CN201373857Y - X fluorescence analyser - Google Patents
X fluorescence analyser Download PDFInfo
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- CN201373857Y CN201373857Y CN200920068392U CN200920068392U CN201373857Y CN 201373857 Y CN201373857 Y CN 201373857Y CN 200920068392 U CN200920068392 U CN 200920068392U CN 200920068392 U CN200920068392 U CN 200920068392U CN 201373857 Y CN201373857 Y CN 201373857Y
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Abstract
The utility model discloses an X fluorescence analyser, which comprises a light source excitation device, a signal detector, a signal processor, a computer as well as a sample test device. A detector is arranged in the single detector; an amplifier connected with the detector as well as an analog-to-digital converter connected with the amplifier are arranged in the signal processor; an electronic refrigeration detector is adopted as the detector; a low power X ray generator is arranged in the light source excitation; the detector is arranged at the position of the best reflection angle of the excitation ray of the low power X ray generator and an optical filter selector is also arranged in front of the X ray generator. The X fluorescence analyser has the advantages of easy operation, convenient use, high precision, good stability, low failure rate, and the like.
Description
Technical field
The utility model relates to a kind of analytical instrument, particularly be a kind of energy dispersion type xrf analysis instrument.
Background technology
Xrf analysis historical long begins the wavelength dispersion X fluorescence analyser from eighties of last century and be used to quick material component analysis, the existing sample analysis that has been widely used in industry-by-industry the sixties; To the latter stage seventies, first energy dispersion xrf analysis instrument is by U.S.'s Lorenz laboratory development success, the eighties, the energy dispersive instrument began to use, China also begins development, succeed in developing to first energy dispersion type xrf analysis instrument of China in 1989, develop unhappy to xrf analysis instrument in 2000 always, main cause is that the critical component-detector of energy dispersion type xrf analysis instrument is to have adopted Si (Li) semiconductor detector, it need could be worked under the cooled with liquid nitrogen state, daily servicing is cumbersome, all will add liquid nitrogen weekly and could work.
For this reason, along with the development of detector technology, after 2005, energy dispersion xrf analysis instrument has just entered high-speed development period.At present, employed energy dispersion xrf analysis instrument, it comprises excitation light source device, signal detecting device, signal processing apparatus, computing machine and puts sampling device; Wherein, the computing machine that excitation light source device and signal processing apparatus are connected respectively, this excitation source are installed in the position near the test sample device, and signal detecting device connects signal processing apparatus, and putting sampling device is to be used to deposit sample.This energy dispersion xrf analysis instrument on-link mode (OLM) is directly to carry out the mode that the multiple tracks data are obtained by fixed interface by computing machine, and this mode connects complexity, failure rate height, operation inconvenience.In addition, be not provided with filter selection device before the x ray generator, thereby the background of sample to be tested is higher, has reduced the sensitivity and the detection limit of analytical element, influenced sample measurement result's degree of accuracy.
The utility model content
At the defective that exists in the prior art, the purpose of this utility model be to provide a kind of easy to use, failure rate is low, precision is high, repeat the good and reliable and stable xrf analysis instrument of performance, has improved the sensitivity and the detection limit of analytical element.
To achieve these goals, the utility model is to realize by the following technical solutions:
The xrf analysis instrument comprises excitation light source device, signal detecting device, signal processing apparatus, computing machine and puts sampling device; Be provided with detector in the described signal detecting device, be provided with amplifier that is connected with detector and the analog to digital converter that is connected with amplifier in the described signal processing apparatus; It is characterized in that, be provided with low power X-ray generator in the described excitation light source device, described detector is on the position of best reflection angle of low power X-ray generator excitation ray, also be provided with filter selection device before the described x ray generator, can reduce the background of element to be measured, improve the sensitivity and the detection limit of analytical element.
Described detector is a SI-PIN electricity refrigeration detector, and described electric refrigeration detector lowest resolution reaches 149eV, makes general sample in 200 seconds, can obtain satisfied result.
In order to reduce the complicacy of data-interface link, reduce failure rate, be provided with at described signal processing apparatus and be connected with analog to digital converter and obtain the single-chip microcomputer of multiple tracks data, described computing machine is provided with USB interface, and described single-chip microcomputer is given computing machine the multiple tracks data transmission of obtaining by USB interface.
According to described xrf analysis instrument, wherein, described excitation light source device also is provided with high-voltage power supply and digital controller, and described high-voltage power supply connects low power X-ray generator and digital controller, and described digital controller connects computing machine.
According to described xrf analysis instrument, wherein, the high pressure of described x ray generator is 50 kilovolts.
According to described xrf analysis instrument, wherein, also be connected with output device on the described computing machine.
According to described xrf analysis instrument, wherein, described output device includes display.
According to described xrf analysis instrument, wherein, described output device also comprises printer.
According to described xrf analysis instrument, wherein, the described sampling device of putting is provided with the sample chamber that can hold samples such as various forms such as solid, liquid, powder, coating.
Principle of work of the present utility model is as follows:
X ray generator sends the excitation of X-rays sample, extranulear electron in each atoms of elements in the sample (particularly K electron) is stimulated and emits, and in situ produce a hole, outer-shell electron this moment (particularly L layer electronics) will be filled this VOID POSITIONS, unnecessary energy is just emitted with the form of characteristic X-ray, these characteristic X-rays enter detector and produce pulse signal, send into the pulse spectroscope amplifier through prime amplifier, amplification and pulse shaping through the pulse spectroscope amplifier, send into analog to digital converter, analog to digital converter becomes digital quantity with analog signal conversion, send into computer interface, software is composed the collection and the control of data by control interface circuit.
The beneficial effects of the utility model are as follows:
1, the utility model has adopted the high resolving power SI-PIN electricity refrigeration detector with U.S.'s imported with original packaging of the international advanced person of imported with original packaging; this detector need not protection of liquid nitrogen; can be applied to each local every field easily; and have high count rate, a high resolving power; minimumly can reach 149eV; make general sample in 200 seconds, can obtain satisfied result.
2, x ray generator of the present utility model adopts positive high voltage to excite, excite with test condition and adopt the digital control of computer software and show, make its processing speed fast, the precision height, reliable and stable, and before x ray generator, increased filter selection device, and can reduce the background of element to be measured, improve the sensitivity and the detection limit of analytical element.
But 3, in the utility model analytical element periodic table by sodium (Na) to the whole elements the uranium (U); Can detect solid, liquid, powder, not need complicated sample making course.
4, the utility model has adopted advanced vacuum automatic control and digital vacuum detecting to show the automaticity height; Advanced instrument drift is revised automatically, guarantees the instrument long-term stability; Have simple to operate, easy to use, degree of accuracy is high, good stability, the advantage that failure rate is low; Can be widely used in industries such as nonferrous mines such as plumbous zinc ore, copper mine, nickel minerals, molybdenum ore, iron ore, bauxite and iron and steel, cement, fire resistive material, geology, petrochemical complex, also can be used for the measurement of various alloy samples, as stainless steel, aluminium alloy, ormolu, lead alloy etc.
Description of drawings
Fig. 1 is the theory diagram of the utility model xrf analysis instrument.
Fig. 2 is the detection synoptic diagram that excites of the present utility model.
Fig. 3 is the contrast spectrogram behind the loading optical filter of the present utility model.
Embodiment
For technological means, creation characteristic that the utility model is realized, reach purpose and effect is easy to understand, below in conjunction with embodiment, further set forth the utility model.
With reference to figure 1 and Fig. 2, xrf analysis instrument of the present utility model comprises excitation light source device, signal detecting device, signal processing apparatus, computing machine and puts sampling device; This signal detecting device is provided with detector 4, is provided with amplifier that is connected with detector 4 and the analog to digital converter that is connected with amplifier in signal processing apparatus; Wherein, this detector 4 be the up-to-date development of U.S. AMPTEK company have the high SI-PIN of a resolution electricity refrigeration detector, need (40 ℃) work at low temperatures, low temperature need be provided by the semiconductor refrigerating mode.This electricity refrigeration detector need not cooled with liquid nitrogen, and Be (beryllium window) thickness is 7.5 microns, and is right
55The resolution of the X ray of Fe 5.9keV when counting rate is 1000CPS is 149eV.And light element Na, Mg, Al, Si, S etc. are had high sensitivity and resolution, make general sample in 200 seconds, can obtain satisfied result.
In the utility model, excitation light source device includes low power X-ray generator 2 and the digital controller that connects on high-voltage power supply, the high-voltage power supply, wherein, with the low-power positive high voltage x ray generator of high pressure 50KV as excitaton source, these x ray generator 2 employing Be (beryllium) window thickness are 125 microns bremstrahlen type, low-power, natural cooling, the X-ray pipe of high life, and according to practical application needs selection target, as selective target be: Rh (rhodium target), Ag (silver-colored target), Mo (molybdenum target), Ti (titanium target) etc.In the utility model, before x ray generator 2, increase filter selection device 3, be used to reduce the background of element to be measured, improved the sensitivity and the detection limit of analytical element.This filter selection device 3 adopts suitable optical filter, can improve the sensitivity for analysis of element-specific, makes the analysis lower limit reach the PPM level.The utility model can be equipped with 4 optical filters adapting to different analysis requirements, and the elementary X ray that produces from x ray generator 2 more can obtain best analysis result by direct excited sample 1 behind the optical filter by the selective excitation condition.
In the present embodiment, as shown in Figure 3, wherein dotted line is a spectrogram when not adding optical filter among the figure, solid line is the spectrogram that adds behind the Ti optical filter, by relatively, the utility model adds that the background of spectrogram has reduced behind the optical filter, and the sensitivity of measuring elements such as Hg, Pb, Br has improved.
On the other hand, in the utility model, this digital controller connects computing machine, also is connected with output device on computers, and this output device includes display and typewriter.In order to reduce the complicacy of data-interface link, reduce failure rate, be provided with the single-chip microcomputer that is connected and can obtains the multiple tracks data with analog to digital converter at signal processing apparatus, described computing machine is provided with USB interface, this single-chip microcomputer is transferred to computing machine to the analysis result that obtains the multiple tracks data by USB interface and shows and add up, and also can print on mini-printer.
In the utility model, the X-ray pipe adopts positive high voltage to excite, and excites with test condition to adopt the digital control of computer software and show.In excitation light source device, the voltage of high-voltage power supply and electric current adopt the digital automatically control of software and show that the X ray degree of stability: 0.3%/8 hour, voltage range: 0V to 50kV was adjustable continuously, and range of current: 0mA to 1mA is adjustable continuously.
In addition, in this enforcement, excitation apparatus adopts unique inversion right angle optical texture design (as shown in Figure 2), and described detector 4 is on the position of best reflection angle of low power X-ray generator 2 excitation rays, is convenient to the ray that detector 4 is accepted reflection.Put sampling device and be provided with the sample chamber that can hold samples such as various forms such as solid, liquid, powder, coating.Also be provided with in the sample chamber and can place the sample tray that diameter reaches the large sample of 200mm, the environment of sample chamber can be selected air, vacuum, can need not manually-operated by software controlled.
During the utility model work, after measuring samples 1 compressing tablet is shaped, place measuring samples 1 in the measuring position, x ray generator 2 send X ray after filtration mating plate 3 excite measuring samples 1, extranulear electron in each atoms of elements in the measuring samples 1 (particularly K electron) is stimulated and emits, and in situ produce a hole, outer-shell electron this moment (particularly L layer electronics) will be filled this VOID POSITIONS, unnecessary energy is just emitted with the form of characteristic X-ray, these characteristic X-rays enter detector 4 and produce pulse signal, send into the pulse spectroscope amplifier through prime amplifier, through the amplification and the pulse shaping of pulse spectroscope amplifier, send into analog to digital converter, analog to digital converter becomes digital quantity with analog signal conversion, send into computer interface, software is composed the collection and the control of data by control interface circuit.Xrf analysis software can obtain result qualitatively by the analysis to various characteristic X-ray energy, know promptly also which kind of element sample contains, again by the intensity of characteristic X-ray is calculated and is analyzed, finally finish the analysis and the printing of each constituent content in the sample, thereby realize the quality control of production.
The utility model is suitable for industries such as iron and steel, geology, mine, cement to be used.Be the on-the-spot actual analysis result of the utility model below to various geological and mineral samples.
1, manganese ore sample measurement
Manganese ore is the higher mineral of economic worth, generally will analyze main content manganese, also analyzes other impurity contents such as P, Fe2O3, SiO2 sometimes.Measuring condition: 150 seconds vacuum free of light filter of 15kv 200uA
Actual manganese ore sample analysis result is to such as table 1:
Table 1
2, copper mine sample measurement
Coloured samples such as copper-lead zinc also can carry out express-analysis on 6000 type instruments,
Measuring condition: 20kv/120uA 100s does not have vacuum Fe optical filter
On-the-spot actual sample is measured comparing result such as table 2:
Table 2
3, navajoite sample analysis
Vanadium metal is used very extensive at steel industry, the navajoite sample is also measured on 6000 easily.
Measuring condition: 15kv 200uA 150s vacuum Ti optical filter
Actual navajoite sample analysis result such as table 3:
Table 3
4, iron ore sample analysis
General iron ore sample adopts the fuse piece mode to measure, and it can eliminate the influence of different mines different minerals structure to iron content, analysis precision height.But this method sample setup time is long, and step is more loaded down with trivial details, therefore also can adopt the compressing tablet mode carry out fast measuring to the situation that requires not to be very high.Following is exactly the analysis result that adopts the direct tablet compressing mode.
Measuring condition: 12kv 300uA 200s vacuum
Actual sample analysis result such as table 4:
Table 4
5, phosphorus ore sample analysis
Phosphorus ore is a primary raw material of producing phosphate fertilizer, utilizes the 6000x fluorescence analyser to be easy to measure.
Measuring condition: 10kv 400uA 150s vacuum
Actual sample analysis result such as table 5:
Table 5
6, the sulphur ore deposit is analyzed
The sulphur ore deposit mainly exists with the troilite form, and sulfur content is higher, carries out express-analysis at the 6000x fluorescence analyser easily.
Measuring condition: 12kv 300uA 150s vacuum
Actual sample analysis result such as table 6:
Table 6
7, silicate sample
The silicate sample comprises: samples such as clay, shale, feldspar, quartz, sandstone, and of many uses.
Measuring condition: 15kv 400uA 200s vacuum
Actual silicon hydrochlorate measuring samples result such as table 7:
Table 7
By on-the-spot actual analysis result verification, the utlity model has the advantage that analysis speed is fast, easy to use, precision is high, cost is low, failure rate is low, Measuring Time is short, but in the analytical element periodic table by sodium (Na) to the whole elements the uranium (U), can reach its intended purposes fully.During analytic sample, generally as long as 100-200 can provide the content of each element second, and can detect samples such as solid, liquid, powder, not need complicated sample making course, be the desirable analytical instrument of industry express-analysis such as nonferrous mine, geology.Thereby, the utility model can be widely used in industries such as nonferrous mines such as plumbous zinc ore, copper mine, nickel minerals, molybdenum ore, iron ore, bauxite and iron and steel, cement, fire resistive material, geology, petrochemical complex, also can be used for the measurement of various alloy samples, as stainless steel, aluminium alloy, ormolu, lead alloy etc.
More than show and described ultimate principle of the present utility model and principal character and advantage of the present utility model.The technician of the industry should understand; the utility model is not restricted to the described embodiments; that describes in the foregoing description and the instructions just illustrates principle of the present utility model; under the prerequisite that does not break away from the utility model spirit and scope; the utility model also has various changes and modifications, and these changes and improvements all fall in claimed the utility model scope.The claimed scope of the utility model is defined by appending claims and equivalent thereof.
Claims (8)
1, xrf analysis instrument comprises excitation light source device, signal detecting device, signal processing apparatus, computing machine and puts sampling device; Be provided with detector in the described signal detecting device, be provided with amplifier that is connected with detector and the analog to digital converter that is connected with amplifier in the described signal processing apparatus;
It is characterized in that, be provided with low power X-ray generator in the described excitation light source device, described detector is on the position of best reflection angle of low power X-ray generator excitation ray, is provided with filter selection device before the described x ray generator.
2, xrf analysis instrument according to claim 1 is characterized in that, also is provided with at described signal processing apparatus to be connected with analog to digital converter and to obtain the single-chip microcomputer of multiple tracks data.
3, xrf analysis instrument according to claim 2 is characterized in that, described computing machine is provided with USB interface, and described single-chip microcomputer is given computing machine the multiple tracks data transmission of obtaining by USB interface.
4, xrf analysis instrument according to claim 1 is characterized in that, the high pressure of described x ray generator is 50 kilovolts.
5, xrf analysis instrument according to claim 1 is characterized in that, also is connected with output device on the described computing machine.
6, xrf analysis instrument according to claim 5 is characterized in that, described output device includes display.
7, xrf analysis instrument according to claim 5 is characterized in that, described output device also comprises printer.
8, xrf analysis instrument according to claim 1 is characterized in that, described detector is electric refrigeration detector.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200920068392U CN201373857Y (en) | 2009-03-04 | 2009-03-04 | X fluorescence analyser |
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| Application Number | Priority Date | Filing Date | Title |
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| CN200920068392U CN201373857Y (en) | 2009-03-04 | 2009-03-04 | X fluorescence analyser |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106908464A (en) * | 2017-03-01 | 2017-06-30 | 四川新先达测控技术有限公司 | Colliery analysis system and method |
| CN109540948A (en) * | 2018-10-29 | 2019-03-29 | 钢研纳克检测技术股份有限公司 | Quickly illuminated X-ray energy spectrum analyzer and analysis method on measurement trace light element |
| CN109668920A (en) * | 2019-02-18 | 2019-04-23 | 上海精谱科技有限公司 | A kind of detection method of upper liquid level radiation modality xrf analysis technology fluid sample elemental analysis |
| CN109738472A (en) * | 2019-02-27 | 2019-05-10 | 上海精谱科技有限公司 | A kind of method that x-ray fluorescence measures light element in silica sol liquid |
-
2009
- 2009-03-04 CN CN200920068392U patent/CN201373857Y/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106908464A (en) * | 2017-03-01 | 2017-06-30 | 四川新先达测控技术有限公司 | Colliery analysis system and method |
| CN109540948A (en) * | 2018-10-29 | 2019-03-29 | 钢研纳克检测技术股份有限公司 | Quickly illuminated X-ray energy spectrum analyzer and analysis method on measurement trace light element |
| CN109668920A (en) * | 2019-02-18 | 2019-04-23 | 上海精谱科技有限公司 | A kind of detection method of upper liquid level radiation modality xrf analysis technology fluid sample elemental analysis |
| CN109668920B (en) * | 2019-02-18 | 2022-03-11 | 上海精谱科技有限公司 | Detection method for liquid sample element analysis by upper liquid surface irradiation mode X fluorescence analysis technology |
| CN109738472A (en) * | 2019-02-27 | 2019-05-10 | 上海精谱科技有限公司 | A kind of method that x-ray fluorescence measures light element in silica sol liquid |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20091230 Termination date: 20120304 |