CN113237717A - Improved high-aluminum slag modifier sample preparation method - Google Patents
Improved high-aluminum slag modifier sample preparation method Download PDFInfo
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- CN113237717A CN113237717A CN202110505228.6A CN202110505228A CN113237717A CN 113237717 A CN113237717 A CN 113237717A CN 202110505228 A CN202110505228 A CN 202110505228A CN 113237717 A CN113237717 A CN 113237717A
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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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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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
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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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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Abstract
The invention provides an improved high-aluminum slag modifier sample preparation method, which comprises the following steps: A) crushing the high-aluminum slag modifier to-10 to-5 mm, and then performing condensation separation to obtain a primary separation sample; B) passing the primarily separated sample through a 3-5 mm sieve, passing the reduced sample through a 1-2 mm sieve for 4 times, passing the obtained sample through a 0.2-0.5 mm sieve for 4 times, weighing the materials on the sieve, detecting the content of metallic aluminum in the materials under the sieve by a chemical analysis method, and calculating according to a formula to obtain the content W of the metallic aluminum in the high-aluminum slag modifier sampleMal. This application is through increasing the grinding of 1 ~ 2mm granularity level, adjusting 0.2 ~ 0.5mm granularity level and grinding number of times and time, has improved and has showing at present that the too much great problem that leads to the testing result fluctuation of the material that can not sieve that exists, has realized that metallic aluminum content in high-alumina slag modifier detects good reproducibility's purpose, can popularize and apply in the metallurgical industry.
Description
Technical Field
The invention relates to the technical field of high-aluminum slag modifier, in particular to an improved sample preparation method of the high-aluminum slag modifier.
Background
The high-aluminum slag modifier is formed by mixing granular metal aluminum and slag modifier, the measurement of the metal aluminum at present consists of two parts of sample preparation link weighing measurement (an upper part of a sieve) and chemical analysis measurement (a lower part of the sieve), the high-aluminum slag modifier is obtained by grinding, sieving and then weighing measurement, and the metal aluminum in the weighing measurement accounts for more than 85 percent.
In the process of measuring the aluminum content in the high-aluminum slag modifier, the metal aluminum has better ductility, can not be completely ground and sieved when an analysis sample is prepared, the slag modifier coated on the surface of the metal aluminum is difficult to separate, the fluctuation of the measurement result of the metal aluminum is large, the detection of the metal aluminum content is influenced, and the repeatability of the detection is poor.
Disclosure of Invention
The invention aims to solve the technical problem of providing an improved sample preparation method for a high-aluminum slag modifier, which aims to realize good repeatability and high accuracy of detection of the content of metallic aluminum in the high-aluminum slag modifier.
In view of this, the application provides an improved high-aluminum slag modifier sample preparation method, which includes the following steps:
A) crushing the high-aluminum slag modifier to-10 to-5 mm, and then performing condensation separation to obtain a primary separation sample;
B) passing the primarily separated sample through a 3-5 mm sieve, passing the contracted sample through a 1-2 mm sieve for 4 times, passing the obtained sample through a 0.2-0.5 mm sieve for 4 times, weighing the material on the sieve, detecting the content of metallic aluminum in the material under the sieve by a chemical analysis method, and calculating according to a formula (I) to obtain the content W of the metallic aluminumMAl；
The time for passing through the 1-2 mm sieve for 4 times is respectively as follows: the first time is 40-35 s, the second time is 35-30 s, the third time is 30-25 s, the fourth time is 25-20 s, and the time is decreased progressively;
the time for passing through a 0.2-0.5 mm sieve for 4 times is respectively as follows: the first time is 40-35 s, the second time is 35-30 s, the third time is 30-25 s, the fourth time is 25-20 s, and the time is decreased progressively;
wherein m isOn the upper partThe mass of the oversize material after the grinding of the 0.2-0.5 mm size fraction is finished, and the unit is gram (g);
mlower partThe mass of the undersize is the mass of the undersize after the grinding of the 0.2-0.5 mm size fraction is finished, and the unit is gram;
mgeneral assemblyIs the total mass in grams used to prepare the assay;
Wunder MAlThe result of undersize detection was%.
Preferably, in the step A), the division is carried out by three dividers and then the dividers are combined together.
Preferably, in step a), the fractionation is followed by drying.
Preferably, the drying temperature is 100-110 ℃.
Preferably, the weighing is specifically as follows: weighing the sample on the sieve to calculate the proportion, and carrying out chemical analysis and determination on the sample on the sieve.
Preferably, step B) is specifically:
passing the primarily separated sample through a 3mm sieve, passing the reduced sample through a 1mm sieve for 4 times, passing the obtained sample through a 0.2mm sieve for 4 times, finally weighing the materials on the sieve, detecting the content of the metallic aluminum in the materials under the sieve by a chemical analysis method, and calculating according to a formula (I) to obtain the content W of the metallic aluminumMal。
Preferably, the time for passing through the 1-2 mm sieve for 4 times is respectively as follows: first 35s, second 30s, third 25s, fourth 20 s.
Preferably, the time for passing through the sieve of 0.2-0.5 mm for 4 times is respectively as follows: first 35s, second 30s, third 25s, fourth 20 s.
The application provides an improved high-aluminum slag modifier sample preparation method, which specifically comprises the following steps: crushing the high-aluminum slag modifier to-10 to-5 mm, and then performing condensation separation to obtain a primary separation sample; then, the primarily separated sample passes through a 3-5 mm sieve, the contracted sample passes through a 1-2 mm sieve for 4 times, the obtained sample passes through a 0.2-0.5 mm sieve for 4 times, and finally, the weight is weighed and the formula is calculated to obtain the content W of the metallic aluminumMAl(ii) a This application is through increasing the grinding of 1 ~ 2mm granularity level, adjusting 0.2 ~ 0.5mm granularity level and grinding number of times and time, has improved and has showing at present that the too much great problem that leads to the testing result fluctuation of the material that can not sieve that exists, has realized that metallic aluminum content in high-alumina slag modifier detects good reproducibility's purpose, can popularize and apply in the metallurgical industry.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
In view of the problems that the sieved materials cannot be completely ground and sieved and are difficult to separate from the slag agent in the prior art, the invention provides an improved high-aluminum slag modifier sample preparation method, which increases grinding times and time of 1-2 mm and 0.2-0.5 mm, gradually reduces the grinding sample amount, makes the fluctuation of a measurement result smaller, and finally makes the detection of metal aluminum have good repeatability and high accuracy. Specifically, the embodiment of the invention discloses an improved high-aluminum slag modifier sample preparation method, which comprises the following steps:
A) crushing the high-aluminum slag modifier to-10 to-5 mm, and then performing condensation separation to obtain a primary separation sample;
B) passing the primarily separated sample through a 3-5 mm sieve, passing the contracted sample through a 1-2 mm sieve for 4 times, passing the obtained sample through a 0.2-0.5 mm sieve for 4 times, weighing the material on the sieve, detecting the content of metallic aluminum in the material under the sieve by a chemical analysis method, and calculating according to a formula (I) to obtain the content W of the metallic aluminumMAl；
The time for passing through the 1-2 mm sieve for 4 times is respectively as follows: the first time is 40-35 s, the second time is 35-30 s, the third time is 30-25 s, the fourth time is 25-20 s, and the time is decreased progressively;
the time for passing through a 0.2-0.5 mm sieve for 4 times is respectively as follows: the first time is 40-35 s, the second time is 35-30 s, the third time is 30-25 s, the fourth time is 25-20 s, and the time is decreased progressively;
wherein m isOn the upper partThe mass of the oversize material after the grinding of the 0.2-0.5 mm size fraction is finished, and the unit is gram (g);
mlower partThe mass of the undersize is the mass of the undersize after the grinding of the 0.2-0.5 mm size fraction is finished, and the unit is gram;
mgeneral assemblyIs the total mass in grams used to prepare the assay;
Wunder MAlThe result of undersize detection was%.
In the sample preparation process of the improved high-aluminum slag modifier, the high-aluminum slag modifier is firstly crushed to-10 mm-5 mm, in a specific embodiment, the high-aluminum slag modifier is crushed to-10 mm, and then the crushed sample is subjected to division, wherein the division specifically comprises the following steps: the crushed samples were passed successively three times through a dicer and then brought together. And drying the reduced sample to obtain a primary separation sample. The drying temperature is 100-110 ℃.
According to the invention, the primarily separated sample is sieved by a 3-5 mm sieve, the condensed sample is sieved by a 1-2 mm sieve for 4 times, and the obtained sample is sieved by a 0.2-0.5 mm sieve for 4 times; in the process, the primarily separated sample is completely crushed and then passes through a 3-5 mm sieve, more specifically a 3mm sieve. And then, separating out a part of samples, and passing through a 1-2 mm sieve for 4 times, specifically passing through the 1mm sieve for 4 times, wherein the time of 4 times is specifically as follows: the first time is 40-35 s, the second time is 35-30 s, the third time is 30-25 s, the fourth time is 25-20 s, and the time is decreased progressively; more specifically: 35s for the first time, 30s for the second time, 25s for the third time and 20s for the fourth time. And finally, sieving the mixture for 4 times through a 0.2-0.5 mm sieve, specifically sieving the mixture for 4 times through a 0.2mm sieve, wherein the time of 4 times is specifically as follows: the first time is 40-35 s, the second time is 35-30 s, the third time is 30-25 s, the fourth time is 25-20 s, and more specifically: 35s for the first time, 30s for the second time, 25s for the third time and 20s for the fourth time. After the division, the sample is screened, the particle size is gradually reduced, and the amount of the ground sample is gradually reduced, so that the grinding is sufficient, and the detection of the aluminum content is facilitated.
According to the invention, the oversize fraction is weighed and proportioned and the undersize fraction is analyzed and determined, the metallic aluminum content is calculated according to a formula, and the oversize fraction can be regarded as pure aluminum after the screening.
In order to further understand the present invention, the following examples are provided to illustrate the sample preparation method of the improved high-alumina slag modifier of the present invention, and the scope of the present invention is not limited by the following examples.
Examples
Crushing a large sample of the high-aluminum slag modifier to-10 mm, continuously passing the sample through a clean and dry two dividers for three times, then combining the samples together, dishing the sample, and putting the sample into a drying oven at 105 +/-5 ℃ for drying; crushing the dried sample by a crusher until the dried sample completely passes through a 3mm sieve, reducing 200g of the sample, grinding the sample to pass through a 1mm sieve (35 s for the first time, 30s for the second time, 25s for the third time and 20s for the fourth time), grinding the sample to pass through a 0.2mm sample sieve (35 s for the first time, 30s for the second time, 25s for the third time and 20s for the fourth time), weighing the part above the sieve to calculate the proportion and analyzing and determining the part below the sieve by using a chemical formula, and calculating the content of the metallic aluminum by using a formula;
in the formula: m isOn the upper part-mass on sieve after grinding of 0.2mm fraction in grams (g);
mlower part-mass under sieve after grinding of 0.2mm fraction in grams (g);
mgeneral assembly-total mass in grams (g) used to prepare the assay;
Wunder MAl-undersize detection,%.
In order to highlight the effect of the technical scheme of the application, several aspects of improvement are performed, and the difference only lies in the difference of test methods in a table, specifically:
one) improving the first and adjusting the grinding times and time of 1mm granularity level
1. Keeping the grinding time consistent and controlling the grinding times
TABLE 1 data sheet of different grinding times and time
2. The grinding times are kept consistent (4 times), the grinding time is controlled (since the aluminum metal particles are malleable and gradually decrease with the grinding amount)
TABLE 2 data sheet for different grinding times
According to the analysis of the experimental results, when the grinding times of the 1mm particle size grade are kept consistent (4 times), the grinding time is controlled to be 35s for the first time, 30s for the second time, 25s for the third time and 20s for the fourth time, the fluctuation is small, and the metal aluminum detection result of the high-aluminum slag modifier is stable.
Second) improving the second, adjusting the grinding times and time of 0.2mm granularity level
1. Keeping the grinding time consistent, controlling the grinding times, and respectively obtaining the following detection results:
TABLE 3 data sheet for different grinding times and times
2. The grinding times are kept consistent (4 times), the grinding time is controlled (since the aluminum metal particles are malleable and the grinding time is gradually reduced along with the reduction of the sample amount), and the detection results are respectively as follows:
TABLE 4 data sheet for different grinding times
According to the analysis of the experimental results, when the grinding times of the 0.2mm particle size grade are kept consistent (4 times), the grinding time is controlled to be 35s for the first time, 30s for the second time, 25s for the third time and 20s for the fourth time, the fluctuation is small, and the metal aluminum detection result of the high-aluminum slag modifier is stable.
Comparative experiment (III)
The method for measuring the content of metallic aluminum in the high-aluminum slag modifier by adopting the existing method is compared with the method, and the measurement result is shown in the following table:
TABLE 5 data comparison of the method of the present invention with the existing methods
From the comparison results in the table, the precision of the method is obviously superior to that of the existing method (the sample preparation method of the high-aluminum slag modifier has no national standard or standard, so that the enterprise standard is used, namely the instruction of the sample preparation and component detection operation of the high-aluminum slag modifier).
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. An improved high-aluminum slag modifier sample preparation method comprises the following steps:
A) crushing the high-aluminum slag modifier to-10 to-5 mm, and then performing condensation separation to obtain a primary separation sample;
B) passing the primarily separated sample through a 3-5 mm sieve, passing the contracted sample through a 1-2 mm sieve for 4 times, passing the obtained sample through a 0.2-0.5 mm sieve for 4 times, weighing the material on the sieve, detecting the content of metallic aluminum in the material under the sieve by a chemical analysis method, and calculating according to a formula (I) to obtain the content W of the metallic aluminumMAl；
The time for passing through the 1-2 mm sieve for 4 times is respectively as follows: the first time is 40-35 s, the second time is 35-30 s, the third time is 30-25 s, the fourth time is 25-20 s, and the time is decreased progressively;
the time for passing through a 0.2-0.5 mm sieve for 4 times is respectively as follows: the first time is 40-35 s, the second time is 35-30 s, the third time is 30-25 s, the fourth time is 25-20 s, and the time is decreased progressively;
wherein m isOn the upper partThe mass of the oversize material after the grinding of the 0.2-0.5 mm size fraction is finished, and the unit is gram (g);
mlower partThe mass of the undersize is the mass of the undersize after the grinding of the 0.2-0.5 mm size fraction is finished, and the unit is gram;
mgeneral assemblyIs the total mass in grams used to prepare the assay;
Wunder MAlThe result of undersize detection was%.
2. A sample preparation method as claimed in claim 1, wherein in step a), the division is performed three times by using a splitter and then combined together.
3. A sample preparation method as claimed in claim 1, characterized in that in step a), the fractionation is followed by drying.
4. A sample preparation method as claimed in claim 3, wherein the drying temperature is 100-110 ℃.
5. A sample preparation method as claimed in claim 1, wherein the weighing is in particular: weighing the sample on the sieve to calculate the proportion, and carrying out chemical analysis and determination on the sample on the sieve.
6. A sample preparation method according to claim 1, wherein step B) is specifically:
passing the primarily separated sample through a 3mm sieve, passing the reduced sample through a 1mm sieve for 4 times, passing the obtained sample through a 0.2mm sieve for 4 times, finally weighing the materials on the sieve, detecting the content of the metallic aluminum in the materials under the sieve by a chemical analysis method, and calculating according to a formula (I) to obtain the content W of the metallic aluminumMal。
7. The sample preparation method according to claim 1, wherein the time for passing through the 1-2 mm sieve for 4 times is respectively as follows: first 35s, second 30s, third 25s, fourth 20 s.
8. The sample preparation method according to claim 1, wherein the time for passing through the 0.2-0.5 mm sieve for 4 times is respectively as follows: first 35s, second 30s, third 25s, fourth 20 s.
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Application publication date: 20210810 |