CN101509873B - Coal quality detecting method based on active marker method - Google Patents
Coal quality detecting method based on active marker method Download PDFInfo
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- CN101509873B CN101509873B CN2009101198856A CN200910119885A CN101509873B CN 101509873 B CN101509873 B CN 101509873B CN 2009101198856 A CN2009101198856 A CN 2009101198856A CN 200910119885 A CN200910119885 A CN 200910119885A CN 101509873 B CN101509873 B CN 101509873B
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Abstract
The invention discloses a coal property detecting method based on an active internal calibrating method, which can be used for online coal property detecting devices based on the laser-induced plasma spectrum principle. The coal property detecting method actively adds a bonding agent with known element concentration and ingredients into coal according to a certain mass proportion, and a calibration is carried out by the mixture, with known mass concentration of each element, of the coal and the bonding agent; the elements with good characteristics are selected as internal calibrating elements, the vertical axis of a calibrating curve obtained by fitting shows the spectral line intensity ratio of elements to be detected to the internal calibrating elements and the horizontal axis shows themass concentration of the elements to be detected. In the detection of coal with unknown ingredients, the spectral line intensity ratio of the elements to be detected to the internal calibrating elements is detected, and the concentration of the elements to be detected can be obtained according to the calibrating curve. The coal property detecting method based on the active internal calibrating method reduces the influence caused by variant coal ingredients, raises the measuring accuracy of the laser-induced plasma spectrum technology, and can realize the online coal multiple-element measurement and provide real-time data of coal ingredients in production process.
Description
Technical field
The present invention relates to a kind of coal quality detecting method.Specifically, the ultimate principle of method is an induced with laser plasma spectrum technology (LIBS), and has used active marker method that ature of coal is carried out the rapid quantitative analysis.
Background technology
Using coal unit,, must in time control the concrete composition of coal on the band conveyor, can in time regulate relevant manufacturing parameter like this according to the variation of coal constituent for production run is carried out in good time regulation and control.Such as in the coal-burning power plant, the coal cost has accounted for 80% of total cost, so understand and factor such as research ature of coal is vital to the influence with coal unit.This can carry out constituent analysis to the coal on the conveying belt in real-time online ground with regard to requiring.But there are shortcomings such as analysis speed is slow, operation is loaded down with trivial details in the off-line analysis that generally adopts at present, generally need several hrs from sampling, sample preparation to quoting of assay, testing result seriously lags behind, can not in time feed back the information of coal, the reference data of real-time online can not be provided for operating personnel, be difficult to adapt to industrial demand.The coal analysis method of off-line has been difficult to satisfy the requirement with coal unit, employing is advanced, analysis means is very necessary fast, particularly develop effective ature of coal on-line measuring device and method, help improving the economy that coal resources in China is rationally utilized ability and improved coal utilization like this.Such as analyzing with 2 300MW coal fired power generation units, be used to into stove coal composition detection as if on-line measuring device, change according to ature of coal and adjust boiler combustion in real time, reduce coal consumption 1g/kWh, then can save 1,500,000 yuan approximately every year.
At present the technology of using in the online detection of ature of coal is the XRF technology, neutron induct prompt gamma-ray analysis technology and dual energy gamma ray through-transmission technique.But the XRF technology only is suitable for measuring atomic number greater than 11 element, and measuring accuracy and sensitivity are not high.Neutron inducts that the prompt gamma-ray analysis technology exists that investment is big, radiation hazard and short shortcoming of radioactive source half life period.And the shortcoming of dual energy gamma ray projective technique maximum be can't full elemental analysis, cost is higher and potential safety hazard is arranged.Because the shortcoming of these technology itself is not so be more widely used.It is higher that each is badly in need of a kind of precision with coal unit, and can realize the ature of coal on-line quick detection method of full elemental analysis.
In recent years, induced with laser plasma spectrum technology (being called for short LIBS) becomes a kind of new laser analysis technology owing to having high sensitivity, need not advantages such as sample pretreatment and the measurement of realization multielement.Because this technology maternal effect is apparent in view, directly precision is not high during the measurement of species composition, has limited the application of this technology in the online detection of ature of coal yet.Quantification measurement accurately is prerequisite and the basis that the LIBS system plays a role in the online detection of ature of coal.
Summary of the invention
The objective of the invention is at present big, the not high enough shortcoming that maybe can not realize full elemental analysis of precision of ature of coal on-line analysis technology existence investment, designed a kind of coal quality detecting method based on active marker method, can in induced with laser plasma spectrum system, use, solve the problem of ature of coal express-analysis.The present invention is by initiatively adding the fixing bonding agent of composition, scaling method is calibrated and is measured in the utilization, the characteristic spectral line of scaled element is eliminated the experiment parameter fluctuation of LIBS in utilizing, and both can realize the full elemental analysis of ature of coal, can improve measuring accuracy again.
Technical scheme of the present invention is:
A kind of coal quality detecting method based on active marker method is characterized in that this method comprises the steps:
1) utilizes one group of known coal of each element mass concentration to calibrate, earlier the sampling of the coal on the belt is smashed, add the known bonding agent of each element mass concentration, be pressed into solid-state calibration sample;
2) in calibration sample, choose the good or mass concentration relative standard deviation of some characteristics less than 20% element as interior scaled element, described in scaled element be as the element of reference standard when detecting;
3) utilize the induced with laser plasma spectrum system that is installed on the coal conveyer belt to detect: with pulsed laser 1 is excitation source, after laser process condenser lens 2 focusing of laser emitting, act on sample 3 surfaces, produce plasma at focus point, plasma cools off in the atmosphere of blanket gas, the radiant light signal that produces is by gathering lens 4 by real-time collecting, gathered by computing machine 7 by optical fiber 5 and through changing into electric signal after spectrometer 6 processing, obtain the characteristic spectrum of each element in the calibration sample, set up calibration curve then;
4) the characteristic spectra line strength I of scaled element in the selection
0As the basis of calculation, with the characteristic spectra line strength I of element to be measured
cCharacteristic spectra line strength I with interior scaled element
0Ratio and element mass concentration C to be measured form data to (C, I
c/ I
0), and it is right to obtain multi-group data at many groups sample, simulates calibration curve then, and the transverse axis of curve is exactly an element mass concentration to be measured, and the longitudinal axis is exactly I
cAnd I
0Ratio;
When 5) coal of each element mass concentration the unknown being detected, earlier the sampling of the coal on the belt is smashed, add the known bonding agent of each element mass concentration then, be pressed into solid-state testing sample;
6) utilize induced with laser plasma spectrum system to measure element to be measured and the corresponding characteristic spectra line strength of interior scaled element I '
cAnd I '
0, on calibration curve, find corresponding point (C ', I '
c/ I '
0), the horizontal ordinate C ' of corresponding point be the concentration C of element to be measured '.
Described coal quality detecting method based on active marker method is characterized in that: described bonding agent adopts inorganic bond, organic bond or both potpourris.
Described coal quality detecting method based on active marker method is characterized in that: described inorganic bond is selected clay, bentonitic clay, pulverized limestone, cement, water glass, gypsum or sodium silicate for use; Described organic bond is selected lignin, organic siliconresin, polyvinyl alcohol (PVA), coal tar, pitch, phenolics, epoxy resin or unsaturated polyester resin for use.
Described blanket gas comprises air, N
2, CO
2Or inert gas.
The present invention has the following advantages:
It is easy that the present invention has analysis, realizes the multielement measurement, and Measuring Time is less, and safe and reliable characteristics.Because interior scaling method is the higher method of precision in the LIBS quantitative analysis,, improved measuring accuracy by adding the known bonding agent of composition.By the element component content in this equipment check and analysis in real time coal,, use coal unit in time to instruct production run according to coal elemental composition for production run provides the real time data of coal elemental composition.
The present invention similarly needing also to can be used for the chemical constitution occasion of detection in real time.But bonding agent will be selected for use according to particular problem.
Description of drawings
Fig. 1 is the concrete synoptic diagram of induced with laser plasma spectrum measurement mechanism among the present invention.
Fig. 2 is a schematic flow sheet of the present invention.
Fig. 3 is the illustration of the calibration curve of match among the present invention.
Embodiment
The present invention is further illustrated with enforcement below in conjunction with accompanying drawing.
A kind of coal quality detecting method based on active marker method provided by the invention is characterized in that this method comprises the steps:
1) utilizes one group of known coal of each element mass concentration to calibrate, earlier the sampling of the coal on the belt is smashed, add the known bonding agent of each element mass concentration, be pressed into solid-state calibration sample.Bonding agent can adopt inorganic bond, such as clay, bentonitic clay, pulverized limestone, cement, water glass, gypsum or sodium silicate; Also can adopt organic bond, such as lignin, organic siliconresin, polyvinyl alcohol (PVA), coal tar, pitch, phenolics, epoxy resin or unsaturated polyester resin.Cardinal rule is should not contain element to be measured in the bonding agent or contain more a spot of element to be measured, in order to avoid influence the coal analysis result, the bond properties of while and coal is better.The bonding agent that adds should keep the certain quality ratio with coal, must make the bonding agent of adding and coal can form solid-state calibration sample, also can determine the size of mass ratio according to the needs of measuring;
2) in calibration sample, choose the good or mass concentration relative standard deviation of some characteristics less than 20% element as interior scaled element, in described scaled element be when detecting as the element of reference standard, generally should the operating characteristic spectral line obviously or mass concentration in calibration sample, change smaller elements.
3) utilize the induced with laser plasma spectrum system that is installed on the coal conveyer belt to detect: with pulsed laser 1 is excitation source; after laser process condenser lens 2 focusing of laser emitting, act on sample 3 surfaces; produce plasma at focus point; plasma cools off in the atmosphere of blanket gas; the radiant light signal that produces is by gathering lens 4 by real-time collecting; gathered by computing machine 7 by optical fiber 5 and through changing into electric signal after spectrometer 6 processing; obtain the characteristic spectrum of each element in the calibration sample; set up calibration curve then, described blanket gas comprises air; N
2, CO
2Or inert gas.
4) the characteristic spectra line strength I of scaled element in the selection
0As the basis of calculation, with the characteristic spectra line strength I of element to be measured
cCharacteristic spectra line strength I with interior scaled element
0Ratio and element mass concentration C to be measured form data to (C, I
c/ I
0), and it is right to obtain multi-group data at many groups sample, simulates calibration curve then, and the transverse axis of curve is exactly an element mass concentration to be measured, and the longitudinal axis is exactly I
cAnd I
0Ratio;
When 5) coal of each element mass concentration the unknown being detected, earlier the sampling of the coal on the belt is smashed, add the known bonding agent of each element mass concentration then, be pressed into solid-state testing sample.The bonding agent that uses in the testing sample should be the same with the bonding agent that uses in the calibration sample, and the bonding agent in mass ratio and the calibration sample of bonding agent and coal and the mass ratio of coal should keep equating in the testing sample, this be for the mass concentration in calibration sample and testing sample of scaled element in guaranteeing constant substantially;
6) utilize induced with laser plasma spectrum system to measure element to be measured and the corresponding characteristic spectra line strength of interior scaled element I '
cAnd I '
0, on calibration curve, find corresponding point (C ', I '
c/ I '
0), the horizontal ordinate C ' of corresponding point be the concentration C of element to be measured '.
Embodiment:
1) be element to be measured with H, take five kinds of stone coal coal samples that each element mass concentration is known, as one group of calibration sample, the mass concentration of element H is respectively 1.00%, 1.32% in this group coal sample, and 1.50%, 1.90%, 2.10%.To every kind of coal sample sampling 50g, the bonding agent pulverized limestone that adds 20g then, be pressed into solid-state sheet sample and enter measurement mechanism, wherein contain Elements C a mass concentration 35%, Elements C mass concentration 12%, element M g mass concentration 8%, element O mass concentration 45% in the bonding agent.Owing to do not contain the H element in this bonding agent,, contain spectral signature Elements C a preferably in the bonding agent simultaneously so can the H element mass concentration of coal sample in the calibration sample not impacted;
2) for this group calibration sample, Elements C a mass concentration relative standard deviation is 3%, remain unchanged substantially, and Elements C a spectral signature is better, and be interior scaled element so select Elements C a;
3) utilize the induced with laser plasma spectrum system that is installed on the coal conveyer belt that calibration sample is detected: with pulsed laser 1 is excitation source, after laser process condenser lens 2 focusing of laser emitting, act on sample 3 surfaces, produce plasma at focus point, plasma cools off in the atmosphere of air, the radiant light signal that produces is by gathering lens 4 by real-time collecting, gathered by computing machine 7 by optical fiber 5 and through changing into electric signal after spectrometer 6 processing, obtain the characteristic spectrum of each element in the calibration sample, set up calibration curve then;
4) select the interior characteristic spectra line strength I that calibrates Elements C a
0As the basis of calculation, with the characteristic spectra line strength I of element H to be measured
cCharacteristic spectra line strength I with interior calibration Elements C
0Ratio and element H mass concentration C to be measured form data to (C, I
c/ I
0), and it is right to obtain multi-group data at many groups sample, simulates calibration curve then, and the transverse axis of curve is exactly an element mass concentration to be measured, and the longitudinal axis is exactly I
cAnd I
0Ratio.As shown in Figure 3, the curve horizontal ordinate is element H mass concentration C to be measured in the calibration sample, and ordinate is the characteristic spectra line strength I of element H to be measured in the calibration sample
cCharacteristic spectra line strength I with interior calibration Elements C
0Ratio.
5) to the coal sampling 50g of each element mass concentration the unknown and smash, add the known bonding agent pulverized limestone of each element mass concentration of 20g then, be pressed into solid-state testing sample, enter measurement mechanism.Wherein contain Elements C a mass concentration 35%, Elements C mass concentration 12%, element M g mass concentration 8%, element O mass concentration 45% in the bonding agent, the adhesive ingredients that uses during with calibration is formed identical;
6) utilize induced with laser plasma spectrum system to measure element H to be measured and the corresponding characteristic spectra line strength of interior calibration Elements C a I '
cAnd I '
0, the ratio of experimental result is I '
c/ I '
0=0.13.On calibration curve, find corresponding point (C ', I '
c/ I '
0)=(1.49,0.13), the horizontal ordinate C ' of corresponding point is concentration C '=1.49% of element H to be measured in the coal of composition the unknown.
7) measurement result shows by computing machine.
Accuracy for verification method, when use element H mass concentration be 1.72% stone coal as testing sample, the mass concentration that obtains its element H after tested is 1.70%, measuring relative errors is 1.1%, as seen this method precision is higher, can meet the production needs.
Comprise pulsed laser 1, condenser lens 2 with the corresponding checkout equipment of said method, gather lens 3, optical fiber 4, CCD spectrometer 5, computing machine 6, it is characterized in that pulsed laser 1 is installed in the top of condenser lens 2, condenser lens 2 is positioned at the top of the coal sample 3 on the belt, gathers the side that lens 4 are positioned at the coal sample.Coal sample 3 on the belt passes through from condenser lens 2 bottoms.Gather lens 4 and link to each other with the input section of spectrometer 6 by optical fiber 5, the output terminal of spectrometer 6 links to each other with computing machine 7.
Principle of work of the present invention is:
Induced with laser plasma spectrum technology is meant that sample can be gasificated into high temperature, highdensity plasma in moment when intense pulse laser shines on the sample through focusing on, and the plasma cognition that is in excited state externally discharges different rays.The wavelength of plasma emission spectroscopy spectral line correspondence and intensity reflect the component in the object surveyed and its concentration respectively.This technology has high detection sensitivity, and cost is lower, can be simultaneously multiple element such as be analyzed at advantage, the application potential that has huge coal analysis to detect.The full element express-analysis that utilizes this technology to realize coal sample.
Interior scaling method is an induced with laser plasma spectrum technology quantitative method commonly used.Because total some test parameters (such as pulsed laser energy) random fluctuation in each process of the test, thereby make test findings have the randomness error.In order to eliminate this error, when setting up calibration curve, need select interior scaled element.Selected element as reference standard is called interior scaled element when utilizing the induced with laser plasma technology to carry out detection by quantitative.(its signal intensity is I to certain bar characteristic spectral line of scaled element in the definite selection of saying so
0), with the characteristic spectra line strength I of element to be measured
cAnd I
0Ratio and required constituent content form data to (C, I
c/ I
0), and it is right to obtain multi-group data at many groups calibration sample, simulate calibration curve then, and the transverse axis of curve is exactly a constituent content to be measured, the longitudinal axis is exactly I
cAnd I
0Ratio.When the sample of principal component does not detect, only need utilize induced with laser plasma spectrum system to measure element to be measured and the corresponding characteristic spectra line strength of interior scaled element I '
cAnd I '
0, on calibration curve, find corresponding point (C ', I '
c/ I '
0), the horizontal ordinate C ' of corresponding point is the concentration of element to be measured.This calibrating method is compared with general LIBS quantitative analysis method, owing to used the signal intensity of interior scaled element to eliminate the fluctuation of test parameters, degree of accuracy is higher.
Claims (4)
1. the coal quality detecting method based on active marker method is characterized in that this method comprises the steps:
1) utilizes one group of known coal of each element mass concentration to calibrate, earlier the sampling of the coal on the belt is smashed, add the known bonding agent of each element mass concentration, be pressed into solid-state calibration sample;
2) in the sample of calibration, choose the good or mass concentration relative standard deviation of some characteristics less than 20% element as interior scaled element, in described scaled element be when detecting as the element of reference standard, and be the element that exists in the bonding agent that initiatively adds;
3) utilize the induced with laser plasma spectrum system that is installed on the coal conveyer belt to detect: with pulsed laser (1) is excitation source, after laser process condenser lens (2) focusing of laser emitting, act on sample (3) surface, produce plasma at focus point, plasma cools off in the atmosphere of blanket gas, the radiant light signal that produces is by gathering lens (4) by real-time collecting, gathered by computing machine (7) by optical fiber (5) and through changing into electric signal after spectrometer (6) processing, obtain the characteristic spectrum of each element in the calibration sample, set up calibration curve then;
4) the characteristic spectra line strength I of scaled element in the selection
0As the basis of calculation, with the characteristic spectra line strength I of element to be measured
cCharacteristic spectra line strength I with interior scaled element
0Ratio and element mass concentration C to be measured form data to C, I
c/ I
0, and it is right to obtain multi-group data at many groups sample, simulates calibration curve then, and the transverse axis of calibration curve is an element mass concentration to be measured, the longitudinal axis is I
cAnd I
0Ratio;
When 5) coal of each element mass concentration the unknown being detected, earlier the sampling of the coal on the belt is smashed, add the known bonding agent of each element mass concentration, be pressed into solid-state testing sample;
6) utilize induced with laser plasma spectrum system to measure element to be measured and the corresponding characteristic spectra line strength of interior scaled element I '
cAnd I '
0, on calibration curve, find corresponding point C ', I '
c/ I '
0, the horizontal ordinate C ' of corresponding point be the concentration C of element to be measured '.
2. the coal quality detecting method based on active marker method according to claim 1 is characterized in that: described bonding agent adopts inorganic bond, organic bond or both potpourris.
3. the coal quality detecting method based on active marker method according to claim 2 is characterized in that: described inorganic bond is selected clay, bentonitic clay, pulverized limestone, cement, water glass, gypsum or sodium silicate for use; Described organic bond is selected lignin, organic siliconresin, polyvinyl alcohol (PVA), coal tar, pitch, phenolics, epoxy resin or unsaturated polyester resin for use.
4. the coal quality detecting method based on active marker method according to claim 1, its feature also is: the blanket gas described in the step 3) comprises air, N
2, CO
2Or inert gas.
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| WO2016206401A1 (en) * | 2015-06-26 | 2016-12-29 | 国电新能源技术研究院 | Device for detecting characteristic nature of coal on-line |
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| CN101949852A (en) * | 2010-07-30 | 2011-01-19 | 清华大学 | Spectral standardization-based coal quality on-line detection method |
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