WO2012075958A1 - Real-time online absorption detection system - Google Patents

Real-time online absorption detection system Download PDF

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Publication number
WO2012075958A1
WO2012075958A1 PCT/CN2011/083719 CN2011083719W WO2012075958A1 WO 2012075958 A1 WO2012075958 A1 WO 2012075958A1 CN 2011083719 W CN2011083719 W CN 2011083719W WO 2012075958 A1 WO2012075958 A1 WO 2012075958A1
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WO
WIPO (PCT)
Prior art keywords
sample
light
real
time online
detector
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PCT/CN2011/083719
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French (fr)
Chinese (zh)
Inventor
刘选斌
潘涛
孙震宏
Original Assignee
霍尼韦尔综合科技(中国)有限公司
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Publication of WO2012075958A1 publication Critical patent/WO2012075958A1/en

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/85—Investigating moving fluids or granular solids
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/255—Details, e.g. use of specially adapted sources, lighting or optical systems
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00—Features of devices classified in G01N21/00
    • G01N2201/06—Illumination; Optics
    • G01N2201/068—Optics, miscellaneous
    • G01N2201/0683—Brewster plate; polarisation controlling elements

Definitions

  • the present invention relates to an absorption detection system.
  • the present invention relates to a real time online absorption detection system.
  • spectrophotometer Current absorption measurements of liquid or solid samples are typically performed on a spectrophotometer.
  • the measurement wavelength can be selected in the ultraviolet, visible or infrared range as needed.
  • spectrophotometers are widely used in the laboratory, but they are expensive.
  • the source of the spectrophotometer uses a xenon lamp.
  • the light of the xenon lamp has a wide range of coverage from ultraviolet to visible to infrared.
  • spectrophotometers can continuously and accurately provide different wavelengths of light in these bands, but this high-performance source and precise grating splitting technology add to the cost of the system.
  • a large number of similar products require only a single wavelength or a few wavelengths for absorption measurements.
  • many measurements of UV absorption require only ultraviolet light with a wavelength of 254 nm.
  • the real-time online absorption detection system provided by the present invention has the advantages of compact structure, simple structure, high reliability, low maintenance requirements, and an increase in the maximum flow rate of the flowing liquid sample in the flow chamber.
  • the real-time online absorption detection system of the present invention is realized by the following technical solutions:
  • An aspect of the present invention provides a real-time online absorption detecting system including a light source that allows only a light path from a light path, a filter disposed along a first light path, and a light beam a conversion unit, a beam splitter, a sample unit, a first detector, and a second detector disposed on the second optical path, the first optical path and the second optical path being separated at the optical splitter, the absorption detecting system further comprising a control module, the control module and The first detector and the second detector are coupled and communicated for obtaining an absorption rate of the sample to be tested in the sample unit, wherein the light source, the filter, the beam converting unit, the beam splitter, the sample unit, and the first detector and the first The second detector is placed in the dark box, and the light transmission path, the optical axis of the beam converting unit and the central axis of the sample unit are coaxially arranged, wherein the light beam emitted by the light source has a stable polarization state, which makes the splitting ratio of
  • a real-time online absorption detecting system wherein the absorption detecting system further comprises a polarizer disposed before or after the beam converting unit, the polarizer passing a maximum polarization component of the light beam emitted from the light source, thereby increasing The intensity of light on the first detector and the second detector.
  • a real-time online absorption detecting system wherein the sample to be tested is a solid sample, a static liquid sample or a flowing liquid sample.
  • a real-time online absorption detection system wherein the light source of the absorption detection system is selected from at least one of ultraviolet, visible or infrared light sources.
  • a real-time online absorption detecting system wherein when a light beam emitted by a light source includes a plurality of operating wavelengths, a plurality of filters corresponding to light beams of respective working wavelengths are required, and at this time, a plurality of filters are The film is arranged on the turntable, and the turntable is controlled by rotation through the control module or by manual rotation, so that the corresponding filter is adjusted to be adapted to the corresponding working wavelength, thereby allowing the light beam of the corresponding working wavelength to pass.
  • a real-time online absorption detecting system wherein a light source is disposed in a casing, and the light transmitting passage is a slit or a hole disposed on the casing adjacent to the optical path side.
  • a real-time online absorption detecting system wherein when the sample to be tested is a flowing liquid sample, the sample unit comprises a hollow body, an inlet and an outlet disposed at both ends of the hollow body, and the flowing liquid sample flows in from the inlet and exits Flow out.
  • a real-time online absorption detecting system wherein the beam converting unit is a lens or a lens group.
  • a real-time online absorption detecting system is provided, wherein the spectrometer has a relative standard deviation of the spectral ratio R of not more than about 5%.
  • the splitting ratio R of the spectroscope is measured by using the real-time online absorption detecting system to measure the light intensity of the standard blank sample and can be obtained by the following two methods:
  • the first mode is calculated by the following formula to obtain the spectral ratio R: where L is the intensity of the sample beam passing through the standard blank sample recorded by the first detector. 1 1 I 2 is the standard blank sample recorded by the second detector. The light intensity of the reference beam.
  • the second way is to use the light intensity of the sample beam passing through the standard blank sample recorded by the first detector for a period of time as the ordinate, and the standard blank sample recorded by the second detector at the same time or at the same time in the same period of time.
  • the light intensity of the reference beam is 1 2 as the abscissa, and then linear fitting is performed to obtain a fitted linear equation:
  • the slope of the fitted line is the split ratio R.
  • Another aspect of the present invention provides a real-time online absorption detecting system including a light source that allows only an optical path from a light-transmitting path, a filter disposed along an optical path, a beam converting unit, a sample unit, and a detector, and an absorption detecting system
  • the utility model further comprises a control module, wherein the control module is coupled with the detector and is used for obtaining the absorption rate of the sample to be tested in the sample unit, wherein the light source, the filter, the beam conversion unit, the sample unit and the detector are placed in the dark box,
  • the optical path, the optical axis of the beam converting unit, and the central axis of the sample unit are coaxially arranged, wherein the light beam emitted by the light source has a stable light intensity, which makes the absorption rate of the same sample to be measured measured at different times stable.
  • a real-time online absorption detecting system wherein the absorption detecting system further comprises a polarizer disposed before or after the beam converting unit, the polarizer passing a maximum polarization component of the light beam emitted from the light source, thereby Increase the light intensity on the detector.
  • a real-time online absorption detecting system wherein the sample to be tested is a solid sample, a static liquid sample or a flowing liquid sample.
  • a real-time online absorption detecting system wherein absorption
  • the light source of the detection system is selected from at least one of an ultraviolet, visible or infrared source.
  • a real-time online absorption detecting system wherein when a light beam emitted from a light source includes a plurality of operating wavelengths, a plurality of filters corresponding to light beams of respective working wavelengths are required, and at this time, a plurality of filters are provided.
  • the light sheet is arranged on the turntable, and the turntable is rotated and controlled by the control module or manually, so that the corresponding filter is adjusted to be adapted to the corresponding working wavelength, thereby allowing the light beam of the corresponding working wavelength to pass.
  • a real-time online absorption detecting system wherein a light source is disposed in a casing, and the light transmitting passage is a slit or a hole provided on the casing adjacent to the optical path side.
  • a real-time online absorption detecting system wherein when the sample to be tested is a flowing liquid sample, the sample unit comprises a hollow body, an inlet and an outlet disposed at both ends of the hollow body, and the flowing liquid sample flows in from the inlet and The exit is out.
  • a real-time online absorption detecting system wherein the beam converting unit is a lens or a lens group.
  • a real-time online absorption detecting system wherein an absorption rate of the same sample to be tested passes through a light intensity of a sample beam of a sample to be tested measured by the real-time online absorption detecting system; The ratio of the light intensity of the sample beam of the sample is correct
  • the real-time online absorption detecting system uses a low-cost light source in combination with a filter to select a measuring beam having a specific wavelength, thereby overcoming the combination of a high-performance light source and a grating of the prior art absorption detecting system. To choose the measurement beam, which leads to the disadvantage of high cost.
  • FIG. 1 shows a real-time online absorption detection system in accordance with one embodiment of the present invention.
  • Figure 2 shows an example of a real-time online absorption detection system as shown in Figure 1.
  • Figure 3 shows an example of a turntable for a real-time online absorption detection system as shown in Figure 1. as well as
  • the real-time online absorption detecting system is a dual optical path absorption detecting system including a light source 1, a power source 2, a filter 3, a polarizer 4, a beam converting unit 5, a beam splitter 6, and a sample unit. 7.
  • the light source 1 is mounted in the casing, and the casing is adjacent to the optical path
  • One side is provided with a light shielding plate 2a, and the light shielding plate 2a is provided with a light transmitting passage 2b for allowing the light beam 11 emitted from the light source to enter the optical path only from the light transmitting path 2b and preventing other light from leaking into the optical path.
  • a real-time online absorption detection system in accordance with one embodiment of the present invention is installed in a black box to ensure that no external light is leaking into the absorption detection system.
  • the light transmission path 2b, the optical axis of the beam converting unit 5, and the central axis of the sample unit 7 are coaxially disposed to ensure the light source having a linear shape.
  • the light beam 11 can pass through the central axis of the sample unit 7, thereby increasing the light intensity of the sample beam 1 la incident on the first detector 8.
  • the positions of a plurality of optical elements such as the light transmitting path 2b, the filter 3, the polarizer 4, the beam converting unit 5, and the beam splitter 6 can be adjusted according to actual needs.
  • the polarizer 4 can be placed in front of the filter 3 or behind the beam converting unit 5.
  • the filter 3 can be placed behind the beam converting unit 5.
  • the light beam 11 emitted by the light source sequentially passes through the light transmission path 2b, the filter 3 and the polarizer 4; then the light beam 11 emitted from the light source passes through the beam converting unit 5; 11 is incident on the beam splitter 6, wherein the beam splitter 6 is disposed at a certain inclination angle with the direction of the light beam 1 1 emitted by the light source; the light beam 11 emitted from the light source passes through the beam splitter 6 and is divided into a sample beam 11a and a reference beam l ib ,
  • the sample beam 11a is incident on the first detector 8 after passing through the sample unit 7, and the reference beam 1 ib is directly incident on the second detector 9, wherein the sample to be tested 7a is disposed in the sample unit 7, and the sample beam 11a passes through the sample to be tested 7a, the first detector 8 records the light intensity of the sample beam 11a passing through the sample 7a to be tested.
  • the second detector 9 records the light intensity of the reference beam l ib /;
  • the splitting ratio R of the spectroscope 6 is determined by the incident angle of the beam 11 emitted from the spectroscope 6 and the light source incident on the spectroscope 6.
  • the control module 10 accepts the light intensity of the sample beam 11a from the first detector 8 and the intensity of the reference beam lib from the second detector 9 and is according to equation (1-1) or (1- 2) Obtain the transmittance T of the sample to be tested 7a:
  • R in the formula (1-1) is given by the following formula (3-1), and R and b in the formula (1-2) are both given by the following formula (3-2), and the formula (1-1) R in the R or R and b in the formula (1-2) are all stored in the control module 10.
  • the control module specifically calculates the transmittance T of the sample to be tested 7a according to the formula (1-1) or the formula (1-2), depending on whether the calculation method of the spectral ratio R is based on the formula (3-1) or the formula (3- 2).
  • the control module 10 obtains the absorption rate A bs of the sample 7 to be tested according to formula (2) :
  • the split ratio R of the spectroscope 6 in the formula (1-1) or the split ratio R and the parameter b of the spectroscope 6 in the formula (1-2) are detected by real-time online absorption using an embodiment of the present invention.
  • the system is tested with a standard blank sample.
  • a standard blank sample is injected into the sample unit 7.
  • the blank sample test should be performed at regular intervals or as needed.
  • the calculation method of the splitting ratio R the following tests are separately described for the blank samples.
  • the first calculation method of the splitting ratio R records the light intensity of the sample beam 11a passing through the standard blank sample by the first detector 8 1
  • the second detector 9 records the light intensity 1 2 of the reference beam l ib of the standard blank sample.
  • the control module 10 obtains the split ratio R of the spectroscope 6 according to the formula (3-1):
  • the second calculation method of the splitting ratio R records the light intensity of the sample beam 11a passing through the standard blank sample by the first detector 8 for a period of time. 1
  • the second detector 9 records the standard at the same time or at the same time in the same period of time.
  • the light intensity of the reference beam l ib of the blank sample is 1 2 .
  • the control module 10 according to the following way to obtain the spectral beam splitter 6 ratio R: that the ordinate, the abscissa to 12, followed by a linear fit, fitting a straight line equation can be obtained:
  • the slope of the fitted line is the split ratio R, and b is the intercept of the fitted line.
  • the real-time online absorption detection system is capable of real-time online measurement of the absorption rate of a sample to be tested of a solid, static liquid or flowing liquid.
  • the control module 10 of the real-time online absorption detection system obtains the absorption rate A bs of the sample to be tested according to the formulas (1)-(3).
  • the light beam emitted by the light source of the real-time online absorption detecting system according to an embodiment of the present invention has a stable polarization state, which makes the splitting ratio R on the spectroscope 6 stable.
  • the fact that the spectral ratio R is stable means that the relative standard deviation of the spectral ratio is usually not more than about 5% within the effective life of the present invention.
  • the stable polarization state refers to the change of the ratio of the S polarization and the P polarization of the light beam emitted by the light source, and generally does not cause the relative polarization ratio R on the spectroscope 6 within the effective lifetime of the real-time online absorption detection system of the present invention.
  • the standard deviation is greater than approximately 5%.
  • a light source 1 of a real-time online absorption detecting system may be selected from at least one of ultraviolet, visible, and infrared light sources, and the light beam emitted by the light source generally includes S-polarized light (vertical polarization).
  • Light and P-polarized light (horizonically polarized light)
  • the operating wavelength of the light source can be single wavelength or multiple wavelengths.
  • the S-polarized light and the P-polarized light respectively represent vertically polarized light and horizontally polarized light, wherein the vertical and horizontal directions refer to a plane formed by the sample beam 11a and the reference beam l ib , and the polarization direction of the light is vertical or parallel.
  • the light transmission path 2b is a slit or a hole. It will be easily understood by those skilled in the art that: the light transmission path 2b can also Other methods are employed, and this will also fall within the scope of the present invention.
  • the filter 3 allows only the single wavelength as the operating wavelength and the wavelength in the vicinity thereof to pass.
  • the operating wavelength of the light source 1 is multiple wavelengths, a plurality of filters 3a, 3b, 3c, and 3d corresponding to a plurality of operating wavelengths are required, and the plurality of filters 3a, 3b, 3c, and 3d may be mounted in one On the turntable 14.
  • the plurality of filters 3a, 3b, 3c, and 3d allow light beams of different operating wavelengths to pass, respectively.
  • the control module 10 rotates the turntable 14 according to the operating wavelength required for the sample to be tested to select the corresponding filter.
  • Fig. 4 shows a perspective view of the turntable 14 on which a plurality of filters are disposed.
  • the turntable 14 includes a body 15, a turntable central shaft 16 disposed at the center of the body 15, and a plurality of mounting holes 15a disposed around the body 15, the mounting holes 15a for mounting the filters 3a, 3b, respectively. 3c and 3d, the turntable 14 is rotatable about its central axis 16.
  • the turntable 14 is rotated by the control module 10 or manually to adjust the corresponding filter to accommodate the corresponding operating wavelength, thereby allowing the beam of the corresponding operating wavelength to pass.
  • the turntable 14 may also be provided with other configurations to mount more than four or less than four filters, and this will also fall within the scope of the present invention.
  • the polarizer 4 has a plane of polarization, the plane of polarization has a transmission axis, and the polarizer 4 allows only polarized light in the plane of polarization parallel to the direction of the transmission axis to pass. Therefore, when the maximum polarization component of the light beam emitted from the light source is S-polarized light, the polarizer 4 allows only the S-polarized light to pass by appropriately placing the polarizer 4, as shown in Fig. 2. It should be noted that when the maximum polarization component of the light beam 11 emitted by the light source is P-polarized light, the polarizer 4 can also allow the P-polarized light to pass only by appropriately placing the polarizer 4, and this will also fall under the protection of the present invention. Within the scope.
  • the polarization state of the light beam emitted by the light source (the ratio of the S-polarized light to the P-polarized light) is stable, this makes the spectral ratio R on the spectroscope 6 also stable, real-time online absorption detection according to an embodiment of the present invention.
  • the system may not include the polarizer 4.
  • the beam transforming unit 5 is a lens or lens group for collimating and concentrating the light beam 11 emitted from the light source.
  • the beam splitter 6 is made of a suitable material to allow the light beam emitted from the light source to be split at a certain splitting ratio R.
  • the sample unit 7 is made of a suitable material to allow the light beam emitted from the light source to pass the most.
  • the sample unit 7 comprises a hollow body 13 and an inlet 13a and an outlet 13b disposed on opposite sides of the hollow body 13, the flow of liquid sample to be tested flowing in from the inlet 13a of the sample unit 7 and from The outlet 13b flows out (as shown in Figure 1).
  • a real-time online absorption detection system according to one embodiment of the present invention is capable of measuring the absorption rate A bs of a flowing liquid sample.
  • the flow rate of the flowing liquid sample in the sample unit 7 of the present invention is remarkably increased.
  • the bubbles in the sample unit 7 easily overflow from the sample unit 7. It will be readily understood by those skilled in the art that the sample unit 7 for flowing liquid samples may also have other configurations, and this will also fall within the scope of the present invention.
  • the first detector 8 and the second detector 9 are capable of recording the intensity of light of a single or multiple operating wavelengths of the beam 11 emitted by the source.
  • the control module 10 is coupled to and communicates with the first detector 8 and the second detector 9 to receive the intensity and reference of the respective sample beams from the sample to be tested and the standard blank sample from the first detector 8 and the second detector 9.
  • the intensity of the beam and based on equations (1) - (3), obtain the absorbance A bs of the sample to be tested.
  • the absorption detecting system is a single optical path absorption detecting system comprising a light source 1, a power source 2, a filter 3, a polarizer 4, a beam converting unit 5, a sample unit 7, a first detector 8, and a control module 10.
  • the light source 1 is mounted in the casing, and the light shielding plate 2a is disposed on a side of the casing near the optical path, and the light shielding plate 2a is provided with a light transmission passage 2b.
  • the function of the light shielding plate 2a is to make the light beam 11 emitted from the light source only from the light transmission path 2b.
  • a real-time online absorption detection system in accordance with another embodiment of the present invention is installed in a black box to ensure that no external light is leaking into the absorption detection system.
  • the light transmission path 2b, the optical axis of the beam converting unit 5, and the central axis of the sample unit 7 are coaxially disposed to ensure a slave light source having a linear shape.
  • the emitted light beam 11 can pass through the central axis of the sample unit 7, thereby increasing the light intensity of the sample beam 11a incident on the first detector 8.
  • the positions of a plurality of optical elements such as the light transmission path 2b, the filter 3, the polarizer 4, and the beam converting unit 5 can be adjusted according to actual needs.
  • the polarizer 4 can be placed in front of the filter 3 or behind the beam converting unit 5.
  • the filter 3 can be placed behind the beam converting unit 5.
  • the light beam 11 emitted from the light source sequentially passes through the light transmission path 2b, the filter 3 and the polarizer 4; then the light beam 11 emitted from the light source passes through the beam converting unit 5; then the converted light beam 11 passes through the sample unit 7 and becomes the sample beam 11a.
  • the sample beam 11a is incident on the first detector 8, wherein the sample unit 7 contains the sample 7a to be tested, the sample beam 11a passes through the sample 7a to be tested, and the first detector 8 records the sample beam passing through the sample 7a to be tested.
  • the control module 10 receives the light intensity of the sample beam 11a from the first detector 8 and obtains the transmittance T of the sample 7a to be tested according to the formula (4):
  • the control module 10 obtains the absorption rate A bs of the sample 7 to be tested according to the formula (2).
  • the standard blank sample is first tested with the absorption measurement system, and then the system is tested with the system.
  • the test of the standard blank sample should be performed once every other time or according to actual needs. Specifically, a standard blank sample (or a sample to be tested) is injected into the sample unit 7, and then the light intensity of the sample beam 11a passing through the standard blank sample (or the sample to be tested) is recorded by the first detector 8 ( / ;).
  • the control module 10 obtains the transmittance T of the sample 7a to be tested according to the formula (4).
  • optical elements such as filters, polarizers, beam transform units, and the like of a single optical path real-time online absorption detecting system according to another embodiment of the present invention and an implementation according to the present invention
  • optical elements such as filters, polarizers, beam transform units, and the like of a single optical path real-time online absorption detecting system according to another embodiment of the present invention and an implementation according to the present invention
  • the corresponding optical components in the dual optical path real-time online absorption detection system are similar, and will not be described here.
  • the single-light path real-time on-line absorption detection system is capable of real-time on-line measurement of the absorption rate of a sample to be tested of a solid, static liquid or flowing liquid.
  • the first detector 8 is capable of recording the intensity of light of a single or multiple operating wavelengths of the beam 11 emitted by the source.
  • the control module 10 is coupled to and communicates with the first detector 8 to receive the intensity of the respective sample beam from the sample to be tested and the standard blank sample from the first detector 8 and obtain the sample to be tested based on equations (2) and (4).
  • Absorption rate A bs Absorption rate
  • the light beam emitted from the light source of the single-light path real-time online absorption detecting system has a stable light intensity, which makes the absorption rate A bs of the same sample to be measured measured at different times stable.
  • the relative standard deviation of the absorption rate of the same sample to be tested is usually no more than about 5%, and the relative standard deviation is defined above.
  • the absorption rate A bs of the same sample to be tested is stable, which means the real-time online absorption test in the present invention.
  • Figure 2 shows an example of a real-time online absorption detection system as shown in Figure 1.
  • the example uses a low-pressure mercury lamp as the light source 1, and the light source 1 can emit an ultraviolet light beam 11 having a wavelength of about 254 nm.
  • the light source 1 is mounted in the casing, and one side of the casing is provided with a light shielding plate 2a, and the light shielding plate 2a is provided with light transmission.
  • the ultraviolet light beam 11 having a wavelength of 254 nm emitted from the light source 1 is transmitted only from the light transmission path 2b which is, for example, a slit or a hole, and the light shielding plate 2a prevents other light from leaking into the optical path.
  • the ultraviolet light beam 11 emitted by the light source 1 having a wavelength of about 254 nm passes through the filter 3, the polarizer 4, and the beam converting unit 5 (for example, a lens or a lens group), and then the light beam 11 is incident on the beam splitter 6 to be divided into two beams: a sample
  • the light beam 11a and the reference light beam l ib, the sample light beam 11a passes through the sample unit 7 and passes through a sample to be tested (or a standard blank sample) disposed therein, and the first detector 8 and the second detector 9 are respectively used for recording incident thereon
  • the intensity of the sample beam 11a and the reference beam l ib The intensity of the sample beam 11a and the reference beam l ib .
  • the control module 10 is coupled to and communicates with the first detector 8 and the second detector 9 to receive the intensity and reference of the respective sample beams from the standard blank sample of the first detector 8 and the second detector 9 and the sample to be tested.
  • the intensity of the beam and based on equations (1) - (3), obtain the absorbance A bs of the sample to be tested at a wavelength of approximately 254 nm.
  • the light beam emitted by the light source according to an example of the real-time online absorption detecting system shown in Fig. 1 has a stable polarization state, which makes the splitting ratio R on the spectroscope 6 stable.
  • a real-time online absorption detecting system may not include the polarizer 4.
  • the filter 3 allows an ultraviolet beam having a wavelength of about 254 nm to pass, and the filter 3 can avoid interference of other wavelengths of light.
  • Beam transform unit 5 for example, a lens or a lens group
  • the beam splitter 6 and the sample unit 7 are prepared using quartz, and the beam splitter 6 can be set, for example, at 45 degrees to the sample beam.
  • the light beam 11 emitted from the light source 1 has a stable polarization state, and the splitting ratio R on the spectroscope 6 remains stable.
  • the split ratio is about 7-8, and the relative standard deviation of the split ratio is less than about 4%.
  • the splitting ratio R on the spectroscope 6 prepared by quartz is about 4-5, and the splitting is performed.
  • the relative standard deviation of the ratio is less than about 2%.
  • a light transmission path 2b of a slit or a hole for example, a beam or a lens group
  • the optical axis of the unit 5 and the central axis of the sample unit 7 are coaxially arranged. This ensures that the ultraviolet beam 11 having a linear shape from the light source and having a wavelength of about 254 nm can pass through the central axis of the sample unit 7, thereby increasing the intensity of the sample beam 11a incident on the first detector 8.
  • the filter 3 allows an ultraviolet light beam having a wavelength of about 254 nm to pass, and the filter 3 can avoid interference of light of other wavelengths.
  • the polarizer 4, the beam converting unit 5 (e.g., lens or lens group), the beam splitter 6, the sample unit 7, and the like are suitably prepared using a material that allows ultraviolet light to pass therethrough. These materials include, but are not limited to, quartz glass, UV-transmissive glass or polymers, high boron glass, sapphire, magnesium fluoride, lithium fluoride, etc., of which quartz is the most widely used material in the ultraviolet region.
  • an ultraviolet lamp having a wavelength of about 254 nm is measured by the system to have a maximum polarization component parallel to the direction of the tube.
  • the polarizer 4 uses quartz as a substrate and is coated with a thin film.
  • the polarization axis of the polarizer 4 allows the polarized light S-polarized light in the ultraviolet light beam having a wavelength of about 254 nm emitted from the light source 1 to pass. Therefore, in order to increase the intensity of the sample beam and the reference beam on the first detector 8 and the second detector 9, the ultraviolet lamp tube is placed vertically (as shown in Fig. 2).
  • the sample unit 7 adopts the structure shown in FIG. 2, the sample unit 7 is prepared by using quartz to ensure that the ultraviolet light beam can pass, and the sample unit 7 has a circular cross section, including the hollow body 13 and the inlet 13a and the outlet 13b disposed at both ends thereof.
  • the test sample flows in from the inlet 13a and flows out from the outlet 13b.
  • sample unit 7 of circular cross section if A slit is provided on the light shielding plate on the side of the ultraviolet lamp, instead of the hole, and the sample unit 7 is placed in a direction parallel to the direction of the slit. If the visor on the side of the ultraviolet lamp is open with a small hole, the orientation of the sample unit 7 is not limited thereto.
  • Other configurations, and this will also fall within the scope of the present invention.
  • the first detector 8 and the second detector 9 employ an ultraviolet responsive type of silicon photo cell.
  • UV-responsive silicon photocells should respond at selected UV operating wavelengths.
  • the effective area of the UV-responsive silicon photocell should be larger than the spot size of the UV beam falling on the UV-responsive silicon photocell to ensure that the UV-responsive silicon photocell can receive the energy of all optical signals.
  • the dual optical path system as shown in 2 can also be simplified into a single optical path system.
  • the optical splitter 6 and the reference beam can be omitted.
  • the polarization from the UV lamp can first be measured. If the beam from the UV lamp is partially polarized, the alignment of the UV lamp should be adjusted to ensure that the maximum polarization of the beam from the UV lamp is parallel to the polarization of the polarizer 4. Therefore, it is ensured that the maximum beam energy can pass through the polarizer 4.
  • the real-time online absorption detecting system uses a low-cost light source in combination with a filter to select a measuring beam having a specific wavelength, thereby overcoming the combination of a high-performance light source and a grating of the prior art absorption detecting system. To choose the measurement beam, which leads to the disadvantage of high cost.

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Abstract

A real-time online absorption detection system comprises a light source (1) entering a first optical path through an optical transmission path, a filter (3) arranged along the first optical path, a polarizer (4), a beam transformation unit (5), a beam splitter (6), a sample unit (7), a first detector (9) and a second detector (8) arranged along a second optical path. The first optical path and the second optical path are separated at the beam splitter, and the system also comprises a control module (10), coupled and in communication with the first detector and the second detector for obtaining the absorption rate of test samples waiting to be measured in the sample unit, wherein the polarizer allows the maximum polarization component of a light beam from the light source to pass through, thus increasing the incidental light intensity of the first detector and the second detector. The system combines the light source and the filter to select a measuring beam with a specific wavelength, and has a lower cost when compared with the traditional absorption detection system combining continuous light source with grating to select a measuring beam.

Description

实时在线吸收检测系统  Real-time online absorption detection system
【技术领域】  [Technical Field]
本发明涉及一种吸收检测系统。 具体而言， 本发明涉及一种实时 在线吸收检测系统。  The present invention relates to an absorption detection system. In particular, the present invention relates to a real time online absorption detection system.
【背景技术】 【Background technique】
目前液体或者固体样品的吸收测量一般在分光光度计上进行。 测 量波长可以根据需要选择紫外、 可见或者红外波段。 作为高精度的科 学吸收检测系统， 分光光度计在实验室中得到广泛的应用， 但其价格 却比较昂贵。  Current absorption measurements of liquid or solid samples are typically performed on a spectrophotometer. The measurement wavelength can be selected in the ultraviolet, visible or infrared range as needed. As a high-precision scientific absorption detection system, spectrophotometers are widely used in the laboratory, but they are expensive.
一般来说， 分光光度计的光源采用氙灯。 氙灯的光 i普范围较宽， 覆盖了从紫外、 可见到红外波段。 通过将氙灯和精确的光栅分光技术 结合， 分光光度计可以连续精确地提供在这些波段中的不同波长的 光， 但这种高性能的光源和精确的光栅分光技术增加了系统的成本。 对一些特定应用而言， 例如大量同类产品的吸收测量仅需要单个波长 或者某几个波长。例如，许多测量紫外吸收的情形仅需要波长为 254nm 的紫外光。 对于这些特定应用， 通常不需要采用昂贵而且占据较大空 间的分光光度计。  In general, the source of the spectrophotometer uses a xenon lamp. The light of the xenon lamp has a wide range of coverage from ultraviolet to visible to infrared. By combining xenon lamps with precise grating spectroscopic techniques, spectrophotometers can continuously and accurately provide different wavelengths of light in these bands, but this high-performance source and precise grating splitting technology add to the cost of the system. For some specific applications, for example, a large number of similar products require only a single wavelength or a few wavelengths for absorption measurements. For example, many measurements of UV absorption require only ultraviolet light with a wavelength of 254 nm. For these specific applications, it is generally not necessary to use a spectrophotometer that is expensive and occupies a large space.
因而， 对于大量同类产品的吸收检测而言， 需要提供特定工作波 长的实时在线吸收检测系统， 以降低成本。  Therefore, for the absorption detection of a large number of similar products, a real-time online absorption detection system with a specific working wavelength is required to reduce the cost.
【发明内容】 [Summary of the Invention]
本发明的目的是提供一种低成本的实时在线吸收检测系统。 本 发明提供的实时在线吸收检测系统具有结构紧凑、 构造简单、 可靠性 高、 维护要求低以及增加了流动室内流动液体样品最大流速的优点。 本发明的实时在线吸收检测系统通过以下技术方案得以实现：  It is an object of the present invention to provide a low cost real time online absorption detection system. The real-time online absorption detection system provided by the present invention has the advantages of compact structure, simple structure, high reliability, low maintenance requirements, and an increase in the maximum flow rate of the flowing liquid sample in the flow chamber. The real-time online absorption detection system of the present invention is realized by the following technical solutions:
本发明的一方面提供了一种实时在线吸收检测系统， 其包括仅允 许从透光通路进入第一光路的光源、 沿第一光路设置的滤光片、 光束 变换单元、 分光器、 样品单元、 第一探测器以及设置在第二光路上的 第二探测器， 第一光路和第二光路在分光器处分开， 吸收检测系统还 包括控制模块， 控制模块与第一探测器和第二探测器耦联并通信， 用 于获得样品单元中待测样品的吸收率， 其中光源、 滤光片、 光束变换 单元、分光器、样品单元以及第一探测器和第二探测器放置在暗箱中， 透光通路、 光束变换单元的光轴以及样品单元的中心轴同轴设置， 其 特征在于， 光源发出的光束具有稳定的偏振态， 这使得分光器的分光 比 R稳-定。 An aspect of the present invention provides a real-time online absorption detecting system including a light source that allows only a light path from a light path, a filter disposed along a first light path, and a light beam a conversion unit, a beam splitter, a sample unit, a first detector, and a second detector disposed on the second optical path, the first optical path and the second optical path being separated at the optical splitter, the absorption detecting system further comprising a control module, the control module and The first detector and the second detector are coupled and communicated for obtaining an absorption rate of the sample to be tested in the sample unit, wherein the light source, the filter, the beam converting unit, the beam splitter, the sample unit, and the first detector and the first The second detector is placed in the dark box, and the light transmission path, the optical axis of the beam converting unit and the central axis of the sample unit are coaxially arranged, wherein the light beam emitted by the light source has a stable polarization state, which makes the splitting ratio of the splitter R stable.
才艮据本发明的一方面提供的实时在线吸收检测系统， 其中吸收检 测系统还包括设置在光束变换单元之前或之后的偏振器， 偏振器使得 光源发出的光束中的最大偏振分量通过， 从而增加第一探测器和第二 探测器上的光强。  According to an aspect of the present invention, there is provided a real-time online absorption detecting system, wherein the absorption detecting system further comprises a polarizer disposed before or after the beam converting unit, the polarizer passing a maximum polarization component of the light beam emitted from the light source, thereby increasing The intensity of light on the first detector and the second detector.
才艮据本发明的一方面提供的实时在线吸收检测系统， 其中待测样 品为固体样品、 静态液体样品或者流动液体样品。  According to an aspect of the present invention, a real-time online absorption detecting system is provided, wherein the sample to be tested is a solid sample, a static liquid sample or a flowing liquid sample.
才艮据本发明的一方面提供的实时在线吸收检测系统， 其中吸收检 测系统的光源选自紫外、 可见或者红外光源中的至少一种。  A real-time online absorption detection system according to one aspect of the invention, wherein the light source of the absorption detection system is selected from at least one of ultraviolet, visible or infrared light sources.
根据本发明的一方面提供的实时在线吸收检测系统， 其中当光源 发出的光束包括多个工作波长时， 则需要与各个工作波长的光束相对 应的多个滤光片， 此时多个滤光片设置在转盘上， 转盘通过控制模块 进行转动控制或者通过手动方式进行转动控制， 以便将相应的滤光片 调整就为与相应的工作波长适应， 从而允许相应工作波长的光束通 过。  According to an aspect of the present invention, a real-time online absorption detecting system is provided, wherein when a light beam emitted by a light source includes a plurality of operating wavelengths, a plurality of filters corresponding to light beams of respective working wavelengths are required, and at this time, a plurality of filters are The film is arranged on the turntable, and the turntable is controlled by rotation through the control module or by manual rotation, so that the corresponding filter is adjusted to be adapted to the corresponding working wavelength, thereby allowing the light beam of the corresponding working wavelength to pass.
根据本发明的一方面提供的实时在线吸收检测系统， 其中光源设 置在罩壳中， 透光通路为设置在罩壳上邻近光路侧的狭缝或者孔。  According to an aspect of the present invention, a real-time online absorption detecting system is provided, wherein a light source is disposed in a casing, and the light transmitting passage is a slit or a hole disposed on the casing adjacent to the optical path side.
根据本发明的一方面提供的实时在线吸收检测系统， 其中当待测 样品为流动液体样品时， 样品单元包括中空本体、 设置在中空本体两 端的入口和出口， 流动液体样品从入口流入并从出口流出。  According to an aspect of the present invention, there is provided a real-time online absorption detecting system, wherein when the sample to be tested is a flowing liquid sample, the sample unit comprises a hollow body, an inlet and an outlet disposed at both ends of the hollow body, and the flowing liquid sample flows in from the inlet and exits Flow out.
才艮据本发明的一方面提供的实时在线吸收检测系统， 其中光束变 换单元为透镜或者透镜组。 才艮据本发明的一方面提供的实时在线吸收检测系统， 其中分光器 的分光比 R的相对标准偏差不大于大约 5%。 分光器的分光比 R通过 采用所述实时在线吸收检测系统测量标准空白样品的光强并可以由 以下两种方式而获得： According to an aspect of the present invention, a real-time online absorption detecting system is provided, wherein the beam converting unit is a lens or a lens group. According to an aspect of the present invention, a real-time online absorption detecting system is provided, wherein the spectrometer has a relative standard deviation of the spectral ratio R of not more than about 5%. The splitting ratio R of the spectroscope is measured by using the real-time online absorption detecting system to measure the light intensity of the standard blank sample and can be obtained by the following two methods:
第一种方式由以下公式计算而获得分光比 R: 其中 L为由第一探测器记录的经过标准空白样品的样品光束的光 强 11 I2为由第二探测器记录的标准空白样品的参考光束的光强。 The first mode is calculated by the following formula to obtain the spectral ratio R: where L is the intensity of the sample beam passing through the standard blank sample recorded by the first detector. 1 1 I 2 is the standard blank sample recorded by the second detector. The light intensity of the reference beam.
第二种方式是以第一探测器在一段时间内记录的经过标准空白 样品的样品光束的光强 为纵坐标， 以第二探测器在同一段时间内相 同时刻或相近时刻记录的标准空白样品的参考光束的光强 12为横坐 标， 然后进行线性拟合， 可得拟合直线方程： The second way is to use the light intensity of the sample beam passing through the standard blank sample recorded by the first detector for a period of time as the ordinate, and the standard blank sample recorded by the second detector at the same time or at the same time in the same period of time. The light intensity of the reference beam is 1 2 as the abscissa, and then linear fitting is performed to obtain a fitted linear equation:
= R x I2 + b， = R x I 2 + b,
拟合直线的斜率即为分光比 R。  The slope of the fitted line is the split ratio R.
本发明的另一方面提供了一种实时在线吸收检测系统， 其包括仅 允许从透光通路进入光路的光源、 沿光路设置的滤光片、 光束变换单 元、 样品单元和探测器， 吸收检测系统还包括控制模块， 控制模块与 探测器耦联并通信， 用于获得样品单元中待测样品的吸收率， 其中光 源、 滤光片、 光束变换单元、 样品单元以及探测器放置在暗箱中， 透 光通路、光束变换单元的光轴以及样品单元的中心轴同轴设置，其中， 光源发出的光束具有稳定的光强， 这使得在不同时刻测量的同一待测 样品的吸收率稳定。  Another aspect of the present invention provides a real-time online absorption detecting system including a light source that allows only an optical path from a light-transmitting path, a filter disposed along an optical path, a beam converting unit, a sample unit, and a detector, and an absorption detecting system The utility model further comprises a control module, wherein the control module is coupled with the detector and is used for obtaining the absorption rate of the sample to be tested in the sample unit, wherein the light source, the filter, the beam conversion unit, the sample unit and the detector are placed in the dark box, The optical path, the optical axis of the beam converting unit, and the central axis of the sample unit are coaxially arranged, wherein the light beam emitted by the light source has a stable light intensity, which makes the absorption rate of the same sample to be measured measured at different times stable.
才艮据本发明的另一方面提供的实时在线吸收检测系统， 其中吸收 检测系统还包括设置在光束变换单元之前或之后的偏振器， 偏振器使 得光源发出的光束中的最大偏振分量通过， 从而增加探测器上的光 强。  According to another aspect of the present invention, there is provided a real-time online absorption detecting system, wherein the absorption detecting system further comprises a polarizer disposed before or after the beam converting unit, the polarizer passing a maximum polarization component of the light beam emitted from the light source, thereby Increase the light intensity on the detector.
才艮据本发明的另一方面提供的实时在线吸收检测系统， 其中待测 样品为固体样品、 静态液体样品或者流动液体样品。  According to another aspect of the present invention, there is provided a real-time online absorption detecting system, wherein the sample to be tested is a solid sample, a static liquid sample or a flowing liquid sample.
才艮据本发明的另一方面提供的实时在线吸收检测系统， 其中吸收 检测系统的光源选自紫外、 可见或者红外光源中的至少一种。 According to another aspect of the present invention, a real-time online absorption detecting system, wherein absorption The light source of the detection system is selected from at least one of an ultraviolet, visible or infrared source.
根据本发明的另一方面提供的实时在线吸收检测系统， 其中当光 源发出的光束包括多个工作波长时， 则需要与各个工作波长的光束相 对应的多个滤光片， 此时多个滤光片设置在转盘上， 转盘通过控制模 块或者通过手动方式进行转动控制， 以便将相应的滤光片调整就为与 相应的工作波长适应， 从而允许相应工作波长的光束通过。  According to another aspect of the present invention, a real-time online absorption detecting system is provided, wherein when a light beam emitted from a light source includes a plurality of operating wavelengths, a plurality of filters corresponding to light beams of respective working wavelengths are required, and at this time, a plurality of filters are provided. The light sheet is arranged on the turntable, and the turntable is rotated and controlled by the control module or manually, so that the corresponding filter is adjusted to be adapted to the corresponding working wavelength, thereby allowing the light beam of the corresponding working wavelength to pass.
才艮据本发明的另一方面提供的实时在线吸收检测系统， 其中光源 设置在罩壳中， 透光通路为设置在罩壳上邻近光路侧的狭缝或者孔。  According to another aspect of the present invention, there is provided a real-time online absorption detecting system, wherein a light source is disposed in a casing, and the light transmitting passage is a slit or a hole provided on the casing adjacent to the optical path side.
根据本发明的另一方面提供的实时在线吸收检测系统， 其中当待 测样品为流动液体样品时， 样品单元包括中空本体、 设置在中空本体 两端的入口和出口， 流动液体样品从入口流入并从出口流出。  According to another aspect of the present invention, there is provided a real-time online absorption detecting system, wherein when the sample to be tested is a flowing liquid sample, the sample unit comprises a hollow body, an inlet and an outlet disposed at both ends of the hollow body, and the flowing liquid sample flows in from the inlet and The exit is out.
才艮据本发明的另一方面提供的实时在线吸收检测系统， 其中光束 变换单元为透镜或者透镜组。  According to another aspect of the present invention, a real-time online absorption detecting system is provided, wherein the beam converting unit is a lens or a lens group.
才艮据本发明的另一方面提供的实时在线吸收检测系统， 其中同一 待测样品的吸收率通过对由所述实时在线吸收检测系统测量的待测 样品的样品光束的光强 /;和空白样品的样品光束的光强 的比值求对  According to another aspect of the present invention, there is provided a real-time online absorption detecting system, wherein an absorption rate of the same sample to be tested passes through a light intensity of a sample beam of a sample to be tested measured by the real-time online absorption detecting system; The ratio of the light intensity of the sample beam of the sample is correct
5%。 5%.
根据本发明上述实施例的实时在线吸收检测系统采用低成本光 源与滤光片结合来选择具有特定波长的测量用光束， 从而克服了现有 技术的吸收检测系统的采用高性能的光源与光栅结合来选择测量用 光束而导致成本高的缺点。  The real-time online absorption detecting system according to the above embodiment of the present invention uses a low-cost light source in combination with a filter to select a measuring beam having a specific wavelength, thereby overcoming the combination of a high-performance light source and a grating of the prior art absorption detecting system. To choose the measurement beam, which leads to the disadvantage of high cost.
【附图说明】 [Description of the Drawings]
参照附图， 本发明的公开内容将变得更易理解。 本领域技术人 员容易理解的是： 这些附图仅仅用于说明的目的， 而并非意在对本发 明的保护范围构成限制。 图中：  The disclosure of the present invention will become more apparent from the drawings. It is to be understood by those skilled in the art that the drawings are only for the purpose of illustration and are not intended to limit the scope of the invention. In the picture:
图 1示出了根据本发明一个实施例的实时在线吸收检测系统。 图 2示出了如图 1所示的实时在线吸收检测系统一个实例。 图 3示出了用于如图 1所示的实时在线吸收检测系统的转盘的 一个实例。 以及 1 shows a real-time online absorption detection system in accordance with one embodiment of the present invention. Figure 2 shows an example of a real-time online absorption detection system as shown in Figure 1. Figure 3 shows an example of a turntable for a real-time online absorption detection system as shown in Figure 1. as well as
图 4示出了根据本发明另一个实施例的实时在线吸收检测系统。 部件及标号列表  4 illustrates a real-time online absorption detection system in accordance with another embodiment of the present invention. List of parts and labels
Figure imgf000007_0001
【具体实施方式】
Figure imgf000007_0001
【Detailed ways】
图 1—4和以下说明描述了本发明的特定实施例以教导本领域技术 人员如何实施和再现本发明的最佳模式。 为了教导发明原理， 已简化 或省略了一些常规方面。 本领域技术人员应该理解源自这些实施例的 变型将落在本发明的保护范围内。 本领域技术人员应该理解下述特征 能够以各种方式结合以形成本发明的多个变型。 由此， 本发明并不局 限于下述特定实施例， 而仅由权利要求和它们的等同物限定。 实施例 1  The Figures 1-4 and the following description describe specific embodiments of the present invention to teach those skilled in the art how to implement and reproduce the invention. Some conventional aspects have been simplified or omitted to teach the principles of the invention. Those skilled in the art will appreciate that variations derived from these embodiments are intended to fall within the scope of the present invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Therefore, the invention is not to be limited to the specific embodiments described below, but only by the claims and their equivalents. Example 1
图 1示出了根据本发明一个实施例的实时在线吸收检测系统。 如 图 1所示， 根据本发明的实时在线吸收检测系统为双光路吸收检测系 统， 其包括光源 1、 电源 2、 滤光片 3、 偏振器 4、 光束变换单元 5、 分光器 6、 样品单元 7、 第一探测器 8、 第二探测器 9和控制模块 10， 其中电源 2用于向光源 1供电， 其包括罩壳 (未示出）， 光源 1安装在 罩壳中， 罩壳靠近光路的一侧设有遮光板 2a， 遮光板 2a上设置有透 光通路 2b，遮光板 2a的作用是允许光源发出的光束 11仅从透光通路 2b进入光路， 并防止其他光泄漏到光路中。 根据本发明一个实施例的 实时在线吸收检测系统安装在一个暗箱中， 以保证没有外部光泄露到 该吸收检测系统中。 在才艮据本发明的一个实施例的实时在线吸收检测 系统中， 透光通路 2b、 光束变换单元 5的光轴以及样品单元 7的中心 轴同轴设置， 以确保具有线性形状的光源发出的光束 11能够通过样 品单元 7的中心轴， 从而增加入射到第一探测器 8上的样品光束 1 la 的光强。 在本发明提供的实时在线吸收检测系统中， 多个光学元件例 如透光通路 2b、 滤光片 3、 偏振器 4、 光束变换单元 5以及分束器 6 的位置可根据实际需要进行调节。 例如， 偏振器 4可放置在滤光片 3 前面或者光束变换单元 5后面。 再例如， 滤光片 3可放置在光束变换 单元 5的后面。  1 shows a real-time online absorption detection system in accordance with one embodiment of the present invention. As shown in FIG. 1, the real-time online absorption detecting system according to the present invention is a dual optical path absorption detecting system including a light source 1, a power source 2, a filter 3, a polarizer 4, a beam converting unit 5, a beam splitter 6, and a sample unit. 7. A first detector 8, a second detector 9 and a control module 10, wherein the power source 2 is for supplying power to the light source 1, which comprises a casing (not shown), the light source 1 is mounted in the casing, and the casing is adjacent to the optical path One side is provided with a light shielding plate 2a, and the light shielding plate 2a is provided with a light transmitting passage 2b for allowing the light beam 11 emitted from the light source to enter the optical path only from the light transmitting path 2b and preventing other light from leaking into the optical path. A real-time online absorption detection system in accordance with one embodiment of the present invention is installed in a black box to ensure that no external light is leaking into the absorption detection system. In the real-time online absorption detecting system according to an embodiment of the present invention, the light transmission path 2b, the optical axis of the beam converting unit 5, and the central axis of the sample unit 7 are coaxially disposed to ensure the light source having a linear shape. The light beam 11 can pass through the central axis of the sample unit 7, thereby increasing the light intensity of the sample beam 1 la incident on the first detector 8. In the real-time online absorption detecting system provided by the present invention, the positions of a plurality of optical elements such as the light transmitting path 2b, the filter 3, the polarizer 4, the beam converting unit 5, and the beam splitter 6 can be adjusted according to actual needs. For example, the polarizer 4 can be placed in front of the filter 3 or behind the beam converting unit 5. For another example, the filter 3 can be placed behind the beam converting unit 5.
光源发出的光束 11依次通过透光通路 2b、 滤光片 3和偏振器 4; 接着光源发出的光束 11经过光束变换单元 5; 随后光源发出的光束 11入射到分光器 6上， 其中分光器 6被设置成与光源发出的光束 1 1 的方向成一定的倾斜角度； 光源发出的光束 11经过分光器 6后分成 样品光束 11a和参考光束 l ib , 样品光束 11a通过样品单元 7后入射 到第一探测器 8上， 参考光束 l ib直接入射到第二探测器 9上， 其中 样品单元 7内设置有待测样品 7a， 样品光束 11a通过待测样品 7a， 第 一探测器 8记录经过待测样品 7a的样品光束 11a的光强 /; 。 第二探 测器 9记录参考光束 l ib的光强 /; 。 分光器 6的分光比 R由分光器 6 和入射到分光器 6上的光源发出的光束 1 1的入射角决定。 控制模块 10接受来自第一探测器 8的样品光束 1 1a的光强 /; 和来自第二探测器 9的参考光束 l ib的光强 /; ， 并根据公式 (1-1)或者 (1-2)获得待测样品 7a的透过率 T:
Figure imgf000009_0001
The light beam 11 emitted by the light source sequentially passes through the light transmission path 2b, the filter 3 and the polarizer 4; then the light beam 11 emitted from the light source passes through the beam converting unit 5; 11 is incident on the beam splitter 6, wherein the beam splitter 6 is disposed at a certain inclination angle with the direction of the light beam 1 1 emitted by the light source; the light beam 11 emitted from the light source passes through the beam splitter 6 and is divided into a sample beam 11a and a reference beam l ib , The sample beam 11a is incident on the first detector 8 after passing through the sample unit 7, and the reference beam 1 ib is directly incident on the second detector 9, wherein the sample to be tested 7a is disposed in the sample unit 7, and the sample beam 11a passes through the sample to be tested 7a, the first detector 8 records the light intensity of the sample beam 11a passing through the sample 7a to be tested. The second detector 9 records the light intensity of the reference beam l ib /; The splitting ratio R of the spectroscope 6 is determined by the incident angle of the beam 11 emitted from the spectroscope 6 and the light source incident on the spectroscope 6. The control module 10 accepts the light intensity of the sample beam 11a from the first detector 8 and the intensity of the reference beam lib from the second detector 9 and is according to equation (1-1) or (1- 2) Obtain the transmittance T of the sample to be tested 7a:
Figure imgf000009_0001
其中公式 (1-1)中的 R由下面公式 (3-1)给出，公式 (1-2)中的 R和 b均由 下面公式 (3-2)给出，并且公式 (1-1)中的 R或者公式 (1-2)中的 R和 b均 存储在控制模块 10中。 控制模块具体采用公式 (1-1)还是公式 (1-2)来 计算待测样品 7a的透过率 T， 取决于分光比 R的计算方法是采用公 式 (3-1)还是公式 (3-2)。 控制模块 10根据公式 (2)获得待测样品 7a的吸 收率 Abs: Wherein R in the formula (1-1) is given by the following formula (3-1), and R and b in the formula (1-2) are both given by the following formula (3-2), and the formula (1-1) R in the R or R and b in the formula (1-2) are all stored in the control module 10. The control module specifically calculates the transmittance T of the sample to be tested 7a according to the formula (1-1) or the formula (1-2), depending on whether the calculation method of the spectral ratio R is based on the formula (3-1) or the formula (3- 2). The control module 10 obtains the absorption rate A bs of the sample 7 to be tested according to formula (2) :
Abs=-log10(T) (2) A bs =-log 10 (T) (2)
实际使用时，公式 (1-1)中的分光器 6的分光比 R或者公式 (1-2)中的分 光器 6的分光比 R和参数 b通过应用本发明一个实施例的实时在线吸 收检测系统测试标准空白样品而获得。 做空白样品的测试时， 将标准 空白样品注入到样品单元 7内。 空白样品的测试应当每隔一段时间进 行一次或者根据实际需要进行。 根据分光比 R的计算方法不同， 下面 对空白样品的测试分别具体描述。 分光比 R的第一种计算方法通过第 一探测器 8记录经过标准空白样品的样品光束 11a的光强 11 第二探 测器 9记录标准空白样品的参考光束 l ib的光强 12。控制模块 10依据 公式 (3-1)获得分光器 6的分光比 R:
Figure imgf000010_0001
In actual use, the split ratio R of the spectroscope 6 in the formula (1-1) or the split ratio R and the parameter b of the spectroscope 6 in the formula (1-2) are detected by real-time online absorption using an embodiment of the present invention. The system is tested with a standard blank sample. When testing a blank sample, a standard blank sample is injected into the sample unit 7. The blank sample test should be performed at regular intervals or as needed. According to the calculation method of the splitting ratio R, the following tests are separately described for the blank samples. The first calculation method of the splitting ratio R records the light intensity of the sample beam 11a passing through the standard blank sample by the first detector 8 1 The second detector 9 records the light intensity 1 2 of the reference beam l ib of the standard blank sample. The control module 10 obtains the split ratio R of the spectroscope 6 according to the formula (3-1):
Figure imgf000010_0001
分光比 R的第二种计算方法通过第一探测器 8在一段时间内记录经过 标准空白样品的样品光束 11a的光强 11 第二探测器 9在同一段时间 内相同时刻或相近时刻记录标准空白样品的参考光束 l ib的光强 12。 控制模块 10依据以下方式获得分光器 6的分光比 R: 以 为纵坐标， 以 12为横坐标， 然后进行线性拟合， 可得拟合直线方程：The second calculation method of the splitting ratio R records the light intensity of the sample beam 11a passing through the standard blank sample by the first detector 8 for a period of time. 1 The second detector 9 records the standard at the same time or at the same time in the same period of time. The light intensity of the reference beam l ib of the blank sample is 1 2 . The control module 10 according to the following way to obtain the spectral beam splitter 6 ratio R: that the ordinate, the abscissa to 12, followed by a linear fit, fitting a straight line equation can be obtained:
Figure imgf000010_0002
Figure imgf000010_0002
拟合直线的斜率即为分光比 R， b为拟合直线的截距。 The slope of the fitted line is the split ratio R, and b is the intercept of the fitted line.
根据本发明的一个实施例的实时在线吸收检测系统能够对固体、 静态液体或者流动液体的待测样品的吸收率进行实时在线测量。 该实 时在线吸收检测系统的控制模块 10根据公式 (1)-(3)获得待测样品的吸 收率 Abs。 根据本发明的一个实施例的实时在线吸收检测系统的光源 发出的光束具有稳定的偏振态， 这使得分光器 6上的分光比 R稳定。 在本发明中， 分光比 R稳定是指在本发明的有效使用期限之内， 分光 比的相对标准偏差通常不大于大约 5%。 在本发明中， 相对标准偏差 ( RSD )是指:标准偏差与测量结果算术平均值的比值， 用公式表示如 下： RSD=S/X， 其中 S为标准偏差， X为测量平均值。 稳定的 偏振态是指光源发出的光束的 S偏振与 P偏振的比例之变化， 在本发 明的实时在线吸收检测系统的有效使用期限之内通常不会引起分光 器 6上的分光比 R的相对标准偏差大于大约 5%。 The real-time online absorption detection system according to one embodiment of the present invention is capable of real-time online measurement of the absorption rate of a sample to be tested of a solid, static liquid or flowing liquid. The control module 10 of the real-time online absorption detection system obtains the absorption rate A bs of the sample to be tested according to the formulas (1)-(3). The light beam emitted by the light source of the real-time online absorption detecting system according to an embodiment of the present invention has a stable polarization state, which makes the splitting ratio R on the spectroscope 6 stable. In the present invention, the fact that the spectral ratio R is stable means that the relative standard deviation of the spectral ratio is usually not more than about 5% within the effective life of the present invention. In the present invention, the relative standard deviation (RSD) is the ratio of the standard deviation to the arithmetic mean of the measurement results, and is expressed as follows: RSD = S / X, where S is the standard deviation and X is the measured average. The stable polarization state refers to the change of the ratio of the S polarization and the P polarization of the light beam emitted by the light source, and generally does not cause the relative polarization ratio R on the spectroscope 6 within the effective lifetime of the real-time online absorption detection system of the present invention. The standard deviation is greater than approximately 5%.
如图 1所示， 根据本发明的一个实施例的实时在线吸收检测系统 的光源 1可选自紫外、 可见、 红外光源中的至少一种光源， 光源发出 的光束通常包括 S偏振光（垂直偏振光）和 P偏振光（水平偏振光）， 光源的工作波长可以为单波长或者多波长。 在本发明中， S偏振光和 P偏振光分别代表垂直偏振光和水平偏振光， 其中的垂直和水平是指 相对样品光束 11a和参考光束 l ib所构成的平面， 光的偏振方向为垂 直或者平行。  As shown in FIG. 1, a light source 1 of a real-time online absorption detecting system according to an embodiment of the present invention may be selected from at least one of ultraviolet, visible, and infrared light sources, and the light beam emitted by the light source generally includes S-polarized light (vertical polarization). Light) and P-polarized light (horizonically polarized light), the operating wavelength of the light source can be single wavelength or multiple wavelengths. In the present invention, the S-polarized light and the P-polarized light respectively represent vertically polarized light and horizontally polarized light, wherein the vertical and horizontal directions refer to a plane formed by the sample beam 11a and the reference beam l ib , and the polarization direction of the light is vertical or parallel.
根据本发明的一个实施例的实时在线吸收检测系统，透光通路 2b 为狭缝或者孔。 本领域技术人员容易理解的是： 透光通路 2b也可以 采用其他的方式， 而这也将落在本发明的保护范围内。 According to a real-time online absorption detecting system according to an embodiment of the present invention, the light transmission path 2b is a slit or a hole. It will be easily understood by those skilled in the art that: the light transmission path 2b can also Other methods are employed, and this will also fall within the scope of the present invention.
当光源 1的工作波长为单波长时， 滤光片 3仅允许作为工作波长 的该单波长及其附近的波长通过。 当光源 1的工作波长为多波长时， 则需要与多个工作波长相对应的的多个滤波片 3a、 3b、 3c以及 3d， 多个滤光片 3a、 3b、 3c以及 3d可安装在一个转盘 14上。 多个滤波片 3a、 3b、 3c以及 3d分别允许不同工作波长的光束通过。 才艮据本发明 的一个实施例的实时在线吸收检测系统工作时， 控制模块 10根据待 测样品所需要的工作波长转动转盘 14， 以选择相应的滤波片。 图 4示 出了上面设置有多个滤光片的转盘 14的斜视图。 如图 4所示， 转盘 14包括本体 15、 设置在本体 15中心处的转盘中心轴 16以及设置在 本体 15周围的多个安装孔 15a， 安装孔 15a分别用于安装滤光片 3a、 3b、 3c以及 3d， 转盘 14可以绕其中心轴 16进行转动。 实际使用时， 通过控制模块 10或者手动方式转动转盘 14， 以便将相应的滤光片调 整就为与相应的工作波长适应， 从而允许相应工作波长的光束通过。 需要说明的是： 转盘 14也可以设置具有其他构造， 以安装多于 4个 或者少于 4个的滤光片， 而这也将落在本发明的保护范围内。  When the operating wavelength of the light source 1 is a single wavelength, the filter 3 allows only the single wavelength as the operating wavelength and the wavelength in the vicinity thereof to pass. When the operating wavelength of the light source 1 is multiple wavelengths, a plurality of filters 3a, 3b, 3c, and 3d corresponding to a plurality of operating wavelengths are required, and the plurality of filters 3a, 3b, 3c, and 3d may be mounted in one On the turntable 14. The plurality of filters 3a, 3b, 3c, and 3d allow light beams of different operating wavelengths to pass, respectively. When the real-time online absorption detecting system according to one embodiment of the present invention operates, the control module 10 rotates the turntable 14 according to the operating wavelength required for the sample to be tested to select the corresponding filter. Fig. 4 shows a perspective view of the turntable 14 on which a plurality of filters are disposed. As shown in FIG. 4, the turntable 14 includes a body 15, a turntable central shaft 16 disposed at the center of the body 15, and a plurality of mounting holes 15a disposed around the body 15, the mounting holes 15a for mounting the filters 3a, 3b, respectively. 3c and 3d, the turntable 14 is rotatable about its central axis 16. In actual use, the turntable 14 is rotated by the control module 10 or manually to adjust the corresponding filter to accommodate the corresponding operating wavelength, thereby allowing the beam of the corresponding operating wavelength to pass. It should be noted that the turntable 14 may also be provided with other configurations to mount more than four or less than four filters, and this will also fall within the scope of the present invention.
偏振器 4具有偏振面， 偏振面具有透光轴， 偏振器 4仅允许偏振 面内与透光轴方向平行的偏振光通过。 因而当光源发出的光束的最大 偏振分量为 S偏振光时， 通过适当放置偏振器 4使得偏振器 4仅允许 S偏振光通过， 如图 2所示。 需要说明的是： 当光源发出的光束 11的 最大偏振分量为 P偏振光时， 通过适当放置偏振器 4也可使得偏振器 4仅允许 P偏振光通过， 而这也将落在本发明的保护范围内。 此外， 当光源发出的光束的偏振态 （ S偏振光和 P偏振光之比） 艮稳定时， 这使得分光器 6上的分光比 R也保持稳定， 根据本发明一个实施例 的实时在线吸收检测系统可以不包括偏振器 4。  The polarizer 4 has a plane of polarization, the plane of polarization has a transmission axis, and the polarizer 4 allows only polarized light in the plane of polarization parallel to the direction of the transmission axis to pass. Therefore, when the maximum polarization component of the light beam emitted from the light source is S-polarized light, the polarizer 4 allows only the S-polarized light to pass by appropriately placing the polarizer 4, as shown in Fig. 2. It should be noted that when the maximum polarization component of the light beam 11 emitted by the light source is P-polarized light, the polarizer 4 can also allow the P-polarized light to pass only by appropriately placing the polarizer 4, and this will also fall under the protection of the present invention. Within the scope. Further, when the polarization state of the light beam emitted by the light source (the ratio of the S-polarized light to the P-polarized light) is stable, this makes the spectral ratio R on the spectroscope 6 also stable, real-time online absorption detection according to an embodiment of the present invention. The system may not include the polarizer 4.
在本发明的一个实施例中， 光束变换单元 5为透镜或者透镜组， 用于对从光源发出的光束 11进行准直和会聚。  In one embodiment of the invention, the beam transforming unit 5 is a lens or lens group for collimating and concentrating the light beam 11 emitted from the light source.
分光器 6由合适的材料制成， 从而允许从光源发出的光束按照一 定的分光比 R进行分光。 样品单元 7由合适的材料制成， 从而允许从光源发出的光束最大 程度地通过。 在才艮据本发明的一个实施例中， 样品单元 7包括中空本 体 13和设置在中空本体 13相对侧上的入口 13a和出口 13b， 待测流 动液体样品从样品单元 7的入口 13a流入并从出口 13b流出 （如图 1 所示） 。 根据本发明一个实施例的实时在线吸收检测系统能够测量流 动液体样品的吸收率 Abs。 在本发明中， 由于入口 13a和出口 13b设 置在样品单元的两端， 使得本发明的样品单元 7内的流动液体样品的 流速显著增加。 样品单元 7内的气泡容易从样品单元 7溢出。 本领域 技术人员容易理解的是： 用于流动液体样品的样品单元 7也可以具有 其他的构造， 而这也将落在本发明的保护范围内。 The beam splitter 6 is made of a suitable material to allow the light beam emitted from the light source to be split at a certain splitting ratio R. The sample unit 7 is made of a suitable material to allow the light beam emitted from the light source to pass the most. In an embodiment in accordance with the invention, the sample unit 7 comprises a hollow body 13 and an inlet 13a and an outlet 13b disposed on opposite sides of the hollow body 13, the flow of liquid sample to be tested flowing in from the inlet 13a of the sample unit 7 and from The outlet 13b flows out (as shown in Figure 1). A real-time online absorption detection system according to one embodiment of the present invention is capable of measuring the absorption rate A bs of a flowing liquid sample. In the present invention, since the inlet 13a and the outlet 13b are disposed at both ends of the sample unit, the flow rate of the flowing liquid sample in the sample unit 7 of the present invention is remarkably increased. The bubbles in the sample unit 7 easily overflow from the sample unit 7. It will be readily understood by those skilled in the art that the sample unit 7 for flowing liquid samples may also have other configurations, and this will also fall within the scope of the present invention.
第一探测器 8和第二探测器 9能够记录光源发出的光束 11的单 个或者多个工作波长的光强。 控制模块 10与第一探测器 8和第二探 测器 9耦联并进行通信， 接受来自第一探测器 8和第二探测器 9的待 测样品和标准空白样品的各自样品光束的强度和参考光束的强度， 并 基于公式（ 1 ) - ( 3 ) 获得待测样品的吸收率 Abs。 实施例 2 The first detector 8 and the second detector 9 are capable of recording the intensity of light of a single or multiple operating wavelengths of the beam 11 emitted by the source. The control module 10 is coupled to and communicates with the first detector 8 and the second detector 9 to receive the intensity and reference of the respective sample beams from the sample to be tested and the standard blank sample from the first detector 8 and the second detector 9. The intensity of the beam, and based on equations (1) - (3), obtain the absorbance A bs of the sample to be tested. Example 2
图 4示出了根据本发明另一个实施例的实时在线吸收检测系统。 该吸收检测系统是单光路吸收检测系统， 其包括光源 1、 电源 2、 滤 光片 3、 偏振器 4、 光束变换单元 5、 样品单元 7、 第一探测器 8以及 控制模块 10。 光源 1安装在罩壳中， 罩壳靠近光路的一侧设有遮光板 2a, 遮光板 2a上设置有透光通路 2b， 遮光板 2a的作用是使得光源发 出的光束 11仅从透光通路 2b进入光路，遮光板 2a可防止其他光泄漏 到光路中。 根据本发明另一个实施例的实时在线吸收检测系统安装在 一个暗箱中， 以保证没有外部光泄露到该吸收检测系统中。 在才艮据本 发明的另一个实施例的实时在线吸收检测系统中， 透光通路 2b、 光束 变换单元 5的光轴以及样品单元 7的中心轴同轴设置， 以确保具有线 性形状的从光源发出的光束 11能够通过样品单元 7的中心轴， 从而 增加入射到第一探测器 8上的样品光束 11a的光强。 在本发明提供的 实时在线吸收检测系统中， 多个光学元件例如透光通路 2b、滤光片 3、 偏振器 4以及光束变换单元 5等的位置可根据实际需要进行调节。 例 如， 偏振器 4可放置在滤光片 3前面或者光束变换单元 5后面。 再例 如， 滤光片 3可放置在束变换单元 5的后面。 4 illustrates a real-time online absorption detection system in accordance with another embodiment of the present invention. The absorption detecting system is a single optical path absorption detecting system comprising a light source 1, a power source 2, a filter 3, a polarizer 4, a beam converting unit 5, a sample unit 7, a first detector 8, and a control module 10. The light source 1 is mounted in the casing, and the light shielding plate 2a is disposed on a side of the casing near the optical path, and the light shielding plate 2a is provided with a light transmission passage 2b. The function of the light shielding plate 2a is to make the light beam 11 emitted from the light source only from the light transmission path 2b. Entering the optical path, the visor 2a prevents other light from leaking into the optical path. A real-time online absorption detection system in accordance with another embodiment of the present invention is installed in a black box to ensure that no external light is leaking into the absorption detection system. In a real-time online absorption detecting system according to another embodiment of the present invention, the light transmission path 2b, the optical axis of the beam converting unit 5, and the central axis of the sample unit 7 are coaxially disposed to ensure a slave light source having a linear shape. The emitted light beam 11 can pass through the central axis of the sample unit 7, thereby increasing the light intensity of the sample beam 11a incident on the first detector 8. Provided by the present invention In the real-time online absorption detecting system, the positions of a plurality of optical elements such as the light transmission path 2b, the filter 3, the polarizer 4, and the beam converting unit 5 can be adjusted according to actual needs. For example, the polarizer 4 can be placed in front of the filter 3 or behind the beam converting unit 5. For another example, the filter 3 can be placed behind the beam converting unit 5.
光源发出的光束 11依次通过透光通路 2b、 滤光片 3和偏振器 4; 接着光源发出的光束 11经过光束变换单元 5; 随后经过变换的光束 11通过样品单元 7后变成样品光束 11 a， 该样品光束 11 a入射到第一 探测器 8上， 其中样品单元 7内容纳有待测样品 7a， 样品光束 11a通 过待测样品 7a， 第一探测器 8记录经过待测样品 7a的样品光束 11a 的光强 /; 。 控制模块 10接受来自第一探测器 8的样品光束 11a的光 强 /; 并根据公式 (4)获得待测样品 7a的透过率 T: The light beam 11 emitted from the light source sequentially passes through the light transmission path 2b, the filter 3 and the polarizer 4; then the light beam 11 emitted from the light source passes through the beam converting unit 5; then the converted light beam 11 passes through the sample unit 7 and becomes the sample beam 11a. The sample beam 11a is incident on the first detector 8, wherein the sample unit 7 contains the sample 7a to be tested, the sample beam 11a passes through the sample 7a to be tested, and the first detector 8 records the sample beam passing through the sample 7a to be tested. 11a light intensity /; The control module 10 receives the light intensity of the sample beam 11a from the first detector 8 and obtains the transmittance T of the sample 7a to be tested according to the formula (4):
Figure imgf000013_0001
Figure imgf000013_0001
控制模块 10根据公式 (2)获得待测样品 7a的吸收率 Abs。 实际使用时， 首先用该吸收测量系统对标准空白样品进行测试， 然后再用该系统对 待测样品进行测试， 标准空白样品的测试应当每隔一段时间进行一次 或者根据实际需要进行。 具体而言， 将标准空白样品（或者待测样品） 注入到样品单元 7内， 并且然后通过第一探测器 8记录经过标准空白 样品（或者待测样品）的样品光束 11a的光强 ^ ( /； )。 控制模块 10 依据公式 (4)获得待测样品 7a的透过率 T。 The control module 10 obtains the absorption rate A bs of the sample 7 to be tested according to the formula (2). In actual use, the standard blank sample is first tested with the absorption measurement system, and then the system is tested with the system. The test of the standard blank sample should be performed once every other time or according to actual needs. Specifically, a standard blank sample (or a sample to be tested) is injected into the sample unit 7, and then the light intensity of the sample beam 11a passing through the standard blank sample (or the sample to be tested) is recorded by the first detector 8 ( / ;). The control module 10 obtains the transmittance T of the sample 7a to be tested according to the formula (4).
需要说明的是， 根据本发明的另一个实施例的单光路实时在线 吸收检测系统的光学元件例如滤光片、 偏振器、 光束变换单元等的选 择、 制造以及设置方式与根据本发明的一个实施例的双光路实时在线 吸收检测系统中相应光学元件类似， 这里不再累述。  It should be noted that the selection, manufacture, and arrangement of optical elements such as filters, polarizers, beam transform units, and the like of a single optical path real-time online absorption detecting system according to another embodiment of the present invention and an implementation according to the present invention The corresponding optical components in the dual optical path real-time online absorption detection system are similar, and will not be described here.
根据本发明的另一个实施例的该单光路实时在线吸收检测系统 能够对固体、 静态液体或者流动液体的待测样品的吸收率进行实时在 线测量。 具体而言， 第一探测器 8能够记录光源发出的光束 11的单 个或者多个工作波长的光强。 控制模块 10与第一探测器 8耦联并进 行通信， 接受来自第一探测器 8的待测样品和标准空白样品的各自样 品光束的强度并基于公式（2 ) 和 （4 )获得待测样品的吸收率 Abs。 根据本发明的另一个实施例的单光路实时在线吸收检测系统的光源 发出的光束具有稳定的光强， 这使得在不同时刻测量的同一待测样品 的吸收率 Abs稳定。 经过实验检测， 同一待测样品的吸收率的相对标 准偏差通常不大于大约 5%， 相对标准偏差的定义见上文。 在本发明 中， 同一待测样品的吸收率 Abs稳定是指在本发明的实时在线吸收检 The single-light path real-time on-line absorption detection system according to another embodiment of the present invention is capable of real-time on-line measurement of the absorption rate of a sample to be tested of a solid, static liquid or flowing liquid. In particular, the first detector 8 is capable of recording the intensity of light of a single or multiple operating wavelengths of the beam 11 emitted by the source. The control module 10 is coupled to and communicates with the first detector 8 to receive the intensity of the respective sample beam from the sample to be tested and the standard blank sample from the first detector 8 and obtain the sample to be tested based on equations (2) and (4). Absorption rate A bs . The light beam emitted from the light source of the single-light path real-time online absorption detecting system according to another embodiment of the present invention has a stable light intensity, which makes the absorption rate A bs of the same sample to be measured measured at different times stable. After experimental testing, the relative standard deviation of the absorption rate of the same sample to be tested is usually no more than about 5%, and the relative standard deviation is defined above. In the present invention, the absorption rate A bs of the same sample to be tested is stable, which means the real-time online absorption test in the present invention.
实施例 3 Example 3
图 2示出了如图 1所示的实时在线吸收检测系统一个实例。 该实例采 用低压汞灯作为光源 1， 光源 1能发出波长大约为 254nm的紫外光束 11， 光源 1安装在罩壳中， 罩壳的一侧设置有遮光板 2a， 遮光板 2a 上设置有透光通路 2b， 光源 1发出的波长为 254nm的紫外光束 11仅 从例如为狭缝或者孔的透光通路 2b透过， 遮光板 2a防止其他光泄漏 到光路中。 光源 1发出的波长大约为 254nm的紫外光束 11依次经过 滤光片 3、 偏振器 4以及光束变换单元 5 (例如透镜或者透镜组） ， 随后光束 11入射到分光器 6上分成两束光：样品光束 11a和参考光束 l ib,样品光束 11a经过样品单元 7并经过设置在其中的待测样品（或 标准空白样品） ， 第一探测器 8和第二探测器 9分别用于记录入射到 其上的样品光束 11a和参考光束 l ib的光强。控制模块 10与第一探测 器 8和第二探测器 9耦联并进行通信， 接受来自第一探测器 8和第二 探测器 9的标准空白样品和待测样品的各自样品光束的强度和参考光 束的强度， 并基于公式（ 1 ) - ( 3 ) 获得待测样品在大约 254nm波长 处的吸收率 Abs。 才艮据如图 1所示的实时在线吸收检测系统一个实例 的光源发出的光束具有稳定的偏振态， 这使得分光器 6上的分光比 R 稳定。 Figure 2 shows an example of a real-time online absorption detection system as shown in Figure 1. The example uses a low-pressure mercury lamp as the light source 1, and the light source 1 can emit an ultraviolet light beam 11 having a wavelength of about 254 nm. The light source 1 is mounted in the casing, and one side of the casing is provided with a light shielding plate 2a, and the light shielding plate 2a is provided with light transmission. In the passage 2b, the ultraviolet light beam 11 having a wavelength of 254 nm emitted from the light source 1 is transmitted only from the light transmission path 2b which is, for example, a slit or a hole, and the light shielding plate 2a prevents other light from leaking into the optical path. The ultraviolet light beam 11 emitted by the light source 1 having a wavelength of about 254 nm passes through the filter 3, the polarizer 4, and the beam converting unit 5 (for example, a lens or a lens group), and then the light beam 11 is incident on the beam splitter 6 to be divided into two beams: a sample The light beam 11a and the reference light beam l ib, the sample light beam 11a passes through the sample unit 7 and passes through a sample to be tested (or a standard blank sample) disposed therein, and the first detector 8 and the second detector 9 are respectively used for recording incident thereon The intensity of the sample beam 11a and the reference beam l ib . The control module 10 is coupled to and communicates with the first detector 8 and the second detector 9 to receive the intensity and reference of the respective sample beams from the standard blank sample of the first detector 8 and the second detector 9 and the sample to be tested. The intensity of the beam, and based on equations (1) - (3), obtain the absorbance A bs of the sample to be tested at a wavelength of approximately 254 nm. The light beam emitted by the light source according to an example of the real-time online absorption detecting system shown in Fig. 1 has a stable polarization state, which makes the splitting ratio R on the spectroscope 6 stable.
根据本发明一个实施例的实时在线吸收检测系统可以不包括偏 振器 4。在该不包括偏振器 4的实时在线吸收检测系统的一个实例中， 滤光片 3允许波长大约为 254nm的紫外光束通过，采用滤光片 3可以 避免其他波长光的干扰。 光束变换单元 5 (例如透镜或者透镜组） 、 分光器 6以及样品单元 7采用石英制备， 并且分光器 6例如可设置成 与样品光束成 45度。 光源 1发出的光束 11具有稳定的偏振态， 分光 器 6上的分光比 R保持稳定。 在本实例中， 经实验测量， 分光比大约 在 7~8左右， 分光比的相对标准偏差小于大约 4%。 居本发明一个 实施例的实时在线吸收检测系统， 当其包括偏振器 4并且偏振器 4只 允许 S偏振通过时， 采用石英制备的分光器 6上的分光比 R大约为 4-5左右， 分光比的相对标准偏差小于大约 2%。 A real-time online absorption detecting system according to an embodiment of the present invention may not include the polarizer 4. In one example of the real-time in-line absorption detection system that does not include the polarizer 4, the filter 3 allows an ultraviolet beam having a wavelength of about 254 nm to pass, and the filter 3 can avoid interference of other wavelengths of light. Beam transform unit 5 (for example, a lens or a lens group), The beam splitter 6 and the sample unit 7 are prepared using quartz, and the beam splitter 6 can be set, for example, at 45 degrees to the sample beam. The light beam 11 emitted from the light source 1 has a stable polarization state, and the splitting ratio R on the spectroscope 6 remains stable. In this example, experimentally measured, the split ratio is about 7-8, and the relative standard deviation of the split ratio is less than about 4%. In a real-time online absorption detecting system according to an embodiment of the present invention, when the polarizer 4 is included and the polarizer 4 only allows S polarization to pass, the splitting ratio R on the spectroscope 6 prepared by quartz is about 4-5, and the splitting is performed. The relative standard deviation of the ratio is less than about 2%.
在如图 1所示的实时在线吸收检测系统一个实例中， 为了保证整 个实时在线吸收检测系统的测量准确性， 例如为狭缝或者孔的透光通 路 2b、例如为透镜或者透镜组的光束变换单元 5的光轴以及样品单元 7的中心轴同轴设置。 这确保具有线性形状的从光源发出的波长大约 为 254nm的紫外光束 11能够通过样品单元 7的中心轴， 从而增加入 射到第一探测器 8上的样品光束 11a的光强。  In an example of the real-time online absorption detection system shown in FIG. 1, in order to ensure the measurement accuracy of the entire real-time online absorption detection system, for example, a light transmission path 2b of a slit or a hole, for example, a beam or a lens group The optical axis of the unit 5 and the central axis of the sample unit 7 are coaxially arranged. This ensures that the ultraviolet beam 11 having a linear shape from the light source and having a wavelength of about 254 nm can pass through the central axis of the sample unit 7, thereby increasing the intensity of the sample beam 11a incident on the first detector 8.
在才艮据本发明又一个实施例的实时在线吸收检测系统中， 滤光 片 3允许波长大约为 254nm的紫外光束通过，采用滤光片 3可以避免 其他波长光的干扰。 偏振器 4、 光束变换单元 5 (例如透镜或者透镜 组）、 分光器 6、 样品单元 7等适合采用允许紫外光通过的材料制备。 这些材料包括但不局限于： 石英玻璃、 紫外透过玻璃或者聚合物、 高 硼玻璃、 蓝宝石、 氟化镁， 氟化锂等， 其中石英是在紫外区域应用的 最广泛的材料。 例如在一个实例中， 波长大约为 254nm的紫外灯， 通 过该系统测得其最大偏振分量与灯管方向平行。 而偏振器 4采用石英 作为衬底并涂覆有薄膜， 偏振器 4的偏振轴允许光源 1发出的波长大 约为 254nm的紫外光束中的偏振分量 S偏振光通过。 因此， 为了增加 第一探测器 8和第二探测器 9上样品光束和参考光束的强度， 使得紫 外灯灯管垂直放置 （如图 2所示） 。  In the real-time online absorption detecting system according to still another embodiment of the present invention, the filter 3 allows an ultraviolet light beam having a wavelength of about 254 nm to pass, and the filter 3 can avoid interference of light of other wavelengths. The polarizer 4, the beam converting unit 5 (e.g., lens or lens group), the beam splitter 6, the sample unit 7, and the like are suitably prepared using a material that allows ultraviolet light to pass therethrough. These materials include, but are not limited to, quartz glass, UV-transmissive glass or polymers, high boron glass, sapphire, magnesium fluoride, lithium fluoride, etc., of which quartz is the most widely used material in the ultraviolet region. For example, in one example, an ultraviolet lamp having a wavelength of about 254 nm is measured by the system to have a maximum polarization component parallel to the direction of the tube. The polarizer 4 uses quartz as a substrate and is coated with a thin film. The polarization axis of the polarizer 4 allows the polarized light S-polarized light in the ultraviolet light beam having a wavelength of about 254 nm emitted from the light source 1 to pass. Therefore, in order to increase the intensity of the sample beam and the reference beam on the first detector 8 and the second detector 9, the ultraviolet lamp tube is placed vertically (as shown in Fig. 2).
样品单元 7采用如图 2所示的结构， 样品单元 7采用石英制备以 保证紫外光束可以通过， 样品单元 7具有圆形截面， 包括中空本体 13 和设置在其两端的入口 13a和出口 13b， 待测样品从入口 13a流入并 从出口 13b流出。 在实际应用中， 对圆形截面的样品单元 7， 如果在 紫外灯一侧的遮光板上设置的是狭缝， 而不是孔， 样品单元 7的放置 方向应与狭缝的方向平行。 如果在紫外灯一侧的遮光板开的是小孔， 则样品单元 7的放置方向不受此限制。本领域技术人员容易理解的是： 其他的构造， 而这也将落在本发明的保护范围内。 The sample unit 7 adopts the structure shown in FIG. 2, the sample unit 7 is prepared by using quartz to ensure that the ultraviolet light beam can pass, and the sample unit 7 has a circular cross section, including the hollow body 13 and the inlet 13a and the outlet 13b disposed at both ends thereof. The test sample flows in from the inlet 13a and flows out from the outlet 13b. In practical applications, for sample unit 7 of circular cross section, if A slit is provided on the light shielding plate on the side of the ultraviolet lamp, instead of the hole, and the sample unit 7 is placed in a direction parallel to the direction of the slit. If the visor on the side of the ultraviolet lamp is open with a small hole, the orientation of the sample unit 7 is not limited thereto. Those skilled in the art will readily appreciate: Other configurations, and this will also fall within the scope of the present invention.
例如在一个实例中， 第一探测器 8和第二探测器 9采用紫外响应 型硅光电池。 紫外响应型硅光电池应该在所选择的紫外工作波长有响 应。 紫外响应型硅光电池有效面积的大小应大于紫外光束落在紫外响 应型硅光电池上的光斑大小， 以确保紫外响应型硅光电池可以接收到 全部光信号的能量。  For example, in one example, the first detector 8 and the second detector 9 employ an ultraviolet responsive type of silicon photo cell. UV-responsive silicon photocells should respond at selected UV operating wavelengths. The effective area of the UV-responsive silicon photocell should be larger than the spot size of the UV beam falling on the UV-responsive silicon photocell to ensure that the UV-responsive silicon photocell can receive the energy of all optical signals.
需要说明的是： 如果紫外灯的输出光强稳定， 则如 2所示的双光 路系统也可以简化为单光路系统， 如图 4所示， 即可以省略分光器 6 和用于参考光束的第二探测器 9。  It should be noted that: if the output intensity of the ultraviolet lamp is stable, the dual optical path system as shown in 2 can also be simplified into a single optical path system. As shown in FIG. 4, the optical splitter 6 and the reference beam can be omitted. Two detectors 9.
为了增加两个探测器的光强， 来自紫外灯的偏振态首先能够被测 量。 如果来自紫外灯的光束是部分偏振光， 则应当调整紫外灯管的对 准方向， 以确保来自紫外灯的光束的最大偏振部分与偏振器 4的偏振 方向平行。 因此， 可确保最大光束能量能够透过偏振器 4。  In order to increase the light intensity of the two detectors, the polarization from the UV lamp can first be measured. If the beam from the UV lamp is partially polarized, the alignment of the UV lamp should be adjusted to ensure that the maximum polarization of the beam from the UV lamp is parallel to the polarization of the polarizer 4. Therefore, it is ensured that the maximum beam energy can pass through the polarizer 4.
根据本发明上述实施例的实时在线吸收检测系统采用低成本光源与 滤光片结合来选择具有特定波长的测量用光束， 从而克服了现有技术 的吸收检测系统的采用高性能的光源与光栅结合来选择测量用光束 而导致成本高的缺点。 The real-time online absorption detecting system according to the above embodiment of the present invention uses a low-cost light source in combination with a filter to select a measuring beam having a specific wavelength, thereby overcoming the combination of a high-performance light source and a grating of the prior art absorption detecting system. To choose the measurement beam, which leads to the disadvantage of high cost.

Claims

1. 一种实时在线吸收检测系统，其包括仅允许从透光通路进入第 一光路的光源、 沿第一光路设置的滤光片、 光束变换单元、 分光器、 样品单元、 第一探测器以及设置在第二光路上的第二探测器， 第一光 路和第二光路在分光器处分开， 所述吸收检测系统还包括控制模块， 控制模块与第一探测器和第二探测器耦联并通信， 用于获得样品单元 中待测样品的吸收率， 其中光源、 滤光片、 光束变换单元、 分光器、 样品单元以及第一探测器和第二探测器放置在暗箱中， 透光通路、 光 束变换单元的光轴以及样品单元的中心轴同轴设置， 其特征在于， 光 源发出的光束具有稳定的偏振态， 这使得分光器的分光比 R稳定。 A real-time online absorption detecting system comprising a light source that allows only a light path from a light path, a filter disposed along a first light path, a beam converting unit, a beam splitter, a sample unit, a first detector, and a second detector disposed on the second optical path, the first optical path and the second optical path being separated at the optical splitter, the absorption detecting system further comprising a control module, the control module being coupled to the first detector and the second detector Communication for obtaining an absorption rate of a sample to be tested in a sample unit, wherein the light source, the filter, the beam conversion unit, the beam splitter, the sample unit, and the first detector and the second detector are placed in a dark box, the light transmission path, The optical axis of the beam converting unit and the central axis of the sample unit are coaxially arranged, characterized in that the light beam emitted from the light source has a stable polarization state, which makes the splitting ratio R of the spectroscope stable.
2. 根据权利要求 1所述的实时在线吸收检测系统， 其特征在于， 所述吸收检测系统还包括设置在光束变换单元之前或之后的偏振器， 偏振器使得光源发出的光束中的最大偏振分量通过， 从而增加第一探 测器和第二探测器上的光强。  2. The real-time online absorption detecting system according to claim 1, wherein the absorption detecting system further comprises a polarizer disposed before or after the beam converting unit, wherein the polarizer causes a maximum polarization component of the light beam emitted from the light source. By, thereby increasing the light intensity on the first detector and the second detector.
3. 根据权利要求 1所述的实时在线吸收检测系统， 其特征在于， 待测样品为固体样品、 静态液体样品或者流动液体样品。  3. The real-time online absorption detection system according to claim 1, wherein the sample to be tested is a solid sample, a static liquid sample or a flowing liquid sample.
4. 根据权利要求 1所述的实时在线吸收检测系统， 其特征在于， 所述吸收检测系统的光源选自紫外、 可见或者红外光源中的至少一 种。  4. The real-time online absorption detection system according to claim 1, wherein the light source of the absorption detecting system is selected from at least one of an ultraviolet, visible or infrared light source.
5. 根据权利要求 1所述的实时在线吸收检测系统， 其特征在于， 当光源发出的光束包括多个工作波长时， 则需要与各个工作波长的光 束相对应的多个滤光片， 此时多个滤光片设置在转盘上， 转盘通过控 制模块进行转动控制或者通过手动方式进行转动控制， 以便将相应的 滤光片调整就为与相应的工作波长相适应， 从而允许相应工作波长的 光束通过。  5. The real-time online absorption detection system according to claim 1, wherein when the light beam emitted by the light source comprises a plurality of operating wavelengths, a plurality of filters corresponding to the light beams of the respective working wavelengths are required, A plurality of filters are arranged on the turntable, and the turntable is rotated or controlled by a control module or manually controlled to adjust the corresponding filter to be adapted to the corresponding operating wavelength, thereby allowing a beam of the corresponding working wavelength. by.
6. 根据权利要求 1所述的实时在线吸收检测系统， 其特征在于， 光源设置在罩壳中， 透光通路为设置在罩壳上邻近光路侧的狭缝或者 孔。 6. The real-time online absorption detection system according to claim 1, wherein the light source is disposed in the casing, and the light transmission path is a slit or a hole disposed on the casing adjacent to the optical path side.
7. 根据权利要求 3所述的实时在线吸收检测系统， 其特征在于， 当待测样品为流动液体样品时， 样品单元包括中空本体、 设置在中空 本体两端的入口和出口， 流动液体样品从入口流入并从出口流出。 7. The real-time online absorption detecting system according to claim 3, wherein when the sample to be tested is a flowing liquid sample, the sample unit comprises a hollow body, an inlet and an outlet disposed at both ends of the hollow body, and a flowing liquid sample from the inlet Flow in and out of the exit.
8. 根据权利要求 1所述的实时在线吸收检测系统， 其特征在于， 光束变换单元为透镜或者透镜组。  8. The real-time online absorption detecting system according to claim 1, wherein the beam converting unit is a lens or a lens group.
9. 根据权利要求 1所述的实时在线吸收检测系统， 其特征在于， 分光器的分光比 R的相对标准偏差不大于大约 5%。  9. The real-time online absorption detection system according to claim 1, wherein the spectrometer has a relative standard deviation of the spectral ratio R of not more than about 5%.
10. 一种实时在线吸收检测系统， 其包括仅允许从透光通路进入 光路的光源、 沿光路设置的滤光片、 光束变换单元、 样品单元和探测 器， 所述吸收检测系统还包括控制模块， 控制模块与探测器耦联并通 信， 用于获得样品单元中待测样品的吸收率， 其中光源、 滤光片、 光 束变换单元、 样品单元以及探测器放置在暗箱中， 透光通路、 光束变 换单元的光轴以及样品单元的中心轴同轴设置， 其特征在于， 光源发 出的光束具有稳定的光强， 这使得在不同时刻测量的同一待测样品的 吸收率稳定。  10. A real-time online absorption detection system comprising a light source that only allows access to an optical path from a light transmissive path, a filter disposed along the optical path, a beam transform unit, a sample unit, and a detector, the absorption detection system further comprising a control module The control module is coupled and communicated with the detector for obtaining the absorption rate of the sample to be tested in the sample unit, wherein the light source, the filter, the beam conversion unit, the sample unit and the detector are placed in the dark box, the light transmission path, the light beam The optical axis of the transform unit and the central axis of the sample unit are coaxially arranged, characterized in that the light beam emitted by the light source has a stable light intensity, which makes the absorption rate of the same sample to be measured measured at different times stable.
11. 根据权利要求 10所述的实时在线吸收检测系统， 其特征在 于， 所述吸收检测系统还包括设置在光束变换单元之前或之后的偏振 器， 偏振器使得光源发出的光束中的最大偏振分量通过， 从而增加探 测器上的光强。  11. The real-time online absorption detecting system according to claim 10, wherein the absorption detecting system further comprises a polarizer disposed before or after the beam converting unit, wherein the polarizer causes a maximum polarization component of the light beam emitted by the light source. Pass to increase the light intensity on the detector.
12. 根据权利要求 10所述的实时在线吸收检测系统， 其特征在 于， 待测样品为固体样品、 静态液体样品或者流动液体样品。  12. The real-time online absorption detection system according to claim 10, wherein the sample to be tested is a solid sample, a static liquid sample or a flowing liquid sample.
13. 根据权利要求 10所述的实时在线吸收检测系统， 其特征在 于， 所述吸收检测系统的光源选自紫外、 可见或者红外光源中的至少 一种。  13. The real-time online absorption detection system of claim 10, wherein the light source of the absorption detection system is selected from at least one of an ultraviolet, visible, or infrared source.
14. 根据权利要求 10所述的实时在线吸收检测系统， 其特征在 于， 当光源发出的光束包括多个工作波长时， 则需要与各个工作波长 的光束相对应的多个滤光片， 此时多个滤光片设置在转盘上， 转盘通 过控制模块或者通过手动方式进行转动控制， 以便将相应的滤光片调 整就为与相应的工作波长相适应， 从而允许相应工作波长的光束通 过。 14. The real-time online absorption detection system according to claim 10, wherein when the light beam emitted by the light source comprises a plurality of operating wavelengths, a plurality of filters corresponding to the light beams of the respective working wavelengths are required, A plurality of filters are disposed on the turntable, and the turntable is controlled by a control module or manually, so that the corresponding filter is adjusted to be compatible with the corresponding operating wavelength, thereby allowing the light beam of the corresponding working wavelength to pass. Over.
15. 根据权利要求 10所述的实时在线吸收检测系统， 其特征在 于， 光源设置在罩壳中， 透光通路为设置在罩壳上邻近光路侧的狭缝 或者孔。  15. The real-time online absorption detection system according to claim 10, wherein the light source is disposed in the casing, and the light transmission path is a slit or a hole disposed on the casing adjacent to the optical path side.
16. 根据权利要求 10所述的实时在线吸收检测系统， 其特征在 于， 当待测样品为流动液体样品时， 样品单元包括中空本体、 设置在 中空本体两端的入口和出口， 流动液体样品从入口流入并从出口流 出。  16. The real-time online absorption detection system according to claim 10, wherein when the sample to be tested is a flowing liquid sample, the sample unit comprises a hollow body, an inlet and an outlet disposed at both ends of the hollow body, and a flowing liquid sample from the inlet Flow in and out of the exit.
17. 根据权利要求 10所述的实时在线吸收检测系统， 其特征在 于， 光束变换单元为透镜或者透镜组。  17. The real-time online absorption detection system according to claim 10, wherein the beam transformation unit is a lens or a lens group.
18. 根据权利要求 10所述的实时在线吸收检测系统， 其特征在 于， 同一待测样品的吸收率通过对由实时在线吸收检测系统测量的待 测样品的样品光束的光强 ι'和空白样品的样品光束的光强 A的比值求  18. The real-time online absorption detection system according to claim 10, wherein the absorption rate of the same sample to be tested is passed through a light intensity ι' and a blank sample of the sample beam of the sample to be tested measured by the real-time online absorption detection system. The ratio of the intensity A of the sample beam
5%。 5%.
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