CN109187369A - A kind of oil plant detection device and detection method applying associated detection technique - Google Patents
A kind of oil plant detection device and detection method applying associated detection technique Download PDFInfo
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- CN109187369A CN109187369A CN201810876562.0A CN201810876562A CN109187369A CN 109187369 A CN109187369 A CN 109187369A CN 201810876562 A CN201810876562 A CN 201810876562A CN 109187369 A CN109187369 A CN 109187369A
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Abstract
The present invention relates to oil plant detection field, especially a kind of oil plant detection device for applying associated detection technique and detection scheme, the oil plant detection device include: excitation component, transfer element, incident eyeglass, grating, photo-electric conversion element and computer；The optical conversion component packet photomultiplier tube and CDD detector, the photomultiplier tube are used to receive and convert the spectrum of multielement threadiness and band spectrum region；The photomultiplier tube is used to receive and convert the spectrum in the region that other need to receive and convert monochromatic spectrum.The present invention is used ccd detector and photomultiplier tube connected applications, the photo-electric conversion element of different type and characteristic is set according to the spectra1 interfer- situation of different zones, other component spectrum interference bring measurement errors can utmostly be avoided, it again can be in the case where guaranteeing compared with high detection sensitivity, measurement range is utmostly improved, precision is improved.
Description
Technical field
The present invention relates to oil plant detection field, especially a kind of oil plant detection device and inspection for applying associated detection technique
Survey scheme.
Background technique
In fields such as atomic spectroscopic analysis, graduating spectroscopy, metering and detections, it is often necessary to occupy to the element of sample and
Its content is analyzed.Traditional spectroscopic analysis methods have: spectra methods mainly has atomic emission spectrometry, atomic absorption light
Spectrometry, UV-Vis Spectrophotometry, red well spectroscopic methodology etc..
With the continuous development of science and technology, oil plant is analyzed using spectrometer also more more and more universal.Existing spectrum glaze
Expect the principle of analysis, i.e. analyzed oil sample excites in the analytical gap of excitation chamber, and then the light of oil sample transmitting passes through optics
Fiber transmission, is introduced to entrance slit, is then divided into various different wave lengths after light reaches grating by incident eyeglass
Spectral line, different spectral lines are divided into the spectral line corresponding to each element in the exit slit focused on curved surface: the focusing curved surface
Photoelectric conversion element is set below, so that luminous energy is become electric energy.In each burning correct time interval will be pressed with electric current
Operation forms the voltage directly proportional to the received light quantity of photoelectric conversion element.This voltage is converted into number by reading circuit
It is worth, the standard curve data comparison stored in measured result and computer can calculate the concentration of element, last entirely to divide
Analysis result shows on the computer screen or is got with printer.
Conventional atom emission spectrum oil content analyzer uses multichannel photomultiplier tube as detector device, although photomultiplier tube has
The features such as having dynamic range big, meeting international standard, but big region, photomultiplier transit are interfered in multielement threadiness and band spectrum
Sense not can avoid other elements spectra1 interfer-, and then the detection error that bring is very big；Therefore existing oil plant detection how is improved
The detection accuracy of device has great importance in this field.
Summary of the invention
In view of the foregoing drawbacks, it is an object of the invention to propose that one kind applies associated detection technique testing result is had
The detection method for having the oil plant detection device of more high measurement accuracy and oil plant being detected using it.
To achieve this purpose, the present invention adopts the following technical scheme:
A kind of oil plant detection device applying associated detection technique comprising: excitation oil sample transmitting characteristic spectrum swashs
Send out component, and the transfer element, incident eyeglass, grating, photo-electric conversion element and the calculating that are successively arranged along spectral transmissions direction
Machine；The transfer element is used to for the spectrum that the excitation component is launched being collected, and transmits injection to the incident mirror
The incidence surface of piece；The grating is set to the light-emitting surface downstream of the incident eyeglass, by the characteristic spectrum color at multiple lists
Color spectrum；The computer is electrically connected in the photo-electric conversion element, records and analyze the electric signal.
More preferably, the optical conversion component includes multiple photomultiplier tubes and CDD detector, the optical conversion component
It is distributed in the injection direction of monochromatic spectrum at arc-shaped, receive each monochromatic spectrum and converts it into electric signal；The photoelectricity times
Increase pipe for receiving and converting the spectrum of multielement threadiness and band spectrum region；The photomultiplier tube is for receiving and converting
Other need to receive and convert the spectrum in the region of monochromatic spectrum.
More preferably, the receiving area of the photo-electric conversion element is divided into zero level optical signal receiving area and non-zero order optical signal
Receiving area；Zero level optical signal receiving area is equipped with diode pump integrator；The diode pump integrator includes photo-diode
Pipe and the integrating counting circuit electrically connected with the photodiode.
More preferably, the photomultiplier tube and CDD detector are all set in non-zero order optical signal receiving area.
More preferably, it is concave grating rowland circle spectrometer that the high-precision cremate light source atomic emission spectrum, which surveys oily device,
The incidence eyeglass, grating and photo-electric conversion element are all set in above Rowland circle, and the grating is concave grating.
More preferably, the transfer element is optical fiber, and the transmitting terminal of the transfer element is set to above the Rowland circle；Institute
Incident eyeglass is stated to be set to above the Rowland circle by angle adjustment device.
Specifically, the excitation component includes: high voltage power supply, metal bar positive electrode and rosette negative electrode；The height
Voltage source is controlled by the computer；The metal bar positive electrode is electrically connected by electric wire with the high voltage power supply, the metal
Disk negative electrode is located at in the oil plant tested and analyzed.
Using a kind of detection method for the oil plant detection device for applying associated detection technique as described above comprising such as
Lower step:
A. the oil sample that analysis to be detected is excited using excitation component, generates characteristic spectrum；
B. characteristic spectrum is penetrated into incident eyeglass, directive grating by transfer element；
C. characteristic spectrum is diffracted into multiple monochromatic spectrums, and directive photo-electric conversion element by grating；
D. the angle of incident eyeglass is adjusted, so that multielement threadiness and band spectrum are incident upon equipped with CDD spy in monochromatic spectrum
Survey the region of device；Other need to receive and convert monochromatic spectrum and be incident upon the region equipped with photomultiplier tube；So that monochromatic spectrum is non-
Zero level optical signal is projected to the non-zero order region of the photo-electric conversion element, obtains just slightly detecting spectrum electric signal, so that monochromatic
The zero level optical signal of spectrum is projected to the zero level region of the photo-electric conversion element, by photodiode and integral calculation electricity
Road obtains intensity electrical signals；
E. computer just slightly will detect spectrum electric signal and intensity electrical signals are normalized, and obtain monochromatic spectrum
Exact value.
More preferably, the detection method further includes following steps: f. adjusts incident lens angle deflection first, makes characteristic light
Spectrum deflects out the range of grating, and photo-electric conversion element receives the spectral information of bias light at this time, obtains bias light interference information；
The operation is repeated, until the background interference information of all monochromatic spectrums is recorded by computer.
More preferably, above-mentioned steps d and f and further include following steps in no particular order: g. as unit of each monochromatic spectrum,
From the background interference information rejected in the step f in the exact value in the step e, the inspection of all monochromatic spectrums is finally obtained
Measured value.
More preferably, the detection method further includes into school step: h. incidence eyeglass is micro- by the carry out controlled from computer
Small angular deflection；Adjusting incident eyeglass is best angle, is penetrating target monochromatic spectrum just in corresponding photo-electric conversion element,
Monochromatic spectrum is set to reach the most intensity values of analysis；Photo-electric conversion element, which receives target monochromatic spectrum and is converted to electric signal, is sent to meter
Calculation machine is analyzed and recorded: computer records different monochromatic spectrums and just penetrates the different angle most believed by force, and with obtained in the step d
Strength signal be combined analysis, and then correct the unstability of the cremate light source of excitation component.
The present invention is used ccd detector and photomultiplier tube connected applications, is interfered in multielement threadiness and band spectrum
Big region carries out spectrum survey using linear array CCD and detects, and other regions small in spectra1 interfer-, such as chromium and sodium
The SPECTRAL REGION of element is detected using the photomultiplier tube of high dynamic range, can utmostly avoid other component spectrums dry
Bring measurement error is disturbed, and can utmostly improve measurement range in the case where guaranteeing compared with high detection sensitivity, is improved
Precision.
Detailed description of the invention
Fig. 1 is the work of one embodiment that heretofore described high-precision cremate light source atomic emission spectrum surveys oily device
Schematic illustration；
Structural schematic diagram when Fig. 2 is heretofore described photo-electric conversion element and grating cooperating；
Fig. 3 is the circuit connection diagram of one embodiment of heretofore described diode pump integrator.
Wherein: computer 1 excites component 2, high voltage power supply 21, metal bar positive electrode 22, rosette negative electrode 23, biography
Defeated element 3, incident eyeglass 4, grating 5, photo-electric conversion element 6, non-zero order optical signal receiving area 62, zero level optical signal reception area
Domain 63；Diode pump integrator 61, photodiode 611, integrating counting circuit 612, photomultiplier tube 621, CDD detector 622.
Specific embodiment
To further illustrate the technical scheme of the present invention below with reference to the accompanying drawings and specific embodiments.
As shown in Figure 1, a kind of oil plant detection device for applying associated detection technique comprising: excitation oil sample transmitting is special
Levy the excitation component 2 of spectrum, and the transfer element 3, the incident eyeglass 4, grating 5, photoelectricity that are successively arranged along spectral transmissions direction
Conversion element 6 and computer 1；The transfer element 3 is used to for the spectrum that the excitation component 2 is launched being collected, and passes
It is defeated to project to the incidence surface of the incident eyeglass 4；The grating 5 is set to the light-emitting surface downstream of the incident eyeglass 4, will be described
Characteristic spectrum color is at multiple monochromatic spectrums；The computer 1 is electrically connected in the photo-electric conversion element 6, records and analyze institute
State electric signal.More have, as shown in Fig. 2, the optical conversion component includes multiple photomultiplier tubes 621 and CDD detector
622, the optical conversion component is distributed in the injection direction of monochromatic spectrum at arc-shaped, receives each monochromatic spectrum and is converted
At electric signal；The photomultiplier tube 621 is used to receive and convert the spectrum of multielement threadiness and band spectrum region；The light
Electric multiplier tube 621 is used to receive and convert the spectrum in the region that other need to receive and convert monochromatic spectrum.
As shown in Figures 2 and 3, the receiving area of the photo-electric conversion element 6 is divided into zero level optical signal receiving area 63 and non-
Zero level optical signal receiving area 62；Zero level optical signal receiving area 63 is equipped with diode pump integrator 61；The diode product
Device 61 is divided to include photoelectric diode and the integrating counting circuit 612 electrically connected with the photodiode 611.Using being currently used for
The zero level optical signal that generation usually not acts at grating 5 in the spectrometer of oil plant is detected to improve detection accuracy, in zero level
Cooperate integrating counting circuit 612 using photodiode 611 at optical signal, so that the work of photodiode 611 is in integral mode
Under, it can detect excitation component 2 while detection elements emission spectrum signal rejects mushing error in spectral signal and swash
The overall strength of the cremate light collection signal of hair, is normalized, and then can correct sharp using this overall strength and spectral signal
Send out the unstability of cremate light source at component 2.
The photomultiplier tube 621 and CDD detector 622 are all set in non-zero order optical signal receiving area 62.Light
Monochromatic spectrum is converted into electric signal, and amplify the electric signal for receiving monochromatic spectrum by electric transition element 6.Photomultiplier tube
621 and CDD detector 622 is the photo-electric conversion element 6 for further increasing photoelectric sensitivity.Photomultiplier tube 621 and CDD detection
Device 622 can carry out highly sensitive and high-precision receiving and conversion for the optical signal of different situations, in actual use can root
According to the monochromatic spectrum situation that oil plant diffraction generates, the photo-electric conversion element 6 of simultaneous selection corresponding types further increases detection essence
Degree.
Classify according to optical texture, it is 5 sieve of concave grating that the high-precision cremate light source atomic emission spectrum, which surveys oily device,
Blue circle spectrometer, the incidence eyeglass 4, grating 5 and photo-electric conversion element 6 are all set in above Rowland circle, and the grating 5 is recessed
Concave grating 5.Incident eyeglass 4, grating 5 and photo-electric conversion element 6 are installed on the same Rowland circle, and compact-sized and relative position is more
Convenient for adjusting, furthermore grating 5 uses concave grating 5, on the one hand may make monochromatic spectrum scatter to be projected to arc-shaped setting
On photo-electric conversion element 6, on the other hand, is conducive to characteristic spectrum and carries out zero level signal and non-zero order signals disperse area after diffraction
It separates, convenient for the setting that photomultiplier tube 621, CDD detector 622 and photodiode 611 more disperse, guarantees photomultiplier transit
Pipe 621 or CDD detector 622 carry out reception conversion to monochromatic spectrum, and photodiode 611, which receive to zero level optical signal, to be turned
Change, monochromatic spectrum and zero level optical signal dispersion degree are bigger, and corresponding receiving area is separated by farther, can more preferably avoid between optical signal
Interfere with each other, further ensure the accuracy and consistency of infomation detection.
The transfer element 3 is optical fiber, and the transmitting terminal of the transfer element 3 is set to above the Rowland circle；It is described enter
Eyeglass 4 is penetrated to be set to above the Rowland circle by angle adjustment device.Because characteristic spectrum is projected to circle by 5 diffraction of grating
When on arcuation photo-electric conversion element 6, the crevice projection angle different to adjustment is needed in different detection process；The incidence eyeglass 4
It can be rotated around angle adjustment device, the specific embodiment of this angle adjustment device has very much, it is only necessary to so that institute
Stating incident eyeglass 4 can horizontally rotate on the Rowland circle, and rotatable incidence eyeglass 4 ensure that from transfer element 3
Angle adjustable between the light of injection and the plane of incidence of itself, so that 5 diffraction of grating is projected to the photoelectric conversion
The regional location and angle of monochromatic spectrum on element are also adjusted；Monochromatic spectrum and zero level letter in the practical operation of big broad aspect
Number reception conversion operation.
The excitation component 2 includes: high voltage power supply 21, metal bar positive electrode 22 and rosette negative electrode 23；The height
Voltage source 21 is controlled by the computer 1；The metal bar positive electrode 22 is electrically connected by electric wire with the high voltage power supply 21, institute
Rosette negative electrode 23 is stated to be located at in the oil plant tested and analyzed.Utilize rosette negative electrode 23 and metal bar positive electrode 22
Between high voltage power supply 21 by each element atom adding in oil sample to excite, institute's radiation feature light through the grating 5 be divided irradiate
Onto photomultiplier tube 621 corresponding with each element, the content of element is directly displayed after processing.2 structure of excitation component
Simply, and high voltage power supply 21 is controlled by computer 1, so that the excitation of excitation component 2 and the rotation of incident eyeglass 4 have
Synchronism, ensuring measurement structure control in this way, more accurately testing result precision is higher.
Using a kind of detection method of such as above-mentioned oil plant detection device for applying associated detection technique comprising as follows
Step:
A. the oil sample that analysis to be detected is excited using excitation component 2, generates characteristic spectrum；
B. characteristic spectrum is penetrated into incident eyeglass 4, directive grating 5 by transfer element 3；
C. characteristic spectrum is diffracted into multiple monochromatic spectrums, and directive photo-electric conversion element 6 by grating 5；
D. the angle of incident eyeglass 4 is adjusted, so that multielement threadiness and band spectrum are incident upon equipped with CDD spy in monochromatic spectrum
Survey the region of device 622；Other need to receive and convert monochromatic spectrum and be incident upon the region equipped with photomultiplier tube 621；So that monochromatic light
The non-zero order optical signal of spectrum is projected to the non-zero order region of the photo-electric conversion element 6, obtains just slightly detecting spectrum electric signal, make
The zero level optical signal for obtaining monochromatic spectrum is projected to the zero level region of the photo-electric conversion element 6, by photodiode 611 and product
Divide counting circuit 612, obtains intensity electrical signals；
E. computer 1 just slightly will detect spectrum electric signal and intensity electrical signals are normalized, and obtain monochromatic spectrum
Exact value.
It is carried out using a kind of above-mentioned oil plant detection device for applying associated detection technique according still further to the detection method
Oil plant detection, can obtain the title and initial survey content of metallic element corresponding to each monochromatic spectrum, not only according to spectral information
Further the mushing error in initial survey content is rejected using the strength signal detected, it can also be using only photoelectricity
The strength signal of zero level optical signal is extracted and is rejected by diode 611 and integrating counting circuit 612, so that final testing result
A possibility that being interfered substantially reduces, and detection accuracy greatly improves.
More have, the detection method further includes following steps: f. adjusts 4 angular deflection of incident eyeglass first, makes feature
Spectrum deflects out the range of grating 5, and photo-electric conversion element 6 receives the spectral information of bias light at this time, obtains bias light interference
Information；The operation is repeated, until the background interference information of all monochromatic spectrums is recorded by computer 1.This step is extractable each out
Bias light interference information in a monochromatic spectrum is ready for subsequent rejecting bias light interference information.
The volume more having, above-mentioned steps d and f in no particular order, and further include following steps: g. is single with each monochromatic spectrum
Position, from the background interference information rejected in the step f in the exact value in the step e, finally obtains all monochromatic spectrums
Detected value.So that the detection accuracy and consistency of the detected value of rejecting bias light interference information are further promoted.
More have, the detection method further includes into school step: h. incidence eyeglass 4 passes through the progress that controls from computer 1
Small angular deflection；Adjusting incident eyeglass 4 is best angle, is penetrating target monochromatic spectrum just in corresponding photoelectric conversion element
Part 6 makes monochromatic spectrum reach the most intensity values of analysis；Photo-electric conversion element 6 receives target monochromatic spectrum and is converted to electric signal hair
Give computer 1 to analyze and record: computer 1 records different monochromatic spectrums and just penetrates the different angle most believed by force, and with the step
Strength signal obtained in rapid d is combined analysis, and then corrects the unstability of the cremate light source of excitation component 2.Passing through will
The angle parameter and strength signal of detection process acquisition feed back to computer 1, and computer 1 is carried out further according to preset parameter information
Analysis, to control the stability of the excitation cremate light source in excitation process of component 2, detection process and excitation cremate light source
Process form automation adjusting；When the stability of cremate light source is higher, the detection accuracy of oil plant testing result and one
Cause property can also further increase.
The features such as photomultiplier tube 621 has dynamic range big, meets international standard；And ccd detector have multiple tracks, easily
The features such as adjusting；But it individually is used as the photo-electric conversion element 6 using any in the two, all it is unable to satisfy actual spectrum
Reception and conversion；The present invention is used 621 connected applications of ccd detector and photomultiplier tube, in multielement threadiness and band-like
The big region of spectra1 interfer- carries out spectrum survey using linear array CCD and detects, and other regions small in spectra1 interfer-, such as chromium
The SPECTRAL REGION of element and sodium element is detected using the photomultiplier tube 621 of high dynamic range, can utmostly be avoided other
Component spectrum interferes bring measurement error, and can utmostly improve and survey in the case where guaranteeing compared with high detection sensitivity
Range is measured, precision is improved.
The technical principle of the invention is described above in combination with a specific embodiment.These descriptions are intended merely to explain of the invention
Principle, and shall not be construed in any way as a limitation of the scope of protection of the invention.Based on the explanation herein, the technology of this field
Personnel can associate with other specific embodiments of the invention without creative labor, these modes are fallen within
Within protection scope of the present invention.
Claims (10)
1. a kind of oil plant detection device for applying associated detection technique, comprising: the excitation portion of excitation oil sample transmitting characteristic spectrum
Part, and the transfer element, incident eyeglass, grating, photo-electric conversion element and the computer that are successively arranged along spectral transmissions direction；
The transfer element is used to for the spectrum that the excitation component is launched being collected, and transmits injection to the incident mirror
The incidence surface of piece；
The grating is set to the light-emitting surface downstream of the incident eyeglass, by the characteristic spectrum color at multiple monochromatic spectrums；
The computer is electrically connected in the photo-electric conversion element, records and analyze the electric signal；
It is characterized in that, the optical conversion component includes multiple photomultiplier tubes and CDD detector, the optical conversion component
It is distributed in the injection direction of monochromatic spectrum at arc-shaped, receive each monochromatic spectrum and converts it into electric signal；
The photomultiplier tube is used to receive and convert the spectrum of multielement threadiness and band spectrum region；The photomultiplier tube
For receiving and converting the spectrum in the region that other need to receive and convert monochromatic spectrum.
2. a kind of oil plant detection device for applying associated detection technique according to claim 1, which is characterized in that described
The receiving area of photo-electric conversion element is divided into zero level optical signal receiving area and non-zero order optical signal receiving area；The zero order light
Signal receiving area is equipped with diode pump integrator；
The diode pump integrator includes photoelectric diode and the integrating counting circuit that electrically connects with the photodiode.
3. a kind of oil plant detection device for applying associated detection technique according to claim 2, which is characterized in that described
Photomultiplier tube and CDD detector are all set in non-zero order optical signal receiving area.
4. a kind of oil plant detection device for applying associated detection technique according to claim 1, which is characterized in that described
It is concave grating rowland circle spectrometer that high-precision cremate light source atomic emission spectrum, which surveys oily device, the incidence eyeglass, grating and
Photo-electric conversion element is all set in above Rowland circle, and the grating is concave grating.
5. a kind of oil plant detection device for applying associated detection technique according to claim 4, which is characterized in that described
Transfer element is optical fiber, and the transmitting terminal of the transfer element is set to above the Rowland circle；The incidence eyeglass passes through angle
Regulating device is set to above the Rowland circle.
6. a kind of oil plant detection device for applying associated detection technique according to claim 1, which is characterized in that described
Exciting component includes: high voltage power supply, metal bar positive electrode and rosette negative electrode；The high voltage power supply is by the computer control
System；The metal bar positive electrode is electrically connected by electric wire with the high voltage power supply, and the rosette negative electrode is located at band detection
In the oil plant of analysis.
7. a kind of oil plant detection device for applying associated detection technique of the application as described in any one of claim 1-6
Detection method, which comprises the steps of:
A. the oil sample that analysis to be detected is excited using excitation component, generates characteristic spectrum；
B. characteristic spectrum is penetrated into incident eyeglass, directive grating by transfer element；
C. characteristic spectrum is diffracted into multiple monochromatic spectrums, and directive photo-electric conversion element by grating；
D. the angle for adjusting incident eyeglass, so that multielement threadiness and band spectrum are incident upon equipped with CDD detector in monochromatic spectrum
Region；Other need to receive and convert monochromatic spectrum and be incident upon the region equipped with photomultiplier tube；So that the non-zero order of monochromatic spectrum
Optical signal is projected to the non-zero order region of the photo-electric conversion element, obtains just slightly detecting spectrum electric signal, so that monochromatic spectrum
Zero level optical signal be projected to the zero level region of the photo-electric conversion element and obtained by photodiode and integrating counting circuit
To intensity electrical signals；
E. computer just slightly will detect spectrum electric signal and intensity electrical signals are normalized, and obtain the accurate of monochromatic spectrum
Value.
8. detection method according to claim 7, which is characterized in that further include following steps:
F. incident lens angle deflection is adjusted first, so that characteristic spectrum is deflected out the range of grating, photo-electric conversion element receives this
When bias light spectral information, obtain bias light interference information；The operation is repeated, until the background interference of all monochromatic spectrums
Information is recorded by computer.
9. detection method according to claim 8, which is characterized in that above-mentioned steps d and f in no particular order, and further include as
Lower step:
G. as unit of each monochromatic spectrum, from the background interference letter rejected in the exact value in the step e in the step f
Breath, finally obtains the detected value of all monochromatic spectrums.
10. detection method according to claim 7, which is characterized in that further include into school step:
H. the incident eyeglass angular deflection small by the progress controlled from computer；Adjusting incident eyeglass is best angle, is made
Target monochromatic spectrum is just being penetrated in corresponding photo-electric conversion element, and monochromatic spectrum is made to reach the most intensity values of analysis；Photoelectric conversion element
Part receives target monochromatic spectrum and is converted to electric signal and is sent to computer and analyzes and record: computer records different monochromatic spectrums
The different angle most believed by force is just penetrated, and is combined analysis with strength signal obtained in the step d, and then correct excitation portion
The unstability of the cremate light source of part.
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| WO2021002286A1 (en) * | 2019-07-04 | 2021-01-07 | コニカミノルタ株式会社 | Spectrometer |
| JP7494851B2 (en) | 2019-07-04 | 2024-06-04 | コニカミノルタ株式会社 | Spectrophotometer |
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