CN107132243B - Sample preparation equipment for X-ray fluorescence spectrum micro powder sample - Google Patents
Sample preparation equipment for X-ray fluorescence spectrum micro powder sample Download PDFInfo
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- CN107132243B CN107132243B CN201710268956.3A CN201710268956A CN107132243B CN 107132243 B CN107132243 B CN 107132243B CN 201710268956 A CN201710268956 A CN 201710268956A CN 107132243 B CN107132243 B CN 107132243B
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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
-
- 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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- 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)
- Analysing Materials By The Use Of Radiation (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides sample preparation equipment for a trace powder sample of an X-ray fluorescence spectrum, belongs to the technical field of sample preparation tools, and is used for preparing the trace powder sample in the detection process of the X-ray fluorescence spectrum. For a trace amount of powder that cannot be prepared as a standard sample, the conventional solution is to mix the trace amount of powder with a binder to prepare the standard sample. However, this method introduces new impurities, increases analysis errors, and affects the lower detection limits of light elements and trace elements. Therefore, the round groove for containing the trace powder is pressed in the adhesive, so that the trace powder to be detected is concentrated at the middle upper part of the adhesive, the trace powder to be detected is prevented from being diluted, and the detection precision is improved.
Description
Technical Field
The invention belongs to the technical field of sample preparation tools, and is used for preparing a trace powder sample in an X-ray fluorescence spectrum detection process.
Background
An X-ray fluorescence spectrometer is a detection instrument for analyzing a substance component by using fluorescent X-rays, and can perform both quantitative analysis and qualitative analysis of a substance. Therefore, the X-ray fluorescence spectrometer has been widely used in the fields of biology, medicine, materials and the like, and the development of various related subjects is promoted.
Currently, when powder samples are tested using an X-ray fluorescence spectrometer, they are typically pressed into compact sheet-like standard samples having a diameter of 3.5 cm and a thickness of 2 mm. When detecting minute amounts of powder, standard samples are often not prepared due to insufficient volume of powder. The conventional solution is to add a certain amount of powder binder with known ingredients to the trace powder and mix it with the trace powder to be measured to prepare a standard sample. However, the use of a binder has three disadvantages, firstly, the addition of the binder will introduce new impurities, increasing analysis errors; second, the low concentration of the element or light element may cause the line intensity to be low due to dilution, and if the binder particle size is large, the particle size effect may be caused, so that quantitative analysis is impossible. Third, the addition of binders can reduce the analytical line strength, affecting the lower detection limit for light and trace elements. Therefore, the invention aims to solve the defects caused by the traditional preparation method of the trace powder sample.
Disclosure of Invention
The invention aims to provide an X-ray fluorescence spectrum powder sample preparation device which is beneficial to solving the defects of the traditional sample preparation method.
The technical scheme of the invention is as follows:
a sample preparation device for an X-ray fluorescence spectrum micro powder sample comprises a bottom plate 1, a guide post 2, a spring 3, a bolt 4, a slideway plate 5, a nut 6, a gasket 7, a functional plate 8, a positioning plate 9 and a positioning post 10;
one end of a plurality of bolts 4 is fixedly connected to two sides of the bottom plate 1 in two rows, the guide posts 2 are sleeved outside the bolts 4, and two slideway plates 5 are sleeved on the guide posts 2; the guide post 2 is sleeved with a spring 3, and the spring 3 is positioned between the bottom plate 1 and the slideway plate 5 to realize limit; the nut 6 is matched and fixed with the other end of the bolt 4, and a gasket 7 is arranged between the nut and the other end;
a step-shaped groove structure is arranged on one side of the slideway plate 5, a groove on the slideway plate is matched with a bulge on the functional plate 8, and the step-shaped structure is clamped and fixed with the step-shaped structure of the functional plate 8;
the functional board 8 is provided with a stepped bulge structure on two sides, and is provided with a knob 11, a large circular pressing piece 12, an annular pressing piece 13, a small circular pressing piece 14 and a sample adding groove 15; the knob 11 and the sample adding groove 15 are arranged on the upper surface of the functional board 8, and the movement of the functional board 8 is realized through controlling the knob 11; the sample adding groove 15 is positioned at the end part of the functional board 8, a feeding hole 16 is arranged on the sample adding groove 15, and a sample enters the sample ring through the feeding hole 16; the large circular pressing piece 12, the annular pressing piece 13 and the small circular pressing piece 14 are arranged on the lower surface of the functional board 8, and the small circular pressing piece 14 is arranged on the annular pressing piece 13 to form a boss structure; in the operation process, firstly, the position of the functional plate 8 is adjusted to enable the central axis of the large circular pressing plate 12 to coincide with the central axis of the sample ring, after the sample in the sample ring is compacted, the functional plate 8 is moved to enable the central axis of the sample ring to coincide with the central axis of the small circular pressing plate 14, and then the sample is pressed again to enable the sample to form a groove; moving the functional plate (8) to enable the central axis of the sample ring to coincide with the central axis of the feeding hole (16), and adding sample powder into the groove pressed by the small circular pressing sheet (14) through the feeding hole (16);
the positioning column 10 is fixed on the bottom plate 1 and used for supporting the positioning plate 9, and the positioning plate 9 realizes positioning of the sample ring;
the positioning plate 9 is a plate with an arc-shaped groove;
the sample ring containing a proper amount of adhesive is arranged at the center of the arc-shaped groove of the positioning plate 9, and the functions of flattening the adhesive surface, extruding the circular groove containing the trace powder and adding the trace powder are realized by sequentially moving the functional plate 8.
The invention has the excellent effects that: in the prepared standard sample, the micro powder to be detected is separated from the binder, so that the defect that the micro powder to be detected and the binder are mixed to prepare the standard sample is avoided, the sample box is combined to realize direct detection of the micro powder, and the detection precision of the X-ray fluorescence spectrometer on the micro powder is improved.
Drawings
FIG. 1 is a schematic diagram showing the overall structure of an apparatus for preparing a trace amount of powder sample by X-ray fluorescence spectrum according to the present invention.
FIG. 2 is a front view of a functional plate in the apparatus for preparing a micro powder sample by X-ray fluorescence spectrum according to the present invention.
FIG. 3 is a top view of a functional plate in the apparatus for preparing a micro powder sample by X-ray fluorescence spectroscopy according to the present invention.
In the figure: 1, a bottom plate; 2, a guide post; 3, a spring; 4 bolts; 5, a slideway plate; 6, a nut; 7, a gasket;
8, a function board; 9, positioning a plate; 10 positioning columns; 11 a knob; 12 big round tabletting; 13, annular tabletting;
14 small round tabletting; 15 sample adding grooves; 16 feed holes.
Detailed Description
The following describes the embodiments of the present invention in detail with reference to the technical scheme and the accompanying drawings.
Examples
Placing a sample preparation device on a horizontal plane, then placing a sample ring containing a proper amount of adhesive at the circle center of an arc-shaped groove of a positioning plate, enabling the circle center of the sample ring to be positioned on the same vertical line with the circle center of a large circular pressing sheet on a functional plate, manually pressing down the slideway plate, enabling the slideway plate to be integrally and downwards translated with the functional plate, using the large circular pressing sheet on the functional plate to flatten the surface of the adhesive, then enabling the slideway plate to reset under the action of a spring, moving the functional plate, enabling the circle center of a small circular pressing sheet on the functional plate to be positioned on the same vertical line with the circle center of the sample ring, manually pressing down the slideway plate again, enabling the slideway plate to be integrally and downwards translated with the functional plate, using the small circular pressing sheet on the functional plate to press out a groove for containing micro powder, after resetting the slideway plate, moving the function plate again, enabling the circle center of a charging hole to be positioned on the same vertical line with the circle center of the sample ring, adding the micro powder placed in the groove of the small circular pressing sheet into a groove, finally moving the sample ring to a pressing machine, compacting the sample ring, and preparing a standard sample.
Claims (1)
1. The sample preparation equipment for the X-ray fluorescence spectrum micro powder sample is characterized by comprising a bottom plate (1), a guide post (2), a spring (3), a bolt (4), a slideway plate (5), a nut (6), a gasket (7), a functional plate (8), a positioning plate (9) and a positioning post (10);
one end of each bolt (4) is fixedly connected to two sides of the bottom plate (1) in two rows, the guide posts (2) are sleeved outside the bolts (4), and the two slideway plates (5) are sleeved on the guide posts (2); the guide post (2) is sleeved with a spring (3), and the spring (3) is positioned between the bottom plate (1) and the slideway plate (5) to realize limit; the nut (6) is matched and fixed with the other end of the bolt (4), and a gasket (7) is arranged between the nut and the other end;
a step-shaped groove structure is arranged on one side of the slideway plate (5), the groove on the slideway plate is matched with the bulge on the functional plate (8), and the step structure is clamped and fixed with the step structure of the functional plate (8);
the functional board (8) is provided with a stepped bulge structure on two sides, and is provided with a knob (11), a large circular pressing piece (12), an annular pressing piece (13), a small circular pressing piece (14) and a sample adding groove (15); the knob (11) and the sample adding groove (15) are arranged on the upper surface of the functional board (8), and the movement of the functional board (8) is realized through the control knob (11); the sample adding groove (15) is positioned at the end part of the functional board (8), a feeding hole (16) is arranged on the sample adding groove (15), and a sample enters the sample ring through the feeding hole (16); the large circular pressing piece (12), the annular pressing piece (13) and the small circular pressing piece (14) are arranged on the lower surface of the functional board (8), and the small circular pressing piece (14) is positioned on the annular pressing piece (13) to form a boss structure; in the operation process, firstly, the position of the functional plate (8) is adjusted to enable the central axis of the large circular pressing plate (12) to coincide with the central axis of the sample ring, after the sample in the sample ring is compacted, the functional plate (8) is moved to enable the central axis of the sample ring to coincide with the central axis of the small circular pressing plate (14), and then the sample is pressed again to enable the sample to form a groove; moving the functional plate (8) to enable the central axis of the sample ring to coincide with the central axis of the feeding hole (16), and adding sample powder into the groove pressed by the small circular pressing sheet (14) through the feeding hole (16);
the positioning column (10) is fixed on the bottom plate (1) and used for supporting the positioning plate (9), and the positioning plate (9) realizes positioning of the sample ring;
the positioning plate (9) is a plate with an arc-shaped groove;
the sample ring is arranged at the center of an arc-shaped groove of the positioning plate (9);
the implementation mode is as follows:
placing sample preparation equipment on a horizontal plane, then placing a sample ring containing an adhesive at the circle center of an arc-shaped groove of a positioning plate (9), enabling the circle center of the sample ring to be positioned on the same vertical line with the circle center of a large circular pressing sheet (12) on a functional plate (8), pressing down a slide plate (5) by hand, enabling the slide plate (5) to be integrally downwards translated with the functional plate (8), flattening the surface of the adhesive by using the large circular pressing sheet (12) on the functional plate (8), resetting the slide plate (5) under the action of a spring (3), moving the functional plate (8) to enable the circle center of a small circular pressing sheet (14) on the functional plate (8) to be positioned on the same vertical line with the circle center of the sample ring, pressing down the slide plate (5) by hand again, enabling the small circular pressing sheet (14) on the functional plate (8) to be integrally downwards translated on the plane of the adhesive, after resetting the slide plate (5), moving the functional plate (8) again, enabling the circle center of a small circular pressing sheet (14) on the functional plate (8) to be positioned on the same vertical line with the sample ring, pressing the small circular pressing sheet (14) to be positioned on the same vertical line, pressing powder, and finally pressing the sample to be pressed into a sample, and finally, pressing the sample to be placed in the sample on the sample to be pressed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710268956.3A CN107132243B (en) | 2017-04-24 | 2017-04-24 | Sample preparation equipment for X-ray fluorescence spectrum micro powder sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710268956.3A CN107132243B (en) | 2017-04-24 | 2017-04-24 | Sample preparation equipment for X-ray fluorescence spectrum micro powder sample |
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| Publication Number | Publication Date |
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| CN107132243A CN107132243A (en) | 2017-09-05 |
| CN107132243B true CN107132243B (en) | 2023-07-18 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710268956.3A Active CN107132243B (en) | 2017-04-24 | 2017-04-24 | Sample preparation equipment for X-ray fluorescence spectrum micro powder sample |
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| CN (1) | CN107132243B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110231318A (en) * | 2019-05-16 | 2019-09-13 | 西安交通大学 | A kind of powder sample method for making sample for low temperature fluorometric investigation |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002350372A (en) * | 2001-05-29 | 2002-12-04 | Tdk Corp | Sample for fluorescence x-ray analysis, fluorescence x-ray analyzing apparatus, and fluorescence x-ray analyzing method |
| CN202453234U (en) * | 2012-01-10 | 2012-09-26 | 重庆普源化工工业有限公司 | Simple tablet press |
| CN203337578U (en) * | 2013-07-09 | 2013-12-11 | 王卿 | X-fluorescence spectrum analysis sample box for powder samples |
| CN105723210A (en) * | 2013-09-19 | 2016-06-29 | Fl史密斯公司 | Front-loading sample preparation apparatus and methods thereof |
| CN106153656A (en) * | 2016-08-31 | 2016-11-23 | 江苏天瑞仪器股份有限公司 | A kind of X fluorescence spectrum method rapid assay methods to heavy metal in soil cadmium element |
| CN206696208U (en) * | 2017-04-24 | 2017-12-01 | 大连理工大学 | The sample making apparatus of X-ray fluorescence spectra little power sample |
-
2017
- 2017-04-24 CN CN201710268956.3A patent/CN107132243B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002350372A (en) * | 2001-05-29 | 2002-12-04 | Tdk Corp | Sample for fluorescence x-ray analysis, fluorescence x-ray analyzing apparatus, and fluorescence x-ray analyzing method |
| CN202453234U (en) * | 2012-01-10 | 2012-09-26 | 重庆普源化工工业有限公司 | Simple tablet press |
| CN203337578U (en) * | 2013-07-09 | 2013-12-11 | 王卿 | X-fluorescence spectrum analysis sample box for powder samples |
| CN105723210A (en) * | 2013-09-19 | 2016-06-29 | Fl史密斯公司 | Front-loading sample preparation apparatus and methods thereof |
| CN106153656A (en) * | 2016-08-31 | 2016-11-23 | 江苏天瑞仪器股份有限公司 | A kind of X fluorescence spectrum method rapid assay methods to heavy metal in soil cadmium element |
| CN206696208U (en) * | 2017-04-24 | 2017-12-01 | 大连理工大学 | The sample making apparatus of X-ray fluorescence spectra little power sample |
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| CN107132243A (en) | 2017-09-05 |
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