Preparation method of semi-quantitative detection sample of fluorescence spectrophotometer

Abstract

The invention relates to the field of X-ray fluorescence spectrophotometer semi-quantitative or qualitative analysis, and discloses a preparation method of a fluorescence spectrophotometer semi-quantitative detection sample, which comprises the following steps: S1, taking a proper amount of powder to-be-detected sample for later use; s2, selecting a plastic ring according to a to-be-tested sample, and filling the plastic ring with the to-be-tested sample; s3, respectively covering the upper and lower sides of the plastic ring with a piece of weighing paper, and placing the weighing paper in the center of the sample pressing table; and S4, performing sample pressing and forming, and then removing the weighing paper to obtain a sample sheet. According to the scheme, the to-be-tested sample can be prevented from being in contact with other substances, pollution is reduced, the equipment requirement and the sample loss are reduced, the sample size can be flexibly adjusted, different analysis requirements are met, the sample preparation method can be mastered without professional training, operation is easy and convenient, cost is low, and efficiency is high; the emulsion sample can be effectively pressed to obtain a sample piece, and the detection effect of the to-be-tested sample is not influenced.

Description

Technical Field

[0001] The invention relates to the field of semi-quantitative or qualitative analysis of X-ray fluorescence spectrometer, and in particular to a method for preparing a sample for semi-quantitative detection by fluorescence spectrometer. Background Art

[0002] Fluorescence spectroscopy, as an advanced scientific analysis method, has been widely used in the field of material composition and content detection due to its unique advantages. This technology does not require complex chemical pretreatment steps or reliance on standard samples, and can achieve non-destructive analysis of unknown substances. Through semi-quantitative and qualitative analysis of fluorescence spectra, researchers can quickly obtain information on the composition and approximate content of substances, which is of great significance to many fields such as materials science, environmental monitoring, and food safety.

[0003] In fluorescence spectroscopy, X-ray fluorescence spectrometer is a commonly used detection instrument. However, for the preparation of powder samples and emulsion samples, the sample preparation process of X-ray fluorescence spectrometer faces certain challenges. At present, there are three main methods for powder tableting of X-ray fluorescence spectrometer: the first is to place the sample directly in a plastic ring and press it into a tablet by applying a certain pressure and time; the second method is to directly press the tablet after mixing the adhesive and the reagent evenly; the third method is to use boric acid edging pads for pressing. These three methods have their own advantages and are suitable for different types of powder samples. However, when it comes to emulsion samples, these three sample preparation methods have obvious limitations. The emulsion sample pressed by the first method is easy to crack and it is difficult to form a complete sheet structure, which directly affects the detection effect of the X-ray fluorescence spectrometer. Although the second method can press the emulsion and the adhesive into tablets, the introduction of the adhesive will interfere with the semi-quantitative and qualitative analysis, reducing the accuracy of the analysis. The third method has poor sample preparation effect due to the poor adhesion between the emulsion and boric acid.

[0004] Due to the limitations of the above-mentioned sample preparation methods, X-ray fluorescence spectrometers have encountered difficulties in semi-quantitative and qualitative analysis of emulsion samples. In order to overcome this problem, researchers usually choose to use plasma spectrometers for alternative analysis. Although the plasma spectrometer requires a series of tedious operating steps such as digestion, transfer, and volume determination during the analysis process, the process is relatively complicated and time-consuming, but its detection effect on emulsion samples is more accurate and reliable. However, this undoubtedly increases the detection cost and time cost, and has a certain impact on the detection efficiency.

[0005] In summary, although fluorescence spectroscopy analysis technology has many advantages, it still faces certain challenges in the detection of emulsion samples. How to optimize the sample preparation method of X-ray fluorescence spectrometer and improve the detection efficiency and accuracy of emulsion samples is a problem that needs to be solved urgently. Summary of the invention

[0006] In view of this, the purpose of the embodiment of the present invention is to propose a method for preparing a sample for semi-quantitative detection by a fluorescence spectrometer. The method has a wide range of applications, avoids the inapplicability of the traditional direct tableting method and the boric acid-rimmed tableting method in emulsion or powder samples, can avoid contact between the sample and other substances, reduce pollution, and reduce equipment requirements and sample loss. The sample size can be flexibly adjusted to meet different analysis requirements. The sample preparation method can be mastered without professional training. The operation is simple, the cost is low, and the efficiency is high. The emulsion sample can be effectively pressed to obtain a sample sheet, and the detection effect of the sample to be tested will not be affected.

[0007] Based on the above purpose, an embodiment of the present invention provides a method for preparing a sample for semi-quantitative detection by a fluorescence spectrometer, comprising: S1, take an appropriate amount of powdered material to be tested; S2, selecting a plastic ring according to the sample to be tested, and filling the plastic ring with the sample to be tested; S3, cover the upper and lower parts of the plastic ring with a piece of weighing paper and place them at the center of the sample pressing table; S4, press the sample into shape, then remove the weighing paper to obtain the sample piece.

[0008] According to one embodiment of the present invention, in step S1, the sample to be tested is dried in an oven at a drying temperature of 105° C. for a drying time of 2 hours.

[0009] According to an embodiment of the present invention, step S1 includes: drying the emulsion to be tested sample to obtain the powder to be tested sample.

[0010] According to one embodiment of the present invention, in step S2, the diameter of the plastic ring is greater than 30 mm.

[0011] According to an embodiment of the present invention, in step S2, the sample to be tested is spread on the inner side of the plastic ring to fill the plastic ring.

[0012] According to one embodiment of the present invention, in step S3, the weighing paper is dry, clean, oily weighing paper.

[0013] According to one embodiment of the present invention, in step S3, the length and width of the weighing paper are greater than the diameter of the plastic ring.

[0014] According to an embodiment of the present invention, in step S4, the effective detection area of ​​the sample piece is not less than 10 mm×10 mm.

[0015] According to one embodiment of the present invention, in step S4, the pressure of the sample pressing is not less than 10 MPa.

[0016] According to one embodiment of the present invention, in step S4, the time for pressing the sample is 10 to 30 seconds.

[0017] The present invention has at least the following beneficial technical effects: The present invention provides a method for preparing a sample for semi-quantitative detection by a fluorescence spectrometer suitable for emulsion and powder samples, which uses a manual sample pressing device to achieve low-pressure molding, without the need for chemical pretreatment and additional adhesives, thereby improving analysis accuracy and practicality. During the sample pressing process, an oily weighing paper is covered on the top and bottom, thereby reducing the contact between the sample and other substances, reducing pollution, and promoting the pressing of the sample into sheets. The manual sample pressing pressure is small, and the sample ring will not crack. The sample size can be flexibly adjusted, which is suitable for different analysis needs. This method reduces equipment requirements, improves sample preparation flexibility, and realizes a pollution-free sample preparation method without the introduction of additional reagents. It will not affect the detection effect of the emulsion sample and can provide reliable analysis results. The operation is simple, the cost is low, and the efficiency is high, which is suitable for daily laboratory analysis. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present invention. For ordinary technicians in this field, other embodiments can be obtained based on these drawings without paying creative work.

[0019] Figure 1 The present invention provides a schematic diagram of an embodiment of a method for preparing a sample for semi-quantitative detection by a fluorescence spectrometer. DETAILED DESCRIPTION

[0020] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the embodiments of the present invention are further described in detail below in combination with specific embodiments and with reference to the accompanying drawings.

[0021] The terms "including" and "having" and any variations thereof in the specification and claims of the present invention and the above-mentioned drawings are intended to cover non-exclusive inclusions; the terms "first", "second", etc. in the specification and claims of the present invention or the above-mentioned drawings are used to distinguish different objects rather than to describe a specific order. "Multiple" means two or more, unless otherwise clearly and specifically defined.

[0022] In addition, reference to "embodiments" herein means that a particular feature, structure, or characteristic described in conjunction with the embodiments may be included in at least one embodiment of the present invention. The appearance of the phrase in various places in the specification does not necessarily refer to the same embodiment, nor is it an independent or alternative embodiment that is mutually exclusive with other embodiments. It is explicitly and implicitly understood by those skilled in the art that the embodiments described herein may be combined with other embodiments.

[0023] like Figure 1 The method for preparing a sample for semi-quantitative detection by a fluorescence spectrometer provided by the present invention comprises the following steps: S1, take an appropriate amount of powdered material to be tested; S2, selecting a plastic ring according to the sample to be tested, and filling the plastic ring with the sample to be tested; S3, cover the upper and lower parts of the plastic ring with a piece of weighing paper and place them at the center of the sample pressing table; S4, press the sample into shape, then remove the weighing paper to obtain the sample piece.

[0024] According to one embodiment of the present invention, by using a manual sample pressing device, a manual sample pressing and tableting method for an emulsion sample or a powder sample is designed, so that a semi-quantitative analysis of the emulsion or powder sample can be completed, and the analysis result is consistent with the analysis result of the plasma spectrometer. In one example, the sample to be tested is an emulsion, and the specific operation steps of the sample pressing method include: (1) Drying treatment of emulsion samples: Dry the emulsion samples in an oven at 105°C for 2 hours to remove moisture and improve the compressibility of the samples; (2) Plastic ring fixation: Select a plastic ring of appropriate size (diameter is generally greater than 30 mm), and spread the emulsion sample on the inside of the plastic ring to ensure that the sample is evenly stressed during the compression process to reduce the risk of breakage; (3) Weighing paper isolation: Cover the upper and lower parts of the plastic ring with oily weighing paper to reduce direct contact between the sample and the equipment and ensure that the sample piece is fully formed; (4) Manual pressing: carefully transfer the weighing paper and plastic ring to the center of the sample pressing table, apply a pressure of 10 MPa and maintain for 10 s, then unload the pressure and carefully remove the weighing paper above and below the sample to obtain a stable sample piece, which is then numbered for later use; (5) XRF analysis: Select the appropriate test area according to the sample size for semi-quantitative analysis.

[0025] According to one embodiment of the present invention, the advantages of the above-mentioned operation steps include: a wide range of applications, avoiding the inapplicability of traditional direct tableting and boric acid-rimmed tableting methods in emulsion or powder samples, and covering the upper and lower parts with an oily weighing paper during the sample pressing process, thereby reducing the contact between the sample and other substances, reducing pollution, and promoting the sample to be pressed into tablets. The manual sample pressing pressure is small, and the sample ring will not crack. The sample size can be flexibly adjusted, which is suitable for different analysis needs. The operation is simple and easy, and the sample preparation method can be mastered without professional training. The method of the present invention reduces equipment requirements and sample loss, improves sample preparation flexibility, realizes a pollution-free sample preparation method without the introduction of additional reagents, does not affect the detection effect of emulsion samples, improves the stability and repeatability of XRF analysis, and can provide reliable analysis results. It avoids the defects of traditional sample preparation methods, improves test accuracy, is suitable for daily laboratory analysis, and has good promotion and application value.

[0026] According to one embodiment of the present invention, in step S1, the sample to be tested is dried in an oven at a drying temperature of 105° C. for a drying time of 2 hours.

[0027] According to an embodiment of the present invention, step S1 includes: drying the emulsion to be tested sample to obtain the powder to be tested sample.

[0028] According to one embodiment of the present invention, in step S2, the diameter of the plastic ring is greater than 30 mm.

[0029] According to an embodiment of the present invention, in step S2, the sample to be tested is spread on the inner side of the plastic ring to fill the plastic ring.

[0030] According to one embodiment of the present invention, in step S3, the weighing paper includes dry, clean oily weighing paper.

[0031] According to one embodiment of the present invention, in step S3, the length and width of the weighing paper are greater than the diameter of the plastic ring.

[0032] According to an embodiment of the present invention, in step S4, the effective detection area of ​​the sample piece is not less than 10 mm×10 mm.

[0033] According to one embodiment of the present invention, in step S4, the pressure of the sample pressing is not less than 10 MPa.

[0034] According to one embodiment of the present invention, in step S4, the time for pressing the sample is 10 to 30 seconds.

[0035] The present invention provides a method for preparing a sample for semi-quantitative detection by a fluorescence spectrometer suitable for emulsion and powder samples, which uses a manual sample pressing device to achieve low-pressure molding, without the need for chemical pretreatment and additional adhesives, thereby improving analysis accuracy and practicality. During the sample pressing process, an oily weighing paper is covered on the top and bottom, thereby reducing the contact between the sample and other substances, reducing pollution, and promoting the pressing of the sample into sheets. The manual sample pressing pressure is small, and the sample ring will not crack. The sample size can be flexibly adjusted, which is suitable for different analysis needs. This method reduces equipment requirements, improves sample preparation flexibility, and realizes a pollution-free sample preparation method without the introduction of additional reagents. It will not affect the detection effect of the emulsion sample and can provide reliable analysis results. The operation is simple, the cost is low, and the efficiency is high, which is suitable for daily laboratory analysis.

[0036] The present invention is further explained below in conjunction with specific embodiments and comparative examples.

[0037] Example 1 (1) Sample processing Take a certain amount of emulsion sample, place it in an oven, and dry it at 105°C for 2 hours to ensure that the sample is free of moisture.

[0038] (2) Sample preparation steps 1. Select a plastic ring that is suitable for the sample size (30 mm or 120 mm is recommended).

[0039] 2. Place the plastic ring on a dry, clean weighing paper.

[0040] 3. Spread the dried emulsion sample evenly on the inside of the plastic ring.

[0041] 4. Cover the plastic ring and the sample with a piece of weighing paper and transfer them to the center of the manual press.

[0042] 5. Apply 10 MPa pressure and maintain for 10 s, then unload the pressure.

[0043] 6. Take out the sample, remove the weighing papers above and below, and number them for later use.

[0044] (3) On-machine testing Select the XRF analysis program with a detection area of ​​10 mm × 10 mm, perform semi-quantitative analysis, and record the element contents.

[0045] Test Results The emulsion sample prepared by this method is consistent with the analysis results of plasma spectrometer (ICP), which proves that this method is suitable for XRF semi-quantitative analysis.

[0046] The present invention provides a method for preparing a sample suitable for semi-quantitative detection of an emulsion by a fluorescence spectrometer, which uses a manual sample pressing device to achieve low-pressure molding, without the need for chemical pretreatment and additional adhesives, thereby improving analysis accuracy and practicality. During the sample pressing process, an oily weighing paper is covered on the top and bottom, thereby reducing the contact between the sample and other substances, reducing pollution, and promoting the pressing of the sample into sheets. The manual sample pressing pressure is small, and the sample ring will not crack. The sample size can be flexibly adjusted, which is suitable for different analysis needs. This method reduces equipment requirements, improves sample preparation flexibility, and achieves a pollution-free sample preparation method without the introduction of additional reagents. It will not affect the detection effect of the emulsion sample and can provide reliable analysis results. It is simple to operate, low cost, and high efficiency, and is suitable for daily laboratory analysis.

[0047] Example 2 (1) Sample processing Take a certain amount of powder sample without drying.

[0048] (2) Sample preparation steps 1. Select a suitable plastic ring (30 mm or 120 mm is recommended).

[0049] 2. Place the plastic ring on a dry, clean weighing paper.

[0050] 3. Spread the powder sample evenly on the inside of the plastic ring.

[0051] 4. Cover the plastic ring and the sample with a piece of weighing paper and transfer them to the center of the manual press.

[0052] 5. Apply 10 MPa pressure and maintain for 30 s, then unload the pressure.

[0053] 6. Take out the sample, remove the weighing papers above and below, and number them for later use.

[0054] (3) On-machine testing Select an appropriate XRF analysis program, perform semi-quantitative analysis, and record the element content.

[0055] Test Results This method effectively solves the problems of direct tableting of powdered samples and failure of tableting with boric acid inserts, increases the sample preparation success rate to over 90%, and has good test repeatability.

[0056] The present invention provides a method for preparing a sample for semi-quantitative detection by a fluorescence spectrometer suitable for powder samples, which uses a manual sample pressing device to achieve low-pressure molding, without the need for chemical pretreatment and additional adhesives, thereby improving analysis accuracy and practicality. During the sample pressing process, an oily weighing paper is covered on the top and bottom, thereby reducing the contact between the sample and other substances, reducing pollution, and promoting the pressing of the sample into sheets. The manual sample pressing pressure is small, and the sample ring will not crack. The sample size can be flexibly adjusted, which is suitable for different analysis needs. This method reduces equipment requirements, improves sample preparation flexibility, and realizes a pollution-free sample preparation method without the introduction of additional reagents. It will not affect the detection effect of powder samples and can provide reliable analysis results. It is simple to operate, low cost, and high efficiency, and is suitable for daily laboratory analysis.

[0057] The above are exemplary embodiments disclosed in the present invention, but it should be noted that various changes and modifications may be made without departing from the scope disclosed in the embodiments of the present invention as defined in the claims. The functions, steps and / or actions of the method claims according to the disclosed embodiments described herein do not need to be performed in any particular order. In addition, although the elements disclosed in the embodiments of the present invention may be described or required in individual form, they may also be understood as multiple unless explicitly limited to the singular.

[0058] It should be understood that, as used herein, the singular forms "a", "an" are intended to include the plural forms as well, unless the context clearly supports an exception. It should also be understood that, as used herein, "and / or" refers to any and all possible combinations including one or more of the associated listed items.

[0059] The serial numbers of the embodiments disclosed in the above embodiments of the present invention are only for description and do not represent the advantages or disadvantages of the embodiments.

[0060] A person skilled in the art should understand that the discussion of any of the above embodiments is only exemplary and is not intended to imply that the scope of the disclosure of the embodiments of the present invention (including the claims) is limited to these examples; under the concept of the embodiments of the present invention, the technical features in the above embodiments or different embodiments can also be combined, and there are many other changes in different aspects of the above embodiments of the present invention, which are not provided in detail for the sake of simplicity. Therefore, any omissions, modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the embodiments of the present invention should be included in the protection scope of the embodiments of the present invention.

Claims

1. A method for preparing a sample for semi-quantitative detection by a fluorescence spectrometer, characterized in that: include: S1, take an appropriate amount of powdered material to be tested; S2, selecting a plastic ring according to the sample to be tested, and filling the plastic ring with the sample to be tested; S3, cover the upper and lower parts of the plastic ring with a piece of weighing paper and place them at the center of the sample pressing table; S4, press the sample into shape, then remove the weighing paper to obtain the sample piece.

2. The preparation method according to claim 1, characterized in that: In step S1, the sample to be tested is dried in an oven at a drying temperature of 105°C for a drying time of 2 hours.

3. The preparation method according to claim 1, characterized in that: Step S1 includes: drying the emulsion to be tested sample to obtain the powder to be tested sample.

4. The preparation method according to claim 1, characterized in that: In step S2, the diameter of the plastic ring is greater than 30 mm.

5. The preparation method according to claim 1, characterized in that: In step S2, the sample to be tested is spread flat on the inner side of the plastic ring to fill the plastic ring.

6. The preparation method according to claim 1, characterized in that: In step S3, the weighing paper is dry, clean, oily weighing paper.

7. The preparation method according to claim 1, characterized in that: In step S3, the length and width of the weighing paper are greater than the diameter of the plastic ring.

8. The preparation method according to claim 1, characterized in that: In step S4, the effective detection area of ​​the sample piece is not less than 10 mm×10 mm.

9. The preparation method according to claim 1, characterized in that: In step S4, the pressure of the sample pressing is not less than 10 MPa.

10. The preparation method according to claim 1, characterized in that: In step S4, the time for pressing the sample is 10 to 30 seconds.

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