Bearing device for measuring sample by glow discharge mass spectrometer

Abstract

The invention provides a bearing device for measuring a sample by a glow discharge mass spectrograph, the bearing device comprises a pressing main body, a sample preparation pressing sheet and a sample base, the pressing main body is provided with a first end face and a second end face which are opposite to each other, the first end face is provided with a positioning groove, the second end face is provided with a handle, and the handle is provided with a clamping groove. The sample preparation pressing sheet is used for wrapping a to-be-tested sample and is located in the positioning groove, and the sample base is in butt joint with the second end face of the pressing main body. According to the invention, effective fixation of small-size block-shaped samples or sheet-shaped samples is realized, introduction of impurities is reduced, and the accuracy of test results is improved.

Description

Technical Field

[0001] The present invention belongs to the technical field of material detection, relates to a glow discharge mass spectrometer, and particularly relates to a carrier device for determining a sample by a glow discharge mass spectrometer. Background Art

[0002] Glow Discharge Mass Spectrometry (GDMS) is an analytical method that uses a glow discharge source as an ion source and is connected to a mass spectrometer for mass spectrometry determination. It is mainly used to detect the content of trace elements in materials, and the corresponding analytical instrument is called a glow discharge mass spectrometer. The sample holders in the discharge chamber of a glow discharge mass spectrometer are generally divided into sheet-shaped and needle-shaped. Among them, the size requirements for the sheet-shaped sample to be measured in the sheet-shaped glow discharge chamber are generally 20mm×20mm×2mm, and the size requirements for the needle-shaped sample to be measured in the needle-shaped glow discharge chamber are generally 20mm×2mm×2mm. However, in the actual production, processing, and use processes, the morphologies of the samples to be measured are various, including irregular blocks, powders, granules, chips, etc., and cannot be effectively fixed by the sample holders in the glow discharge chamber, seriously hindering the progress of GDMS analysis.

[0003] For samples to be measured with small sizes, the prior art has disclosed some loading components for samples to be measured that can be effectively fixed by sample holders. For example, CN205374369U discloses a loading device for determining powder samples by a glow discharge mass spectrometer, including a base, on which four vertical surfaces are provided, two of which are parallel and relatively arranged planes, and the other two vertical surfaces are arc surfaces for connecting the two planes; a through hole is provided at the center of the top surface of the base, and an elastic washer is detachably connected in the through hole. CN212542352U discloses a rod-shaped indium carrier for testing needle-shaped samples, with a hole opened on the end surface at one end, and a groove opened at a position corresponding to the hole on the side surface, and a base provided at the other end. The needle-shaped sample is fixed by applying pressure to the positioning of the sample through the groove, which can not only be reused, but also adjust the size of the hole according to the sample size, neither causing the sample to fall nor requiring customization.

[0004] However, the current fixing methods for small-sized block or sheet samples have cumbersome steps, time-consuming, low sample preparation success rate, are prone to introducing impurities, and the molds used are not reusable, reducing the detection efficiency. Therefore, there is an urgent need to develop a carrier for block or sheet samples that can make the samples to be measured into a size that can be detected by GDMS without introducing impurities for rapid analysis. Summary of the Invention

[0005] Aiming at the deficiencies of the existing technology, the purpose of the present invention is to provide a loading device for samples measured by a glow discharge mass spectrometer, which simplifies the operation steps, realizes the effective fixation of small-sized block samples or sheet samples, reduces the introduction of impurities, and improves the accuracy of test results.

[0006] To achieve this purpose, the present invention adopts the following technical solutions:

[0007] The present invention provides a loading device for samples measured by a glow discharge mass spectrometer. The loading device includes a pressing main body, a sample preparation pressing sheet, and a sample base. The pressing main body has opposite first and second end faces. A positioning groove is provided on the first end face, and a handle is provided on the second end face. The sample preparation pressing sheet is used to wrap the sample to be measured and is located in the positioning groove. The sample base is docked with the second end face of the pressing main body.

[0008] The loading device provided by the present invention has a reasonable structure, simple sample preparation operation, can effectively fix the sample to be measured, reduce the introduction of impurities in the measured sample, and greatly improve the success rate of sample preparation.

[0009] As a preferred technical solution of the present invention, the pressing main body has a frustum of a cone structure, and the diameter of the first end face is larger than the diameter of the second end face.

[0010] As a preferred technical solution of the present invention, the positioning groove is a rectangular groove, a circular groove, or a U-shaped groove.

[0011] As a preferred technical solution of the present invention, the depth of the positioning groove is 2-5 mm, for example, it can be 2 mm, 2.5 mm, 3 mm, 3.5 mm, 4 mm, 4.5 mm, or 5 mm, but is not limited to the listed values. Other unlisted values within this numerical range are equally applicable.

[0012] As a preferred technical solution of the present invention, the sample preparation pressing sheet is an indium sheet.

[0013] Preferably, the purity of the sample preparation pressing sheet is ≥7N.

[0014] As a preferred technical solution of the present invention, the thickness of the sample preparation pressing sheet is 1-3 mm, for example, it can be 1 mm, 1.2 mm, 1.5 mm, 1.8 mm, 2 mm, 2.2 mm, 2.5 mm, 2.8 mm, or 0.3 mm, but is not limited to the listed values. Other unlisted values within this numerical range are equally applicable.

[0015] As a preferred technical solution of the present invention, the orthographic projection of the unfolded sample preparation pressing sheet on the second end face covers the positioning groove.

[0016] Preferably, the unfolded sample preparation pressing sheet is rectangular or circular.

[0017] In the present invention, the indium sheet has a soft texture. After being subjected to a certain pressure, it gradually deforms and wraps the sample to be measured. Moreover, the purity of the indium sheet is ≥7N, avoiding the introduction of other impurities that may affect the sample measurement result. The size of the prepared sample tablet after unfolding is larger than the size of the positioning groove, ensuring that it can completely wrap the sample to be measured and avoiding the introduction of other impurities.

[0018] As a preferred technical solution of the present invention, the cross-section of the sample base is circular.

[0019] The diameter of the sample base is equal to the diameter of the second end face of the pressing body.

[0020] That is, the side wall of the sample base in the present invention is flush with the side edge of the second end face of the pressing body.

[0021] Preferably, the height of the sample base is 20 - 40 mm. For example, it can be 20 mm, 22 mm, 25 mm, 26 mm, 28 mm, 30 mm, 32 mm, 35 mm, 36 mm, 38 mm or 40 mm, but is not limited to the listed values. Other unlisted values within this numerical range are equally applicable.

[0022] As a preferred technical solution of the present invention, the diameter of the second end face of the pressing body is 80 - 120 mm. For example, it can be 80 mm, 85 mm, 90 mm, 95 mm, 100 mm, 105 mm, 110 mm, 115 mm or 120 mm, but is not limited to the listed values. Other unlisted values within this numerical range are equally applicable.

[0023] Preferably, the height of the pressing body is 60 - 80 mm. For example, it can be 60 mm, 62 mm, 65 mm, 66 mm, 68 mm, 70 mm, 72 mm, 75 mm, 78 mm or 80 mm, but is not limited to the listed values. Other unlisted values within this numerical range are equally applicable.

[0024] As a preferred technical solution of the present invention, the height of the handle is 20 - 30 mm. For example, it can be 20 mm, 21 mm, 22 mm, 23 mm, 24 mm, 25 mm, 26 mm, 27 mm, 28 mm, 29 mm or 30 mm, but is not limited to the listed values. Other unlisted values within this numerical range are equally applicable.

[0025] Exemplarily, a method for testing using a loading device for sample determination by glow discharge mass spectrometry provided by the present invention includes:

[0026] (1) Pickling the sample to be measured and the loading device respectively;

[0027] (2) Place the sample to be tested on the sample base, unfold the sample preparation sheet and lay it flat on the surface of the sample to be tested;

[0028] (3) Press the sample to be tested by applying pressure through the handle, so that the sample preparation sheet wraps the sample to be tested and then extends into the positioning groove to complete the loading;

[0029] (4) The container loaded with the sample to be tested in step (3) is transferred to a glow discharge mass spectrometer for sample measurement.

[0030] The sample to be tested in the present invention is a block sample or a sheet sample.

[0031] Compared with the prior art, the present invention has the following beneficial effects:

[0032] The present invention provides a carrier device for measuring samples by a glow discharge mass spectrometer, which achieves effective fixation of small-sized block or sheet samples, and the carrier device can be reused, has strong practicality, reduces the introduction of impurities, improves sample preparation quality and detection accuracy, and increases the success rate of sample preparation. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 This is a schematic diagram of the structure of a carrier device for measuring samples using a glow discharge mass spectrometer provided in Example 1 of the present invention.

[0034] Among them, 1-pressing body; 2-sample pressing tablet; 3-sample base; 4-handle; 5-positioning groove; 6-first end face; 7-second end face. DETAILED DESCRIPTION

[0035] It should be understood that, in the description of the present invention, the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", etc., indicating the orientation or positional relationship are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention. In addition, the terms "first", "second", etc. are only used for descriptive purposes, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, the features defined as "first", "second", etc. may explicitly or implicitly include one or more of the features. In the description of the present invention, unless otherwise specified, "multiple" means two or more.

[0036] It should be noted that in the description of the present invention, unless otherwise clearly defined and limited, the terms "arranged", "connected" and "coupled" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the communication inside two components. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood through specific situations.

[0037] The technical solution of the present invention will be further described below with reference to the accompanying drawings and through specific embodiments.

[0038] In a specific embodiment, the present invention provides a loading device for determining a sample by a glow discharge mass spectrometer, including a pressing main body, a sample preparation tablet and a sample base. The pressing main body has opposite first and second end faces. A positioning groove is provided on the first end face, and a handle is provided on the second end face. The sample preparation tablet is used to wrap the sample to be measured and is located in the positioning groove. The sample base is docked with the second end face of the pressing main body. During the actual sample preparation process, first place the sample to be measured on the sample base, place the unfolded sample preparation tablet on the surface of the sample to be measured, then align the positioning groove of the pressing main body with the sample preparation tablet, and apply pressure using the handle. After being pressed, the sample preparation tablet gradually wraps the sample to be measured and extends into the positioning groove, realizing the effective fixation of the sample to be measured.

[0039] The loading device of the present invention has no requirements for the material and shape of the sample to be measured. The sample to be measured can contain elements such as potassium, sodium, calcium, magnesium, iron, silicon, silver, arsenic, boron, phosphorus, selenium, tellurium or thallium, or semiconductors, and the sample to be measured can be in a regular shape, or an irregular block or sheet. The present invention uses the pressing main body to fix the sample preparation tablet and the sample to be measured, which can reduce the introduction of impurities, and then place the entire loading device with the sample to be measured in the sample clamp of the glow discharge mass spectrometer for measurement.

[0040] The loading device in the present invention has the characteristics of high temperature resistance, impact resistance and acid and alkali resistance. The material of the loading device can be polytetrafluoroethylene well-known to those skilled in the art to avoid introducing other impurities.

[0041] In some embodiments, the pressing body has a frustum of a cone structure, and the diameter of the first end face is larger than that of the second end face. That is, the positioning groove is formed on the end face with a larger area, and the handle is arranged on the end face with a smaller area, which is convenient for applying pressure and avoiding the falling off of the sample to be measured. Specifically, the positioning groove is a rectangular groove, a circular groove or a U-shaped groove. The depth of the positioning groove is 2-5 mm. Those skilled in the art can adjust the size of the positioning groove according to the actual size of the sample to be measured. The handle has an operating end and a connecting end. The operating end is the side that bears force, and the connecting end is butt-jointed with the second end face of the pressing body. Specifically, both the operating end and the connecting end are cylindrical structures, and the diameter of the operating end is larger than that of the connecting end, and the diameter of the connecting end is equal to the diameter of the second end face, which is not only convenient for operation but also ensures the structural strength.

[0042] In some embodiments, the sample preparation pressing sheet is an indium sheet, which is soft in texture. After being subjected to a certain pressure, it gradually deforms and wraps the sample to be measured. Moreover, the purity of the indium sheet is ≥7N, and the thickness of the sample preparation pressing sheet is 1-3 mm. The orthographic projection of the unfolded sample preparation pressing sheet on the second end face covers the positioning groove, and the unfolded sample preparation pressing sheet is rectangular or circular. After a certain pressure is applied to the pressing body, the sample preparation pressing sheet wraps the sample to be measured and extends into the positioning groove to form a carrier for the sample to be measured. No other tools are required during the entire fixing process, avoiding the introduction of impurities.

[0043] In addition, the carrying device of the present invention can be reused. Even if it is contaminated, it can be reused after cutting and pickling treatment.

[0044] In some embodiments, the cross-section of the sample base is circular, and the diameter of the sample base is equal to the diameter of the second end face of the pressing body.

[0045] Specifically, the height of the sample base is 20-40 mm. The diameter of the second end face of the pressing body is 80-120 mm, and the height of the pressing body is 60-80 mm. The height of the handle is 20-30 mm.

[0046] In another specific embodiment, the present invention provides a method for testing by using the carrying device for a sample to be measured by a glow discharge mass spectrometer described in a specific embodiment, which specifically includes the following steps:

[0047] (1) Pickle the sample to be measured and the carrying device respectively with concentrated nitric acid.

[0048] (2) Place the sample to be measured on the sample base, and unfold and lay the sample preparation pressing sheet on the surface of the sample to be measured.

[0049] (3) The sample to be tested is pressed by applying pressure through the handle, so that the sample preparation pressing sheet wraps the sample to be tested and then extends into the positioning groove to complete the loading.

[0050] (4) The container loaded with the sample to be tested in step (3) is transferred to a glow discharge mass spectrometer for sample measurement.

[0051] Wherein, the sample to be tested is a block sample or a sheet sample. The sample to be tested is a high-purity metal conductor or semiconductor.

[0052] The present invention does not specifically limit the working conditions of the glow discharge mass spectrometer. Those skilled in the art can adjust the discharge current, discharge voltage, cooling time and sputtering process parameters of the glow discharge mass spectrometer according to different samples and test requirements.

[0053] Example 1

[0054] This embodiment provides a sample carrier device for measuring a sample by a glow discharge mass spectrometer, such as Figure 1 As shown, it includes a pressing body 1, a sample pressing sheet 2 and a sample base 3. The pressing body 1 is a truncated cone structure, having a first end face 6 and a second end face 7 opposite to each other, and the diameter of the first end face 6 is greater than the diameter of the second end face 7. The first end face 6 is provided with a positioning groove 5, and the positioning groove 5 is a rectangular groove, and its size is 7mm×5mm×3mm. The second end face 7 is provided with a handle 4, the height of the handle 4 is 25mm, the diameter of the second end face 7 is 100mm, and the height of the pressing body 1 is 67mm. The sample pressing sheet 2 is used to wrap the sample to be tested and is located in the positioning groove 5. The sample pressing sheet 2 is an indium sheet with a thickness of 2mm. After the sample pressing sheet 2 is unfolded, the positive projection on the second end face 7 covers the positioning groove 5, and the unfolded sample pressing sheet 2 is rectangular. The cross section of the sample base 3 is circular, and it butts the second end face 7 of the pressing body 1. The diameter of the sample base 3 is equal to the diameter of the second end face 7 of the pressing body 1, and the height of the sample base 3 is 30mm.

[0055] The bulk semiconductor sample is measured by using the sample carrier device for measuring the sample by a glow discharge mass spectrometer provided in this embodiment, which specifically includes the following steps:

[0056] (1) Use concentrated nitric acid to pickle the sample to be tested and the carrier device respectively.

[0057] (2) Place the sample to be tested on the sample base 3, and unfold the sample preparation sheet 2 and lay it flat on the surface of the sample to be tested.

[0058] (3) The pressing body 1 is moved by the handle 4 so that the positioning groove 5 is aligned with the block-shaped sample to be tested, and then the sample to be tested is pressed by applying pressure by the handle 4 so that the sample preparation pressing sheet 2 wraps the sample to be tested and then extends into the positioning groove 5 to complete the loading.

[0059] (4) Transfer the loading device loaded with the sample to be measured into a VG9000 glow discharge mass spectrometer for sample measurement.

[0060] Example 2

[0061] This example provides a loading device for measuring samples by a glow discharge mass spectrometer, including a pressing main body 1, a sample preparation tablet 2 and a sample base 3. The pressing main body 1 has a frustum of a cone structure with opposite first end face 6 and second end face 7. The diameter of the first end face 6 is larger than that of the second end face 7. A positioning groove 5 is provided on the first end face 6, and the positioning groove 5 is a rectangular groove with dimensions of 7 mm × 6 mm × 4 mm. A handle 4 is provided on the second end face 7. The height of the handle 4 is 20 mm, the diameter of the second end face 7 is 80 mm, and the height of the pressing main body 1 is 60 mm. The sample preparation tablet 2 is used to wrap the sample to be measured and is located in the positioning groove 5. The sample preparation tablet 2 is an indium sheet with a thickness of 1 mm. The orthographic projection of the unfolded sample preparation tablet 2 on the second end face 7 covers the positioning groove 5, and the unfolded sample preparation tablet 2 is circular. The cross-section of the sample base 3 is circular. It is butt-jointed with the second end face 7 of the pressing main body 1. The diameter of the sample base 3 is equal to the diameter of the second end face 7 of the pressing main body 1, and the height of the sample base 3 is 20 mm.

[0062] Using the loading device for measuring samples by a glow discharge mass spectrometer provided in this example to measure bulk samples specifically includes the following steps:

[0063] (1) Pickle the sample to be measured and the loading device respectively with concentrated nitric acid.

[0064] (2) Place the sample to be measured on the sample base 3, and unfold and lay the sample preparation tablet 2 flat on the surface of the sample to be measured.

[0065] (3) Move the pressing main body 1 by the handle 4 so that the positioning groove 5 is aligned with the bulk sample to be measured, and then press the sample to be measured by applying pressure through the handle 4, so that the sample preparation tablet 2 wraps the sample to be measured and extends into the positioning groove 5 to complete the loading.

[0066] (4) Transfer the loading device loaded with the sample to be measured in step (3) into a VG9000 glow discharge mass spectrometer for sample measurement.

[0067] Example 3

[0068] This embodiment provides a loading device for determining samples by glow discharge mass spectrometer, including a pressing main body 1, a sample preparation pressing sheet 2 and a sample base 3. The pressing main body 1 has a frustum of a cone structure, with opposite first end face 6 and second end face 7. The diameter of the first end face 6 is larger than that of the second end face 7. The first end face 6 is provided with a positioning groove 5, and the positioning groove 5 is a rectangular groove with dimensions of 6mm×6mm×5mm. The second end face 7 is provided with a handle 4, the height of the handle 4 is 30mm, the diameter of the second end face 7 is 120mm, and the height of the pressing main body 1 is 80mm. The sample preparation pressing sheet 2 is used to wrap the sample to be measured and is located in the positioning groove 5. The sample preparation pressing sheet 2 is an indium sheet with a thickness of 3mm. The orthographic projection of the unfolded sample preparation pressing sheet 2 on the second end face 7 covers the positioning groove 5, and the unfolded sample preparation pressing sheet 2 is circular. The cross-section of the sample base 3 is circular, and it is butt-jointed with the second end face 7 of the pressing main body 1. The diameter of the sample base 3 is equal to the diameter of the second end face 7 of the pressing main body 1, and the height of the sample base 3 is 35mm.

[0069] Using the loading device for determining samples by glow discharge mass spectrometer provided in this embodiment to determine bulk samples, specifically including the following steps:

[0070] (1) Pickle the sample to be measured and the loading device respectively with concentrated nitric acid.

[0071] (2) Place the sample to be measured on the sample base 3, and unfold and lay the sample preparation pressing sheet 2 on the surface of the sample to be measured.

[0072] (3) Move the pressing main body 1 by the handle 4 so that the positioning groove 5 is aligned with the bulk sample to be measured, and then press the sample to be measured by applying pressure through the handle 4, so that the sample preparation pressing sheet 2 wraps the sample to be measured and extends into the positioning groove 5 to complete the loading.

[0073] (4) Transfer the loading device loaded with the sample to be measured in step (3) to a VG9000 glow discharge mass spectrometer for sample determination.

[0074] The present invention realizes the effective fixation of small-sized bulk or sheet samples for determination by glow discharge mass spectrometer, reduces the introduction of impurities in the pretreatment process, and also simplifies the sample pretreatment process.

[0075] The applicant declares that the above description is only the specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention fall within the protection scope and the disclosure scope of the present invention.

Claims

1. A sample carrier for glow discharge mass spectrometer, characterized in that: The carrying device includes a pressing body, a sample-preparing pressing sheet and a sample base. The pressing body has a first end face and a second end face relative to each other. The first end face is provided with a positioning groove, and the second end face is provided with a handle. The sample-preparing pressing sheet is used to wrap the sample to be tested and is located in the positioning groove. The sample base is connected to the second end face of the pressing body.

2. The sample carrier for glow discharge mass spectrometer measurement according to claim 1, characterized in that: The pressing body is in a truncated cone structure, and the diameter of the first end surface is greater than the diameter of the second end surface.

3. The sample carrier for glow discharge mass spectrometer measurement according to claim 1, characterized in that: The positioning groove is a rectangular groove, a circular groove or a U-shaped groove.

4. The sample carrier for glow discharge mass spectrometer measurement according to claim 1, characterized in that: The depth of the positioning groove is 2-5 mm.

5. The sample carrier for glow discharge mass spectrometer measurement according to claim 1 or 2, characterized in that: The sample preparation pressed sheet is an indium sheet; Preferably, the purity of the sample preparation tablet is ≥7N.

6. The sample carrier for glow discharge mass spectrometer measurement according to claim 1 or 5, characterized in that: The thickness of the sample preparation pressed sheet is 1 to 3 mm.

7. The sample carrier for glow discharge mass spectrometer measurement according to claim 1, characterized in that: After the sample preparation pressed sheet is unfolded, the orthographic projection on the second end surface covers the positioning groove; Preferably, the sample preparation pressed sheet after unfolding is rectangular or circular.

8. The sample carrier for glow discharge mass spectrometer measurement according to claim 1, characterized in that: The cross section of the sample base is circular; Preferably, the diameter of the sample base is equal to the diameter of the second end surface of the pressing body; Preferably, the height of the sample base is 20-40 mm.

9. The sample carrier device for glow discharge mass spectrometer measurement according to claim 2, characterized in that: The diameter of the second end surface of the pressing body is 80 to 120 mm; Preferably, the height of the pressing body is 60-80 mm.

10. The sample carrier for glow discharge mass spectrometer measurement according to claim 9, characterized in that: The height of the handle is 20-30 mm.

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