CN110596168A - Sample preparation method of silicon-manganese alloy molten sample for spectral analysis - Google Patents
Sample preparation method of silicon-manganese alloy molten sample for spectral analysis Download PDFInfo
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- CN110596168A CN110596168A CN201911028234.6A CN201911028234A CN110596168A CN 110596168 A CN110596168 A CN 110596168A CN 201911028234 A CN201911028234 A CN 201911028234A CN 110596168 A CN110596168 A CN 110596168A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
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Abstract
The invention discloses a sample preparation method of a silicon-manganese alloy molten sample for spectral analysis, which comprises the steps of weighing a silicon-manganese sample, lithium carbonate, strontium nitrate and potassium nitrate according to a certain proportion, grinding and uniformly mixing; and (3) placing lithium tetraborate in a crucible, embedding the mixture in the lithium tetraborate in S3, placing in a sample melting furnace, performing a pre-oxidation step and a melting step, and finally cooling to finish the sample preparation. The invention simplifies the process steps, reduces the pretreatment stage of the platinum crucible protective film and reduces the operation time; meanwhile, the operation difficulty is reduced, and the accuracy is improved. In the oxidation and melting stage, the step of oxidation in a muffle furnace is omitted, so that the use of the muffle furnace is reduced, and meanwhile, the energy is saved; in the melting furnace, the pre-oxidation and melting processes can be automatically completed through self-contained programs, personnel are not required to watch, 90% of manual operation is reduced, and the working intensity and the labor cost are saved.
Description
Technical Field
The method belongs to the field of raw material analysis measurement and test, and particularly relates to a sample preparation method of a silicon-manganese alloy molten sample for spectral analysis, which is applied to X-ray fluorescence (XRF) analysis.
Background
In the prior art, when a silicon-manganese alloy melting sample is prepared by X-ray fluorescence (XRF) spectrum analysis, the silicon-manganese alloy has strong oxidizability and may corrode a crucible, so that the preparation method is complicated and comprises the following specific steps:
firstly, 7.0000g of lithium tetraborate is weighed by a tester in a platinum crucible, 1ml of ammonium iodide solution is added as a release agent, then the platinum crucible is placed in a muffle furnace with the temperature raised to 1000 ℃, after a flux is melted, the crucible is taken out, the crucible is slowly rotated, the lithium tetraborate is uniformly paved on the inner wall of the crucible, and a lithium tetraborate protective layer is formed after cooling;
and secondly, weighing 0.2000g of sample, 1.0000g of mixed flux, 2.0000g of barium peroxide and 0.2000g of lithium bromide, putting the weighed materials into a crucible for manufacturing a lithium tetraborate protective layer, and uniformly mixing. Then placing the crucible into a muffle furnace heated to 800 ℃ for pre-oxidation, wherein the crucible needs to be preheated at a furnace door for 1-2min, then slowly enters a hearth in steps for about 30min, a sample is flowable liquid after oxidation is completed, the pre-oxidation process needs to be operated by an operator all the time on site and operated continuously in a high-temperature environment, and the step needs to be carried out by the muffle furnace to increase the power consumption;
and thirdly, after the pre-oxidation is finished, transferring the crucible to a sample melting furnace for melting, and obtaining a glass fuse piece for XRF analysis after the pre-oxidation is finished.
In conclusion, the existing silicon-manganese alloy melting sample preparation method has the disadvantages of complicated steps, high operation difficulty and low working efficiency, and is not suitable for the rapid analysis requirement in the current production process.
Disclosure of Invention
The invention aims to provide a sample preparation method of a silicon-manganese alloy molten sample for spectral analysis, which aims to solve the problems in the prior art.
The invention is realized by the following technical scheme: a sample preparation method of a silicon-manganese alloy molten sample for spectral analysis is characterized by comprising the following steps: the method comprises the following steps:
s1, weighing lithium carbonate, strontium nitrate and potassium nitrate according to the mass ratio of 1:1:1.5, placing the lithium carbonate, the strontium nitrate and the potassium nitrate into a grinding bowl, grinding and uniformly mixing the lithium carbonate, the strontium nitrate and the potassium nitrate, and placing the mixture into a dryer for later use;
s2, weighing the silicomanganese sample according to the mass ratio of the silicomanganese sample to the mixture of 1:14, grinding and uniformly mixing the silicomanganese sample and the mixture, and putting the mixture into a dryer for later use;
s3, weighing lithium tetraborate according to the mass ratio of 64:14 of the lithium tetraborate to the mixture in the S2, and placing the lithium tetraborate in a crucible;
s4, embedding the mixture obtained in the S2 in the lithium tetraborate in the S3;
s5, placing the crucible in a sample melting furnace, wherein the temperature is 450 ℃, and the time is 2 minutes;
s6, keeping the temperature rise rate of the sample melting furnace at 8 ℃/min until the temperature rises to 850 ℃, keeping the temperature for 8 minutes, wherein the swinging angle of the crucible is 0 ℃ and the swinging rate is 0 time/min;
s7, keeping the temperature rise rate of the sample melting furnace at 8 ℃/min until the temperature rises to 1050 ℃, and keeping the crucible swinging angle at 0 ℃ and the swinging rate at 0 time/min;
s8, keeping 1050 ℃ at a constant temperature, and melting for 5 minutes under the conditions that the crucible swinging angle is 10 degrees and the swinging speed is 10 times/min; melting for 5 minutes under the conditions that the crucible swinging angle is 20 degrees and the swinging speed is 20 times/min; melting for 8 minutes under the conditions of a swing angle of 25 degrees and a swing speed of 30 times/min, and standing for 2 minutes;
and S9, automatically pouring the melted mixture into a mold, and cooling to room temperature to finish the preparation of the sample.
Further: the silicon-manganese alloy is 0.1250g, and 0.5000g of lithium carbonate, 0.5000g of strontium nitrate, 0.7500g of potassium nitrate and 8.0000g of lithium tetraborate flux are taken.
Further: the fineness of the silicomanganese sample is 200 meshes.
The invention has the advantages that: 1. the process steps are simplified, the pretreatment stage of the platinum crucible protective film is reduced, and the operation time is reduced by 10 minutes; meanwhile, the operation difficulty is reduced, and the accuracy is improved. 2. In the oxidation and melting stage, the step of oxidation in a muffle furnace is omitted, so that the use of the muffle furnace is reduced, and meanwhile, the energy is saved; 3. in the melting furnace, the pre-oxidation and melting processes can be automatically completed through self-contained programs, personnel are not required to watch, 90% of manual operation is reduced, and the working intensity and the labor cost are saved.
Detailed Description
The invention discloses a sample preparation method of a silicon-manganese alloy molten sample for spectral analysis, which comprises the following steps:
a burdening stage:
s1, weighing 0.5000 +/-0.003 g of lithium carbonate, 0.5000 +/-0.0003 g of strontium nitrate and 0.7500 +/-0.003 g of potassium nitrate in a surface dish respectively, placing the materials in a grinding bowl, grinding and uniformly mixing the materials, and placing the materials in a dryer for later use;
s2, accurately weighing 0.1250 +/-0.0003 g of silicomanganese (200 meshes) sample, grinding and uniformly mixing the silicon manganese sample and the mixture, and putting the mixture into a dryer for later use; in order to save time, under the premise of ensuring uniform mixing, the materials S1 and S2 can be ground and mixed together;
s3, adding 7.0000 +/-0.0003 g of lithium tetraborate flux into the platinum crucible;
s4, embedding the mixture (i.e. the unmelted sample) obtained in S2 in the lithium tetraborate in S3, and covering a layer of 1.0000 +/-0.0003 g of lithium tetraborate around the sample; note that the sample cannot be in direct contact with the crucible;
a pre-oxidation stage:
s5, placing the crucible in a sample melting furnace, wherein the temperature is 450 ℃, and the time is 2 minutes;
s6, keeping the temperature rise rate of the sample melting furnace at 8 ℃/min until the temperature rises to 850 ℃, keeping the temperature for 8 minutes, wherein the swinging angle of the crucible is 0 ℃ and the swinging rate is 0 time/min;
s7, keeping the temperature rise rate of the sample melting furnace at 8 ℃/min until the temperature rises to 1050 ℃, and keeping the crucible swinging angle at 0 ℃ and the swinging rate at 0 time/min;
melting stage
S8, keeping 1050 ℃ at a constant temperature, and melting for 5 minutes under the conditions that the crucible swinging angle is 10 degrees and the swinging speed is 10 times/min; melting for 5 minutes under the conditions that the crucible swinging angle is 20 degrees and the swinging speed is 20 times/min; melting for 8 minutes under the conditions of a swing angle of 25 degrees and a swing speed of 30 times/min, and standing for 2 minutes;
cooling stage
And S9, automatically pouring the melted mixture into a mold, and cooling to room temperature to finish the preparation of the sample.
In the scheme, main test instruments and reagents comprise an electronic balance, a sample melting furnace (such as the THEOX ADVG type of CLAISSE company in Canada), and a platinum crucible which are all conventional instruments and are sold in the market; and the lithium carbonate, the strontium nitrate, the potassium nitrate and the lithium tetraborate flux are high-grade purities. For experimental purposes, 4 sets of replicates were generally weighed out as described above and ready for use. The sample prepared by the scheme has good stability, small difference of experimental results and high reliability.
Compared with the prior art, the method reduces the pretreatment stage of the platinum crucible protective film and reduces the operation time by 10 minutes. In the oxidation and melting stage, the oxidation stage in a muffle furnace is omitted, so that the investment of instrument equipment is saved, the energy is also saved, the method can simultaneously complete the oxidation and melting process of the sample in a sample melting furnace, the process can be completed through the arrangement of the instrument, the control viscosity is high, the labor cost is low, and the manual operation is reduced by 90%.
Claims (3)
1. A sample preparation method of a silicon-manganese alloy molten sample for spectral analysis is characterized by comprising the following steps: the method comprises the following steps:
s1, weighing lithium carbonate, strontium nitrate and potassium nitrate according to the mass ratio of 1:1:1.5, placing the lithium carbonate, the strontium nitrate and the potassium nitrate into a grinding bowl, grinding and uniformly mixing the lithium carbonate, the strontium nitrate and the potassium nitrate, and placing the mixture into a dryer for later use;
s2, weighing the silicomanganese sample according to the mass ratio of the silicomanganese sample to the mixture of 1:14, grinding and uniformly mixing the silicomanganese sample and the mixture, and putting the mixture into a dryer for later use;
s3, weighing lithium tetraborate according to the mass ratio of 64:14 of the lithium tetraborate to the mixture in the S2, and placing the lithium tetraborate in a crucible;
s4, embedding the mixture obtained in the S2 in the lithium tetraborate in the S3;
s5, placing the crucible in a sample melting furnace, wherein the temperature is 450 ℃, and the time is 2 minutes;
s6, keeping the temperature rise rate of the sample melting furnace at 8 ℃/min until the temperature rises to 850 ℃, keeping the temperature for 8 minutes, wherein the swinging angle of the crucible is 0 ℃ and the swinging rate is 0 time/min;
s7, keeping the temperature rise rate of the sample melting furnace at 8 ℃/min until the temperature rises to 1050 ℃, and keeping the crucible swinging angle at 0 ℃ and the swinging rate at 0 time/min;
s8, keeping 1050 ℃ at a constant temperature, and melting for 5 minutes under the conditions that the crucible swinging angle is 10 degrees and the swinging speed is 10 times/min; melting for 5 minutes under the conditions that the crucible swinging angle is 20 degrees and the swinging speed is 20 times/min; melting for 8 minutes under the conditions of a swing angle of 25 degrees and a swing speed of 30 times/min, and standing for 2 minutes;
and S9, automatically pouring the melted mixture into a mold, and cooling to room temperature to finish the preparation of the sample.
2. The sample preparation method according to claim 1, wherein: the silicon-manganese alloy is 0.1250g, and 0.5000g of lithium carbonate, 0.5000g of strontium nitrate, 0.7500g of potassium nitrate and 8.0000g of lithium tetraborate flux are taken.
3. The sample preparation method according to claim 1, wherein: the silicomanganese sample is 200 meshes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911028234.6A CN110596168A (en) | 2019-10-28 | 2019-10-28 | Sample preparation method of silicon-manganese alloy molten sample for spectral analysis |
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| CN201911028234.6A CN110596168A (en) | 2019-10-28 | 2019-10-28 | Sample preparation method of silicon-manganese alloy molten sample for spectral analysis |
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| US20170276580A1 (en) * | 2014-09-15 | 2017-09-28 | Materiaux Nieka Inc. | Method and apparatus for preparing an analytical sample by fusion |
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Application publication date: 20191220 |