CN101196482B - Testing apparatus and method for X-ray fluorescence analysis - Google Patents
Testing apparatus and method for X-ray fluorescence analysis Download PDFInfo
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- CN101196482B CN101196482B CN2007101942077A CN200710194207A CN101196482B CN 101196482 B CN101196482 B CN 101196482B CN 2007101942077 A CN2007101942077 A CN 2007101942077A CN 200710194207 A CN200710194207 A CN 200710194207A CN 101196482 B CN101196482 B CN 101196482B
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Abstract
The invention provides a testing device measuring the chlorine content through X Rays fluorometric analysis, which utilizes a high voltage generator to receive the electric current from outside to generate high-voltage electric current and utilizes the voltage controller to control the high-voltage electric current into the operating voltage in the range of 5 to 15 kv; a light tube is motivated by the operating voltage to send up X Rays, a filter filters the X Rays from the light tube to filter off the noises and sends out fluorescence after shining sample, and the tester receives the fluorescence to form testing signal; then, the testing sample of arithmetic processor is compared to count the content of microcontent chlorine.
Description
Technical field
The invention relates to a kind of pick-up unit and detection method of x-ray fluorescence analysis, refer to especially utilize x-ray fluorescence analysis to detect the pick-up unit and the detection method of micro-chlorine.
Background technology
The idea that whole world response environmental protection is helped planet Earth is arrived gradually, environmental protection standard in response to European RoHS, in electronic product at the restriction of halogen family element, the concentration summation of bromine (Br) and chlorine (Cl) must be below 1500ppm (per mille concentration), and the concentration of each halogen family element also must be below 900ppm.
When using x-ray fluorescence analyzer to detect noxious material in the past, the bromine of trace can be checked out, but, the chlorine of 1000ppm to 50000ppm scope can only be measured at chlorine.Because in the PVC material, have the chlorine of high concentration, still be free from chloride PE material for the PVC material so the past on practice, can only be used for detecting resolution sample thing.
At present under the environmental protection standard of RoHS, need check out the chlorine of trace,, make the product compliant and the market of marketing to avoid contaminated environment, but the operation manual with the existing machine of present x-ray fluorescence analyzer is tested, and all can't record the existence of the following micro-chlorine of 1000ppm.
Therefore, fundamental purpose of the present invention is to provide a kind of pick-up unit and the detection method of x-ray fluorescence analysis to detect micro-chlorine of utilizing, to improve the problems referred to above.
Summary of the invention
Purpose of the present invention can be checked out the micro-chlorine of trace as 100ppm in pick-up unit that a kind of x-ray fluorescence analysis is provided and detection method, so that product meets the environmental protection standard of European RoHS, not only expands business opportunity, and can accomplish environmental protection conscientiously.
The invention relates to a kind of pick-up unit and detection method of x-ray fluorescence analysis, in order to analyze the chlorine of trace in the sample.This pick-up unit further comprises a high-pressure generator, a voltage controller, a light pipe, a wave filter (filter), a detecting device and an operation processing unit.
This high-pressure generator receives electric current from the outside to produce high-tension current.The high-tension current that this voltage controller is given birth to this high-pressure generator is controlled to be 5 kilovolts (KV) to the operating voltage between 15 kilovolt range.
This light pipe is excited by the electric current of this operating voltage that this voltage controller produces, and penetrates an X ray.This wave filter filter the emitted X ray of this light pipe with elimination 0.3 keV (kev) to the noise between the keV scope, and this sample of the x-ray bombardment after will filtering makes this sample be subjected to disengage a fluorescence behind this excitation of X-rays.
This detecting device receives this fluorescence, to form an inspection amount signal.Comparing an inspection amount sample, the result by comparison is to calculate the content of micro-chlorine according to this inspection amount signal for this operation processing unit.
The detection method of x-ray fluorescence analysis provided by the invention comprises the following step: receive electric current from the outside to produce high-tension current; This high-tension current is controlled to be the operating voltage between 5 kilovolts to 15 kilovolts scope; Excited by the electric current of described operating voltage, penetrate an X ray; Filter emitted X ray with the noise between elimination 0.3 keV to 4 keV scope; The described sample of x-ray bombardment with after filtering makes this sample be subjected to disengage a fluorescence behind this excitation of X-rays; Receive described fluorescence to form an inspection amount signal; And according to described inspection amount signal comparing an inspection amount sample, the result by comparison is to calculate the content of micro-chlorine.
Therefore; pick-up unit and detection method by x-ray fluorescence analysis of the present invention; utilize the control of operating voltage and assisting of elimination particular range noise; can check out the micro-chlorine of trace as 100PPM; so that detect the environmental protection standard that the made product of thing meets European RoHS; not only expand business opportunity, and can accomplish environmental protection conscientiously.
Can be further understood by the following detailed description and accompanying drawings about the advantages and spirit of the present invention.
Description of drawings
Fig. 1 is the synoptic diagram of pick-up unit of the present invention;
Fig. 2 is the synoptic diagram of energy spectral intensity (CPS) figure among the present invention;
Fig. 3 is the synoptic diagram of the present invention energy spectral intensity-cl concn graph of a relation RD and inspection amount line sample SL;
Fig. 4 is the control group synoptic diagram of reactive filter;
Fig. 5 is the control group synoptic diagram of carrying out with the 30KV operating voltage;
Fig. 6 is the process flow diagram of detection method of the present invention; And
Fig. 7 makes the process flow diagram of inspection amount line sample SL for the present invention.
Drawing reference numeral:
Pick-up unit 30 samples 32
High-pressure generator 40 voltage controllers 42
Light pipe 44 X ray 44L
Wave filter 46 aluminium sheets 4602
Detecting device 48 fluorescence 32L
Operation processing unit 49 inspection amount line sample SL
Can spectral intensity-cl concn graph of a relation RD
Embodiment
See also Fig. 1, Fig. 1 is the synoptic diagram of pick-up unit 30 of the present invention.The invention relates to the pick-up unit 30 that a kind of XRF 32L analyzes, in order to analyze the chlorine that is lower than the 1000PPM trace in the sample 32, even can detect as the chlorine of 100PPM trace, so that sample 32 made commodity can meet the environmental protection standard of European RoHS.Pick-up unit 30 further comprises a high-pressure generator 40, a voltage controller 42, a light pipe 44, a wave filter 46, a detecting device 48 and an operation processing unit 49.
High-pressure generator 40 receives the electric current from the outside, after transformation to produce high-tension current.The high-tension current that voltage controller 42 is given birth to high-pressure generator 40 is controlled to be 5 kilovolts (KV) to the operating voltage between 15 kilovolts scope.
Light pipe 44 is excited by the electric current of voltage controller 42 this operating voltage that produces, and penetrates an X ray 44L.After testing, find, this voltage controller 42 suitable operating voltage range of controlling, approximately be 2 to 3 times of chlorine element electron-volt, the electron-volt of chlorine element is 2.62 keVs (kev), the operating voltage range of being controlled when voltage controller 42 at 5 kilovolts (KV) to 15 kilovolts, follow-uply get desirable energy spectral intensity (CPS) figure,, can obtain better energy spectral intensity (CPS) figure if operating voltage range is contracted to 5.24 kilovolts (KV) between 7.86 kilovolts scope.
Wave filter 46 is arranged on the optical path of X ray 44L, filter the emitted X ray 44L of light pipe 44 with elimination 0.3 keV (kev) to the noise between 4 keV scopes, and the X ray 44L after will filtering irradiation sample 32, disengage a fluorescence 32L after making sample 32 excited by X ray 44L.Comprise an aluminium sheet 4602 in the wave filter 46, light pipe 44 emitted X ray 44L pass aluminium sheet 4602 with the elimination noise, and it is good between between the scope of 0.09mm to 0.11mm that the thickness of aluminium sheet 4602 needs.
Detecting device 48 receives fluorescence 32L, and detected energy intensity is to form an inspection amount signal.Wherein, this inspection amount signal be can spectral intensity (CPS) with electron-volt related.
High-pressure generator 40 or be called high pressure generator, circuit for producing high voltage or be called high-voltage pulse circuit (High Voltage Pulser Circuits), be all existing part at present with voltage controller (voltage controller) 42, light pipe (X-RayTube) and detecting device (fluorescence detector) 48, be used in auxiliary enforcement technical characterictic of the present invention among the present invention, finish purpose of the present invention and effect, the principle of satisfying indivedual existing elements repeats no more in this.Because the present invention goes out the usefulness that had not had by described existing elements combination, to solve existing problem, so the present invention possesses progressive really.
Cooperate Fig. 1 to see also Fig. 2, Fig. 2 is the synoptic diagram of energy spectral intensity (CPS) figure among the present invention.Use 15 kilovolts the operating voltage and the wave filter 46 of 0.1mm thickness aluminium sheet, produce the associated diagram of energy spectral intensity-electron-volt, the power spectrum intensity crest that can see the 2.62kev part among the figure is obvious, and this is the energy spectral intensity of chlorine.
Operation processing unit (processor) the 49th, comparing an inspection amount sample, the result by comparison is to calculate the content of micro-chlorine according to this inspection amount signal.Wherein, the content of described micro-chlorine is the concentration of chlorine, generally is to represent with per mille concentration (PPM).
Further see also Fig. 3, Fig. 3 is the synoptic diagram of the present invention energy spectral intensity-cl concn graph of a relation RD and inspection amount line sample SL.Described inspection amount sample is an inspection amount line sample SL, and inspection amount line sample SL is the linear relationship of this energy spectral intensity and this concentration unit.Wherein, the making of inspection amount line sample SL, the standard model of the known and variable concentrations of at least two parts of samplings earlier, in the legend two duplicate samples of 1200PPM and 2500PPM, after the energy spectral intensity of measuring chlorine (2.62kev place) respectively is 400CPS and 1000CPS, relation with its energy spectral intensity-cl concn in energy spectral intensity-cl concn graph of a relation RD indicates two position A, B (representing this two parts of known standard samples), and inspection amount line sample SL is made in two position A, B extension according to this again.
Follow-up, at the measured energy spectral intensity of sample 32, can converse due concentration unit by self check amount line sample SL.The using method of Fig. 3 is described with Fig. 2 example, when the energy spectral intensity of micro-chlorine such as Fig. 2 are measured as 34CPS, in Fig. 3 the sample 32 of 34CPS being inserted inspection amount line sample SL with interpolation method converts, the cl concn of derived sample 32 is 407PPM, by this, can measure the existence that converses micro-chlorine in the sample 32, particularly at chlorine micro-below the 1000PPM.With method of the present invention even can record chlorine as 100PPM easily, the following commodity that make with this sample 32 are just can meet the environmental protection standard of European RoHS.
At Fig. 2, please further consult Fig. 4 and Fig. 5, Fig. 4 is the control group synoptic diagram of reactive filter 46.Fig. 5 is the control group synoptic diagram of carrying out with the 30KV operating voltage.As seen from Figure 4, also have many noise crests in the scope of 2.62kev to 3kev, compare the signal of Fig. 2 of the present invention, Fig. 4 changes digitizing for waveform and judges, or directly judges with naked eyes, all is easy to generate erroneous judgement.As seen from Figure 5, with operating voltage up to 30KV, near chlorine 2.62kev, acomia at all evoke tangible can spectral intensity (CPS), compare the signal of Fig. 2 of the present invention, Fig. 5 can't measure running at all.So, suffice to show that the effect that Fig. 2 the technology of the present invention feature is shown, really improve problem in the past and have obvious progressive.
See also Fig. 6, Fig. 6 is the process flow diagram of detection method of the present invention.The present invention also is the detection method that a kind of XRF 32L analyzes, in order to analyze the chlorine of trace in the sample 32.This detection method comprises the following step:
Step S02: receive electric current from the outside to produce high-tension current.
Step S04: this high-tension current is controlled to be 5 kilovolts (KV) to the operating voltage between 15 kilovolts scope.Further, particularly with 5.24 kilovolts (KV) to better between 7.86 kilovolts scope.
Step S06: excited by the electric current of this operating voltage, light pipe 44 penetrates an X ray 44L.
Step S08: filter emitted X ray 44L with elimination 0.3 keV (kev) to the noise between 4 keV scopes.Wherein, emitted X ray 44L passes an aluminium sheet 4602 with the elimination noise, and the thickness of aluminium sheet 4602 is between the scope of 0.09mm to 0.11mm.
Step S10: X ray 44L after will filtering irradiation sample 32, disengage a fluorescence 32L after making sample 32 excited by X ray 44L.
Step S12: receiving fluorescence 32L to form an inspection amount signal, should inspection amount signal be an energy spectral intensity (CPS) wherein.
Step S14: comparing an inspection amount sample, the result by comparison is to calculate the content of micro-chlorine according to this inspection amount signal, and the content of wherein said micro-chlorine is the concentration of chlorine, and available PPM represents.This inspection amount sample is an inspection amount line sample SL, and inspection amount line sample SL is the linear relationship of this energy spectral intensity and cl concn.
Further see also Fig. 7, Fig. 7 makes the process flow diagram of inspection amount line sample SL for the present invention.Fig. 7 makes inspection amount line sample SL and comprises the following step:
Step S20: the standard model of at least two parts of known and variable concentrations of taking a sample, measure can spectral intensity to make the position of two standard models in can spectral intensity-cl concn graph of a relation RD.
Step S22: in graph of a relation RD, utilize these at least two parts of standard models to extend and make inspection amount line sample SL.
Step S24: follow-up basis is by the measured energy spectral intensity of sample 32, can self check amount line sample SL, converse the due concentration of micro-chlorine with interpolation method.
Therefore; pick-up unit 30 and detection method by XRF 32L analysis of the present invention; utilize the control of operating voltage and assisting of elimination particular range noise; can check out the micro-chlorine of trace as 100ppm; so that detect the environmental protection standard that the made product of thing meets European RoHS; not only expand business opportunity, and can accomplish environmental protection conscientiously.
By the above detailed description of preferred embodiments, be to wish to know more to describe feature of the present invention and spirit, and be not to come category of the present invention is limited with the above-mentioned preferred embodiment that is disclosed.On the contrary, its objective is that hope can contain in the category of claim of being arranged in of various changes and tool equality institute of the present invention desire application.
Claims (12)
1. the pick-up unit of an x-ray fluorescence analysis in order to analyze the chlorine of trace in the sample, is characterized in that this pick-up unit further comprises:
One high-pressure generator receives electric current from the outside to produce high-tension current;
One voltage controller with the high-tension current that described high-pressure generator is given birth to, is controlled to be the operating voltage between 5 kilovolts to 15 kilovolts scope;
One light pipe is excited by the electric current of the operating voltage that described voltage controller produces, and penetrates an X ray;
One wave filter filters the emitted X ray of described light pipe with the noise between elimination 0.3 keV to 4 keV scope, and the described sample of the x-ray bombardment after will filtering, and makes this sample be subjected to disengage a fluorescence behind the described excitation of X-rays;
One detecting device receives described fluorescence, to form an inspection amount signal; And
One operation processing unit, comparing an inspection amount sample, the result by comparison is to calculate the content of micro-chlorine according to described inspection amount signal.
2. pick-up unit as claimed in claim 1 is characterized in that, described inspection amount signal is an energy spectral intensity.
3. pick-up unit as claimed in claim 2 is characterized in that, the content of described micro-chlorine is the concentration of chlorine.
4. pick-up unit as claimed in claim 3 is characterized in that, described inspection amount sample is an inspection amount line sample, and this inspection amount line sample is the linear relationship of described energy spectral intensity and described concentration.
5. pick-up unit as claimed in claim 4, it is characterized in that the standard model of the known and variable concentrations of two parts of described inspection amount line sample samplings is made described inspection amount line sample, follow-up according to measured energy spectral intensity, can converse due concentration from described inspection amount line sample.
6. pick-up unit as claimed in claim 1 is characterized in that, comprises an aluminium sheet in the described wave filter, and the emitted X ray of described light pipe passes described aluminium sheet with the elimination noise, and the thickness of this aluminium sheet is between the scope of 0.09mm to 0.11mm.
7. the detection method of an x-ray fluorescence analysis in order to analyze the chlorine of trace in the sample, is characterized in that this detection method comprises the following step:
Reception from the electric current of outside to produce high-tension current;
This high-tension current is controlled to be the operating voltage between 5 kilovolts to 15 kilovolts scope;
Excited by the electric current of described operating voltage, penetrate an X ray;
Filter emitted X ray with the noise between elimination 0.3 keV to 4 keV scope;
The described sample of x-ray bombardment with after filtering makes this sample be subjected to disengage a fluorescence behind this excitation of X-rays;
Receive described fluorescence to form an inspection amount signal; And
Comparing an inspection amount sample, the result by comparison is to calculate the content of micro-chlorine according to described inspection amount signal.
8. detection method as claimed in claim 7 is characterized in that, described inspection amount signal is an energy spectral intensity.
9. detection method as claimed in claim 8 is characterized in that, the content of described micro-chlorine is the concentration of chlorine.
10. detection method as claimed in claim 9 is characterized in that, described inspection amount sample is an inspection amount line sample, and described inspection amount line sample is the linear relationship of described energy spectral intensity and concentration.
11. detection method as claimed in claim 10, it is characterized in that, described detection method further comprises the following step, the take a sample standard model of two parts of known and variable concentrations, make described inspection amount line sample, follow-up according to measured energy spectral intensity, can converse due concentration from described inspection amount line sample.
12. detection method as claimed in claim 7 is characterized in that, emitted X ray passes an aluminium sheet with the elimination noise, and the thickness of described aluminium sheet is between the scope of 0.09mm to 0.11mm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2007101942077A CN101196482B (en) | 2007-12-12 | 2007-12-12 | Testing apparatus and method for X-ray fluorescence analysis |
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| CN2007101942077A CN101196482B (en) | 2007-12-12 | 2007-12-12 | Testing apparatus and method for X-ray fluorescence analysis |
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| CN101196482B true CN101196482B (en) | 2010-06-23 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106442593A (en) * | 2016-11-10 | 2017-02-22 | 中铝广西国盛稀土开发有限公司 | Rare earth product quality online monitoring instrument |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109613036A (en) * | 2015-12-01 | 2019-04-12 | 中国计量科学研究院 | For the filter disc of XRF element determination, filter disc preparation method, determination box, element determination method |
| CN109030528A (en) * | 2018-09-26 | 2018-12-18 | 云南驰宏锌锗股份有限公司 | A kind of method that X-ray fluorescence spectra analyzes fluorine chlorine in smelting smoke dust |
| CN112198182B (en) * | 2020-10-10 | 2023-07-14 | 中国兵器工业第五九研究所 | Device and method for detecting chloride ion content in atmospheric environment |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86208769U (en) * | 1986-10-30 | 1988-02-10 | 成都地质学院 | Filter for locating goldmine in portable x-ray fluorometer |
| CN1624463A (en) * | 2003-09-04 | 2005-06-08 | 精工电子纳米科技有限公司 | X-ray analyzer for analyzing plastics |
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- 2007-12-12 CN CN2007101942077A patent/CN101196482B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86208769U (en) * | 1986-10-30 | 1988-02-10 | 成都地质学院 | Filter for locating goldmine in portable x-ray fluorometer |
| CN1624463A (en) * | 2003-09-04 | 2005-06-08 | 精工电子纳米科技有限公司 | X-ray analyzer for analyzing plastics |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106442593A (en) * | 2016-11-10 | 2017-02-22 | 中铝广西国盛稀土开发有限公司 | Rare earth product quality online monitoring instrument |
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