CN111289548B - Sample powder arrangement method during sample wafer pressing for XRFS analysis - Google Patents
Sample powder arrangement method during sample wafer pressing for XRFS analysis Download PDFInfo
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- CN111289548B CN111289548B CN202010183744.7A CN202010183744A CN111289548B CN 111289548 B CN111289548 B CN 111289548B CN 202010183744 A CN202010183744 A CN 202010183744A CN 111289548 B CN111289548 B CN 111289548B
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- 239000000843 powder Substances 0.000 title claims abstract description 62
- 238000004458 analytical method Methods 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000003825 pressing Methods 0.000 title claims abstract description 19
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 40
- 239000010959 steel Substances 0.000 claims abstract description 40
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000004327 boric acid Substances 0.000 claims abstract description 17
- 239000002356 single layer Substances 0.000 claims abstract description 4
- 238000007790 scraping Methods 0.000 claims description 8
- 229910000851 Alloy steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 238000005056 compaction Methods 0.000 claims 1
- 230000006835 compression Effects 0.000 claims 1
- 238000007906 compression Methods 0.000 claims 1
- 239000003826 tablet Substances 0.000 description 18
- 238000004846 x-ray emission Methods 0.000 description 17
- 235000012431 wafers Nutrition 0.000 description 13
- 238000005265 energy consumption Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 2
- 230000008092 positive effect Effects 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000007891 compressed tablet Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009957 hemming Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000009700 powder processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000004876 x-ray fluorescence Methods 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
- 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
-
- 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
- G01N23/2204—Specimen supports therefor; Sample conveying means therefore
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to a method for arranging sample powder during sample wafer pressing for XRFS analysis. The technical scheme is as follows: the square steel plates with the thicknesses of 2.0mm and 1.0mm are provided with the same corner holes and large round holes, and the large round hole of the square steel plate with the thickness of 2.0mm is provided with a counter bore; and (3) movably connecting the corner holes of the two square steel plates by using a cylindrical pin, wherein the side with the counter bore faces upwards, and flatly laying a single-layer tissue between the two square steel plates to obtain the paper bottom sample loading tray. Placing 1.5-2.0 g of boric acid on a lower pressure head in a bin of a tablet press, filling a paper bottom sample loading disc with sample powder to be pressed and leveling, loading a paper towel sample loading disc and the sample powder to be pressed into a loading bin of the tablet press, and pressing the sample powder to be pressed and the paper bottom of the paper bottom sample loading disc to the loading bin of the tablet press from the upper plane of the paper towel sample loading disc by using a pressure lever, thus finishing the arrangement of the sample powder. The invention has the characteristics of simple structure of the paper bottom sample loading plate, high sample loading speed, small sample quality fluctuation and high sample piece strength.
Description
Technical Field
The invention belongs to the technical field of sample wafer pressing for XRFS analysis. In particular to a method for arranging sample powder when sample wafers for XRFS analysis are pressed.
Background
In the application of X-ray fluorescence spectroscopy (XRFS) analysis, the preparation of sample pieces for analytical measurement has been a technology-intensive task. At present, mature sample slice preparation technologies comprise a method for preparing a glass slice by melting borate, a method for preparing a metal slice by remelting in an induction furnace and a method for tabletting powder. Wherein, the powder tabletting method has wide application due to high speed and low cost of preparing the sample tablet; in the tableting analysis, the particle size of the test piece powder has a large influence on the analysis result, the tableting rate of the compressed tablet and the strength of the test piece.
In order to improve the accuracy of the analysis results and reduce the effect of particle size, the influence of particle size effect on X-ray fluorescence spectroscopy analysis of sintered ore [ J ] metallurgical analysis, 2006, 26 (3): 92-93) and document 2 (Liu Sha, etc.. the influence of particle size of sample powder processing on the analysis results was studied using a tabletting method with an X-ray fluorescence analyzer for analyzing clinker components [ J ] cement technology, 2004(6):96-99), and an appropriate particle size and appropriate processing method suitable for each of the samples were found, although the preparation process was simplified with respect to melt tabletting, the sample loading speed was still slow with respect to tabletting technology with a fast tabletting speed in tabletting with boric acid substrate hemming; in the tabletting method using the plastic ring, the amount of the sample powder and the effective pressed sample powder cannot be controlled, and the tabletting efficiency and the strength of the sample are affected.
In order to solve the problem of avoiding using a binding agent when coal samples are pressed, in the document 3 (Li-Li et al. high pressure sample preparation X-ray fluorescence spectrometry for measuring 17 elements and ash content [ J ]. analytical chemistry, 2014, 42 (2): 283-.
In order to improve the strength and the sample loading speed of sample wafers for analysis, "a tabletting method for XRFS sample wafers for analysis of boric acid substrate" (CN201910728811.6) patent technology, it is proposed that a backing film is spread on a boric acid substrate layer, and then sample powder is spread so that the backing film is completely covered with the sample powder, which solves the problem that the amount of sample powder used is large, but the fluctuation of the amount of the same type of sample powder is still large, and in order to improve the strength of sample wafers, the sample powder is spread as much as possible during sample loading, and it still takes a long time to completely cover a paper substrate with the sample powder by a sample spoon and to smear the sample.
In summary, the technical defects of the prior art are as follows: the sample loading is assisted by using a backing film, so that the sample powder surface flattening process is long, and the sample loading time is long; the quality fluctuation of the effective sample powder is large during tabletting; when higher pressure is used for tabletting, the energy consumption is high; the tablet press and the matched equipment have large investment and consumption.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide a method for arranging sample powder when sample wafers for XRFS analysis are pressed, wherein the sample wafers for XRFS analysis are simple in structure, high in sample loading speed, small in sample quality fluctuation, low in tabletting energy consumption and high in sample wafer strength.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
step one, a square steel plate with the thickness of 1.0mm and the side length of 45mm is provided with an angle hole with the aperture of 2.2mm and a large round hole with the aperture of 36mm, and an upper hole frame is obtained.
The hole center of the corner hole is positioned on the angular bisector of any right angle of the square steel plate, the distance between the hole center of the corner hole and the right angle is 3mm, and the center of the large round hole is positioned at the center of the square steel plate.
And step two, firstly, forming a corner hole and a large round hole which are the same as the hole diameter and the hole center position of the upper hole frame on a square steel plate with the thickness of 2.0mm and the side length of 45mm, and then forming a counter bore at the hole opening of the large round hole, wherein the diameter of the counter bore is 38.5mm, and the hole depth of the counter bore is 1.0 mm. The side with the counter bore is called the front side of the square steel plate, and vice versa; then, the wall of the counter bore is processed into teeth, the tooth space is 0.7mm, the width of the tooth space is 0.5mm, and the radial depth of the tooth space is 0.2 mm.
4 small round holes with the diameter of 1.0mm are uniformly formed by taking the center of the large circle as the symmetrical center, and the 4 small round holes are positioned on the circumference with the diameter of 37 mm. And respectively inserting steel columns with the length of 3mm and the diameter of 1.0mm into each small circular hole, wherein one end of each of 4 steel columns is 0-0.2 mm higher than the front surface of the square steel plate, and thus obtaining the lower hole frame.
And step three, movably connecting the upper hole frame and the lower hole frame through the corner holes of the upper hole frame and the corner holes of the lower hole frame by using cylindrical pins with the diameters of 2.0mm, wherein the upper hole frame is positioned on the lower hole frame, the front side of a square steel plate of the lower hole frame faces upwards, and the column length of the cylindrical pins is 3.5-6 mm, so that the sample loading frame is obtained.
And step four, rotating the upper hole frame of the sample loading frame around the cylindrical pin, covering a single-layer tissue piece with the side length of 40mm on the lower hole frame, rotating the upper hole frame around the cylindrical pin to be completely superposed with the lower hole frame, pressing the tissue piece by the upper hole frame, and fixing the upper hole frame and the lower hole frame by using a spring clamp to obtain the sample loading tray for the paper bottom.
And fifthly, placing 1.5-2.0 g of boric acid on a lower pressure head in a bin of the tablet press to enable the boric acid to cover all the pressure surfaces.
And step six, filling the sample tray with the sample powder to be pressed into the paper bottom, scraping the sample powder to be pressed by using a scraping blade with the width of 40mm, and removing the redundant sample powder to be pressed.
And step seven, firstly, loading the paper towel sample loading disc and the powder sample to be pressed into a loading bin of a tablet press, then pressing the powder sample to be pressed and the paper bottom of the paper bottom sample loading disc to the loading bin of the tablet press from the upper plane of the paper towel sample loading disc by using a pressing rod with the outer diameter of 35.0mm, and then removing a sample loading frame to finish the arrangement of the powder sample.
The square steel blocks in the first step and the second step are made of medium and low alloy steel or stainless steel.
The steel column is made of medium and low alloy steel or stainless steel.
The paper towel is one of napkin paper, roll paper and toilet paper.
The boric acid is chemically pure or more.
The tablet press is a powder tablet press for XRFS analysis with a nominal pressure of 80 tons.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
1. the invention directly assembles the paper bottom on the sample-loading frame, and the prepared sample-loading plate with the paper bottom has simple structure and is easy to prepare.
2. According to the invention, after the sample loading disc at the bottom of the paper is filled with the sample powder to be pressed, the sample powder to be pressed is scraped by the scraping blade, and the process of finely leveling the sample powder to be pressed is not needed, so that the sample loading speed is high.
3. The paper bottom sample loading discs prepared by the invention have the same sample loading volume, so the sample quality fluctuation is small.
4. The invention uses a common XRFS tablet press, does not need a high-pressure tablet press, and has low energy consumption for tabletting.
5. According to the invention, the teeth of the countersink wall are utilized to cut the square tissue into the circular tissue with the diameter of 38.5mm, and the friction action of 4 steel columns and the tissue is utilized, so that the free falling distance of the sample powder to be pressed is reduced, the influence of the falling of the sample powder to be pressed on the flatness is reduced, and the sample strength for analysis is high.
Therefore, the invention has the characteristics of simple structure of the paper bottom sample loading plate, high sample loading speed, small sample quality fluctuation, low tabletting energy consumption and high sample wafer strength for analysis.
Detailed Description
The invention is further described with reference to specific embodiments, without limiting its scope.
In this embodiment:
the square steel blocks in the first step and the second step are made of medium and low alloy steel or stainless steel;
the steel column is made of medium-low alloy steel or stainless steel;
the paper towel is one of napkin paper, roll paper and toilet paper;
the boric acid is chemically pure or more;
the tablet press is a powder tablet press for XRFS analysis with a nominal pressure of 80 tons.
The detailed description is omitted in the embodiments.
Example 1
A method of arranging sample powder for XRFS analysis when pressing a sample wafer. The preparation method of the embodiment comprises the following steps:
step one, a square steel plate with the thickness of 1.0mm and the side length of 45mm is provided with an angle hole with the aperture of 2.2mm and a large round hole with the aperture of 36mm, and an upper hole frame is obtained.
The hole center of the corner hole is positioned on the angular bisector of any right angle of the square steel plate, the distance between the hole center of the corner hole and the right angle is 3mm, and the center of the large round hole is positioned at the center of the square steel plate.
And step two, firstly, forming a corner hole and a large circular hole which have the same aperture and hole center positions as those of the upper hole frame on a square steel plate with the thickness of 2.0mm and the side length of 45mm, and then forming a counter bore at the hole position of the large circular hole, wherein the diameter of the counter bore is 38.5mm, and the hole depth of the counter bore is 1.0 mm. The side with the counter bore is called the front side of the square steel plate, and vice versa; and then, processing the hole wall of the counter bore into a tooth shape, wherein the tooth space is 0.7mm, the width of each tooth space is 0.5mm, and the radial depth of each tooth space is 0.2 mm.
4 small round holes with the diameter of 1.0mm are uniformly formed by taking the center of the large circle as the symmetrical center, and the 4 small round holes are positioned on the circumference with the diameter of 37 mm. And respectively inserting steel columns with the length of 3mm and the diameter of 1.0mm into each small circular hole, wherein one end of each of 4 steel columns is 0-0.2 mm higher than the front surface of the square steel plate, and thus obtaining the lower hole frame.
And step three, movably connecting the upper hole frame and the lower hole frame through the corner holes of the upper hole frame and the corner holes of the lower hole frame by using cylindrical pins with the diameters of 2.0mm, wherein the upper hole frame is positioned on the lower hole frame, the front side of a square steel plate of the lower hole frame faces upwards, and the column length of the cylindrical pins is 3.5-6 mm, so that the sample loading frame is obtained.
And step three, movably connecting the upper hole frame and the lower hole frame through the corner holes of the upper hole frame and the corner holes of the lower hole frame by using cylindrical pins with the diameters of 2.0mm, wherein the upper hole frame is positioned on the lower hole frame, the front side of the square steel plate of the lower hole frame faces upwards, and the column length of the cylindrical pins is 3.5-6 mm, so that the sample loading frame is obtained.
And step four, rotating the upper hole frame of the sample loading frame around the cylindrical pin, covering a single-layer tissue piece with the side length of 40mm on the lower hole frame, rotating the upper hole frame around the cylindrical pin to be completely superposed with the lower hole frame, pressing the tissue piece by the upper hole frame, and fixing the upper hole frame and the lower hole frame by using a spring clamp to obtain the sample loading tray for the paper bottom.
And step five, placing 2.0g of boric acid on a lower pressure head in a bin of the tablet press, and enabling the boric acid to cover all the pressure surfaces.
And step six, filling the sample tray with the sample powder to be pressed into the paper bottom, scraping the sample powder to be pressed by using a scraping blade with the width of 40mm, and removing the redundant sample powder to be pressed.
And step seven, firstly, loading the paper towel sample loading disc and the powder sample to be pressed into a loading bin of a tablet press, then pressing the powder sample to be pressed and the paper bottom of the paper bottom sample loading disc to the loading bin of the tablet press from the upper plane of the paper towel sample loading disc by using a pressing rod with the outer diameter of 35.0mm, and then removing a sample loading frame to finish the arrangement of the powder sample.
Example 2
A method of arranging sample powder for XRFS analysis when the sample pieces are pressed. Except for step five, the same procedure as in example 1 was followed:
and fifthly, placing 1.8g of boric acid on a lower pressure head in a bin of the tablet press to enable the boric acid to cover all the pressure surfaces.
Example 3
A method of arranging sample powder for XRFS analysis when pressing a sample wafer. The same procedure as in example 1 was repeated except for step five:
and fifthly, placing 1.5g of boric acid on a lower pressure head in a bin of the tablet press to enable the boric acid to cover all the pressure surfaces.
Compared with the prior art, the specific implementation mode has the following positive effects:
1. the embodiment directly assembles the paper bottom on the sample loading frame, and the prepared paper bottom sample loading plate is simple in structure and easy to prepare.
2. According to the embodiment, after the sample loading disc at the bottom of the paper is filled with the sample powder to be pressed, the sample powder to be pressed is scraped by the scraping blade, and the process of finely flattening the sample powder to be pressed is not needed, so that the sample loading speed is high.
3. The paper bottom sample loading plate prepared by the embodiment has the same sample loading volume, so that the sample quality fluctuation is small.
4. This embodiment uses ordinary XRFS tablet press, does not need the high pressure tablet press, so the preforming energy consumption is low.
5. The square tissue piece is cut into the circular tissue piece with the diameter of 38.5mm by the teeth of the hole sinking wall, the free falling distance of the sample powder to be pressed is reduced by the friction action of 4 steel columns and the tissue, the influence of the falling of the sample powder to be pressed on the flatness is reduced, and the sample piece for analysis has high strength.
Therefore, the specific embodiment has the characteristics of simple structure of the paper bottom sample loading plate, high sample loading speed, small sample quality fluctuation, low tabletting energy consumption and high sample wafer strength for analysis.
Claims (6)
1. A method of arranging sample powder for XRFS analysis upon compaction of the sample, the method comprising the steps of:
step one, a square steel plate with the thickness of 1.0mm and the side length of 45mm is provided with an angle hole with the aperture of 2.2mm and a big round hole with the aperture of 36mm, and an upper hole frame is obtained;
the hole center of the corner hole is positioned on the angular bisector of any right angle of the square steel plate, the distance between the corner hole and the right angle is 3mm, and the center of the large round hole is positioned at the center of the square steel plate;
step two, firstly, forming a corner hole and a large round hole which are the same as the hole diameter and the hole center position of the upper hole frame on a square steel plate with the thickness of 2.0mm and the side length of 45mm, and then forming a counter bore at the hole opening of the large round hole, wherein the diameter of the counter bore is 38.5mm, and the hole depth of the counter bore is 1.0 mm; one side with the counter bore is called as the front side of the square steel plate, then the wall of the counter bore is processed into teeth, the tooth space is 0.7mm, the width of the inter-tooth space is 0.5mm, and the radial depth of the inter-tooth space is 0.2 mm;
4 small round holes with the diameter of 1.0mm are uniformly formed by taking the circle center of the big circle as the symmetric center, and the 4 small round holes are positioned on the circumference with the diameter of 37 mm; respectively inserting steel columns with the length of 3mm and the diameter of 1.0mm into each small circular hole, wherein one end of each of 4 steel columns is 0-0.2 mm higher than the front side of the square steel plate, and thus obtaining a lower hole frame;
step three, movably connecting the upper hole frame and the lower hole frame through the corner holes of the upper hole frame and the corner holes of the lower hole frame by using cylindrical pins with the diameters of 2.0mm, wherein the upper hole frame is positioned on the lower hole frame, the right side of a square steel plate of the lower hole frame faces upwards, and the column length of the cylindrical pins is 3.5-6 mm, so that a sample loading frame is obtained;
step four, rotating an upper hole frame of the sample loading frame around the cylindrical pin, covering a single-layer tissue piece with the side length of 40mm on a lower hole frame, rotating the upper hole frame around the cylindrical pin to be completely superposed with the lower hole frame, pressing the tissue piece by the upper hole frame, and fixing the upper hole frame and the lower hole frame by using a spring clamp to obtain a sample loading tray at the bottom of the paper;
placing 1.5-2.0 g of boric acid on a lower pressure head in a bin of a tablet press to enable the boric acid to cover all the pressed surfaces;
step six, filling a paper bottom sample loading disc with sample powder to be pressed, scraping the sample powder to be pressed by using a scraping blade with the width of 40mm, and removing redundant sample powder to be pressed;
and step seven, firstly, loading the paper towel sample loading disc and the powder sample to be pressed into a loading bin of a tablet press, then pressing the powder sample to be pressed and the paper bottom of the paper bottom sample loading disc to the loading bin of the tablet press from the upper plane of the paper towel sample loading disc by using a pressing rod with the outer diameter of 35.0mm, and then removing a sample loading frame to finish the arrangement of the powder sample.
2. The method of arranging sample powder during sample pressing for XRFS analysis as claimed in claim 1, wherein said square steel plate of step one and step two is made of medium low alloy steel or stainless steel.
3. The method of arranging sample powder during sample pressing for XRFS analysis as claimed in claim 1, wherein said steel column is made of medium low alloy steel or stainless steel.
4. The method of arranging sample powder as pressed from a sample wafer for XRFS analysis according to claim 1, wherein said tissue is one of napkin, roll-paper and toilet-paper.
5. The method of arranging sample powders for XRFS analysis upon pressing of the sample wafer according to claim 1 wherein said boric acid is chemically pure or more.
6. The method of arranging sample powder upon compression of a tablet for XRFS analysis according to claim 1, wherein the tablet press is a powder tablet press for XRFS analysis having a pressure rating of 80 tons.
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