CN101949852B - Spectral standardization-based coal quality on-line detection method - Google Patents
Spectral standardization-based coal quality on-line detection method Download PDFInfo
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Abstract
The invention relates to a spectral standardization-based coal quality on-line detection method, which can be used for coal quality on-line detection based on a laser induced plasma spectra principle. In the method, a calibrating model is established by using the intensity of an atomic characteristic spectral line after spectral standardization as a vertical coordinate and using the concentration of an element corresponding to the atomic characteristic spectral line as a horizontal coordinate. When the coal with unknown components is detected, the concentration of an element to be tested can be obtained according to the calibrating model after the spectral standardization. In the method, plasma temperature, electronic density, density ratio of ion to atom of the same element and a boltzmann's law are taken into consideration, so that the fluctuation of experiment parameters is compensated and the measuring precision is improved. The method can also be applied to the similar occasions requiring on-line real-time detection of chemical components.
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 the spectroscopic standard method that ature of coal is carried out online 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 coal resources in China like this and rationally utilize ability and the economy that improves coal utilization.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 adjustment boiler combustion in real time based on ature of coal, reduce coal consumption 1g/kWh, then can practice thrift 1,500,000 yuan approximately every year.
The technology of using in the online detection of ature of coal at present 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 prompt gamma-ray analysis technology exists that investment is big, radiation hazard and short shortcoming of radioactive source half life period.And the maximum shortcoming of dual energy gamma ray projective technique 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, and also having limited should the application of technology in the online detection of ature of coal.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 to 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; A kind of coal quality detecting method based on spectroscopic standardization is provided; Can in induced with laser plasma spectrum system, use, to solve the problem of the online express-analysis of ature of coal.
Technical scheme of the present invention is:
A kind of ature of coal online test method based on spectroscopic standardization is characterized in that this method comprises the steps:
1) utilize the induced with laser plasma spectrum system that is installed on the coal conveyer belt to set up calibration curve: with pulsed laser 1 is excitation source; The calibration coal sample that each element mass concentration is known places the atmosphere of blanket gas; The laser that goes out from laser emitting acts on calibration coal sample surface after focusing on through condenser lens 2; Produce plasma at focus point; Through gathering lens real-time collecting plasma resonance light signal, this signal changes into electric signal and is input to computing machine and handles through optical fiber and after spectrometer is handled, obtain each atoms of elements characteristic spectral line and ion characteristic spectral line in the said calibration coal sample;
2) ask for the temperature and the plasma electron density of plasma;
3) for each atoms of elements characteristic spectral line in the calibration coal sample; Utilize the ion atoms density ratio and the Boltzmann law of element; Green strength to the atomic features spectral line carries out standardization, and the atomic features line strength after the standardization is
Wherein, n
II/ n
I=(2 π m
eKT/h
2)
3/22U
II(T)/U
I(T) exp ((E
Ion-Δ E)/(kT))/n
e
In the following formula,
For atom transits to down the green strength of atomic features spectral line that energy level j is discharged and that received by detector from last energy level i, F representes instrument parameter, and for the experiment condition of confirming, F is constant, A
Ij, g
i, U
I(T) and U
II(T) represent respectively transition probability, go up statistical weight, the partition function of atom and the partition function of ion of energy level; E
i, T, k
BTemperature, Boltzmann constant and Planck's constant with h difference representative element excited energy, plasma; n
I, n
IIAnd n
eRepresent atomic density, ion concentration and electron density respectively, E
IonBe the ionization energy of ground state atom, Δ E is that ionization energy reduces the factor;
4) for one group of calibration coal sample that each concentration of element is different; Repeating step 1), 2) and 3); Obtain each atoms of elements characteristic spectral line intensity; Utilize
and set up calibration curve, C representes the mass concentration of element;
5) utilize induced with laser plasma spectrum system to measure atoms of elements characteristic spectra line strength to be measured
according to step 2), 3) spectrum is carried out standardization; Obtain atomic features line strength
after the standardization and on calibration curve, find the horizontal ordinate C of corresponding point
corresponding point, C is the mass concentration of element to be measured;
Blanket gas described in the step 1) of technique scheme comprises air, N
2, CO
2Or inert gas.Step 2) method of asking for plasma temperature described in adopts Boltzmann method, Saha Boltzmann method or multielement Saha Boltzmann method; Step 2) method of asking for plasma electron density described in adopts spectral line Stark broadening method.
The present invention has the following advantages and the high-lighting effect: because the spectroscopic standard method can improve the precision of LIBS quantitative analysis significantly; The present invention is through utilizing the plasma physics parameter; Spectrum is carried out standardization; Eliminate the experiment parameter fluctuation of LIBS, both can realize the full elemental analysis of ature of coal, can improve measuring accuracy again.It is easy that the present invention has analysis, realizes the multielement measurement, and Measuring Time is less, and safe and reliable characteristics.The element component content of this method in can real-time online check and analysis coal for production run provides the real time data of coal elemental composition, can in time instruct production run according to coal elemental composition with coal unit.
The present invention also can be used for the similarly real-time occasion that detects of the online chemical constitution of needs.
Description of drawings
Fig. 1 is the structural principle synoptic diagram of induced with laser plasma spectrum measurement mechanism among the present invention.
Fig. 2 is the illustration of the calibration curve of match among the present invention.
Fig. 3 is the process flow diagram of measuring method of the present invention.
Embodiment
The present invention is further described with implementing below in conjunction with accompanying drawing.
A kind of ature of coal online test method based on spectroscopic standardization provided by the invention is characterized in that this method comprises the steps:
1) utilize the induced with laser plasma spectrum system that is installed on the coal conveyer belt to set up calibration curve: with pulsed laser 1 is excitation source; The calibration coal sample 3 that each element mass concentration is known places the atmosphere of blanket gas; The laser that goes out from laser emitting acts on calibration coal sample 3 surfaces after focusing on through condenser lens 2; Produce plasma at focus point; Through gathering lens 4 real-time collecting plasma resonance light signals, this signal is through optical fiber 5 and after spectrometer 6 is handled, change into electric signal and be input to into processing of computing machine 7, obtains each atoms of elements characteristic spectral line and ion characteristic spectral line in the said calibration coal sample;
2) ask for the temperature and the plasma electron density of plasma;
3) for each atoms of elements characteristic spectral line in the calibration coal sample; Utilize the ion atoms density ratio and the Boltzmann law of element; Green strength to the atomic features spectral line carries out standardization, and the atomic features line strength after the standardization is
Atomic features line strength after the standardization
derivation is following:
(1)
do not consider the variation of Boltzmann's law and ion concentration atomic density ratio; Promptly think to not homogeneous measurement; Atomic density is constant with the ratio of the atomic density that is in energy level, and the ion concentration atomic density is than constant; Since the mass concentration C of element and atoms of elements density and ion concentration and be directly proportional; So the meval atom characteristic spectral line intensity of element is directly proportional with the mass concentration of element, promptly utilizes
and set up calibration curve.
(2)
Be out of shape:
Consider Boltzmann's law, but do not consider the variation of ion atoms density ratio, promptly think and measure that ion atoms density is than constant, and the ratio of the atomic density that is in the i energy level and atomic density changes for homogeneous not; Promptly utilize
and set up calibration curve.
(3)
Be out of shape:
Wherein, n
II/ n
I=(2 π m
eKT/h
2)
3/22U
II(T)/U
I(T) exp ((E
Ion-Δ E)/(kT))/n
e
Consideration Boltzmann law, and the variation of consideration ion atoms density ratio think that promptly for not homogeneous measurement, ion atoms density ratio changes, and are in the ratio variation of atomic density with the atomic density of i energy level; Promptly utilize
and set up calibration line.In the following formula, in the following formula,
For atom transits to down the green strength of atomic features spectral line that energy level j is discharged and that received by detector from last energy level i, F representes instrument parameter, and for the experiment condition of confirming, F is constant, A
Ij, g
i, U
I(T) and U
II(T) represent respectively transition probability, go up statistical weight, the partition function of atom and the partition function of ion of energy level; E
i, T, k
BTemperature, Boltzmann constant and Planck's constant with h difference representative element excited energy, plasma; n
I, n
IIAnd n
eRepresent atomic density, ion concentration and electron density respectively, E
IonBe the ionization energy of ground state atom, Δ E is that ionization energy reduces the factor;
4) for one group of calibration coal sample that each concentration of element is different; Repeating step 1), 2) and 3); Obtain each atoms of elements characteristic spectral line intensity; Utilize
and set up calibration curve, C representes the mass concentration of element;
5) utilize induced with laser plasma spectrum system to measure atoms of elements characteristic spectra line strength to be measured
according to step 2), 3) spectrum is carried out standardization; Obtain
and on calibration curve, find the horizontal ordinate C of corresponding point
corresponding point, C is the concentration of element to be measured;
Embodiment:
1) get six kinds of known stone coal coal samples of each element mass concentration, as one group of calibration coal sample, the mass concentration of elemental nitrogen N is respectively 0.24%, 0.29% in this group coal sample, and 0.51%, 0.85%, 1.10%, 1.14%.To calibrate the coal sample measurement mechanism of packing into;
2) utilize the induced with laser plasma spectrum system that is installed on the coal conveyer belt to set up calibration curve: with pulsed laser 1 is excitation source, and the calibration coal sample 3 that each element mass concentration is known places the protection atmosphere of air (also can place N
2, CO
2Or in the inert gas atmosphere); The laser that goes out from laser emitting acts on calibration coal sample surface after focusing on through condenser lens 2; Produce plasma at focus point; Through gathering lens 4 real-time collecting plasma resonance light signals, this signal changes into electric signal and is input to computing machine 7 and handles through optical fiber 5 and after spectrometer 6 is handled, obtain each atoms of elements characteristic spectral line and ion characteristic spectral line in the said calibration coal sample;
3) ask for the temperature and the plasma electron density of plasma; Utilize the Boltzmann method to try to achieve plasma temperature, utilize spectral line Stark broadening method to try to achieve plasma and be 1.1*10^23/m^3 for 9041K (also can utilize other method such as Saha Boltzmann method or multielement Saha Boltzmann method);
4) for each atoms of elements characteristic spectral line in the calibration coal sample; Utilize the ion atoms density ratio and the Boltzmann law of element; Green strength to the atomic features spectral line carries out standardization, and the atomic features line strength after the standardization is
Wherein, n
II/ n
I=(2 π m
eKT/h
2)
3/22U
II(T)/U
I(T) exp ((E
Ion-Δ E)/(kT))/n
e
In the following formula,
For atom transits to down the green strength of atomic features spectral line that energy level j is discharged and that received by detector from last energy level i, F representes instrument parameter, and for the experiment condition of confirming, F is constant, A
Ij, g
i, U
I(T) and U
II(T) represent respectively transition probability, go up statistical weight, the partition function of atom and the partition function of ion of energy level; E
i, T, k
BTemperature, Boltzmann constant and Planck's constant with h difference representative element excited energy, plasma; n
I, n
IIAnd n
eRepresent atomic density, ion concentration and electron density respectively, E
IonBe the ionization energy of ground state atom, Δ E is that ionization energy reduces the factor;
5) for one group of calibration coal sample that the N concentration of element is different; Repeating step 1) 2) 3); Obtain each atoms of elements characteristic spectral line intensity; Utilize
and set up calibration curve, C representes the mass concentration of element;
6) utilize induced with laser plasma spectrum system to measure temperature and electron density that the corresponding characteristic spectra line strength of element N to be measured
is obtained plasma; Through the spectral intensity standardization, experimental result
is 3.79.On calibration curve, find corresponding point
so the horizontal ordinate C of corresponding point is concentration C=0.72% of element N to be measured in the unknown coal of composition
7) measurement result shows through computing machine.
Accuracy for verification method; When use element N mass concentration be 0.78% stone coal as testing sample, the mass concentration that obtains its element N after tested is 0.76%, measuring relative errors is 2.56%; It is thus clear that this method precision is higher, can accords with production need.
Comprise pulsed laser 1, condenser lens 2 with the corresponding online detection instrument 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 through 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.Wavelength that the plasma emission spectroscopy spectral line is corresponding and intensity reflect the component and its concentration in the object of surveying 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 ature of coal on-line analysis to detect.Utilize this technology to realize online full element express-analysis to coal sample.
In LIBS measured, because the fluctuation of experiment parameter (like laser energy, ablation quality etc.), one of shortcoming of LIBS was that repeatability is smart low.The present invention considers the physical parameter of plasma fluctuation in the calibration model and goes, thereby described the relation between atomic features spectral line and the element mass concentration more accurately, fluctuation that therefore can the compensation experiment parameter, the precision of raising calibration model.
Ablate (Stoichiometric ablation) in theoretical proportioning (be in the plasma concentration of element concentration of element in the representative sample) fully and the assumed condition of local thermodynamic equilibrium (LTE) under; Based on the result of calculation of plasma electron temperature and electron density, draw a kind of new calibration model of revising the change of plasma physics parameter theoretically.
What the conventional single variable calibration model used is atoms of elements spectral line or ion line, and the mode of use regression fit draws the relation of element mass concentration and line strength.This calibration process is to be based upon under the constant hypothesis of the ion atoms density ratio of identity element.The atomic spectral line of wall scroll or ion line intensity basically can only representative element atomic concentration or ion concentration, and the direct total concentration of the total particle of representative element (atom+ion).The conventional single variable calibration model thinks that the concentration of ion or atom is into positive correlation with the total particle concentration of element, and this pass ties up in the analytic process and remains unchanged.In reality, because the change of matrix effect and experiment parameter, the ratio of ion atoms is along with the variation of plasma physics parameter changes.Could set up in the time of can ignoring so the hypothesis of traditional single argument calibration model can only change in the plasma physics parameter, this is one of important source of univariate model error.The present invention derives a kind of calibration model of considering the spectroscopic standardization that the plasma physics parameter changes theoretically; When calibration is calculated plasma temperature and electron density; And the ion atoms density of identity element compares and ANALOGY OF BOLTZMANN DISTRIBUTION is considered to come in; Thereby reach the fluctuation of compensation experiment parameter, improve the purpose of measuring accuracy.
Claims (3)
1. the ature of coal online test method based on spectroscopic standardization is characterized in that this method comprises the steps:
1) utilize the induced with laser plasma spectrum system that is installed on the coal conveyer belt to set up calibration curve: with pulsed laser (1) is excitation source; The calibration coal sample (3) that each element mass concentration is known places the atmosphere of blanket gas; After focusing on through condenser lens (2), the laser that goes out from laser emitting acts on calibration coal sample (3) surface; Produce plasma at focus point; Through gathering lens (4) real-time collecting plasma resonance light signal, this signal changes into electric signal and is input to computing machine (7) and handles through optical fiber (5) and after spectrometer (6) processing, obtain each atoms of elements characteristic spectral line and ion characteristic spectral line in the said calibration coal sample;
2) ask for the temperature and the plasma electron density of plasma;
3) for each atoms of elements characteristic spectral line in the calibration coal sample, the ion atoms density of utilizing element than and the Boltzmann law, the green strength of atomic features spectral line is carried out standardization, the atomic features line strength after the standardization is:
Wherein, n
II/ n
I=(2 π m
eKT/h
2)
3/22U
II(T)/U
I(T) exp ((E
Ion-Δ E)/(kT))/n
e
In the following formula,
Be the atomic features line strength after the standardization,
For atom transits to down the green strength of atomic features spectral line that energy level j is discharged and that received by detector from last energy level i, F representes instrument parameter, and for the experiment condition of confirming, F is constant; A
Ij, g
i, U
I(T) and U
II(T) represent respectively transition probability, go up statistical weight, the partition function of atom and the partition function of ion of energy level; E
i, T, k and h temperature, Boltzmann constant and the Planck's constant of representative element excited energy, plasma respectively; n
In
IIAnd n
eRepresent atomic density, ion concentration and electron density respectively, E
IonBe the ionization energy of ground state atom, Δ E is that ionization energy reduces the factor;
4) for one group of calibration coal sample that each concentration of element is different; Repeating step 1), 2) and 3); Obtain atomic features line strength after the standardization in one group of calibration sample; With the mass concentration C of element, calibration curve is set up in the standardization
that element is corresponding;
5) utilize induced with laser plasma spectrum system to measure atoms of elements characteristic spectra line strength to be measured
according to step 2), 3) spectrum is carried out standardization; The atomic features line strength
that obtains after the standardization is found corresponding point (C on calibration curve;
) pairing horizontal ordinate C, C is the concentration of element to be measured.
2. a kind of ature of coal online test method based on spectroscopic standardization according to claim 1, its characteristic also is: the blanket gas described in the step 1) comprises air, N
2, CO
2Or inert gas.
3. a kind of ature of coal online test method according to claim 1 based on spectroscopic standardization, its characteristic also is: the method for asking for plasma temperature step 2) adopts Boltzmann method, Saha Boltzmann method or multielement Saha Boltzmann method; The described method of asking for plasma electron density adopts spectral line Stark broadening method.
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