CN1195976C - On-line near-infrared spectrograph - Google Patents
On-line near-infrared spectrograph Download PDFInfo
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- CN1195976C CN1195976C CN 02125852 CN02125852A CN1195976C CN 1195976 C CN1195976 C CN 1195976C CN 02125852 CN02125852 CN 02125852 CN 02125852 A CN02125852 A CN 02125852A CN 1195976 C CN1195976 C CN 1195976C
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Abstract
The present invention discloses an online near-infrared spectrometer composed of a light source, a lens set, a fiber coupler, an optical fiber, an optical fiber switch, an optical fiber sample measurer, a blank reference cell, a standard filter, slits, a plane mirror, grating, a flat-field orthogonal optical set and a detector of a charge coupled device of a linear array. The near-infrared spectrometer has the advantages of high resolution, low cost, easy maintenance and fine stability.
Description
Technical field
The invention relates to a kind of in-line meter, further say so about a kind of online near infrared spectrometer.
Background technology
Tradition laboratory analytical technology is measured data needs several hours or more time, and the data feedback speed is very slow, is not suitable for the timely and accurately control of device, can not carry out the operation of quality edge.And in-line meter can provide parameter to control system apace, control system can in time be optimized and precise control device according to these parameters, therefore, device severity and energy consumption can reduced, save as high added value components such as gasoline blend components, ensuring equipment even running under higher production load, and improve automaticity, aspects such as reduction cost of labor all play a significant role.
Traditional various in-line analyzers are that similar lab investigation instrument is improved mostly, its measuring principle remains unchanged, as do, condensation point, freezing point, pour point, flash-point etc., be generally the chemistry or the physical property mode of direct measurement oil product, because principle limits, its measuring process is often time-consuming many with the factor that influences degree of accuracy as a result.
Existing online near infrared spectrometer product type is divided according to the beam split mode, mainly comprises optical filter, raster scanning, Fourier transform, grating photodiode array detection, acousto-optic tunable type.
The process that the online near infrared spectrometer of optical filtering chip that USP5406084, CN1215837A, CN114472A and USP4286327 mention is applied in industries such as agricultural product, food processing, papermaking mostly detects.The characteristics of the type instrument are: principle is simple, and operation and maintenance are convenient, and manufacturing cost is low relatively; Mainly be limited as spectrally resolved rate variance, wavelength is selected to be restricted, and the sample message that obtains is few.Therefore, be mainly used in and measure moisture, albumen and starch etc., be restricted for high analysis indexes of resolution requirement such as hydrocarbon composition etc.
The raster scan type near infrared spectrometer that USP5187368 discloses belongs to the conventional spectrometers type, and principle is simple, and resolution is moderate, and wavelength coverage is wide; Its mechanical bearing long-time continuous that mainly is limited as grating is used wearing and tearing easily, influences the precision and the reappearance of wavelength, and anti-vibration resistance is relatively poor.
The Fourier transform type near infrared spectrometer resolution height that USP6072579 discloses, the luminous flux height, highly sensitive, wavelength coverage is wide; Its core component interferometer that mainly is limited as instrument has moving-member, and anti-vibration and long-time stability are had relatively high expectations to field environmental condition and instrument maintenance relatively, and online permanence is subjected to certain limitation.
The common feature of the disclosed grating diode array of USP5406084 and USP5751421 type, the disclosed acousto-optic tunable type of USP5317379 near infrared spectrometer product is no moving-member, and sweep velocity is fast, is suitable for online in-site measurement; But both prices are all very expensive.
The linear charge-coupled array detecting device, its light path is fixed, no moving-member, it is fast to have a corresponding speed, the high advantage of measured value and the signal to noise ratio (S/N ratio) of can adding up repeatedly.
Do not see with the linear charge-coupled array to be the near infrared spectrometer that detecting device is used for industrial on-line measurement so far.
Summary of the invention
The object of the present invention is to provide a kind of resolution height, price is low, easy care, the online near infrared spectrometer that stability is good.
Online near infrared spectrometer provided by the invention is made up of light source, lens combination, fiber coupler, optical fiber, fiber switch, sample measuring device of optical fiber, blank reference cell, basic filter, slit, level crossing, grating, flat field quadrature optical group and linear charge-coupled array detecting device.
Said fiber coupler, can select different modes for use, directly be coupled or Lens Coupling as optical fiber, wherein preferred lens coupling, here the lens of indication comprise end face globe lens, post lens, convex lens, conical lens, GRIN Lens, other special-shaped lens, or by the synthetic lens combination of these lens combination, also the optical fibre rod of available variable refractivity replaces.
The light-guide material of said optical fiber is common low hydroxyl quartz, as long as can transmit the light of near infrared region, and the also optical fiber of available other material.The material of fibre cladding can be selected as required, as polyimide covering etc.The scope of fiber core diameter is 50-1500 μ m.The optical fiber appearance can be carried out various protection according to on-the-spot needs, as plastic casing or stainless steel helix tube etc.The length of optical fiber according to actual needs in 0.5-500 rice.
Said fiber switch can be selected different implementation structures for use, as mechanical type, electric light formula, magneto-optic formula, acousto-optic formula etc.Preferred mechanical formula wherein, the mechanical type of indication comprises following two kinds of forms here, the portable and optical fiber of prism moves directly to formula.
Said sample measuring device of optical fiber has different forms according to actual needs, to transparency liquid preferred transmission flow cell or transmission probe, to translucent, solid or the preferred diffuse reflection probe of semi-solid sample, light path is regulated in 1 millimeter-100 millimeters scope according to different situations.
Said charge-coupled image sensor, it is to convert optical information to the directly proportional quantity of electric charge of light intensity a kind of photoelectric commutator, is divided into linear array and face battle array two classes; Online near infrared spectrometer provided by the invention is selected linear charge-coupled array for use.
Linear charge-coupled array mainly is made up of sensitive element, driver, video processor and A/D card etc.The picture dot number of the linear charge-coupled array of different model is also inequality, and online near infrared spectrometer can use the linear charge-coupled array of various picture dot numbers (as 1024,2048,3456 etc.).The wavelength response range of the used linear charge-coupled array of online near infrared spectrometer is preferably 700～1100nm, also can adopt (the linear charge-coupled array of 1100nm～2500nm) of long wavelength more.
Basic filter is a kind of standard of wavelength material with characteristic absorption peak, and its absorption peak is sharp keen and stable.In online near infrared spectrometer, it is mainly used to examine and determine the accuracy and the repeatability of wavelength, automatically the displacement of tuning wavelength.Can select the multiple standards optical filter for use, as praseodymium rubidium optical filter and holimium oxide optical filter etc.Optical filter in the online near infrared spectrometer is a praseodymium rubidium optical filter, and its characteristic absorption peak position is 807.6nm.
Reference cell is mainly used to hold reference material such as air or CCl
4Reagent etc. are used for the measurement of background.Can use sample measuring device of optical fiber to do reference cell, also can use the sample cell of other type to do reference cell.
In addition, the spectrometer that this invention provides can also be provided with annex, sample pre-treatments annex for example, because in some occasion, the sample pre-treatments annex can be controlled and the bubble in the sample, moisture and mechanical impurity are carried out filtering pressure, temperature and the flow velocity of fluid sample; Liquid communication pond constant temperature annex according to actual conditions, carries out constant temperature to the liquid communication pond, and the constant temperature scope is 5 ℃～100 ℃; On-the-spot explosion-proof annex in petroleum refinery, petrochemical complex and chemical process, requires to have explosion prevention function, needs online near infrared spectrometer is equipped with on-the-spot explosion-proof annex, and the type of explosion-proof tank and grade be flexible configuration as required; Abnormal sample appears in the sample annex of taking a sample automatically, and when needing measure with classic method, this annex can be reserved sample automatically; Standard model circulation annex, for setting up the analytical model that is fit to in-site measurement, this annex circulates to standard model, and the motion state of simulation actual sample is come the spectrum of measurement standard sample.
Online near infrared spectrometer provided by the invention, in the measurement for online material, can be in conjunction with Chemical Measurement, at a certain passage of measuring, at first choose the representational sample of some, measure its character or composition with basic methods (standard method or conventional method), measure the spectrum of these samples again with online near infrared spectrometer, the spectrum of measuring is carried out necessary pre-service (as differential, smoothly, polynary scatter correction, the average centralization, standardization, orthogonal signal processing etc.) after, use multivariate calibration methods (as multiple linear regression, principal component regression, partial least squares regression, artificial neural network etc.) spectrogram and character (or composition) data that obtain are set up calibration model.To unknown on-line sample, only need to measure its near infrared spectrum, utilize the analytical model of having built just can calculate its character or composition apace.
Online near infrared spectrometer provided by the invention can be measured the multiple nature parameters of the material of a plurality of measurement points simultaneously, and measurement result is directly delivered to user's set control system (as DCS etc.); Control system is divided into line top (being responsible for instrument control, measurement and data transmission) and line lower part (being responsible for data archiving, foundation and TRANSFER MODEL etc. to measuring); The line lower part has database function, particularly with the duty parameter storage of the nature parameters corresponding intrument of tested material, is the huge information bank of device operation storage.
Online near infrared spectrometer provided by the invention has following characteristics:
1, its optical system is a quadrature flat field light path design, and no movable part makes complete machine dependable performance and long-term stability.
2, because the linear charge-coupled array detecting device need not freeze, and spectrometer is easy to operate, the life-span prolongs.
3, time twin-beam design, the transient measurement background signal makes the anti-drift of complete machine strong.
4, spectrometer is built-in with standard substance, detects the stability of spectrometer in real time, carries out the spectral wavelength calibration automatically, and security performance is improved greatly.
Description of drawings
In the accompanying drawings, 1 expression light source, 2,16 is lens combination, 3,5,7,11,13,15 is fiber coupler, and 4,14 is optical fiber, and 6,12 is fiber switch, 8 is sample measuring device of optical fiber, 9 is blank reference, and 10 is standard substance, and 17 is slit, 18 is level crossing, 19 is grating, and 20 is flat field quadrature optical group, and 21 is linear array coupled apparatus detecting device.
Embodiment
Below in conjunction with accompanying drawing, further specify online near infrared spectrometer provided by the invention.
In the accompanying drawings, 1 expression light source, 2,16 is lens combination, 3,5,7,11,13,15 is fiber coupler, and 4,14 is optical fiber, and 6,12 is fiber switch, 8 is sample measuring device of optical fiber, 9 is blank reference cell, and 10 is basic filter, and 17 is slit, 18 is level crossing, 19 is grating, and 20 is flat field quadrature optical group, and 21 is linear array coupled apparatus detecting device.
Online near infrared spectrometer provided by the invention, its optical transmission process is: the light that light source (1) sends becomes directional light after the filtering of lens combination (2) collimation, import light into optical fiber (4) through fiber coupler (3), through fiber coupler (5), fiber switch (6) and fiber coupler (7) switch light and enter each road sample measuring device of optical fiber (8) successively, blank reference cell (9) and basic filter (10) light path, each Lu Guangjing fiber coupler (11), photoswitch (12) and fiber coupler (13) enter optical fiber (14) successively, import light into lens combination (16) by fiber coupler (15) again, optical convergence is changed direction by level crossing (18) with light to slit (17) back reflex to grating (19), light beam is by after grating (19) beam split, enter flat field quadrature optical group (20), by flat field quadrature optical group (20) light is become the flat field orthogonal optical and shine on the linear array coupled apparatus detecting device (21).
Claims (12)
1, a kind of online near infrared spectrometer is characterized in that this spectrometer is made up of light source (1), lens combination (2), (16), fiber coupler (3), (5), (7), (11), (13), (15), optical fiber (4), (14), fiber switch (6), (12), sample measuring device of optical fiber (8), blank reference cell (9), basic filter (10), slit (17), level crossing (18), grating (19), flat field quadrature optical group (20) and linear charge-coupled array detecting device (21).
2, according to the described online near infrared spectrometer of claim 1, the optical fiber coupling scheme that it is characterized in that said fiber coupler are directly coupling or Lens Coupling of optical fiber.
3, according to the described spectrometer of claim 2, said optical fiber coupling scheme are Lens Coupling.
4, according to the described spectrometer of claim 1, said lens are selected from the lens combination of a kind of or their combinations in end face globe lens, post lens, convex lens, conical lens or the GRIN Lens.
5, according to the described spectrometer of claim 2, said lens can replace with the optical fibre rod of variable refractivity.
6, according to the described spectrometer of claim 1, said fiber switch is a kind of in mechanical type, electric light formula, magneto-optic formula or the acousto-optic formula.
7, according to the described spectrometer of claim 6, the form of said mechanical type fiber switch is selected from the prism movable type or optical fiber moves directly to formula.
8, according to the described spectrometer of claim 1, during to the measurement of transparency liquid, said sample measuring device of optical fiber is selected transmission flow cell or transmission probe for use.
9, according to the described spectrometer of claim 1, during to the measurement of translucent, solid or semi-solid sample, said sample measuring device of optical fiber is the diffuse reflection probe.
10, according to the described spectrometer of claim 1, said basic filter is a praseodymium rubidium optical filter.
11, according to the described spectrometer of claim 1, said linear charge-coupled array detecting device wavelength response range is 700nm～2500nm.
12, according to the described spectrometer of claim 11, said linear charge-coupled array detecting device wavelength response range is 700～1100nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02125852 CN1195976C (en) | 2002-07-30 | 2002-07-30 | On-line near-infrared spectrograph |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02125852 CN1195976C (en) | 2002-07-30 | 2002-07-30 | On-line near-infrared spectrograph |
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| Publication Number | Publication Date |
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| CN1472525A CN1472525A (en) | 2004-02-04 |
| CN1195976C true CN1195976C (en) | 2005-04-06 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 02125852 Expired - Lifetime CN1195976C (en) | 2002-07-30 | 2002-07-30 | On-line near-infrared spectrograph |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100443885C (en) * | 2005-09-27 | 2008-12-17 | 重庆大学 | Miniature portable infrared spectrograph |
| CN100538289C (en) * | 2007-09-30 | 2009-09-09 | 中国科学院安徽光学精密机械研究所 | Differential absorption spectrometer import optic block |
| CN103364360B (en) * | 2013-03-14 | 2015-09-30 | 深圳先进技术研究院 | Moisture teller |
| CN103411887A (en) * | 2013-08-21 | 2013-11-27 | 南通海辰蛋白科技有限公司 | Simple oil body concentration detection device |
| CN103728023B (en) * | 2014-01-02 | 2015-12-30 | 张守明 | Lovibond colour scale spectrometer color measuring device and method for measuring color thereof |
| CN103884673B (en) * | 2014-03-31 | 2017-04-26 | 西安交通大学 | Online infrared spectroscopy monitoring system and method for hard drug taking condition |
| CN104458581B (en) * | 2014-12-16 | 2017-01-11 | 公安部消防产品合格评定中心 | Portable near-infrared three-way optical router |
| CN105699323A (en) * | 2016-03-08 | 2016-06-22 | 中国科学院合肥物质科学研究院 | Drug detection system based on Fourier transform NIRSA (near infrared spectroscopy analysis) technology |
| CN106841125B (en) * | 2017-01-04 | 2019-09-10 | 天津大学 | A kind of optical fiber integration liquid probe based on transmission measurement |
| CN106706523A (en) * | 2017-01-13 | 2017-05-24 | 清华大学 | Near-infrared spectrometer based on upconversion material |
| CN110987024B (en) * | 2019-12-30 | 2023-04-11 | 西安北方光电科技防务有限公司 | Device for measuring drift by utilizing infrared light plane mirror imaging and using method |
| CN113920113B (en) * | 2021-12-06 | 2022-03-18 | 深圳市海谱纳米光学科技有限公司 | Method and system for point-to-point white reference correction of hyperspectral image |
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2002
- 2002-07-30 CN CN 02125852 patent/CN1195976C/en not_active Expired - Lifetime
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