CN1289919A - Sequentially inductor coupled plasma spectrometer with automatic wavelength correction and its application method - Google Patents
Sequentially inductor coupled plasma spectrometer with automatic wavelength correction and its application method Download PDFInfo
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- CN1289919A CN1289919A CN 99119642 CN99119642A CN1289919A CN 1289919 A CN1289919 A CN 1289919A CN 99119642 CN99119642 CN 99119642 CN 99119642 A CN99119642 A CN 99119642A CN 1289919 A CN1289919 A CN 1289919A
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Abstract
A sequential conductance coupled plasma spectrometer with automatic wavelength correction function features that it has an automatic wavelength corrector, whose temp sensor in the case of monochromator is connected with temp sensor interface card in a slot on computer motherboard via interface and line and its wavelength correction subroutine is embedded in the master program of computer. Its advantages include no need of preheating and scanning each analyzed line, and high precision to locate spectral peak and measure the light intensity at speak.
Description
The invention belongs to automatic analytical and testing instrument field, particularly the order inductively-coupled plasma spectrometer and the application process of automatic wavelength calibration.
Existing inductively-coupled plasma spectrometer (being called for short ICP-AES), be the large-scale precision instrument that is used to finish the quantitative test of inorganic elements composition, form by electromechanical assembly, logical drive system, RF generator, matching system, sampling system, air-path control system, induction coil, plasma torch pipe, plasma torch flame, computing machine, display, keyboard, printer, computing machine master routine and the local constant temperature system of monochromator, incident light illumination system, photomultiplier PMT, control system, photometric system, rotating grating usually.
Because the Effect of Environmental such as systematic error of temperature variation, wavelength variations and inductively-coupled plasma spectrometer; following phenomenon usually can take place in ICP-AES: when the operator imports the wavelength value λ of the spectrum line that will measure; the ICP-AES actual measurement to be not the light intensity at λ place, but the light intensity at λ+Δ λ place.Have only when the incoming wave long value of ICP-AES is λ 1, the ICP-AES actual measurement to be only the light intensity that wavelength is the λ place.We claim Δ λ=λ 1-λ to be the skew of spectrum line peak, and it is not a constant, and the peak skew is relevant with the variation of temperature variation, wavelength variations and environmental factor.Present both at home and abroad optical instrument factory (company) in order to eliminate spectrum line peak skew that temperature variation the produces influence to order ICP-AES measuring accuracy, generally adopts local thermostat and adopts two kinds of traditional methods of scanning survey.For example, the Optima3000 ICP Emission Spectrometer inductively coupled plasma quantometer that U.S. PERKIN-ELMER company released in 1998, and the last word Trace Scan that U.S. ThermoJarrell Ash company produces has adopted local constant temperature system on the ICP quantometer in proper order.Fig. 1 provides the synoptic diagram of local constant temperature system principle of work.
Local thermostat is that an interlayer is installed outside the monochromator of ICP-AES, and the gas in the electricity consumption heater heats interlayer, electric fan flow the gas circulation in the interlayer.Temperature controller makes the gas temperature in the interlayer constant on the some temperature spots that are higher than in a year high ambient temperature, usually constant a certain temperature spot between 35-38 ℃.Local thermostat was worked under above state 8-10 hour, and the temperature in the ICP-AES could the constant equably temperature value that is setting.The shortcoming of this device is:
1. preheating time is long.Especially for research unit and universities and colleges, the time of actual usually use ICP-AES is shorter, have only tens minutes sometimes service time, and preheating time is very long, and is very inconvenient.
2. make the structure complicated of inductively-coupled plasma spectrometer, this just makes troubles for the maintenance of instrument and the re-graduation of light path, and increases the cost of instrument.
Do not adopt the ICP-AES of local constant temperature, adopt the scanning survey method more, or classical trace mensuration.The scanning survey method needs to open a measurement window near the spectral line peak position, measures the light intensity of about 10-20 point, therefrom finds out maximal value and is decided to be the peak light intensity.The shortcoming of scanning survey method is:
1. Measuring Time is long, and the Measuring Time lengthening can cause the measuring accuracy variation usually; Simultaneously, consumption gas, power consumption is big.
2. generally do not have the one-point measurement function, when the spectral line light intensity was very weak, the degree of accuracy of measurement was relatively poor.
Do not adopt the order ICP-AES of local constant temperature can make detecting device with CCD yet, open a measurement window and carry out scanning survey, can eliminate with photomultiplier and carry out some shortcomings that scanning survey brought, but the price of higher this class detecting device of resolution is very expensive as detecting device.
The object of the present invention is to provide a kind of order inductively-coupled plasma spectrometer and application process of automatic wavelength calibration, it is the national inventing patent (ZL94119410.8) that utilizes the applicant, make order ICP-AES increase the new function of automatic wavelength calibration, and can be used for replacing traditional local constant temperature system among the order ICP-AES that the merchant sells, it is simple in structure, cheap, easy and simple to handle, do not need preheating when using, and can improve measuring accuracy.
The order inductively-coupled plasma spectrometer of the automatic wavelength calibration of the present invention comprises grating monochromator, incident light illumination system, photomultiplier PMT, control system, photometric system, the electromechanical assembly of rotating grating, the logical drive system, the RF generator, matching system, sampling system, air-path control system, induction coil, the plasma torch pipe, the plasma torch flame, computing machine, display, keyboard, printer and computing machine master routine, it is characterized in that: in this spectrometer, the one automatic wavelength calibration device that is connected with lead with grating monochromator and computing machine is arranged, this device by temperature sensor with the interface board of its temperature sensor that is connected with lead, and the wavelength calibration subroutine in the order inductively-coupled plasma spectrometer computer program of automatic wavelength calibration is formed.Be provided with temperature sensor in this means for correcting, it is positioned at the cabinet of grating monochromator, be connected with the interface board of temperature sensor by parallel interface and lead, the temperature sensor interface plate is inserted in the groove of computer motherboard, and the wavelength calibration subroutine is organized in this spectrometer computer program in advance.
Wherein the interface board of temperature sensor is made up of constant-current source circuit, amplifying circuit, A/D change-over circuit and interface circuit; Temperature sensor constantly is defeated by temperature value the wavelength calibration subroutine by the interface board of temperature sensor, and wavelength value is then imported by keyboard, or accesses from database, and the wavelength calibration subroutine is carried out real-time wavelength calibration according to wavelength value and temperature value.
Automatic wavelength calibration method of the present invention comprises: by the RF generator, matching system, air-path control system, sampling system, induction coil, the plasma torch pipe, the characteristic emission spectrum of the various elements that the plasma torch flame is produced, the beam split of the grating monochromator by incident light illumination system and the control of logical drive system, make the analytical line of analytical element can pass through exit slit successively exactly, and imaging is on the photocathode of photomultiplier, the electric signal of analytical line light intensity is input in the computing machine through measuring system, the computing machine master routine obtains each concentration of element value the standard model by keyboard or from database, and the light intensity value of each analytical line of measuring system input, and be respectively ordinate and horizontal ordinate with standard specimen concentration and analytical line peak light intensity, draw the pairing working curve of each analytical line, after measuring the light intensity value of each elemental characteristic analytical line in the testing sample, on working curve, calculate the concentration value of each element to be measured in the sample solution successively, it is characterized in that: after so-called spectral analysis line is the correction of the automatic wavelength calibration device of analysis of line wavelength value process by exit slit successively exactly, make selected analytical line pass through exit slit, be the interface board of temperature sensor by temperature sensor, constantly send the real time temperature value in the monochromator chamber to the wavelength calibration subroutine, the real time temperature value T of the interface board input by the analytical line standard wave long value λ that from database, selects and temperature sensor, calculate each analytical line spectral line peak shifted by delta λ, and revise wavelength value λ
1λ
1Be fed to control system and drive system, drive unit stops the spectral line peak position of analytical line according to the rotation of this value correction grating successively exactly on exit slit, measure each analytical line peak light intensity exactly.
Polynomial equation (1) is shown below:
Δ λ
w=A
0+ A
1λ+A
2λ
2+ A
3λ
3+ A
4λ
4+ A
5λ
5(1) wherein: A
0=-14.864
A
1=0．181
A
2=-8．74E-4
A
3=2．105E-6
A
4=-2．516E-9
A
5=1．179E-12
R=0．9998
Polynomial equation (2) is shown below:
Δ λ
T=A
0+ A
1T+A
2T
2+ A
3T
3+ A
4T
4+ A
5T
5(2) wherein:
A
0=3．861
A
1=-0．958
A
2=0．891E-1
A
3=-0．410E-2
A
4=9．474E-5
A
5=-8．676E-7
R=0．9996
The present invention starts automatic wavelength calibration subroutine, accesses I bar analytical line and respective wavelength value λ (I) thereof from database, and imports real-time temperature value T from the interface board of temperature sensor; If be to move automatic wavelength calibration subroutine for the first time after the order ICP-AES start, earlier the fixing spectrum line of certain bar is carried out the spectrum line trace with regard to needing, and according to the Δ λ of real-time temperature value T to polynomial equation 1 and 2
W, Δ λ
TValue is revised; If ICP-AES has moved a period of time, this fixing spectrum line was carried out the spectrum line trace, with regard to successively analytical line directly being carried out wavelength calibration, promptly from I=1.
When the fixing spectrum line of certain bar is carried out trace: the wavelength value λ of input trace spectrum line
M, and to λ
MTrace is measured its spectrum line peak position λ
MAXIf λ
MAXValue is zero, then returns trace again; If non-vanishing, then calculate λ
MThe real-time spectral line peak shifted by delta λ of spectrum line
M, Δ λ wherein
M=λ
MAX-λ
MIf Δ λ
MValue has surpassed permissible value greater than 1nm, and also need return this moment, carries out λ again
MThe spectral line trace of spectrum line; If be no more than 1nm, or allow it to surpass 1nm under special circumstances, will carry out next step, two polynomial equation formulas are revised.
At first polynomial equation formula 1 is revised: utilize polynomial equation formula 1 to calculate λ
MSpectral line peak shifted by delta λ
M1Thereby, draw Δ λ in the polynomial equation formula 1
WModified value Δ λ
WD=Δ λ
M-Δ λ
M1Then polynomial equation formula 2 is revised:, obtain its spectrum line peak offset value delta λ the wavelength value substitution polynomial equation formula 1 of hg spectrum line 435.8nm
HGAnd real-time peak shifted by delta λ
HG+ Δ λ
WDUtilize polynomial equation formula 2 to obtain the pairing spectral line of real time temperature value T peak calculations of offset value Δ λ again
TMThereby, obtain Δ λ in the polynomial equation formula 2
TModified value Δ λ
TW=Δ λ
HG+ Δ λ
WD-Δ λ
TMSo far, finish, begin I bar analytical line is carried out the wavelength correction to the spectral line trace of the fixing spectrum line of certain bar and to the correction work of two polynomial equation formulas.
I bar analytical line λ (I) is carried out wavelength calibration: begin during I=1, to utilize polynomial equation formula 1 to obtain the spectral line peak offset value delta λ of λ (1) to the correction that circulates of the maximal value of I from I=1
1(1) and in real time peak shifted by delta λ
1(1)+Δ λ
WD, the correction wavelength X of λ (1) then
1(1)=λ (1)+Δ λ
1(1)+Δ λ
WDBefore being carried out wavelength calibration, next bar analytical line gathers real time temperature T again one time
I, utilize polynomial equation formula 2 to obtain real time temperature value T
IThe spectral line peak offset value delta λ of following hg spectrum line 435.8nm
TMIAnd real-time peak shifted by delta λ
TMI+ Δ λ
TWThereby, calculate the real-time modified value Δ λ of polynomial equation formula 1
WI=Δ λ
TMI+ Δ λ
TW-Δ λ
HG, and with Δ λ
WIValue is given Δ λ
WDSo analogize, to I bar analytical line circulation carrying out wavelength calibration; When I 〉=analytical line total, circulation correction is finished, with the I bar correction wavelength value λ of λ (I)
1(I) return data storehouse, the wavelength calibration subprogram activation finishes automatically.
The principle of work of the order inductively-coupled plasma spectrometer of automatic wavelength calibration:
RF generator 10 provides RF power supply by matching system 9 and induction coil 7 to plasma torch pipe 6, produces plasma torch flame 8.Sample solution 13 enters plasma torch flame 8 by sampling system 12 and air-path control system 11 with aerosol form, and sub-ization of atomic weight under hot environment in the gasoloid or ionization also excite the characteristic emission spectrum that produces each element.The light that light source 8 is produced by illuminator 14 with the imaging of plasma torch flame on the entrance slit 30 of monochromator 15, the function of monochromator 15 is the monochromatic collimated beams that the chromatic dispersion of a branch of polychrome incident light become each elemental characteristic spectrum of multi beam, and with the picture imaging of the entrance slit 30 of monochromatic collimated beam on exit slit 31.The electromechanical assembly 23 of rotating grating can make the grating 24 two-way rotations of monochromator, make the spectrum peak energy of selected analytical line pass through exit slit 31 successively exactly by automatic wavelength calibration device, and imaging is on the photocathode of photomultiplier 16.The analytical line light intensity signal that photomultiplier 16 will receive successively is input to computing machine 18 through measuring system 17.Each concentration of element value in the standard model solution that the master routine utilization of computing machine 18 is imported from keyboard 20 or database, and the light intensity value of each analytical line of measuring system 17 inputs, with the light intensity is ordinate, and the concentration of element value is a horizontal ordinate, makes the working curve of each analytical element.After measuring the light intensity value of each elemental characteristic analytical line in the testing sample, utilize the working curve of each analytical element, just can calculate the concentration value of each element to be measured in the sample solution successively.
Temperature sensor 25 constantly transfers to wavelength calibration subroutine 18 with the real time temperature value in monochromator 15 chambeies by the interface board of temperature sensor.The interface board of temperature sensor is made up of constant current source 26, amplifying circuit 27, A/D change-over circuit 28 and interface circuit 29.Wavelength calibration subroutine 18 is that theoretical foundation is written as with polynomial equation formula 1,2, it is by the real time temperature value T of the interface board input of the standard analysis line wavelength value λ that selects from database and temperature sensor, calculate analytical line spectral line peak shifted by delta λ, and revise wavelength value λ
1λ
1Be fed to control system 17 and drive system 22, the electromechanical assembly 23 of rotating grating is revised the rotation of grating 24 according to this value, the spectral line peak position that makes analytical line reaches to improve and seeks analytical line peak position precision, the accurately purpose of Measurement and analysis line peak light intensity successively exactly by exit slit 31.
Automatically the explanation of wavelength calibration subroutine flow chart
Start automatic wavelength calibration subroutine, access I bar analytical line and wavelength value λ (I) thereof from database, and from the real-time temperature value T of automatic wavelength calibration device input.If order ICP-AES moves for the first time automatic wavelength calibration subroutine after the energized, the spectrum line that just needs earlier certain bar to be fixed carry out the spectrum line trace, and according to real-time temperature value to the Δ λ in polynomial equation 1 and 2
W, Δ λ
TValue is revised, because when environmental factor slightly changes, the position of function relation curve also slightly changes, and need revise.If order ICP-AES has operated a period of time, and this fixing spectrum line is carried out the spectrum line trace, so just need not carry out above operation steps again, can directly carry out wavelength calibration (from I=1) to analytical line successively.
At first consider to carry out certain bar fixed light spectral line the situation of spectral line trace: the wavelength value λ of input trace spectrum line
M, and to λ
MTrace is measured its spectrum line peak position λ
MAXIf λ
MAXValue is zero, then returns trace again.If non-vanishing, as then to calculate λ
MThe real-time spectral line peak shifted by delta λ of spectrum line
M, Δ λ
M=λ
MAX-λ
MIf Δ λ
MValue has surpassed permissible value greater than 1nm, and also need return this moment, carries out λ again
MThe spectral line trace of spectrum line.If be no more than 1nm, or allow it to surpass 1nm under special circumstances, will carry out next step, two polynomial equation formulas are revised.
At first polynomial equation formula 1 is revised: utilize polynomial equation formula 1 to calculate λ
MSpectral line peak shifted by delta λ
M1Thereby, draw Δ λ in the polynomial equation formula 1
WModified value Δ λ
WD=Δ λ
M-Δ λ
M1Then polynomial equation formula 2 is revised:, obtain its spectrum line peak offset value delta λ the wavelength value substitution polynomial equation formula 1 of hg spectrum line 435.8nm
HGAnd real-time peak shifted by delta λ
HGTen Δ λ
WDUtilize polynomial equation formula 2 to obtain the pairing spectral line of real time temperature value T peak calculations of offset value Δ λ again
TMThereby, obtain Δ λ in the polynomial equation formula 2
TModified value Δ λ
TW=Δ λ
HG+ Δ λ
WD-Δ λ
TMSo far, finish to the spectral line trace of certain bar fixed light spectral line and to the correction work of two polynomial equation formulas.Below begin I bar analytical line is carried out the wavelength correction.
I bar analytical line λ (I) is carried out wavelength calibration: begin to the correction that circulates of the maximal value of I from I=1.During I=1.Utilize polynomial equation formula 1 to obtain the spectral line peak offset value delta λ of λ (1)
1(1) and in real time peak shifted by delta λ
1(1)+Δ λ
WD, the correction wavelength X of λ (1) then
1(1)=λ (1)+Δ λ
1(1)+Δ λ
WDIn order to improve the precision of wavelength calibration, before being carried out wavelength calibration, next bar analytical line imports one time real time temperature value T again
I, so that polynomial equation formula 1 is once revised again.Utilize polynomial equation formula 2 to obtain real time temperature T
IThe spectral line peak offset value delta λ of following hg spectrum line 435.8nm
TMIAnd real-time peak shifted by delta λ
TMI+ Δ λ
TWThereby, can calculate the real-time modified value Δ λ of polynomial equation formula 1
WI=Δ λ
TMI+ Δ λ
TW-Δ λ
HG, and with Δ λ
WIValue is given Δ λ
WDSo analogize, to I bar analytical line circulation carrying out wavelength calibration.When I 〉=analytical line total, circulation correction is finished, with the I bar correction wavelength value λ of λ (I)
1(I) return data storehouse, the wavelength calibration subprogram activation finishes automatically
The order inductively-coupled plasma spectrometer of the automatic wavelength calibration of the present invention has the one-point measurement pattern, both just under the condition of not using local thermostat, behind spectrum line of trace, can directly directly carry out the peak luminous intensity measurement in the peak position of all selected analytical lines; And the order ICP-AES that does not sell with the merchant of local thermostat can only carry out scanning survey.In general, the measuring accuracy of one-point measurement than the measuring accuracy height of scanning survey, save time, easy and simple to handle.
The present invention compares with order ICP-AES with local constant temperature system, is very different on the method for operating of instrument, and its feature is:
1. at present the order ICP-AES that sells of merchant is carrying out before the elementary composition analysis, all will be to every spectrum line trace or scanning to seek the peak position of spectrum line.The shortcoming of this method of operating is, original only the need measured a peak light intensity in the spectrum line peak position, became will be on 10-20 some photometry spectral line light intensity, by relatively the largest light intensity value being decided to be the peak light intensity, thus the spectral line peak position of definite this spectrum line.Just can carry out the mensuration of peak light intensity and the measurement of elementary composition after finding the peak position of every spectrum line.
2. automatically the order ICP-AES of wavelength calibration need only spectral line of trace, find out its spectrum line peak position after, all other real-time peak positions of spectral line of analyzing spectrum lines can both be calculated by automatic wavelength calibration device.So the order ICP-AES of wavelength calibration need not every spectrum line is scanned or trace automatically, can directly measure the peak light intensity of every spectrum line, directly carries out the elementary composition analysis.Automatically the order ICP-AES spectrometer of wavelength calibration is because of having the new function of automatic wavelength calibration, therefore in operation, have quick, save time, the characteristics of power saving.
3. the order ICP-AES that various merchants sell mostly in carrying out sample the elementary composition analysis all wanted preheating 8-10 hour in the past.And the order ICP-AES of wavelength calibration need not preheating automatically.
The present invention has fixed point and scan-type measurement function, can reduce environmental factor effectively and change the skew of caused spectral line peak.
Below in conjunction with drawings and Examples technical scheme of the present invention is further described.
Fig. 1. the schematic diagram of local constant temperature system;
Fig. 2. the structural drawing of the order inductively-coupled plasma spectrometer of the automatic wavelength calibration of the present invention;
Function relation curve between skew of Fig. 3 .JY38 ICP-AES spectral line peak and the wavelength;
Function relation curve between skew of Fig. 4 .JY38 ICP-AES spectral line peak and the temperature;
Fig. 5. the process flow diagram of the automatic wavelength calibration subroutine of the present invention.
1. well heater 2. electric fans 3. spectroscopes 4. cycling hot air-flows 5. heat insulation layers
6. plasma torch pipe 7. induction coils 8. plasma torch flames 9. matching systems
10.RF generator 11. air-path control systems 12. sampling systems 13. analytic sample solution
14. incident light illumination system 15. monochromators, 16. photomultipliers
17. measuring system and control system 18. computing machines, master routine and wavelength calibration subroutine
19. display 20. keyboards 21. printers 22. logical drive systems
23. grating 25. temperature sensors of electromechanical assembly 24. monochromators of rotating grating
26. the amplifying circuit in the constant current source 27. temperature sensor interface plates in the temperature sensor interface plate
28. the interface circuit in the A/D change-over circuit 29. temperature sensor interface plates in the temperature sensor interface plate
30. the interface board of exit slit 32. temperature sensors of entrance slit 31. monochromators of monochromator
Under different measurement patterns, relatively use automatic wavelength calibration device and the order ICP-AES that does not use automatic wavelength calibration device to measure the analysis result of the elementary composition in the various standard substances.Table 1-1 has provided 6751 sintering deposit standard specimens, table 1-2 has provided BH0124-5 blast furnace slag standard specimen, and table 1-3 has provided the analysis result of five kinds of elementary compositions in the 7114 blast furnace slag standard specimens.
Table 1-1
| Measurement pattern | Elemental composition | |||||
| SiO 2／％ | MnO／％ | MgO／％ | Al 2O 3／％ | CaO／％ | ||
| The trace method | Single element is measured (RSD) | 11．79 (0．7) | 0．32 (0．4) | 3．77 (0．6) | 0．94 (0．1) | 14．97 (0．4) |
| Multielement proceeding measurement (RSD) | 11．99 (0．4) | 0．32 (0．1) | 3．76 (1．6) | 1．04 (0．5) | 15．12 (1．4) | |
| The scanning survey method | Single element is measured (RSD) | 11．89 (0．2) | 0．32 (0．1) | 3．79 (0．7) | 0．99 (0．4) | 15．72 (0．4) |
| Multielement proceeding measurement (RSD) | 11．79 (0．4) | 0．31 (0．4) | 3．76 (0．3) | 0．91 (0．1) | 15．08 (0．3) | |
| Automatic wavelength calibration method | Single element is measured (RSD) | 11．87 (0．3) | 0．32 (0．1) | 3．77 (0．4) | 0．94 (0．1) | 14．95 (0．6) |
| Multielement proceeding measurement (RSD) | 11．81 (0．3) | 0．32 (0．4) | 3．71 (1．1) | 1．06 (0．4) | 15．25 (0．7) | |
| Standard specimen evaluation value | 11．57 | ?0．31 | ?3．73 | ?0．94 | ?14．95 | |
Table 1-2
| Measurement pattern | Elemental composition | |||||
| SiO 2／％ | MnO／％ | MgO／％ | A1 2O 3／％ | CaO／％ | ||
| The trace method | Single element is measured (RSD) | 40．23 (0．4) | 0．092 (0．1) | 8．06 (0．0) | 8．72 (0．3) | 40．66 (0．2) |
| Multielement proceeding measurement (RSD) | 40．96 (0．5) | 0．093 (0．2) | 8．09 (0．7) | 8．79 (0．4) | 41．17 (1．0) | |
| The scanning survey method | Single element is measured (RSD) | 40．17 (0．6) | 0．084 (0．4) | 8．03 (0．6) | 8．97 (0．2) | 40．70 (0．5) |
| Multielement proceeding measurement (RSD) | 40．61 (0．6) | 0．091 (0．3) | 8．14 (0．4) | 9．06 (0．1) | 40．92 (0．9) | |
| Automatic wavelength calibration method | Single element is measured (RSD) | 40．61 (0．7) | 0．091 (0．3) | 8．09 (0．7) | 8．76 (0．3) | 40．64 (0．6) |
| Multielement proceeding measurement (RSD) | 40．67 (0．2) | 0．088 (0．3) | 7．98 (0．5) | 8．68 (0．4) | 40．99 (1．5) | |
| Standard specimen evaluation value | 40．30 | ?0．093 | ?7．97 | ?8．91 | ?40．64 | |
Table 1-3
| Measurement pattern | Elemental composition | |||||
| SiO 2／％ | MnO／％ | ?MgO／％ | Al 2O 3／％ | CaO／％ | ||
| The trace method | Single element is measured (RSD) | 29．37 (0．1) | 0．576 (0．3) | 6．66 (0．7) | 9．13 (0．1) | 40．68 (0．4) |
| Multielement proceeding measurement (RSD) | 30．07 (0．7) | 0．565 (0．5) | 6．63 (1．0) | 9．24 (0．5) | 41．12 (0．7) | |
| The scanning survey method | Single element is measured (RSD) | 29．03 (0．6) | 0．565 (0．3) | 6．56 (0．4) | 8．88 (0．1) | 40．06 (0．3) |
| Multielement proceeding measurement (RSD) | 30．37 (0．5) | 0．576 (0．2) | 6．78 (0．3) | 8．93 (0．3) | 41．44 (0．3) | |
| Automatic wavelength calibration method | Single element is measured (RSD) | 30．15 (1．0) | 0．576 (0．2) | 6．72 (0．3) | 9．22 (0．1) | 41．28 (0．1) |
| Multielement proceeding measurement (RS D) | 29．84 (0．5) | 0．565 (0．4) | 6．59 (0．1) | 9．13 (0．5) | 40．80 (1．1) | |
| Standard specimen evaluation value | 29．71 | 0．576 | 6．86 | 9．16 | 41．16 | |
As can be seen, under above six kinds of measurement patterns, the precision of measurement of various measurement patterns is all about 1%, and the single element one-point measurement is than the well about 0.1-0.3% of the precision of multielement proceeding measurement.Trace method and about 1% with the relative error of the analysis result of the single element one-point measurement of automatic wavelength calibration device and standard specimen evaluation value, the relative error about 2% of scanning survey method analysis result and standard specimen evaluation value.Measuring accuracy when adopting automatic wavelength calibration device and accuracy and classical trace method are suitable, analysis result is basically identical also, be better than the scanning survey method, this explanation, automatically the order ICP-AES of wavelength calibration both just also can carry out elementary composition analysis accurately under the condition of not using local constant temperature system, and can carry out the elementary composition analysis with the traditional trace method of one-point measurement pattern replacement.Order ICP-AES with automatic wavelength calibration carries out the elementary composition analysis, and is simple to operate, quick.Table 1-4 has provided under above six kinds of measurement patterns, measures the inferior time spent of 30 elements relatively.Obviously, the trace method with the order ICP-AES of automatic wavelength calibration device during than wavelength calibration device automatically will be economized one times of time, saves time about five times than scanning method.
Table 1-4
Embodiment 2.
| Analytical approach | Measurement pattern | Total time spent/second (30 elements are inferior) | The average time spent (second/element) |
| The trace method | The single element one-point measurement | 1500 | 50 |
| The multielement proceeding measurement | 1200 | 40 | |
| Automatically wavelength calibration | The single element one-point measurement | 900 | 30 |
| The multielement proceeding measurement | 720 | 24 | |
| Scanning method | The single element scanning survey | 3300 | 110 |
| The multielement proceeding measurement | 4200 | 140 |
The present invention is applied in automatic wavelength calibration device on the JY38 PLUS order ICP-AES.Fig. 3 has provided the spectral line peak shifted by delta λ that records on JY38 PLUS order ICP-AES
WAnd the function relation curve between the wavelength variations λ, R are related coefficient, temperature value T=22.4 ± 0.1 ℃.The polynomial equation of this curve is shown below:
Δ λ
W=A
0+ A
1λ+A
2λ
2+ A
3λ
3+ A
4λ
4+ A
5λ
5(1) wherein: A
0=-14.864
A
1=0．181
A
2=-8．74E-4
A
3=2．105E-6
A
4=-2．516E-9
A
5=1．179E-12
R=0．9998
The calculating of polynomial equation (1) coefficient is: 9 wavelength value λ that utilize 9 different wave length spectrum lines
i, measure their corresponding 9 spectral line peak offset value delta λ by experiment
i, with 9 groups of λ
i, Δ λ
iValue substitution normal equations:
(∑0)A
0+(∑1)A
1+(∑2)A
2+……+(∑M)A
M=∑Δλ01
(∑1)A
0+(∑2)A
1+(∑3)A
2+……+(∑M+1)A
M=∑Δλ11
(∑2)A
0+(∑3)A
1+(∑4)A
2+……+(∑M+2)A
M=∑Δλ21
(∑ M) A
0+ (∑ M+1) A
1+ (∑ M+2) A
2+ ... + (∑ M+M) A
M=∑ Δ λ M1 wherein
Through calculating the coefficient A that can obtain polynomial equation (1)
0, A
1, A
2, A
3, A
4, A
5, it is worth as previously shown.
Fig. 4 has provided the spectral line peak shifted by delta λ that records on JY38 PLUS order ICP-AES
TAnd the function relation curve between the temperature variation T.R is a related coefficient, and used spectrum line is Hg435.8nm.The polynomial equation of this curve is shown below:
Δ λ
T=A
0+ A
1T+A
2T
2+ A
3T
3+ A
4T
4+ A
5T
5(2) wherein the coefficient of polynomial equation (2) is respectively:
A
0=3．861
A
1=-0．958
A
2=0．891E-1
A
3=-0．410E-2
A
4=9．474E-5
A
5=-8．676E-7
R=0．9996
The calculating of polynomial equation (2) coefficient is: the temperature value T that utilizes 37 temperature spots
i, measure their corresponding 37 spectral line peak offset value delta λ by experiment
i, with 37 groups of T
i, Δ λ
iValue substitution normal equations:
(∑0)A
0+(∑1)A
1+(∑2)A
2+……+(ΣM)A
M=∑Δλ01
(∑1)A
0+(∑2)A
1+(∑3)A
2+……+(∑M+1)A
M=∑Δλ11
(∑2)A
0+(∑3)A
1+(∑4)A
2+……+(∑M+2)A
M=∑Δλ21
(∑ M) A
0+ (∑ M+1) A
1+ (∑ M+2) A
2+ ... + (∑ M+M) A
M=∑ Δ λ M1 wherein
Through calculating the coefficient A that can obtain polynomial equation (2)
0, A
1, A
2, A
3, A
4, A
5, it is worth as previously shown.According to above two polynomial equations, with the VB language compilation wavelength calibration subroutine of JY38 PLUS order ICP-AES, and the wavelength calibration subroutine is organized in the order inductively-coupled plasma spectrometer computer program in advance, temperature sensor places in the cabinet of monochromator, the temperature sensor interface plate that is connected with temperature sensor by parallel interface and lead is inserted in the groove of computer motherboard, and it has been transformed into the order ICP-AES of an automatic wavelength calibration.
Automatically the temperature sensor of wavelength calibration device constantly with the interface circuit of real-time temperature value T by amplifying circuit, A/D transducer and temperature sensor, is imported computing machine, and temperature measurement accuracy is ± 0.02 ℃.Wavelength calibration subroutine so that equation (1,2) is write in advance for the basis is stored in the computing machine.The wavelength calibration subroutine calculates real-time tuning wavelength value λ according to temperature value T and operator wavelength selected value λ from database of input
1, photo gate driver is according to λ
1Value is revised the rotation of grating, makes the peak position of every analytical line in proper order, accurately pass through exit slit, and accurately measures their peak light intensity.
The order JY38 ICP-AES that table 2 has provided improved automatic wavelength calibration measures the analysis result of six kinds of elementary compositions in the BH0124-4 blast furnace slag standard specimen:
Table 2
| Elemental composition | SiO 2 | ?MnO | ?Tfe | ?MgO | ?Al 2O 3 | ?CaO |
| Measured value/% RSD/% | 36．9 0．5 | ?0．29 ?0．4 | ?0．20 ?0．1 | ?3．5 ?0．3 | ?10．7 ?0．3 | ?44．6 ?0．1 |
| Evaluation value/% | 37．8 | ?0．29 | ?0．21 | ?3．5 | ?11．0 | ?45．5 |
Annotate: the RSD value in the table is the relative standard deviation of 3 measurement results.
From above data as can be seen, the standard specimen measured value of the order JY38 ICP-AES of automatic wavelength calibration and the evaluation value basically identical of standard specimen.Precision of measurement RSD about 1%.
Order JY38 ICP-AES with automatic wavelength calibration has carried out the spectral line trace to ten analytical lines, and table 3 has provided real-time spectral line trace value λ
2, the automatic calculated value λ of wavelength calibration device
1And the difference DELTA λ between them:
Table 3
| Element | Standard wavelength λ/nm | Tuning wavelength λ 1／nm | The trace wavelength X 2／nm | △λ=λ 2-λ 1????／nm |
| ????Al | ????309．271 | ????309．320 | ????309．320 | ????0．000 |
| ????Ba | ????455．403 | ????455．346 | ????455．350 | ????0．004 |
| ????Ca | ????422．673 | ????422．718 | ????422．716 | ????-O．002 |
| ????Cu | ????324．754 | ????324．782 | ????324．780 | ????-0．002 |
| ????Fe | ????259．940 | ????259．930 | ????259．932 | ????O．002 |
| ?Mn | ?257．6lO | ?257．608 | ?257．608 | ????O．000 |
| ????Pb | ????283．306 | ????283．286 | ????283．288 | ????0．002 |
| ????Si | ????251．611 | ????251．572 | ????251．574 | ????0．002 |
| ????Sn | ????283．399 | ????283．982 | ????283．984 | ????0．002 |
| ????Y | ????371．030 | ????371．096 | ????371．094 | ????-0．002 |
In addition, in the different time, under the different environment temperatures, measured the tuning wavelength and the actual trace wavelength of Fe 259.940nm analytical line.Measurement data sees Table 4:
Table 4.
| Time | Standard wavelength λ/nm | Tuning wavelength λ 1/nm | The trace wavelength X 2/nm | △λ＝λ 2-λ 1 1/nm |
| Measure for the first time | 259.940 | 299.930 | 259.932 | 0.002 |
| Measure for the second time | 259.940 | 259.910 | 259.912 | 0.002 |
From table 3,4 as can be seen, the tuning wavelength that the wavelength calibration subroutine is calculated and the real-time trace peak position basically identical of analytical line, and difference DELTA λ is less than ± 0.005nm.This order ICP-AES peak-seeking that automatic wavelength calibration of the present invention is described is accurate, rapid, can carry out the elementary composition analysis under the condition of the trace method of not using traditional local constant temperature system, classics or scanning survey method.Embodiment 4.
With elementary composition analysis in the BH0124-4 blast furnace slag standard specimen in the table 2 is example.
Start automatic wavelength calibration subroutine, access Si from database, Mn, Fe, Mg, Al, six analytical lines of six elements of Ca, its wavelength value is respectively Si 251.6nm, Mn 257.6nm, Fe 259.9nm, Mg 280.3nm, Ca 317.9nm, Al 396.1nm, and from the real-time temperature value T of automatic wavelength calibration device input.If order ICP-AES moves for the first time automatic wavelength calibration subroutine after the energized, just need carry out the spectrum line trace to the spectrum line Al 396.1nm that fixes earlier, and according to real-time temperature value to the Δ λ in polynomial equation 1 and 2
W, Δ λ
TValue is revised.If order ICP-AES has operated a period of time, Al396.1nm was carried out the spectrum line trace, so just need not carry out above operation steps again, can directly carry out wavelength calibration (from article one spectrum line Si 251.6nm) to analytical line successively.
At first consider to carry out Al 396.1nm spectrum line the situation of trace: the wavelength value λ of input trace spectrum line
M=396.152nm measures its spectrum line peak position λ then to Al 396.152nm spectrum line trace
MAXIf λ
MAXValue is zero, then returns trace again.If non-vanishing, as then to calculate λ
MThe real-time spectral line peak shifted by delta λ of spectrum line
M, Δ λ
M=λ
MAX-λ
MIf Δ λ
MValue has surpassed permissible value greater than 1nm, and also need return this moment, carries out the spectral line trace of Al 396.1nm spectrum line again.If be no more than 1nm, or allow it to surpass 1nm under special circumstances, will carry out next step, two polynomial equation formulas are revised.
At first polynomial equation formula 1 is revised: utilize polynomial equation formula 1 to calculate the spectral line peak shifted by delta λ of Al 396.152nm
M1Thereby, draw Δ λ in the polynomial equation formula 1
WModified value Δ λ
WD=Δ λ
M-Δ λ
M1
Then polynomial equation formula 2 is revised:, obtain its spectrum line peak offset value delta λ the wavelength value substitution polynomial equation formula 1 of hg spectrum line 435.8nm
HG=0.031nm, and real-time peak shifted by delta λ
HG+ Δ λ
WDUtilize polynomial equation formula 2 to obtain the pairing spectral line of mercury 435.8nm spectrum line peak calculations of offset value Δ λ under the real time temperature value T again
TMThereby, obtain Δ λ in the polynomial equation formula 2
TModified value Δ λ
TW=Δ λ
HG+ Δ λ
WD-Δ λ
TMSo far, finish to the spectral line trace of Al 396.1nm spectrum line and to the correction work of two polynomial equation formulas.Below begin six analytical lines are carried out the wavelength correction.
Six analytical line λ (I) are carried out wavelength calibration: begin to the correction that circulates of the maximal value 6 of I from I=1.During I=1.Utilize polynomial equation formula 1 to obtain the spectral line peak offset value delta λ of λ (1)=251.6nm
1(1)=-0.018nm, and real-time peak shifted by delta λ
1(1)+Δ λ
WD, the correction wavelength X of λ (1) then
1(1)=λ (1)+Δ λ
1(1)+Δ λ
WDIn order to improve the precision of wavelength calibration, before being carried out wavelength calibration, next bar analytical line imports one time real time temperature value T again
2, so that polynomial equation formula 1 is once revised again.Utilize polynomial equation formula 2 to obtain real time temperature value T
2Spectral line peak offset value delta λ
TMIAnd real-time peak shifted by delta λ
TMI+ Δ λ
TWThereby, can calculate the real-time modified value Δ λ of polynomial equation formula 1
WI=Δ λ
TMI+ Δ λ
TW-Δ λ
HG, and with Δ λ
WIValue is given Δ λ
WDSo analogize, to 6 analytical line circulation carrying out wavelength calibrations.When I 〉=6, circulation correction is finished, and six of λ (I) are revised wavelength value λ
1(1), λ
1(2), λ
1(3), λ
1(4), λ
1(5), λ
1(6) return data storehouse, the wavelength calibration subprogram activation finishes automatically.
Automatically the master routine of the order ICP-AES of wavelength calibration is revised wavelength value λ with these six
1(I) flow to the drive system of the electromechanical assembly of the control system of this instrument and rotating grating, drive system is according to λ
1(I) value is revised the rotation of grating, makes the peak position of six spectrum lines of λ (I) pass through exit slit successively exactly.Photomultiplier is measured six peak light intensity values of these six spectrum lines successively on the peak position.
Automatically the master routine of the order ICP-AES of wavelength calibration utilizes each concentration of element value in the standard model solution of importing again from keyboard or database, and the light intensity value of these ultimate analysis lines of measuring of measuring system, with the light intensity is ordinate, the concentration of element value is a horizontal ordinate, makes the working curve of each analytical element spectrum line.Utilize the working curve of these analytical lines, according to measured λ
1The peak light intensity value of six spectrum lines (I), the concentration value that can calculate six elements to be measured in the BH0124-4 blast furnace slag sample solution successively on corresponding analytical line working curve divides other to be SiO
2=36.9%, MnO=0.29%, TFe=0.20%, MgO=3.5%, CaO=44.6%, Al
2O
3=10.7%.
Claims (4)
1. the order inductively-coupled plasma spectrometer of an automatic wavelength calibration, comprise grating monochromator, incident light illumination system, photomultiplier PMT, control system, photometric system, the electromechanical assembly of rotating grating, the logical drive system, the RF generator, matching system, sampling system, air-path control system, induction coil, the plasma torch pipe, the plasma torch flame, computing machine, display, keyboard, printer and computing machine master routine, it is characterized in that: in this spectrometer, the one automatic wavelength calibration device that is connected with lead with grating monochromator and computing machine is arranged, be provided with temperature sensor in this means for correcting, it is positioned at the cabinet of grating monochromator, be connected with the interface board of temperature sensor by interface and lead, the temperature sensor interface plate is inserted in the groove of computer motherboard, and the wavelength calibration subroutine is organized in this spectrometer computer program in advance.
2. the order inductively-coupled plasma spectrometer of automatic wavelength calibration as claimed in claim 1 is characterized in that the interface board of described temperature sensor is made up of constant-current source circuit, amplifying circuit, A/D change-over circuit and interface circuit.
3. automatic wavelength calibration method as the order inductively-coupled plasma spectrometer of the described automatic wavelength calibration of claim 1～2, comprise: by the RF generator, matching system, air-path control system, sampling system, induction coil, the plasma torch pipe, the characteristic emission spectrum of the various elements that the plasma torch flame is produced, the beam split of the grating monochromator by incident light illumination system and the control of logical drive system, make the analytical line of analytical element can pass through exit slit successively exactly, and imaging is on the photocathode of photomultiplier, the electric signal of analytical line light intensity is input in the computing machine through measuring system, the computing machine master routine obtains each concentration of element value the standard model by keyboard or from database, and the light intensity value of each analytical line of measuring system input, and be respectively ordinate and abscissa with standard specimen concentration and analytical line peak light intensity, draw the pairing working curve of each analytical line, after measuring the light intensity value of each elemental characteristic analytical line in the testing sample, on working curve, calculate the concentration value of each element to be measured in the sample solution successively, it is characterized in that: after so-called spectral analysis line is the correction of the automatic wavelength calibration device of analysis of line wavelength value process by exit slit successively exactly, make selected analytical line pass through exit slit, be the interface board of temperature sensor by temperature sensor, constantly send the real time temperature value in the monochromator chamber to the wavelength calibration subroutine, the real time temperature value T of the interface board input by the analytical line standard wave long value λ that from database, selects and temperature sensor, calculate each analytical line spectral line peak shifted by delta λ, and revise wavelength value λ
1λ
1Be fed to control system and drive system, drive unit stops the spectral line peak position of analytical line according to the rotation of this value correction grating successively exactly on exit slit, measure each analytical line peak light intensity exactly.
4. the automatic wavelength calibration method of the order inductively-coupled plasma spectrometer of automatic wavelength calibration as claimed in claim 3, it is characterized in that described automatic wavelength calibration subroutine is: access I bar analytical line and respective wavelength value λ (I) thereof from database, and import real-time temperature value T from the interface board of temperature sensor; If be to move automatic wavelength calibration subroutine for the first time after the order ICP-AES start, just need carry out the spectrum line trace to the fixing spectrum line of certain bar earlier, and polynomial equation (1) is reached Δ λ in (2) according to real-time temperature value T
W, Δ λ
TValue is revised; If ICP-AES has moved a period of time, this fixing spectrum line was carried out the spectrum line trace, with regard to successively analytical line directly being carried out wavelength calibration, promptly from I=1;
When the fixing spectrum line of certain bar is carried out trace: the wavelength value λ of input trace spectrum line
M, and to λ
MTrace is measured its spectrum line peak position λ
MAXCalculate λ
MThe real-time spectral line peak shifted by delta λ of spectrum line
M, Δ λ wherein
M=λ
MAX-λ
MNext step will be revised two polynomial equation formulas;
At first polynomial equation formula (1) is revised: utilize polynomial equation formula (1) to calculate λ
MSpectral line peak shifted by delta λ
M1Thereby, draw Δ λ in the polynomial equation formula (1)
WModified value Δ λ
WD=Δ λ
M-Δ λ
M1Then polynomial equation formula (2) is revised:, obtain its spectrum line peak offset value delta λ the wavelength value substitution polynomial equation formula (1) of hg spectrum line 435.8nm
HGAnd real-time peak shifted by delta λ
HG+ Δ λ
WDUtilize polynomial equation formula (2) to obtain the pairing spectral line of real time temperature value T peak calculations of offset value Δ λ again
TMThereby, obtain Δ λ in the polynomial equation formula (2)
TModified value Δ λ
TW=Δ λ
HG+ Δ λ
WD-Δ λ
TMSo far, finish, begin I bar analytical line is carried out the wavelength correction to the spectral line trace of the fixing spectrum line of certain bar and to the correction work of two polynomial equation formulas;
I bar analytical line λ (I) is carried out wavelength calibration: begin during I=1, to utilize polynomial equation formula (1) to obtain the spectral line peak offset value delta λ of λ (1) to the correction that circulates of the maximal value of I from I=1
1(1) and in real time peak offset value delta λ
1(1)+Δ λ
WD, the correction wavelength X of λ (1) then
1(1)=λ (1)+Δ λ
1(1)+Δ λ
WDBefore being carried out wavelength calibration, next bar analytical line gathers real time temperature T again one time
I, utilize polynomial equation formula (2) to obtain real time temperature value T
IThe spectral line peak offset value delta λ of following hg spectrum line 435.8nm
TMIAnd real-time peak shifted by delta λ
TMI+ Δ λ
TWThereby, calculate the real-time modified value Δ λ of polynomial equation formula (1)
WI=Δ λ
TMI+ Δ λ
TW-Δ λ
HG, and with Δ λ
WIValue is given Δ λ
WDSo analogize, to I bar analytical line circulation carrying out wavelength calibration; When I 〉=analytical line total, circulation correction is finished, with the I bar correction wavelength value λ of λ (I)
1(I) return data storehouse, the wavelength calibration subprogram activation finishes automatically.
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|---|---|---|---|
| CN 99119642 CN1117971C (en) | 1999-09-23 | 1999-09-23 | Sequentially inductor coupled plasma spectrometer with automatic wavelength correction and its application method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99119642 CN1117971C (en) | 1999-09-23 | 1999-09-23 | Sequentially inductor coupled plasma spectrometer with automatic wavelength correction and its application method |
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| Publication Number | Publication Date |
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| CN1117971C CN1117971C (en) | 2003-08-13 |
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|---|---|---|---|
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102023135A (en) * | 2010-11-19 | 2011-04-20 | 中国航空工业集团公司北京航空材料研究院 | Method for analyzing slanting peak locating spectrum |
| CN101576498B (en) * | 2009-06-23 | 2011-06-15 | 中国船舶重工集团公司第十二研究所 | Method for analyzing and detecting alloying elements in beryllium-aluminum alloy |
| CN103226095A (en) * | 2013-04-08 | 2013-07-31 | 南京国电环保科技有限公司 | Fast calibration method of spectrometer wavelength |
| CN104949962A (en) * | 2014-03-25 | 2015-09-30 | 日本株式会社日立高新技术科学 | ICP atomic emission spectrophotometer |
| CN106018383A (en) * | 2015-03-31 | 2016-10-12 | 日本株式会社日立高新技术科学 | Sequential ICP optical emission spectrometer and method for correcting measurement wavelength |
| CN110780021A (en) * | 2019-10-30 | 2020-02-11 | 广船国际有限公司 | Method and device for determining standard substance, terminal and storage medium |
| CN114127540A (en) * | 2019-07-31 | 2022-03-01 | 塞莫费雪科学（不来梅）有限公司 | Peak determination in two-dimensional spectra |
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1999
- 1999-09-23 CN CN 99119642 patent/CN1117971C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101576498B (en) * | 2009-06-23 | 2011-06-15 | 中国船舶重工集团公司第十二研究所 | Method for analyzing and detecting alloying elements in beryllium-aluminum alloy |
| CN102023135A (en) * | 2010-11-19 | 2011-04-20 | 中国航空工业集团公司北京航空材料研究院 | Method for analyzing slanting peak locating spectrum |
| CN103226095A (en) * | 2013-04-08 | 2013-07-31 | 南京国电环保科技有限公司 | Fast calibration method of spectrometer wavelength |
| CN103226095B (en) * | 2013-04-08 | 2014-12-24 | 南京国电环保科技有限公司 | Calibration method of spectrometer wavelength |
| CN104949962A (en) * | 2014-03-25 | 2015-09-30 | 日本株式会社日立高新技术科学 | ICP atomic emission spectrophotometer |
| CN106018383A (en) * | 2015-03-31 | 2016-10-12 | 日本株式会社日立高新技术科学 | Sequential ICP optical emission spectrometer and method for correcting measurement wavelength |
| CN106018383B (en) * | 2015-03-31 | 2020-07-24 | 日本株式会社日立高新技术科学 | Sequential ICP emission spectrometer and measurement wavelength correction method |
| CN114127540A (en) * | 2019-07-31 | 2022-03-01 | 塞莫费雪科学（不来梅）有限公司 | Peak determination in two-dimensional spectra |
| CN110780021A (en) * | 2019-10-30 | 2020-02-11 | 广船国际有限公司 | Method and device for determining standard substance, terminal and storage medium |
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