CN101813646A - Method and device for correcting instrument drift during X-ray fluorescence quantitative detection - Google Patents

Method and device for correcting instrument drift during X-ray fluorescence quantitative detection Download PDF

Info

Publication number
CN101813646A
CN101813646A CN 201019114089 CN201019114089A CN101813646A CN 101813646 A CN101813646 A CN 101813646A CN 201019114089 CN201019114089 CN 201019114089 CN 201019114089 A CN201019114089 A CN 201019114089A CN 101813646 A CN101813646 A CN 101813646A
Authority
CN
China
Prior art keywords
sample
reference sample
instrument
measured
ray pipe
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN 201019114089
Other languages
Chinese (zh)
Inventor
赵宇
周俊武
徐宁
赵建军
高扬
李传伟
杨树亮
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beijing General Research Institute of Mining and Metallurgy
Original Assignee
Beijing General Research Institute of Mining and Metallurgy
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Beijing General Research Institute of Mining and Metallurgy filed Critical Beijing General Research Institute of Mining and Metallurgy
Priority to CN 201019114089 priority Critical patent/CN101813646A/en
Publication of CN101813646A publication Critical patent/CN101813646A/en
Pending legal-status Critical Current

Links

Images

Abstract

The invention discloses a method and a device for correcting instrument drift during X-ray fluorescence quantitative detection.A reference mechanism controlled by an instrument is arranged between an X-ray tube and a measurement sample box; a reference sample pressed according to the metal element to be detected is arranged on the mechanism; and measuring the reference sample by using an X fluorescence analyzer to obtain the pulse counting rate of the reference sample as an original target intensity value. When the X fluorescence analyzer is used for online operation measurement, the counting rate of the reference sample is measured before the ore pulp sample is measured each time, the ratio of the counting rate to the original target intensity of the reference sample is used as a standardization coefficient, and the pulse counting rate of the ore pulp sample measured each time is corrected by using the calculated standardization coefficient to obtain the standard pulse counting rate of online ore pulp measurement. The drift of the instrument on the performance index caused by long-term or short-term can be compensated in real time, and the stability and the measurement accuracy index of the instrument are improved.

Description

The bearing calibration of instrument drift and device during the XRF detection by quantitative
Technical field
The present invention relates to the real-Time Compensation technology of a kind of radionetric survey analytical equipment drift, the bearing calibration and the device of instrument drift when especially relating to a kind of XRF detection by quantitative.
Background technology
In the mineral process, usually with the xrf analysis instrument mine slurry grade is carried out online detection, instrument is in operation, As time goes on reach the continuous variation of surrounding environment factor, its running status is also little by little changing, and the long term drift of the short-term fluctuation of instrument or drift and instrument all can cause the measuring accuracy of fluorescent spectroscopy.The stability of short-term is caused by the fluctuation of environment temperature, atmospheric pressure, AC network, X-ray pipe power supply, detector and drift institute.The long term drift of instrument then causes owing to the instrument component aging, comprising X-ray pipe electric power output voltage wearing out along with resistance and other elements, the light pipe target surface spot may occur and metal sublimate accumulation arrives the window inside surface, cause the ray output intensity to descend, the diffraction crystal reflection efficiency reduces, and detective quantum efficiency descends or the like.
In the prior art,, generally be rule of thumb, after instrument moves a period of time, instrument returned zero correction the bearing calibration of xrf analysis instrument drift.
There is following shortcoming at least in above-mentioned prior art:
Be difficult to the drift on automatic, the real-time compensation apparatus measuring accuracy, the stability and the measuring accuracy of instrument are lower.
Summary of the invention
The purpose of this invention is to provide a kind of can be automatically, the drift on the real-Time Compensation Instrument measuring precision, the bearing calibration of instrument drift when improving the XRF detection by quantitative of the stability of instrument and measuring accuracy.
The objective of the invention is to be achieved through the following technical solutions:
The bearing calibration of instrument drift during XRF detection by quantitative of the present invention comprises step:
At first, prepare the reference sample, and repeatedly measure the pulsimeter digit rate of the metallic element to be measured in the described reference sample with the xrf analysis instrument according to metallic element to be measured and content thereof;
Then, get repeatedly the mean value of pulsimeter digit rate of the metallic element to be measured in the reference sample of measuring as the original object intensity level;
Afterwards, before described xrf analysis instrument is measured testing sample at every turn, at first measure once described reference sample, and pulsimeter digit rate and the described original object intensity level of the metallic element to be measured of this time measurement compared, with the result of comparison correction factor as this measurement;
At last, measure testing sample, and this result who measures testing sample is revised with described correction factor.
The device of the bearing calibration of instrument drift during the above-mentioned XRF detection by quantitative of realization of the present invention, comprise the X-ray pipe, the place ahead of described X-ray pipe is provided with sample box, be provided with the reference sample between described X-ray pipe and the sample box, described reference sample can shift out or move between described X-ray pipe and the sample box.
As seen from the above technical solution provided by the invention, the bearing calibration and the device of instrument drift during XRF detection by quantitative of the present invention are owing between X-ray pipe and measuring samples box, be provided with a reference mechanism that controlled by instrument; The reference sample that is pressed into by metallic element to be measured is installed in this mechanism; Use the xrf analysis instrument to measure the reference sample, the pulsimeter digit rate that obtains reference is as the original object intensity level.When xrf analysis instrument on-line operation is measured, all to measure the counting rate of a reference before each measurement ore pulp sample, and with the ratio of this counting rate and reference original object intensity as normalisation coefft, utilize the normalisation coefft that calculates that the pulsimeter digit rate of the ore pulp sample of each measurement is revised, obtain the full sized pules counting rate of online ore pulp.Can be automatically, the drift on the performance index brought because of long-term or short-term of real-Time Compensation instrument, improve the stability and the measuring accuracy index of instrument.
Description of drawings
The process flow diagram of Fig. 1 bearing calibration specific embodiment of instrument drift during for XRF detection by quantitative of the present invention;
The structural representation of the device specific embodiment of the bearing calibration of instrument drift when Fig. 2 realizes the XRF detection by quantitative for the present invention.
Embodiment
The bearing calibration of instrument drift during XRF detection by quantitative of the present invention, its preferable embodiment comprises step as shown in Figure 1:
At first, prepare the reference sample, and repeatedly measure the pulsimeter digit rate of the metallic element to be measured in the described reference sample with the xrf analysis instrument according to metallic element to be measured and content thereof;
Then, get repeatedly the mean value of pulsimeter digit rate of the metallic element to be measured in the reference sample of measuring as the original object intensity level;
Afterwards, before described xrf analysis instrument is measured testing sample at every turn, at first measure once described reference sample, and pulsimeter digit rate and the described original object intensity level of the metallic element to be measured of this time measurement compared, with the result of comparison correction factor as this measurement;
At last, measure testing sample, and this result who measures testing sample is revised with described correction factor.
The device of the bearing calibration of instrument drift during the above-mentioned XRF detection by quantitative of realization of the present invention, its preferable embodiment be as shown in Figure 2:
Comprise the X-ray pipe, the place ahead of described X-ray pipe is provided with sample box, is provided with the reference sample between described X-ray pipe and the sample box, and described reference sample can shift out or move between described X-ray pipe and the sample box.
Described reference sample can be fixed in the reference mechanism, and described reference mechanism can drive described reference sample and shift out or move between described X-ray pipe and the sample box.
The correct detection method and the device of instrument drift are under the cooperation of reference mechanism during XRF detection by quantitative of the present invention, by a kind of standardization measuring method, calculate the drift correction constant, the processing procedure of carrying out the correction of spectrometer pulse value.Be used to overcome instrument because of long-term or short term drift to the influence that the target strength value causes, improved the measuring accuracy of target strength, thereby improved the grade analysis precision of analyser.
Also the present invention is described in detail in conjunction with the accompanying drawings below by specific embodiment:
Again referring to Fig. 1, Fig. 2:
Between X-ray pipe and measuring samples box, a reference mechanism that is subjected to instrument control is set; By metallic element to be measured and content, prepare the reference sample with powder art sample, compression moulding is installed in the reference sample position among Fig. 1; When reference corrected was carried out in the needs measurement, reference mechanism entered between X-ray pipe and the sample box reference sample.
After finishing measurement, reference mechanism leaves between X-ray pipe and the sample box reference sample, make it can the measuring samples box the ore pulp sample.
Flow process according to Fig. 2, before the normal use of instrument input, the reference sample enters the measuring position, and the xrf analysis instrument is measured this reference sample of certain number of times, draw reference measure in the mean value of the pulsimeter digit rate of element separately, as reference original object intensity level;
After, during analyser instrument on-line operation, at first carrying out standardization measures, all to measure the counting rate of a reference before promptly each measurement ore pulp sample, and be exactly normalisation coefft with the result of the ratio of this counting rate and reference original object intensity level, as the compensation correction factor of instrument drift.
At last, the normalisation coefft that utilize to calculate is revised the pulsimeter digit rate of the ore pulp sample of this measurement, obtains the full sized pules counting rate of online ore pulp, with compensation apparatus because of for a long time or the drift on the performance index brought of short-term.
The present invention can be used for the metal element content detecting instrument equipment of online x-ray fluorescence analyzer, and the drift on the performance index brought because of long-term or short-term of compensation apparatus well improves the stability and the measuring accuracy index of instrument.
The above; only for the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, and anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.

Claims (3)

1. the bearing calibration of instrument drift during an XRF detection by quantitative is characterized in that, comprises step:
At first, prepare the reference sample, and repeatedly measure the pulsimeter digit rate of the metallic element to be measured in the described reference sample with the xrf analysis instrument according to metallic element to be measured and content thereof;
Then, get repeatedly the mean value of pulsimeter digit rate of the metallic element to be measured in the reference sample of measuring as the original object intensity level;
Afterwards, before described xrf analysis instrument is measured testing sample at every turn, at first measure once described reference sample, and pulsimeter digit rate and the described original object intensity level of the metallic element to be measured of this time measurement compared, with the result of comparison correction factor as this measurement;
At last, measure testing sample, and this result who measures testing sample is revised with described correction factor.
2. the device of the bearing calibration of an instrument drift when realizing the described XRF detection by quantitative of claim 1, comprise the X-ray pipe, the place ahead of described X-ray pipe is provided with sample box, it is characterized in that, be provided with the reference sample between described X-ray pipe and the sample box, described reference sample can shift out or move between described X-ray pipe and the sample box.
3. the device of the bearing calibration of instrument drift during realization XRF detection by quantitative according to claim 2, it is characterized in that, described reference sample is fixed in the reference mechanism, and described reference mechanism drives described reference sample and shifts out or move between described X-ray pipe and the sample box.
CN 201019114089 2010-02-26 2010-02-26 Method and device for correcting instrument drift during X-ray fluorescence quantitative detection Pending CN101813646A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201019114089 CN101813646A (en) 2010-02-26 2010-02-26 Method and device for correcting instrument drift during X-ray fluorescence quantitative detection

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 201019114089 CN101813646A (en) 2010-02-26 2010-02-26 Method and device for correcting instrument drift during X-ray fluorescence quantitative detection

Publications (1)

Publication Number Publication Date
CN101813646A true CN101813646A (en) 2010-08-25

Family

ID=42620958

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 201019114089 Pending CN101813646A (en) 2010-02-26 2010-02-26 Method and device for correcting instrument drift during X-ray fluorescence quantitative detection

Country Status (1)

Country Link
CN (1) CN101813646A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103323872A (en) * 2012-03-20 2013-09-25 西门子公司 Method for energy calibrating quantum-counting x-ray detectors in a dual-source computed-tomography scanner

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH1048161A (en) * 1996-07-31 1998-02-20 Shimadzu Corp X-ray analyzer
JP2000105208A (en) * 1998-09-30 2000-04-11 Rigaku Industrial Co Fluorescent x-ray analyzer
CN201373858Y (en) * 2009-03-04 2009-12-30 上海精谱仪器有限公司 Energy chromatic dispersion X fluorescence analyser

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH1048161A (en) * 1996-07-31 1998-02-20 Shimadzu Corp X-ray analyzer
JP2000105208A (en) * 1998-09-30 2000-04-11 Rigaku Industrial Co Fluorescent x-ray analyzer
CN201373858Y (en) * 2009-03-04 2009-12-30 上海精谱仪器有限公司 Energy chromatic dispersion X fluorescence analyser

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103323872A (en) * 2012-03-20 2013-09-25 西门子公司 Method for energy calibrating quantum-counting x-ray detectors in a dual-source computed-tomography scanner
US9039284B2 (en) 2012-03-20 2015-05-26 Siemens Aktiengesellschaft Method for energy calibrating quantum-counting x-ray detectors in a dual-source computed-tomography scanner
CN103323872B (en) * 2012-03-20 2015-11-18 西门子公司 X-ray detector for counting quantum carries out the method for energy calibration

Similar Documents

Publication Publication Date Title
CN101509872B (en) Coal quality on-line detecting analytical method based on regression analysis
CN103837558B (en) Multielement composition and content detection device and detection method in a kind of aqueous solution based on PGNAA technology
CN102313722B (en) Proximate analyzing method for coal quality based on multivariate linear regression
CN101949852B (en) Spectral standardization-based coal quality on-line detection method
CN201909767U (en) Energy dispersive X-ray fluorescence spectrometer for analyzing irregular samples directly
CN102004097B (en) Coal quality on-line detecting method based on dominating factor and combined with partial least squares method
CN109085136B (en) Method for measuring content of oxide components in cement raw material by near-infrared diffuse reflection spectrum
CN103323319A (en) Enriching and detecting equipment for particles
CN108693204B (en) Potassium salt composition on-line measuring device
CN105651801B (en) Online analysis method for ore pulp minerals
CN107703097A (en) Utilize the method and its application of decay total reflection probe and the model of near infrared spectrometer structure fast prediction oil property
CN201373858Y (en) Energy chromatic dispersion X fluorescence analyser
CN107860743A (en) Utilize the method and its application of the model of reflective near infrared fibre-optical probe structure fast prediction oil property
CN103076351A (en) Method for measuring Mo element in tungstenic ferro-molybdenum alloy through X-ray fluorescence spectrum analysis
CN101086477A (en) Method for determining carbon content of non-ferrous metal smelting material
CN103196935B (en) Uranium plutonium on-line measurement device in platform experiment 1AP
CN203824940U (en) Handheld type X-ray fluorescence analyzer
US10816488B2 (en) Process for calibrating a sensor, automated method for online monitoring of the changes to a liquid body and associated sensor
CN103293175A (en) Method for measuring chemical components of liquid sodium silicate
CN108680592B (en) A kind of sylvite ingredient online test method
CN106442474A (en) Cement raw meal three moduli measuring method based on partial least squares
CN101813646A (en) Method and device for correcting instrument drift during X-ray fluorescence quantitative detection
CN201034950Y (en) Vacuum X fluorescent energy color dispersion spectrometer
CN103837559B (en) The quick sulphur meter of many target scans formula
Jia et al. A new distance correction method for sulfur analysis in coal using online XRF measurement system

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
C12 Rejection of a patent application after its publication
RJ01 Rejection of invention patent application after publication

Open date: 20100825