CN115639232A - Fluorescent sulfur, chlorine and silicon element integrated tester based on single-wavelength dispersion - Google Patents
Fluorescent sulfur, chlorine and silicon element integrated tester based on single-wavelength dispersion Download PDFInfo
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- CN115639232A CN115639232A CN202211192122.6A CN202211192122A CN115639232A CN 115639232 A CN115639232 A CN 115639232A CN 202211192122 A CN202211192122 A CN 202211192122A CN 115639232 A CN115639232 A CN 115639232A
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Abstract
The invention discloses a fluorescent sulfur-chlorine-silicon element integrated tester based on single-wavelength dispersion, which comprises an X-ray light pipe, a sample chamber, a hyperboloid curved crystal, a first detector, a second detector, a third detector, a first crystal, a second crystal and a third crystal; the hyperboloid curved crystal is arranged on one side of the X-ray light pipe, the sample chamber is arranged on one side of the hyperboloid curved crystal, the first crystal, the second crystal and the third crystal are respectively arranged on one side of the sample chamber, the first detector is arranged on one side of the first crystal to receive sulfur element detection light, the second detector is arranged on one side of the second crystal to receive chlorine element detection light, and the third detector is arranged on one side of the third crystal to receive silicon element detection light; through the structure, the measurement of total sulfur, total chlorine and total silicon elements is concentrated in one instrument, three elements can be analyzed at one time, the environment is protected, energy is saved, and the operation efficiency is greatly improved.
Description
Technical Field
The invention relates to the technical field of chemical product detection, in particular to a fluorescent sulfur, chlorine and silicon element integrated tester based on single-wavelength dispersion.
Background
With the expansion of the application field of the trace element X-ray fluorescence measuring instrument, more X-ray fluorescence measuring instruments for measuring one element are available in the market, and only a plurality of instruments can be purchased to measure the content of various elements, so that the great resource waste is caused.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide an integrated tester for fluorescent sulfur, chlorine and silicon elements based on single-wavelength dispersion.
The technical scheme adopted by the invention is as follows:
a fluorescent sulfur-chlorine-silicon element integrated tester based on single-wavelength dispersion comprises an X-ray light pipe, a sample chamber for introducing a sample, a hyperboloid curved crystal, a first detector, a second detector, a third detector, a first crystal, a second crystal and a third crystal; the hyperboloid curved crystal is arranged on one side of the X-ray light pipe to receive incident light, the sample chamber is arranged on one side of the hyperboloid curved crystal to receive diffracted light, the first crystal, the second crystal and the third crystal are respectively arranged on one side of the sample chamber to correspondingly receive sulfur element fluorescent light, chlorine element fluorescent light and silicon element fluorescent light, the first detector is arranged on one side of the first crystal to receive sulfur element detection light, the second detector is arranged on one side of the second crystal to receive chlorine element detection light, and the third detector is arranged on one side of the third crystal to receive silicon element detection light.
Further, the hyperboloid curved crystal is arranged on one side of the X-ray light pipe, so that the crystal face of any point of the hyperboloid curved crystal, which is irradiated by the characteristic X-ray emitted by the X-ray light pipe, meets the Bragg condition.
Further, the first detector and the first crystal are located on one side of the diffracted light.
Further, the second detector, the third detector, the second crystal and the third crystal are positioned on the other side of the diffracted light.
Further, the X-ray tube temperature control device further comprises a constant temperature device, and the X-ray tube is placed in the constant temperature device.
Further, constant temperature equipment includes constant temperature control circuit, temperature sensor, heat abstractor and refrigerating plant, temperature sensor with constant temperature control circuit connects for detect the apparent temperature of X-ray tube and send the temperature value for constant temperature control circuit, constant temperature control circuit with heat abstractor and refrigerating plant are connected for according to the temperature value control heat abstractor and refrigerating plant work.
The system further comprises a single chip microcomputer and an upper computer, wherein the output ends of the first detector, the second detector and the third detector are connected with the single chip microcomputer, and the single chip microcomputer is communicated with the upper computer.
Additional aspects and advantages of the present application will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the present application.
Drawings
In order to more clearly illustrate the detailed description of the invention or the technical solutions in the prior art, the drawings that are needed in the detailed description of the invention or the prior art will be briefly described below. Throughout the drawings, like elements or portions are generally identified by like reference numerals. In the drawings, elements or portions are not necessarily drawn to scale.
FIG. 1 is a schematic structural diagram of an integrated measuring instrument for measuring sulfur, chlorine and silicon elements based on single-wavelength dispersion fluorescence provided by an embodiment of the application;
fig. 2 is a schematic structural diagram of a thermostat device provided in an embodiment of the present application.
The device comprises an X-ray light pipe 1, a hyperboloid curved crystal 2, a sample chamber 3, a first crystal 4, a second crystal 5, a third crystal 6, a first detector 7, a second detector 8, a third detector 9, a constant temperature device 10, a temperature sensor 101, a constant temperature control circuit 102, a heat dissipation device 103 and a refrigeration device 104.
Detailed Description
Embodiments of the present invention will be described in detail with reference to specific embodiments. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains.
Referring to fig. 1-2, the integrated tester for fluorescent sulfur, chlorine and silicon elements based on single wavelength dispersion comprises an X-ray light pipe 1, a sample chamber 3 for introducing a sample, a hyperboloid curved crystal 2, a first detector 7, a second detector 8, a third detector 9, a first crystal 4, a second crystal 5 and a third crystal 6; the hyperboloid curved crystal 2 is arranged on one side of the X-ray light pipe 1 to receive incident light, the sample chamber 3 is arranged on one side of the hyperboloid curved crystal 2 to receive diffracted light, the first crystal 4, the second crystal 5 and the third crystal 6 are respectively arranged on one side of the sample chamber 3 to correspondingly receive sulfur element fluorescent light, chlorine element fluorescent light and silicon element fluorescent light, the first detector 7 is arranged on one side of the first crystal 4 to receive sulfur element detection light, the second detector 8 is arranged on one side of the second crystal 5 to receive chlorine element detection light, and the third detector 9 is arranged on one side of the third crystal 6 to receive silicon element detection light.
Through the structure, the measurement of total sulfur, total chlorine and total silicon elements is concentrated in one instrument, three elements can be analyzed at one time, the environment is protected, energy is saved, and the operation efficiency is greatly improved.
The X-ray light pipe 1 adopts a micro focal spot cadmium target thin beryllium window X-ray tube which is used as a point light source and is used for emitting characteristic X-rays.
The fluorescent ray energy of the three elements of silicon, sulfur and chlorine is respectively as follows: 1.74Kev, 2.31Kev, 2.62Kev, absorption limits are: 1.84Kev, 2.47Kev and 2.82Kev, and the micro-focal-spot cadmium target thin beryllium window X-ray tube is selected to ensure that elastically scattered and non-scattered X-rays in a sample do not overlap with fluorescence lines of required detection elements.
The hyperboloid curved crystal 2 adopts a full-focusing hyperboloid curved crystal 2, and is arranged on one side of the X-ray tube 1 to ensure that a crystal face of any point of the hyperboloid curved crystal 2, which is irradiated by characteristic X-rays, meets Bragg conditions, and is strictly focused to an emergent point on the surface of a Rowland circle, so that high-intensity point-to-point diffraction focusing is realized, and a high-intensity target material characteristic spectrum in an emergent spectrum of the X-ray tube is subjected to monochromatization focusing and is irradiated into a sample.
The hyperboloid curved crystal 2 is used for diffracting and focusing a high-intensity target material characteristic spectral line and a crystal secondary target material characteristic spectral line in the characteristic X-ray to a sample surface, irradiating the sample in a monochromatization mode, improving the characteristic element excitation efficiency by energy focusing, greatly improving the signal-to-noise ratio, and solving the problems of low element excitation efficiency and low detection precision.
The sample chamber 3 is used for introducing a sample and is arranged on one side of the hyperboloid curved crystal 2, and diffraction light rays formed by diffraction of characteristic X rays from the hyperboloid curved crystal 2 are focused on the center of a sample surface of the sample chamber 3.
The first detector 7, the second detector 8 and the third detector 9 are used to convert the detected elemental signature fluorescence signal into an electrical signal. The first detector 7, the second detector 8 and the third detector 9 all adopt high-resolution silicon drift detectors, which have high resolution at high counting rate and can detect low-content elements.
The first detector 7 and the first crystal 4 are positioned on one side of the diffracted light, and the first detector 7 is used for detecting sulfur element in the sample.
The second detector 8, the third detector 9, the second crystal 5 and the third crystal 6 are positioned on the other side of the diffracted light; the second detector 8 is used for detecting chlorine element in the sample, and the third detector 9 is used for detecting silicon element in the sample.
In order to process data conveniently, the system further comprises a single chip microcomputer and an upper computer, output ends of the first detector 7, the second detector 8 and the third detector 9 are connected with the single chip microcomputer, and the single chip microcomputer is communicated with the upper computer.
The first detector 7, the second detector 8 and the third detector 9 convert element characteristic fluorescence signals detected in the sample into electric signals, the electric signals are subjected to noise reduction, suppression and amplification processing and then sent to the single chip microcomputer, the single chip microcomputer sends data to the upper computer, and the upper computer processes the signals to obtain detection data.
During data processing, mathematical models such as a basic parameter method and a nonlinear least square method can be adopted to fit curves, influences such as spectral line overlapping interference among elements, absorption enhancement effect among elements, matrix effect and the like are reduced, X-ray fluorescence intensity is obtained and subjected to non-standard quantitative calculation, a working curve is established by using a non-standard calculated value and a standard sample set value, the calculated value is calibrated, and a final test result is obtained.
When the X-ray light pipe 1 works, certain heat can be generated on the outer surface of the pipe, certain influence is generated on electronic devices and other precise components in the instrument, the heat is radiated on an outer surface shell of the instrument, the temperature of the outer surface shell is higher, and in order to effectively reduce the heat generated when the X-ray light pipe 1 works and prolong the service life of the instrument, the X-ray tube constant temperature device 10 is further included, and the X-ray tube is arranged in the constant temperature device 10.
The constant temperature device 10 comprises a constant temperature control circuit 102, a temperature sensor 101, a heat dissipation device 103 and a refrigeration device 104, wherein the temperature sensor 101 is connected with the constant temperature control circuit 102 and used for detecting the surface temperature of the X-ray tube and sending a temperature value to the constant temperature control circuit 102, and the constant temperature control circuit 102 is connected with the heat dissipation device 103 and the refrigeration device 104 and used for controlling the heat dissipation device 103 and the refrigeration device 104 to work according to the temperature value.
After a standard sample is introduced into the sample chamber 3, an element characteristic spectral line is excited under the irradiation of X-rays, a counting pulse signal is output after the detector detects energy, and an energy spectrum is drawn after a series of processing on the signal, so that the whole process of one-time sample detection is completed.
The method comprises the steps of respectively introducing standard samples with different concentrations to obtain different counting rates, automatically calculating characteristic parameters and correlation coefficients of curves according to different counting rate systems, drawing standard curves according to the counting rates, and testing the content of unknown samples according to the standard curves.
After the test is started, the thermostatic control circuit 102 is powered on and works, the temperature sensor 101 detects the temperature, and when the temperature is less than or equal to 20 ℃, the refrigerating device 104 and the heat dissipation device 103 do not work. When the detected temperature is more than 20 ℃, the refrigerating device 104 and the heat sink 103 start to work, in the working process, the real-time temperature of the temperature sensor 101 is circularly detected, and when the temperature of the temperature sensor 101 is detected to be less than or equal to 20 ℃, the refrigerating device 104 and the heat sink stop.
By adopting the tester, a high-temperature combustion sample is not needed, the sample is simple to process, the environment is protected, the energy is saved, the reliability is high, the stability is high, various elements can be analyzed at one time, the detection speed is high, and the operation and maintenance cost is low.
In this application, unless expressly stated or limited otherwise, the terms "connected," "secured," and the like are to be construed broadly and can include, for example, fixed connections, removable connections, or integral combinations thereof; may be an electrical connection; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the description of the present invention, numerous specific details are set forth. It is understood, however, that embodiments of the invention may be practiced without these specific details. In some instances, well-known methods, systems, and techniques have not been shown in detail in order not to obscure an understanding of this description.
In the description of the specification, reference to the description of "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" or the like means that a particular feature, system, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, systems, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Moreover, various embodiments or examples and features of various embodiments or examples described in this specification can be combined and combined by one skilled in the art without being mutually inconsistent.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.
Claims (7)
1. The integrated tester based on the single-wavelength dispersion fluorescence sulfur, chlorine and silicon elements comprises an X-ray light pipe and a sample chamber for introducing a sample, and is characterized by further comprising a hyperboloid curved crystal, a first detector, a second detector, a third detector, a first crystal, a second crystal and a third crystal; the hyperboloid curved crystal is arranged on one side of the X-ray light pipe to receive incident light, the sample chamber is arranged on one side of the hyperboloid curved crystal to receive diffracted light, the first crystal, the second crystal and the third crystal are respectively arranged on one side of the sample chamber to correspondingly receive sulfur element fluorescent light, chlorine element fluorescent light and silicon element fluorescent light, the first detector is arranged on one side of the first crystal to receive sulfur element detection light, the second detector is arranged on one side of the second crystal to receive chlorine element detection light, and the third detector is arranged on one side of the third crystal to receive silicon element detection light.
2. The integrated determinator based on single-wavelength dispersion fluorescent S-Cl-Si element according to claim 1, wherein the hyperboloid curved crystal is arranged on one side of the X-ray light pipe, so that a crystal face of any point of the hyperboloid curved crystal, which is incident to the characteristic X-ray emitted by the X-ray light pipe, meets Bragg condition.
3. The integrated single-wavelength dispersion fluorescence-based S-Cl-Si element tester as claimed in claim 1, wherein the first detector and the first crystal are located at one side of the diffracted light.
4. The integrated tester for measuring the silicon, sulfur and chlorine elements based on the single wavelength dispersion fluorescence according to claim 1, wherein the second detector, the third detector, the second crystal and the third crystal are positioned on the other side of the diffracted light.
5. The single-wavelength dispersion fluorescence-based S, cl and Si element integrated tester according to any one of claims 1-4, further comprising a constant temperature device, wherein the X-ray tube is arranged in the constant temperature device.
6. The single-wavelength dispersion fluorescence sulfur-chlorine-silicon element-based integrated measuring instrument according to claim 5, wherein the constant temperature device comprises a constant temperature control circuit, a temperature sensor, a heat dissipation device and a refrigeration device, the temperature sensor is connected with the constant temperature control circuit and used for detecting the surface temperature of the X-ray tube and sending a temperature value to the constant temperature control circuit, and the constant temperature control circuit is connected with the heat dissipation device and the refrigeration device and used for controlling the heat dissipation device and the refrigeration device to work according to the temperature value.
7. The integrated determinator based on single-wavelength dispersion fluorescence sulfur-chlorine-silicon element according to claim 5 is characterized by further comprising a single chip microcomputer and an upper computer, wherein the output ends of the first detector, the second detector and the third detector are all connected with the single chip microcomputer, and the single chip microcomputer is communicated with the upper computer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211192122.6A CN115639232A (en) | 2022-09-28 | 2022-09-28 | Fluorescent sulfur, chlorine and silicon element integrated tester based on single-wavelength dispersion |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211192122.6A CN115639232A (en) | 2022-09-28 | 2022-09-28 | Fluorescent sulfur, chlorine and silicon element integrated tester based on single-wavelength dispersion |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116124814A (en) * | 2023-04-07 | 2023-05-16 | 太仓市建设工程质量检测中心有限公司 | Method for detecting sulfur dioxide content in atmosphere by single wavelength dispersion X-ray fluorescence |
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2022
- 2022-09-28 CN CN202211192122.6A patent/CN115639232A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116124814A (en) * | 2023-04-07 | 2023-05-16 | 太仓市建设工程质量检测中心有限公司 | Method for detecting sulfur dioxide content in atmosphere by single wavelength dispersion X-ray fluorescence |
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