CN117571416A - Soil conductivity standard substance and preparation method thereof - Google Patents
Soil conductivity standard substance and preparation method thereof Download PDFInfo
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- CN117571416A CN117571416A CN202311607181.XA CN202311607181A CN117571416A CN 117571416 A CN117571416 A CN 117571416A CN 202311607181 A CN202311607181 A CN 202311607181A CN 117571416 A CN117571416 A CN 117571416A
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- 239000002689 soil Substances 0.000 title claims abstract description 133
- 239000000126 substance Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000011159 matrix material Substances 0.000 claims abstract description 47
- 238000000227 grinding Methods 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000007873 sieving Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000004927 clay Substances 0.000 claims description 23
- 239000013076 target substance Substances 0.000 claims description 23
- 238000007605 air drying Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims 2
- 239000013077 target material Substances 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 7
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 238000003860 storage Methods 0.000 abstract description 3
- 239000010949 copper Substances 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 7
- 239000010419 fine particle Substances 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000002734 clay mineral Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910000365 copper sulfate Inorganic materials 0.000 description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- WYMDDFRYORANCC-UHFFFAOYSA-N 2-[[3-[bis(carboxymethyl)amino]-2-hydroxypropyl]-(carboxymethyl)amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)CN(CC(O)=O)CC(O)=O WYMDDFRYORANCC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001637 plasma atomic emission spectroscopy Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229960001763 zinc sulfate Drugs 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
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/043—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a granular material
-
- 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
- G01N2001/2893—Preparing calibration standards
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to a standard substance for soil detection, in particular to a soil conductivity standard substance and a preparation method thereof. The invention discloses a soil conductivity standard substance and a preparation method thereof, wherein the method specifically comprises the following steps: preparing a soil matrix; adding a supporting substance; preparing a soil conductivity standard substance; drying; secondary grinding and sieving; according to the invention, the supporting material is added into the soil matrix, and the specific adding time of the supporting material is adopted, so that the uniformity and stability of the soil conductivity standard substance in the prior art can be improved by combining the follow-up grinding process based on the adsorption performance of the supporting material and the similarity of the components of the supporting material and the soil matrix material, and the standard substance with high measuring result uniformity and high storage stability can be provided for the detection of the soil conductivity.
Description
Technical Field
The invention relates to a standard substance for soil detection, in particular to a soil conductivity standard substance and a preparation method thereof.
Background
The standard substance is a standard instrument, a measuring method and a reference substance with reliable checking analysis and test results. Plays an extremely important role in production practice. Standard samples have been widely used in various fields such as industrial production and scientific research since the beginning of the century.
The soil conductivity (soil conductivity) is the sum of anions and cations in the soil extract and represents the salt content of the soil, meaning the ability of the soil to conduct current, expressed by measuring the conductivity of the soil extract, and the unit of measurement is expressed in mS/m (i.e., 10. Mu.S/cm). The determination of the soil conductivity can directly reflect the content of the mixed salt of the soil, and has great significance for determining the difference of space-time distribution of various field parameters, thereby laying a foundation for the popularization and popularization of modern fine agriculture based on information and knowledge.
Through investigation, no report on the soil conductivity standard substance is found at home and abroad, so that the soil conductivity standard substance and the preparation method thereof have important significance for the characterization of soil components, and Chinese patent CN113884349A is a preparation method of the standard substance for soil environment detection: the method comprises the following steps: collecting representative soil according to the characteristics of soil in different regions, and removing impurities through air drying and sieving to obtain a soil matrix; adding proper target substances into the soil matrix according to detection requirements, and then uniformly mixing and aging for a plurality of days; and drying, grinding, uniformly mixing, split charging and setting the obtained soil containing the specific target substances. The preparation method has strong designability, can select soil and additives according to national standards and market demands, prepare the soil matrix standard substance meeting the quality control requirements of soil environment detection, and solve the technical problem that the existing soil detection industry lacks the targeted soil matrix standard substance.
However, the preparation of the soil standard substance based on the method has poor uniformity of distribution of the target substance in the soil, and the stability of the target substance is reduced along with long-term storage of the soil standard sample, which is a key factor that leads to the inability of prolonging the shelf life of the soil standard sample, so that the preparation of the soil conductivity standard substance with good stability and excellent dispersion performance of the target substance is of great significance.
Disclosure of Invention
The invention aims to provide a soil conductivity standard substance with good stability and excellent dispersion performance of a target substance and a preparation method thereof.
The preparation method of the soil conductivity standard substance comprises the following steps:
(1) Soil matrix preparation
(2) Addition of supporting substance: and adding a supporting substance into the soil matrix, and grinding to obtain a soil standard substance matrix material.
(3) Preparing a soil conductivity standard substance: and (3) adding a target substance into the soil standard substance matrix material prepared in the step (2), and grinding at a certain temperature.
(4) And (3) drying: placing the soil added with the different target substances in the step (3) into an oven for drying;
(5) Secondary grinding and sieving: placing the dried soil in the step (4) into a ball mill for secondary grinding to 100-200 meshes;
(6) And (3) setting: and (3) fixing the value of the sample prepared in the step (5) to obtain the soil conductivity standard substance containing the target substance component.
Further, the preparation steps of the soil matrix in the step (1) are as follows: according to the characteristics of the soil sample to be detected, selecting a soil matrix material, air-drying, grinding and sieving.
Further, in the step (2), the supporting material is clay, and the clay is an aggregate of fine particles formed by decomposing and breaking minerals in the rock and mainly consists of fine particles of clay minerals. Clay is soil containing clay mineral fine particles. According to the invention, the clay is preferentially used as the supporting material, the analysis object element is adhered to the supporting material and is strongly supported due to the plasticity of the clay, so that the analysis object element can be uniformly dispersed, the dispersibility and uniformity of the element to be analyzed in the soil matrix are improved, and in addition, the storage stability of the conductivity standard substance is greatly improved due to the supporting and adsorption effects of the clay, so that the service life of the standard substance is prolonged.
Further, in the step (2), the grinding temperature is room temperature, and the grinding is carried out until the particle size is 100-200 meshes.
Further, the target substance in the step (3) is an element type of the soil conductivity commonly used in the art, and the target substance is not particularly limited as long as it is an element or a compound constituting a solid or a liquid at normal temperature and normal pressure, and preferably, the target substance of the present invention may be one or more selected from Cu, zn, ca, al, mg elements.
Further, the content of the relevant elements in the target substance in the step (3) is 0.05-0.2% of the supporting material.
The inventor finds that, due to partial difference of the components of the supporting material and the soil matrix material, when the adding amount of the target substance is low, the relative content of the supporting material in the system is increased to further influence the testing precision, and when the content of the target substance is high, the relative content of the supporting material is reduced to reduce the dispersibility and the adsorption performance of the supporting material on the target substance to further influence the uniformity of the soil conductivity standard substance.
Further, the grinding temperature in the step (3) is 100-250 ℃.
The invention carries out grinding treatment within a specific temperature range, and can promote the absorption and diffusion of target elements into the clay and the soil matrix of the support body under the temperature condition, thereby further improving the dispersion uniformity of the target elements in the soil.
The beneficial effects of the invention are as follows:
according to the preparation method of the soil conductivity standard substance, the soil matrix material and the supporting material are mixed uniformly by grinding preferentially, and then the target substance is added, so that the distribution uniformity and stability of the target substance in soil can be improved compared with a process of mixing the supporting material and the target substance uniformly and then mixing the supporting material and the soil matrix.
The invention adopts clay as a supporting material, and the clay is an aggregate of fine particles formed by decomposing and destroying minerals in rock and mainly consists of the fine particles of clay minerals. The clay is soil containing clay mineral fine particles, and based on the similarity of clay and soil components, the dispersion uniformity of the support material in the soil matrix can be improved, in addition, the clay has a certain adsorption property, and the target element is strongly supported due to the plasticity of the clay or the clay after being adhered on the support material, so that the target element can be relatively stably present in a soil system, and the dispersion uniformity is higher.
According to the invention, after the soil matrix, the supporting material and the elements to be analyzed are mixed, the target object elements can be adsorbed, diffused and the like in the soil matrix and the supporting material by heating and grinding in a specific temperature range, so that the analysis object elements are uniformly and stably dispersed in the soil matrix and the supporting material.
Detailed Description
The following detailed description of embodiments of the invention is exemplary and intended to be illustrative of the invention and not to be construed as limiting the invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise.
Example 1
(1) Preparing a soil matrix: taking a soil sample, wherein the soil sample in the embodiment is yellow tide soil of Henan Anyang, air-drying, fully grinding, sieving with a 100-mesh sieve, and sieving out large particles to obtain a soil matrix.
(2) Addition of supporting substance: and adding ground clay into the soil matrix, wherein the addition amount of the clay is 0.2% of that of the soil matrix, and grinding at room temperature to obtain the soil standard substance matrix material.
(3) Preparing a soil conductivity standard substance: and (3) adding copper sulfate into the soil standard substance matrix material prepared in the step (2) so that the content of Cu element is 0.1% of that of the supporting material, and grinding at 250 ℃.
(4) And (3) drying: placing the soil added with the Cu-containing substances in the step (3) into an oven for drying;
(5) Secondary grinding and sieving: placing the dried soil in the step (4) into a ball mill for secondary grinding to 150-200 meshes;
(6) And (3) setting: and (3) fixing the value of the sample prepared in the step (5) to obtain the Cu-containing soil conductivity standard substance.
Example 2
(1) Preparing a soil matrix: taking a soil sample, wherein the soil sample in the embodiment is yellow tide soil of Henan Anyang, air-drying, fully grinding, sieving with a 100-mesh sieve, and sieving out large particles to obtain a soil matrix.
(2) Addition of supporting substance: the ground clay was added to the soil matrix in the same amount as in example 1, and ground at room temperature to obtain a soil standard substance matrix material.
(3) Preparing a soil conductivity standard substance: and (3) adding zinc sulfate into the soil standard substance matrix material prepared in the step (2) so that the content of Zn element is 0.1% of that of the support material, and grinding at 110 ℃.
(4) And (3) drying: placing the soil added with the Zn-containing substances in the step (3) into an oven for drying;
(5) Secondary grinding and sieving: placing the dried soil in the step (4) into a ball mill for secondary grinding to 150-200 meshes;
(6) And (3) setting: and (3) fixing the value of the sample prepared in the step (5) to obtain the Zn-containing soil conductivity standard substance.
Comparative example 1
(1) Preparing a soil matrix: taking a soil sample, wherein the soil sample in the embodiment is yellow tide soil of Henan Anyang, air-drying, fully grinding, sieving with a 100-mesh sieve, and sieving out large particles to obtain a soil matrix.
(2) Addition of supporting substances and target elements: copper sulfate was added to clay so that the content of Cu element was 0.1% of the support material, and the clay matrix containing the target element was obtained by grinding, and the addition amount of clay was the same as in example 1.
(3) Preparing a soil conductivity standard substance: mixing the soil matrix prepared in the step (1) and the step (2) with a clay matrix containing Cu element, and grinding at 250 ℃.
(4) And (3) drying: placing the soil added with the Cu-containing substances in the step (3) into an oven for drying;
(5) Secondary grinding and sieving: placing the dried soil in the step (4) into a ball mill for secondary grinding to 100-200 meshes;
(6) And (3) setting: and (3) fixing the value of the sample prepared in the step (5) to obtain the Cu-containing soil conductivity standard substance.
Fixed value of standard substance:
uniformity characterization: 20 parts of standard substance sample are randomly taken and placed in a glass bottle, so that soil is fully leached, and the analysis is carried out by adopting a plasma emission spectrometry (ICP-AES). F, checking and verifying the consistency of the product, and determining the value in the next step if the product meets the requirement.
Table 1 results of characterization of examples and comparative examples uniformity tests
n is the number of measurements, x is the arithmetic mean, s is the standard deviation, and RSD is the relative standard deviation. The Fa value of the standard sample prepared by the embodiment of the application is smaller, and the test precision is relatively high, so that the uniformity of the effective components of the sample is good.
Stability test: and randomly extracting the prepared soil standard substances at the 1 st month, the 6 th month, the 8 th month and the 18 th month respectively, and detecting the copper content by adopting the same method. And verifying the stability by adopting a linear fitting method, and further determining the value if the stability meets the requirement. The results of the stability test described in examples 1-2 and comparative examples are as follows.
TABLE 2 stability test results for examples 1-2 and comparative examples
Based on the data of the embodiment, the invention selects the specific adding time of the supporting substance, and the analysis object element can be adsorbed, diffused, gasified, condensed and the like by heating and grinding in a specific temperature range after the soil matrix, the supporting material and the target substance are mixed, so that the analysis object element is immobilized in the soil matrix and the supporting material, and the uniformity and the stability of the standard substance are improved.
(3) And (3) setting: after random sampling of the soil samples of the examples, the copper content of example 1 of the present invention was found to be 2.17.+ -. 0.07ug.g by DPTA leaching (1:2) -ICP-AES -1 。
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (10)
1. The preparation method of the soil conductivity standard substance is characterized by comprising the following steps:
(1) Preparing a soil matrix;
(2) Adding a supporting substance: adding a supporting substance into a soil matrix to obtain a soil standard substance matrix material, and grinding at a certain temperature;
(3) Preparing a soil conductivity standard substance: adding a target substance into the soil standard substance matrix material prepared in the step (2), and grinding at a certain temperature;
(4) And (3) drying: placing the soil added with the target elements in the step (3) into an oven for drying;
(5) Secondary grinding and sieving: placing the dried soil in the step (4) into a ball mill for secondary grinding;
(6) And (3) setting: and (3) fixing the value of the sample prepared in the step (5) to obtain the soil conductivity standard substance containing the target substance component.
2. The method for preparing a soil conductivity standard according to claim 1, wherein the step (1) of preparing the soil matrix comprises the steps of: according to the characteristics of the soil sample to be detected, selecting a soil matrix material, air-drying, grinding and sieving.
3. The method of claim 1, wherein the support material in step (2) is clay.
4. A method for preparing a soil conductivity standard according to claim 3, wherein said clay is added in the amount of 0.2% of the soil matrix in step (2).
5. The method for preparing a soil conductivity standard according to claim 1, wherein the grinding temperature in the step (2) is room temperature, and the grinding is performed to 100-200 mesh.
6. The method of claim 1, wherein the target material in step (3) is selected from one or more of Cu, zn, ca, al, mg elements.
7. The method for preparing a soil conductivity standard according to claim 1, wherein the content of the target substance in the step (3) is 0.05-0.2% of the supporting material.
8. The method for preparing a soil conductivity standard according to claim 1, wherein said grinding temperature in step (3) is 100-250 ℃.
9. The method for preparing a soil conductivity standard according to claim 1, wherein the ball milling conditions in the step (5) are: ball milling the soil to the particle size of 100-200 meshes.
10. A soil conductivity standard prepared by the method for preparing a soil conductivity standard according to any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311607181.XA CN117571416B (en) | 2023-11-29 | 2023-11-29 | Soil conductivity standard substance and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311607181.XA CN117571416B (en) | 2023-11-29 | 2023-11-29 | Soil conductivity standard substance and preparation method thereof |
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| CN117571416A true CN117571416A (en) | 2024-02-20 |
| CN117571416B CN117571416B (en) | 2024-06-14 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007178198A (en) * | 2005-12-27 | 2007-07-12 | Canon Inc | Investigation method for direction of soil contamination |
| JP2009036550A (en) * | 2007-07-31 | 2009-02-19 | Kankyo Technos Kk | Manufacturing method of soil reference material |
| KR20160001832A (en) * | 2014-06-27 | 2016-01-07 | 강원대학교산학협력단 | Method of inhibiting transport of antibiotics in soil using biochars |
| CN113884349A (en) * | 2021-08-27 | 2022-01-04 | 坛墨质检科技股份有限公司 | Preparation method of standard substance for soil environment detection |
| CN115127888A (en) * | 2022-06-28 | 2022-09-30 | 山东省计量科学研究院 | Method for preparing and valuing volatile organic matter standard substance in soil |
| JP7238195B1 (en) * | 2022-07-20 | 2023-03-13 | 日本製紙株式会社 | soil conditioner |
-
2023
- 2023-11-29 CN CN202311607181.XA patent/CN117571416B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007178198A (en) * | 2005-12-27 | 2007-07-12 | Canon Inc | Investigation method for direction of soil contamination |
| JP2009036550A (en) * | 2007-07-31 | 2009-02-19 | Kankyo Technos Kk | Manufacturing method of soil reference material |
| KR20160001832A (en) * | 2014-06-27 | 2016-01-07 | 강원대학교산학협력단 | Method of inhibiting transport of antibiotics in soil using biochars |
| CN113884349A (en) * | 2021-08-27 | 2022-01-04 | 坛墨质检科技股份有限公司 | Preparation method of standard substance for soil environment detection |
| CN115127888A (en) * | 2022-06-28 | 2022-09-30 | 山东省计量科学研究院 | Method for preparing and valuing volatile organic matter standard substance in soil |
| JP7238195B1 (en) * | 2022-07-20 | 2023-03-13 | 日本製紙株式会社 | soil conditioner |
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