 114755081 B CN114755081 B CN 114755081B CN 202210309237 A CN202210309237 A CN 202210309237A CN 114755081 B CN114755081 B CN 114755081B
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李盟军
艾绍英
王荣辉
申建
姚建武
宁建凤
王思源
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract

The invention relates to the technical field of soil detection and analysis, in particular to a method for reducing influence of a grinder on analysis accuracy of soil sample preparation components, which aims to reduce influence of a soil grinding process on a soil component analysis result.

Description

Method for reducing influence of grinding instrument on analysis accuracy of soil sample preparation components
Technical Field
The invention relates to the technical field of soil detection and analysis, in particular to a method for reducing influence of a grinding instrument on analysis accuracy of soil sample preparation components.
Background
The soil is used as an essential element for agricultural product production, and the quality of soil fertility and environmental quality directly influences the yield and safety quality of agricultural products. Therefore, the monitoring and scientific research work of soil fertility and soil environment quality is more and more, and the task load of soil sample preparation is heavier and heavier, especially in the soil grinding stage (grinding the soil to the particle size of about 100 meshes). Because the soil is uneven under the influence of various factors such as nature, human factors and the like, the sample preparation before the analysis of the soil sample is very important, and the soil sample preparation before the analysis is very important. The traditional soil sample preparation method comprises the following steps: firstly, the air-dried soil is put on organic glass or wood boards to be crushed, then is porphyrized by a wooden stick or is porphyrized by a porcelain mortar and an agate mortar, and finally is sieved by a soil sieve with a certain mesh number. With the development of industrial technology, more and more soil sample preparation devices are produced, such as planetary ball mills, disk stone grinders, jaw crushing grinders, mortar grinders and the like, wherein the disk grinders and the jaw grinders are highly favored by users due to the advantages of labor saving, time saving and high discharge rate. The material of the grinding instrument cavity comprises various types of agate, zirconia, stainless steel, manganese steel, carbide, corundum and the like, but the material quality of different manufacturers is different, so that the influence degree of the soil grinding instrument on the soil sample preparation quality is different. However, the preparation of soil samples is an extremely important step for obtaining accurate data of soil. Therefore, basic information which influences the grinding quality, such as background values of different elements, the minimum processing amount required by the grinding equipment, the influence of soil residues on the next sample and the like of the grinding equipment in the soil sample preparation process, is mastered, so that the interference pollution in the sample preparation process is reduced, and the soil analysis accuracy is improved.
At present, because there is no clear determination method for the grinding equipment for the key information such as background values of different elements, minimum processing amount and minimum wetting and grinding amount required by the grinding equipment, the influence of the factors on the analysis result is generally ignored when people prepare soil samples, and the result of the soil component analysis may have certain deviation. Therefore, it is necessary to provide a clear measuring method for factors affecting soil analysis, such as a sample preparation background value, a minimum treatment amount, and a minimum wetting amount of a soil grinder, so as to improve the accuracy of soil component analysis.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a method for reducing the influence of a grinder on the analysis accuracy of soil sample preparation components.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides a method for reducing influence of a grinder on analysis accuracy of soil sample preparation components, namely, when the grinder is used for soil sample preparation, the ground sample amount is ensured to be larger than the minimum treatment amount; before the soil sample to be prepared is formally ground, the soil sample not less than the minimum amount of lubrication grinding is taken and put into a grinding instrument for lubrication grinding, and after the lubrication grinding is finished, formal sample preparation is carried out; when the soil sample composition is analyzed, the content of each element in the soil is the value obtained by subtracting the corresponding sample preparation background value from the measured value of each element.
In the soil sample preparation component analysis process, firstly, a grinding instrument is adopted to grind a soil sample to prepare the soil sample, and then subsequent component analysis is carried out, but the grinding equipment influences the result of the soil component analysis on the background values of different elements, the minimum processing amount and the minimum lubricating and grinding amount required by the grinding equipment, and the like, so that a certain deviation exists in the measurement result. Therefore, when the soil sample is prepared, the grinding sample amount is ensured to be larger than the minimum treatment amount, the soil sample not smaller than the minimum grinding amount is firstly taken and put into the grinding instrument for grinding, and then the formal sample preparation is carried out after the grinding is finished, and finally, when the soil sample component is analyzed, the content of each element in the soil is set to be a value obtained by subtracting the corresponding sample preparation background value from the measured value of each element, so that the influence of the grinding instrument on the soil sample preparation analysis is effectively reduced, and the soil component analysis accuracy is improved.
Preferably, the minimum throughput measurement method is: selecting soil with the particle size of less than 5mm, accurately weighing 3-8 parts of soil with different masses according to the gradient, grinding the soil by using a grinder in sequence, collecting and accurately weighing the soil, then calculating the soil loss and the loss rate of the soil in the sample preparation process according to the formulas (1), (2) and (3), and finally obtaining the minimum handling capacity;
m Δ =M 0 -M------(1);
Figure GDA0004073454070000021
Figure GDA0004073454070000022
in the formula: m is a unit of Δ G is the amount of soil lost;
M 0 g, soil mass before grinding;
m is the ground soil mass, g;
s is the soil loss rate,%;
M min minimum throughput of the mill, g;
Figure GDA0004073454070000031
the average value of the soil loss amount is g;
SD is the standard deviation of soil loss, g;
S A acceptable soil loss rate,%; s A The value in the industry is generally 3% and is not more than 5%.
Specifically, when the minimum treatment amount is measured, the selected soil has a mass of 25-1000 g.
Preferably, the method for measuring the minimum amount of lubrication is as follows: selecting soil with the particle size of less than 5mm, grinding the soil with a certain mass by a grinder, purging and cleaning a cavity of the grinder according to a normal soil sample preparation procedure, then selecting 3-6 parts of quartz sand with the same mass, grinding the quartz sand by the grinder in sequence, collecting ground quartz sand samples respectively, determining the content of different elements in the quartz sand samples, and when the content of each element in the quartz sand samples begins to be stable, accumulating the amount of the quartz sand entering the grinder to obtain the minimum wet grinding amount.
Specifically, when the minimum amount of the lubricating and grinding is measured, the mass of the selected soil is 100-500g, and the mass of the selected quartz sand is 15-500 g.
Preferably, the method for measuring the sample preparation background value comprises the following steps: weighing 4-8 parts of quartz sand with the same mass and the particle size of less than 5mm, grinding by using a grinder, respectively collecting ground quartz sand samples, determining the content of different elements in the quartz sand, and when the content of each element in the quartz sand samples begins to be stable, subtracting a blank value of the quartz sand from the content value of the different elements to obtain a numerical value, namely a sample preparation background value of the element in the sample preparation process of the grinder.
Specifically, when the sample preparation background value is measured, the mass of the selected quartz sand is 15-500 g.
Specifically, in the sample preparation background value measurement, the different elements measured in the quartz sand comprise Cd, pb, cr, hg, as, ni, cu, zn, N, P, K, ca, mg, S, mo, B, mn and Fe.
Preferably, the grinder includes, but is not limited to, a disc grinder, a jaw grinder.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a method for reducing influence of a grinder on analysis accuracy of soil sample preparation components, which comprises the steps of providing a method for measuring minimum processing amount, minimum lubricating amount and sample preparation background value in soil grinding and subsequent soil component analysis processes, accurately controlling the minimum processing amount and the minimum lubricating amount of a soil sample preparation sample in the soil grinding process, and removing the sample preparation background value of the soil grinder in the subsequent soil component analysis process, so that the influence of the grinder on the soil sample preparation is effectively reduced, and the accuracy of the soil component analysis is improved.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The quartz sand used in the following examples was previously immersed in 10 to 50% hydrochloric acid, and then the immersed acid was washed with water, repeatedly washed with pure water, and dried for use.
For the disk grinder with discontinuous sample introduction, the maximum quantity is not more than two thirds of the grinding cavity.
Example 1 method for measuring minimum throughput, minimum wet abrasion amount and sample preparation background value of disk grinder
1. Method for measuring minimum throughput
Selecting three kinds of soil with different textures, namely clay, loam and sandy soil with the particle size smaller than 2mm, accurately weighing 3-6 parts of 25-200 g of soil with different textures in each soil according to gradient, grinding the soil by using a disc grinder in sequence, cleaning a cavity of the grinder after each ground sample is swept, grinding the next sample, collecting and accurately weighing the soil, calculating the loss amount and the loss rate of the soil with different textures in the sample preparation process according to formulas (1), (2) and (3), and finally obtaining the minimum treatment capacity of the soil;
m Δ =M 0 -M------(1);
Figure GDA0004073454070000041
Figure GDA0004073454070000042
in the formula: m is Δ G is the amount of soil lost;
M 0 g, soil mass before grinding;
m is the ground soil mass, g;
s is the soil loss rate,%;
M min minimum throughput of the mill, g;
Figure GDA0004073454070000051
the average value of the soil loss amount is g;
SD is the standard deviation of soil loss, g;
S A acceptable soil loss rate,%; s A The value in the industry is generally 3% and is not more than 5%.
The influence of the cavity material of the disc type grinding instrument on the soil loss degree in the grinding process can be evaluated by the measuring method, S A Calculated by 3 percent, doThe minimum treatment amounts of selected sandy soil, loam soil and clay on a disc grinder were determined to be 46, 48g and 50g, respectively.
2. Method for measuring minimum lubrication grinding amount
Selecting heavy metal heavily-polluted soil with the particle size of less than 2mm, weighing 100-500g of heavy metal heavily-polluted soil, grinding by using a disc grinder, purging and cleaning a cavity of the grinder according to a normal soil sample preparation procedure, then weighing 3-6 parts of 15-75 g of analytical pure quartz sand with the same mass, grinding by using the disc grinder in sequence, respectively collecting ground quartz sand samples, and determining the content of Cd, pb, cr, hg, as, ni, cu, zn, N, P, K, ca, mg, S, mo, B, mn and Fe in the ground quartz sand samples, wherein when the content of each element in the ground quartz sand samples begins to be stable, the accumulated amount of the quartz sand entering the grinder is the minimum wet grinding amount. The minimum wet grinding amount for evaluating the influence degree of the material and equipment structure of the disc grinder and the residual quantity of the soil with different pollution degrees on the next sample preparation is 15g.
3. Method for measuring sample preparation background value
Weighing 4-8 parts of 25-200 g of analytical pure quartz sand with the same mass and the particle size of less than 2mm, grinding by using a disc grinder, respectively collecting ground quartz sand samples, determining the content of Cd, pb, cr, hg, as, ni, cu, zn, N, P, K, ca, mg, S, mo, B, mn and Fe in the quartz sand, determining the content of different elements in the sample preparation process of the disc grinder, and evaluating the degree of the influence of the material of the disc grinder contacting with the soil on the soil in the grinding process. When the content of each element in the quartz sand sample begins to be stable, the numerical value obtained by subtracting the content value of the corresponding element in the unground quartz sand from the content value of the different elements is the sample preparation background value of the element in the sample preparation process of the disc grinder. The background values of Pb, cd, cr, cu, zn, ni, hg and As sample preparation in the sample preparation process of the disc grinder are respectively 0.962, undetected, 0.056, undetected and 0.064
Example 2 method for measuring minimum throughput, minimum wet-out and sample preparation background values of jaw grinder
1. Method for measuring minimum throughput
Selecting three kinds of soil with different textures of clay, loam and sandy soil with the particle size of 1-5mm, accurately weighing 4-8 parts of 100-1000 g of soil with different textures in each soil according to gradient, grinding the soil by using a jaw grinder in sequence, cleaning a cavity of the grinder after each grinding, grinding the next sample, collecting and accurately weighing the soil, calculating the loss amount and the loss rate of the soil with different textures in the sample preparation process according to formulas (1), (2) and (3), and finally obtaining the minimum treatment capacity of the soil;
m Δ =M 0 -M------(1);
Figure GDA0004073454070000061
Figure GDA0004073454070000062
in the formula: m is Δ Is the soil loss, g;
M 0 g, soil mass before grinding;
m is the ground soil mass, g;
s is the soil loss rate,%;
M min minimum throughput, g;
Figure GDA0004073454070000063
the average value of the soil loss amount is g;
SD is the standard deviation of soil loss, g;
S A acceptable soil loss rate,%; s A The value in the industry is generally 3% and is not more than 5%.
The influence of cavity materials of the jaw grinder equipment on the soil loss degree in the grinding process can be evaluated through the measuring method, and the minimum treatment capacity of the selected sand, loam and clay on the jaw grinder is respectively determined to be 113 g, 177g and 204g.
2. Method for measuring minimum lubrication grinding amount
Selecting heavy metal heavily-polluted soil with the grain size of 1-5mm, weighing 250-500 g of heavy metal heavily-polluted soil, grinding by using a jaw grinder, purging and cleaning a cavity of the grinder according to a normal soil sample preparation procedure, then weighing 4-6 parts of 25-500 g of analytical pure quartz sand with the same mass, grinding by using the jaw grinder in sequence, respectively collecting ground quartz sand samples, and determining the content of Cd, pb, cr, hg, as, ni, cu, zn, N, P, K, ca, mg, S, mo, B, mn and Fe in the ground quartz sand samples, wherein when the content of each element in the ground quartz sand samples begins to be stable, the accumulated amount of the quartz sand entering the grinder is the minimum wet grinding amount. The method is used for evaluating the influence degree of jaw grinder material and equipment structure and the residual quantity of soil with different pollution degrees on the next sample preparation sample and determining the minimum wetting grinding quantity of 50g for thoroughly eliminating the residual influence.
3. Method for measuring sample preparation background value
Weighing 4-8 parts of 100-500g of analytically pure quartz sand with the same mass and the particle size of 1-3 mm, grinding by using a jaw grinder, respectively collecting ground quartz sand samples, determining the contents of Cd, pb, cr, hg, as, ni, cu, zn, N, P, K, ca, mg, S, mo, B, mn and Fe in the quartz sand, determining background values of different elements in the sample preparation process of the jaw grinder, and evaluating the degree of influence of the jaw grinder material contacting with soil on the soil in the grinding process. When the content of each element in the quartz sand sample begins to be stable, the numerical value obtained by deducting the content of the corresponding element in the quartz sand which is not ground from the content of the different elements is the sample preparation background value of the element in the jaw grinder sample preparation process. The background values of Pb, cd, cr, cu, zn, ni, hg and As sample preparation in the sample preparation process of the jaw grinding instrument are all undetected.
Embodiment 3 method for reducing influence of grinding instrument on analysis accuracy of soil sample preparation components
Crushing soil on a hard wood board, sorting out impurities, dividing a crushed soil sample with required weight by a quartering method, enabling the particle size of the crushed soil sample to be smaller than 10mm, uniformly mixing, and then feeding the mixture into a grinder (a disc grinder or a jaw grinder) through a feed opening for grinding until all the mixture passes through a 100-mesh sieve. Before actual polishing, the minimum treatment amount, minimum wet polishing amount and sample preparation background value in a disc-type polishing machine or a jaw-type polishing machine were measured in the same manner as in example 1 or example 2. Then, the soil is formally ground.
When preparing a soil sample, ensuring that the sample preparation amount is larger than the minimum treatment amount; before the prepared soil sample is formally ground, putting the soil sample with the minimum grinding amount into a grinding instrument for instrument grinding, and formally preparing a sample after the grinding is finished; and when the soil composition is analyzed, the content of each element in the soil is a value obtained by subtracting the corresponding sample preparation background value from the measured value of each element. Thereby effectively reduced the influence of grinding appearance to soil system appearance analysis, improved soil composition analysis's accuracy.
The traditional soil grinding method does not pay attention to the influence of the minimum treatment amount and the minimum lubrication amount on the soil grinding, and does not consider the sample preparation background value of the grinding equipment when the soil components are ground.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.

Claims (6)

1. A method for reducing influence of a grinding instrument on analysis accuracy of soil sample preparation components is characterized in that when the grinding instrument is used for soil sample preparation, the ground sample amount is ensured to be larger than the minimum processing amount; before the soil sample to be prepared is formally ground, the soil sample with the minimum amount of lubrication grinding is taken firstly and put into a grinding instrument for lubrication grinding, and formally sample preparation is carried out after the lubrication grinding is finished; when the soil sample composition is analyzed, the content of each element in the soil is a value obtained by subtracting the corresponding sample preparation background value from the measured value of each element;
the method for measuring the minimum treatment capacity comprises the following steps: selecting soil with the particle size of less than 5mm, accurately weighing 3-8 parts of soil with different masses according to the gradient, grinding the soil by using a grinding instrument in sequence, collecting and accurately weighing the soil, then calculating the soil loss and the loss rate of the soil in the sample preparation process according to the formulas (1), (2) and (3), and finally obtaining the minimum treatment capacity:
m Δ =M 0 -M ------(1);
Figure FDA0004073454060000011
Figure FDA0004073454060000012
in the formula: m is Δ Is the soil loss, g;
M 0 g, soil mass before grinding;
m is the ground soil mass, g;
s is the soil loss rate,%;
M min minimum throughput of the mill, g;
Figure FDA0004073454060000013
the average value of the soil loss amount is g;
SD is the standard deviation of soil loss, g;
S A acceptable soil loss rate,%; s. the A The value of (A) is 3% -5%;
the method for measuring the minimum lubrication and abrasion amount comprises the following steps: selecting soil with the particle size of less than 5mm, firstly selecting soil with a certain mass, grinding by a grinding instrument, purging and cleaning a cavity of the grinding instrument according to a soil sample preparation procedure, then selecting 3-6 parts of quartz sand with the same mass of each part of quartz sand, grinding by the grinding instrument in sequence, respectively collecting ground quartz sand samples, determining the content of different elements in the samples, and when the content of each element in the quartz sand samples begins to be stable, accumulating the amount of the quartz sand entering the grinding instrument before the stabilization to be the minimum wet grinding amount;
the method for measuring the sample preparation background value comprises the following steps: weighing 4-8 parts of quartz sand with the same mass and the particle size smaller than 5mm, grinding by using a grinder, respectively collecting ground quartz sand samples, determining the content of different elements in the ground quartz sand, and when the content of each element in the quartz sand samples begins to be stable, subtracting the value of the content of the corresponding element in the unground quartz sand from the content of the different elements to obtain the sample preparation background value of the corresponding element in the sample preparation process of the grinder.
2. The method of claim 1, wherein the soil is selected to have a mass of 15-1000 g for minimum throughput measurement.
3. The method for reducing the influence of the grinder on the analysis accuracy of the soil sample preparation components as claimed in claim 1, wherein in the measurement of the minimum wet grinding amount, the soil is selected to have a mass of 100-500g, and then the quartz sand is selected to have a mass of 15-100 g.
4. The method for reducing the influence of the grinder on the analysis accuracy of the soil sample preparation components as claimed in claim 1, wherein the mass of the selected quartz sand in the determination of the sample preparation background value is 15-500 g.
5. The method for reducing influence of the grinding instrument on analysis accuracy of soil sample preparation components As claimed in claim 1, wherein in sample preparation background value determination, different elements determined in the quartz sand comprise Cd, pb, cr, hg, as, ni, cu, zn, N, P, K, ca, mg, S, mo, B, mn and Fe.
6. The method for reducing influence of the grinder on analysis accuracy of soil sample preparation components according to claim 1, wherein the grinder is a disc grinder or a jaw grinder.
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