CN203275323U - X-ray fluorescence analyser - Google Patents
X-ray fluorescence analyser Download PDFInfo
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- CN203275323U CN203275323U CN 201320220323 CN201320220323U CN203275323U CN 203275323 U CN203275323 U CN 203275323U CN 201320220323 CN201320220323 CN 201320220323 CN 201320220323 U CN201320220323 U CN 201320220323U CN 203275323 U CN203275323 U CN 203275323U
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Abstract
The utility model discloses an X-ray fluorescence analyser which comprises an excitation light source device, a signal detecting device, a signal processing device, a computer and a sample testing device, wherein the signal detecting device is internally provided with a detector; the signal processing device is internally provided with an amplifier connected with the detector and an analog-to-digital converter connected with the amplifier; a latest DP5SI-PIN electrical refrigeration detector is adopted as the detector; the excitation light source device is internally provided with a low-power X-ray generator; the detector is positioned on a position of the best reflection angle for activating rays by the low-power X-ray generator; a ray filter selecting device and a collimator selecting device are also arranged in front of the X-ray generator; and in order to conveniently observe the shapes and positions of samples, the X-ray fluorescence analyser is also provided with a high-resolution camera. The X-ray fluorescence analyser disclosed by the utility model has the advantages of simpleness in operation, convenience in use, high precision, good stability, low failure rate and the like.
Description
Technical field
The utility model relates to a kind of analytical instrument, relates in particular to a kind of easy to use, failure rate is low, precision is high, Repeatability good and reliable and stable 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 the Quick material constituent analysis, the existing sample analysis that has been widely used in industry-by-industry the sixties, to the latter stage seventies, the First X-ray Fluorescence Analyzer is by U.S.'s Lorenz laboratory development success, the eighties, the energy dispersive instrument began to use, China also begins development, Chinese First energy dispersion type xrf analysis instrument was succeeded in developing by 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 to could be worked under the cooled with liquid nitrogen state, daily servicing is cumbersome, all will add weekly liquid nitrogen could work.
For this reason, along with the development of detector technology, after 2005, X-ray Fluorescence Analyzer has just entered high-speed development period.At present, the X-ray Fluorescence Analyzer that uses, 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 connect respectively, this excitation source is arranged on the position near the test sample device, and signal detecting device connects signal processing apparatus, and putting sampling device is be used to depositing sample.This X-ray Fluorescence Analyzer on-link mode (OLM) is directly to carry out the mode of multiple tracks data acquisition by fixed interface by computing machine, and this mode connects complexity, failure rate is high, operation inconvenience.In addition, be not provided with filter selection device before x ray generator, thereby the background of sample to be tested is higher, has reduced sensitivity and the detection limit of analytical element, affected the degree of accuracy of sample measurement result.
The utility model content
For the problems referred to above, fundamental purpose of the present utility model is to provide a kind of easy to use, failure rate is low, precision is high, Repeatability good and reliable and stable xrf analysis instrument, has improved sensitivity and the detection limit of analytical element.
The utility model solves above-mentioned technical matters by following technical proposals: a kind of xrf analysis instrument, and described xrf analysis instrument comprises excitation light source device, signal detecting device, signal processing apparatus and computing machine and puts sampling device; Be provided with detector in described signal detecting device, be provided with the amplifier that is connected with detector and the analog to digital converter that is connected with amplifier in described signal processing apparatus; Described xrf analysis instrument also comprises the sample position finder; Be provided with low power X-ray generator in 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 and collimating apparatus selecting arrangement before described x ray generator.
In specific embodiment of the utility model: described sample position finder is camera, and described camera is arranged on the bottom of measuring sample.
In specific embodiment of the utility model: described signal processing apparatus also is provided with and is connected with analog to digital converter and obtains the single-chip microcomputer of multiple tracks data.
In specific embodiment of the utility model: described computing machine is provided with USB, RS232 serial ports, three kinds of interface modes of ethernet communication, described single-chip microcomputer by USB interface, RS232 serial ports, ethernet communication the multiple tracks data transmission of obtaining to computing machine.
In specific embodiment of the utility model: the high pressure of described x ray generator is 50 kilovolts.
In specific embodiment of the utility model: also be connected with output device on described computing machine.
In specific embodiment of the utility model: described output device includes display and printer.
In specific embodiment of the utility model: described detector is electric refrigeration detector, and USB, RS232 serial ports and ethernet interface are installed on described detector.
Positive progressive effect of the present utility model is: the xrf analysis instrument that the utility model provides has following advantage:
1, the utility model has adopted the high resolving power DP5SI-PIN electricity refrigeration detector with imported with original packaging international state-of-the-art U.S. of new generation imported with original packaging, this detector need not protection of liquid nitrogen, can be applied to easily each local every field, and have more high count rate, a high resolving power more, minimumly can reach 145eV, make general sample in 200 seconds, can obtain satisfied result; But this detector has all choice for uses of USB, RS232 serial ports, three kinds of modes of ethernet interface, and antijamming capability strengthens.
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, precision is high, reliable and stable, and increased filter selection device before x ray generator, and can reduce the background of element to be measured, improve sensitivity and the detection limit of analytical element; Increased the collimating apparatus selecting arrangement before x ray generator, can select suitable collimating apparatus and shooting conditions for the sample of different industries, made the adaptability of instrument broader.
But 3, in the utility model analytical element periodic table by sodium (Na) to the whole elements uranium (U); Can detect Gu Ti ﹑ Ye Ti ﹑ powder, not need complicated sample making course.
4, the utility model has adopted advanced vacuum automatic control and digital vacuum detecting to show, automaticity is high; Advanced instrument drift is revised automatically, guarantees that instrument is steady in a long-term; Have simple to operate, easy to use, degree of accuracy is high, good stability, the advantage of failure rate is low; Can be widely used in the industries such as the 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 schematic diagram that excites of the present utility model.
Fig. 3 is the contrast spectrogram after loading optical filter of the present utility model.
Fig. 4 is three kinds of communication modes selection figure of detector of the present utility model.
Embodiment
Provide the utility model preferred embodiment below in conjunction with accompanying drawing, to describe the technical solution of the utility model in detail.
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, sample finder; This signal detecting device is provided with detector 5, is provided with the amplifier that is connected with detector 5 and the analog to digital converter that is connected with amplifier in signal processing apparatus; Wherein, this detector 5 be the development of U.S. AMPTEK company recent development have a high DP5SI-PIN electricity refrigeration detector of resolution, need (40 ℃) work at low temperatures, low temperature need to be provided by the semiconductor refrigerating mode.This electricity refrigeration detector need not cooled with liquid nitrogen, Be(beryllium window) thickness is 7.5 microns, and is right
55The resolution of the X ray of Fe5.9keV when counting rate is 1000CPS is 145eV.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, high-voltage power supply, wherein, with the low-power positive high voltage x ray generator of high pressure 50KV as excitaton source, this x ray generator 2 adopts Be(berylliums) window thickness is that the bremstrahlen Xing ﹑ Di Gong of 125 microns is Shuaied the X-ray tube of the right Leng Que of ﹑ Zi ﹑ high life, and select target according to the practical application needs, as selective target be: Rh(rhodium target), Ag(silver target), the Mo(molybdenum target), Ti(titanium target) etc.In the utility model, increase filter selection device 3 before x ray generator 2, for reducing the background of element to be measured, improved 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 to adapt to different analysis requirements; Increased collimating apparatus selecting arrangement 4 before x ray generator, can be for the sample of different industries, select suitable collimating apparatus 4 and shooting conditions, make the adaptability of instrument broader, the initial X-ray that produces from x ray generator 2 by optical filter and collimating apparatus after direct excited sample 1, more can obtain best analysis result by the selective excitation condition.
In the present embodiment, as shown in Figure 3, wherein in figure, dotted line is spectrogram when not adding optical filter, solid line is the spectrogram that adds after the Ti optical filter, by relatively, the utility model adds that the background of spectrogram has reduced after optical filter, and the sensitivity of measuring the elements such as Hg, Pb, Br has improved.
Fig. 4 is three kinds of communication modes selection figure of detector of the present utility model.As shown in Figure 4: USB, RS232 serial ports and ethernet interface are installed on detector 5.
On the other hand, in the utility model, this digital controller connects computing machine, also is connected with on computers output device, 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 with analog to digital converter and can obtains the multiple tracks data 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, X-ray tube 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 software digital control and demonstration automatically, and 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 5 is on the position of best reflection angle of low power X-ray generator 2 excitation rays, is convenient to the ray that detector 5 is accepted reflection.Put sampling device and be provided with the sample chamber of samples such as can holding various forms such as Gu Ti ﹑ Ye Ti ﹑ Fen Mo ﹑ coating, for the ease of observing shape and the position of sample, apparatus installation has high-resolution camera 6.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 empty gas ﹑ vacuum, can automatically be controlled by software, need not manually-operated.
during the utility model work, after measuring sample 1 compressing tablet shaping, place and measure sample 1 in the measuring position, x ray generator 2 sends X ray and excites after mating plate 3 and collimating apparatus 4 after filtration and measure sample 1, make the extranulear electron (particularly K electron) in the atom of measuring each element in sample 1 be stimulated and emit, 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, 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 data acquisition and controlling of data by control interface.Xrf analysis software can obtain result qualitatively by the analysis to various characteristic X-ray energy, know namely also which kind of element sample contains, again by the intensity of characteristic X-ray is calculated and is analyzed, finally complete analysis and the printing of each constituent content in sample, thereby realize the quality control of production.
The utility model is suitable for the industries such as iron and steel, geology, mine, cement to be used.The below is that the utility model is to the on-the-spot actual analysis result of 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, sometimes also analyzes other impurity contents such as P, Fe2O3, SiO2.Measuring condition: 15kv200uA150 vacuum second free of light filter
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/120uA100s is without 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 easily measured on 6000.
Measuring condition: 15kv200uA150s vacuum Ti optical filter
Actual navajoite sample analysis result such as table 3:
Table 3
4, iron ore sample analysis
General ironstone sample adopts the fuse piece mode to measure, and it can eliminate different mines different minerals structure to the impact of iron content, and analysis precision is high.But the method preparation of samples time is long, and step is more loaded down with trivial details, therefore also can adopt the compressing tablet mode to carry out Fast Measurement 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: 12kv300uA200s vacuum
Actual sample analysis result such as table 4:
Table 4
5, phosphorus ore sample analysis
Phosphorus ore is the primary raw material of producing phosphate fertilizer, utilizes the 6000x fluorescence analyser to be easy to measure.
Measuring condition: 10kv400uA150s 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, easily carries out express-analysis at the 6000x fluorescence analyser.
Measuring condition: 12kv300uA150s vacuum
Actual sample analysis result such as table 6:
Table 6
7, silicate sample
The silicate sample comprises: the samples such as clay, shale, feldspar, quartz, sandstone, and of many uses.
Measuring condition: 15kv400uA200s vacuum
Actual silicate measurement sample result such as table 7:
Table 7
By on-the-spot actual analysis result verification, the utlity model has that analysis speed is fast, easy to use, precision is high, cost is low, failure rate is low, the short advantage of Measuring Time, but in the analytical element periodic table by sodium (Na) to the whole elements uranium (U), can reach the purpose of expection fully.During analytic sample, generally as long as 100-200 can provide the content of each element second, and can detect the sample such as Gu Ti ﹑ Ye Ti ﹑ powder, not need complicated sample making course, be the desirable analytical instrument of the industry express-analysis such as nonferrous mine, geology.Thereby, the utility model can be widely used in the industries such as the 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.
Above demonstration 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 above-described embodiment and 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; these changes and improvements all fall in claimed the utility model scope, and the claimed scope of the utility model is defined by appending claims and equivalent thereof.
Claims (8)
1. xrf analysis instrument, described xrf analysis instrument comprises excitation light source device, signal detecting device, signal processing apparatus and computing machine and puts sampling device; Be provided with detector in described signal detecting device, be provided with the amplifier that is connected with detector and the analog to digital converter that is connected with amplifier in described signal processing apparatus; It is characterized in that: described xrf analysis instrument also comprises the sample position finder; Be provided with low power X-ray generator in 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 and collimating apparatus selecting arrangement before described x ray generator.
2. xrf analysis instrument according to claim 1, it is characterized in that: described sample position finder is camera, described camera is arranged on the bottom of measuring sample.
3. xrf analysis instrument according to claim 1 is characterized in that: described signal processing apparatus also is provided with and is connected with analog to digital converter and obtains the single-chip microcomputer of multiple tracks data.
4. xrf analysis instrument according to claim 3, it is characterized in that: described computing machine is provided with USB, RS232 serial ports, three kinds of interface modes of ethernet communication, described single-chip microcomputer by USB interface, RS232 serial ports, ethernet communication the multiple tracks data transmission of obtaining to computing machine.
5. xrf analysis instrument according to claim 1, it is characterized in that: the high pressure of described x ray generator is 50 kilovolts.
6. xrf analysis instrument according to claim 1, is characterized in that: also be connected with output device on described computing machine.
7. xrf analysis instrument according to claim 6, it is characterized in that: described output device includes display and printer.
8. xrf analysis instrument according to claim 1, it is characterized in that: described detector is electric refrigeration detector, and USB, RS232 serial ports and ethernet interface are installed on described detector.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109374664A (en) * | 2018-12-07 | 2019-02-22 | 南京航空航天大学 | A kind of online xrf analysis method of automatic sampling type cement slurry |
| CN110530915A (en) * | 2019-10-14 | 2019-12-03 | 中钢集团马鞍山矿山研究院有限公司 | A kind of mine slurry grade measurement and analytical equipment for mineral processing production |
| RU2764394C1 (en) * | 2020-11-23 | 2022-01-17 | Акционерное общество "Иркутский научно-исследовательский институт благородных и редких металлов и алмазов" АО "Иргиредмет" | Method for x-ray radiometric enrichment of manganese ores |
| CN115763616A (en) * | 2023-01-06 | 2023-03-07 | 威海栖桐科技发展有限公司 | X-ray detector, and online ore composition analysis device and method |
-
2013
- 2013-04-26 CN CN 201320220323 patent/CN203275323U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109374664A (en) * | 2018-12-07 | 2019-02-22 | 南京航空航天大学 | A kind of online xrf analysis method of automatic sampling type cement slurry |
| CN110530915A (en) * | 2019-10-14 | 2019-12-03 | 中钢集团马鞍山矿山研究院有限公司 | A kind of mine slurry grade measurement and analytical equipment for mineral processing production |
| RU2764394C1 (en) * | 2020-11-23 | 2022-01-17 | Акционерное общество "Иркутский научно-исследовательский институт благородных и редких металлов и алмазов" АО "Иргиредмет" | Method for x-ray radiometric enrichment of manganese ores |
| CN115763616A (en) * | 2023-01-06 | 2023-03-07 | 威海栖桐科技发展有限公司 | X-ray detector, and online ore composition analysis device and method |
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Granted publication date: 20131106 Termination date: 20160426 |