CN115575340B - Absorbance detection device and method - Google Patents
Absorbance detection device and method Download PDFInfo
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- CN115575340B CN115575340B CN202211393413.1A CN202211393413A CN115575340B CN 115575340 B CN115575340 B CN 115575340B CN 202211393413 A CN202211393413 A CN 202211393413A CN 115575340 B CN115575340 B CN 115575340B
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- 238000001514 detection method Methods 0.000 title claims abstract description 80
- 238000002835 absorbance Methods 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 121
- 230000005540 biological transmission Effects 0.000 claims abstract description 44
- 238000004458 analytical method Methods 0.000 claims description 21
- 238000011144 upstream manufacturing Methods 0.000 claims description 8
- 239000013307 optical fiber Substances 0.000 description 5
- 238000002798 spectrophotometry method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052768 actinide Inorganic materials 0.000 description 2
- 150000001255 actinides Chemical class 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 229910052747 lanthanoid Inorganic materials 0.000 description 2
- 150000002602 lanthanoids Chemical class 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
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- 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
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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Abstract
The invention provides an absorbance detection device and a method, wherein the absorbance detection device comprises a pump and a transmission pipeline; the two bubble detection units are sequentially arranged on the transmission pipeline and are respectively used for detecting bubbles in the liquid to be detected in the transmission pipeline; the liquid to be measured enters the transmission pipeline and the liquid core waveguide; the measuring light emitted by the light source enters the liquid core waveguide, and the detector is used for receiving the measuring light emitted from the liquid core waveguide; and the calculation unit obtains the absorbance A of the liquid to be measured by using the parameters of the bubbles, the transmission pipeline and the liquid core waveguide and the measuring light. The invention has the advantages of accurate detection and the like.
Description
Technical Field
The invention relates to liquid analysis, in particular to an absorbance detection device and method.
Background
When lanthanide and actinide elements are researched and analyzed in a solution, chemical analysis methods such as extraction separation and ion exchange are complicated, and the valence state of the elements is changed to influence accurate determination in the process of adjusting reaction conditions and operating. Because each valence state of lanthanide series and actinide series elements has characteristic absorption peak, the spectrophotometry method is selected to directly measure without separation. Spectrophotometry is used for quantitatively and qualitatively analyzing a substance to be detected by measuring the absorbance of the substance at a specific wavelength or within a certain wavelength range, and the absorption selectivity of the substance to light complies with the principle of Lambert-beer law.
In the field of trace element research and analysis by using a spectrophotometry, the sensitivity and the detection limit of an analysis sample are improved by using a liquid core waveguide capillary pool by utilizing the characteristic of high sensitivity of a long optical path. In the measuring process, the problem that bubbles remained in the long-optical-path liquid flow cell influence the detection signal is solved, and the detection efficiency is greatly influenced. When using liquid core waveguide at present, avoid the processing method of bubble influence, more adoption is with capillary flow-through cell degasification processing, specifically as follows:
1. and introducing a vacuum environment, placing the liquid core waveguide tube in a vacuum container, and permeating the tiny bubbles adsorbed on the inner wall into the vacuum environment through the tube wall by utilizing the permeability characteristic of the Teflon AF material.
2. The sample is degassed by centrifugation using a gas permeable microchannel.
However, the above method is only suitable for the first type liquid core waveguide with gas permeability of the capillary, and is not suitable for the second type liquid core waveguide with a coating layer in the capillary; in addition, the centrifugal device increases the complexity of the whole device, and the centrifugal device can cause interference influence such as vibration on the detection device.
Disclosure of Invention
In order to overcome the defects in the prior art scheme, the invention provides an absorbance detection device.
The purpose of the invention is realized by the following technical scheme:
the absorbance detection device comprises a pump and a transmission pipeline; the absorbance detection device further includes:
the two bubble detection units are sequentially arranged on the transmission pipeline and are respectively used for detecting bubbles in the liquid to be detected in the transmission pipeline;
the liquid to be detected enters the transmission pipeline and the liquid core waveguide; the measuring light emitted by the light source enters the liquid core waveguide, and the detector is used for receiving the measuring light emitted from the liquid core waveguide;
and the calculation unit is used for obtaining the absorbance A of the liquid to be measured by using the parameters of the bubbles, the transmission pipeline and the liquid core waveguide and the measuring light.
The invention also aims to provide an absorbance detection method, and the invention aims to be realized by the following technical scheme:
an absorbance detection method, comprising:
the liquid to be measured enters the transmission pipeline and the liquid core waveguide;
two bubble detection units which are sequentially arranged on the transmission pipeline detect the parameters of bubbles in the liquid to be detected;
measuring light emitted by the light source enters the liquid core waveguide, passes through the liquid core waveguide and is received by the detector, and output signals are sent to the computing unit;
and the computing unit obtains the absorbance A of the liquid to be measured by using the parameters of the bubbles, the parameters of the transmission pipeline and the output signal.
Compared with the prior art, the invention has the following beneficial effects:
the detection result is accurate;
two bubble detection units are arranged to obtain bubble information, correct the calculation of absorbance, eliminate the influence of bubbles on spectral data, remarkably reduce the error of an analysis result and improve the detection accuracy;
the problem that bubbles entering liquid through the liquid core waveguide easily affect detection signals is solved, the stability of the signals can be greatly improved, the detection mode of the liquid core waveguide is more reliable, the problem that residual bubbles in a long-optical-path liquid flow cell affect the detection signals is solved, and the detection efficiency is greatly improved;
the invention has wide application scene and no limit to the type of the liquid core waveguide; the device is simple and easy to operate; the device and other environment interference influence is less; and the debugging is easy to realize.
Drawings
The disclosure of the present invention will become more readily understood with reference to the accompanying drawings. As is readily understood by those skilled in the art: these drawings are only for illustrating the technical solutions of the present invention and are not intended to limit the scope of the present invention. In the figure:
fig. 1 is a schematic structural view of an absorbance detection device according to an embodiment of the present invention.
Detailed Description
Fig. 1 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and reproduce the invention. Some conventional aspects have been simplified or omitted for the purpose of teaching the technical solutions of the present invention. Those skilled in the art will appreciate that variations or substitutions from these embodiments will be within the scope of the 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. Thus, the present invention is not limited to the following alternative embodiments, but is only limited by the claims and their equivalents.
Example 1:
fig. 1 schematically shows a schematic configuration diagram of an absorbance detection device according to an embodiment of the present invention, and as shown in fig. 1, the absorbance detection device includes:
a pump 3 and a transfer pipe 2;
the two bubble detection units 5-6 are sequentially arranged on the transmission pipeline 2 and are respectively used for detecting bubbles in the liquid to be detected in the transmission pipeline 2;
the liquid to be detected enters the transmission pipeline 2 and the liquid core waveguide 7; the measuring light emitted by the light source enters the liquid core waveguide 7, and the detector is used for receiving the measuring light emitted from the liquid core waveguide 7;
and the calculation unit is used for obtaining the absorbance A of the liquid to be measured by using the parameters of the bubbles, the transmission pipeline 2 and the liquid core waveguide 7 and the measuring light.
In order to accurately obtain the absorbance A, further, the absorbanceN is the initial intensity of the measuring light emitted by the light source, N 0 The intensity of the measuring light received by the detector, D the diameter of the transmission pipeline 2, T the time required for each bubble in the liquid to be detected to pass through any bubble detection unit, T the time required for each bubble in the liquid to be detected to pass through the two bubble detection units 5-6, and l the distance between the two bubble detection units 5-6;
r is the radius of the capillary of the liquid core waveguide 7, zeta is the refractive index of the measuring light in the liquid to be measured, v is the kinematic viscosity of the liquid to be measured, rho is the density of the liquid to be measured, T p Is the temperature, R, of the liquid to be measured e Is the radius of curvature of the bubble and λ is the wavelength of the measuring light.
In order to improve the accuracy of absorbance detection, the pump 3 and the liquid core waveguide 7 are further disposed upstream and downstream of the two bubble detecting units 5-6, respectively.
In order to improve the accuracy of bubble detection, further, the bubble detection unit includes:
the light receiving module is used for receiving the light which is emitted by the light emitting module and passes through the transmission pipeline 2, converting the light into an electric signal and sending the electric signal to the analysis module;
and the analysis module acquires bubble information according to the change of the electric signal, wherein the bubble information comprises parameters T and T.
In order to accurately detect the bubbles in the liquid to be detected, further, the parameter T is the time difference between the 2 n-th change and the (2 n-1) -th change of the electric signal in the same bubble detecting unit, n is a positive integer, the parameter T is the time difference between the (2 m-1) -th change of the electric signal in the downstream bubble detecting unit and the 2 m-th change of the electric signal in the upstream bubble detecting unit, and m is a positive integer.
In order to obtain the absorbance of different wavelengths, further, the absorbance detecting device further comprises:
and the light splitting unit is used for spatially separating the polychromatic light emitted from the liquid core waveguide 7 and receiving the polychromatic light by the detector.
The absorbance detection method provided by the embodiment of the invention comprises the following steps:
the liquid to be measured enters the transmission pipeline 2 and the liquid core waveguide 7;
two bubble detection units 5-6 which are sequentially arranged on the transmission pipeline 2 detect the parameters of bubbles in the liquid to be detected;
the measuring light emitted by the light source enters the liquid core waveguide 7, passes through the liquid core waveguide 7 and is received by the detector, and the output signal is sent to the computing unit;
and the computing unit obtains the absorbance A of the liquid to be measured by using the parameters of the bubbles, the parameters of the transmission pipeline 2 and the output signal.
To accurately obtain the absorbance A, further, the absorbanceDegree of rotationN is the initial intensity of the measuring light emitted by the light source, N 0 The intensity of the measuring light received by the detector, D the diameter of the transmission pipeline 2, T the time required for each bubble in the liquid to be detected to pass through any bubble detection unit, T the time required for each bubble in the liquid to be detected to pass through the two bubble detection units 5-6, and l the distance between the two bubble detection units 5-6;
r is the radius of the capillary of the liquid core waveguide 7, zeta is the refractive index of the measuring light in the liquid to be measured, v is the kinematic viscosity of the liquid to be measured, rho is the density of the liquid to be measured, T p Is the temperature, R, of the liquid to be measured e Is the radius of curvature of the bubble and λ is the wavelength of the measuring light.
In order to improve the accuracy of bubble detection, further, the obtaining manner of the parameters of the bubbles is as follows:
the light receiving module receives the light which is emitted by the light emitting module and passes through the transmission pipeline 2, converts the light into an electric signal and sends the electric signal to the analysis module;
and the analysis module obtains bubble information according to the change of the electric signal, wherein the bubble information comprises parameters T and T.
In order to accurately detect the bubbles in the liquid to be detected, further, the parameter T is the time difference between the 2 n-th change and the (2 n-1) -th change of the electrical signal in the same bubble detecting unit, n is a positive integer, the parameter T is the time difference between the (2 m-1) -th change of the electrical signal in the downstream bubble detecting unit and the 2 m-th change of the electrical signal in the upstream bubble detecting unit, and m is a positive integer.
Example 2:
an application example of the absorbance detection apparatus and method according to embodiment 1 of the present invention.
In the application example, as shown in fig. 1, a transmission pipeline 2 is connected with a liquid core waveguide 7 and a sample bottle 1, a pump 3 and two bubble detection units 5-6 are sequentially arranged on the transmission pipeline 2, and the pump 3 adopts a peristaltic pump; the bubble detection unit adopts a non-contact optical fiber sensor and comprises a light emitting module, a light receiving module and an analysis module, wherein the light receiving module is used for receiving light which is emitted by the light emitting module and passes through the transmission pipeline 2, converting the light into an electric signal and sending the electric signal to the analysis module; the analysis module obtains bubble information according to the change of the electric signal, wherein the bubble information comprises parameters T and T; the parameter T is the time difference between the 2 nth change and the (2 n-1) th change of the electric signal in the same bubble detection unit, n is a positive integer, the parameter T is the time difference between the (2 m-1) th change of the electric signal in the downstream bubble detection unit and the 2m th change of the electric signal in the upstream bubble detection unit, and m is a positive integer;
the ultraviolet-visible spectrophotometer 9 comprises an ultraviolet-visible light source, emits polychromatic measuring light, then enters a capillary of the liquid core waveguide 7 through the optical fiber 10, the measuring light which is emitted out of the liquid core waveguide 7 enters a grating (or a prism) through the optical fiber 10 for light splitting, a linear array detector receives the light, and finally the light is sent to an analysis unit, wherein the analysis unit is the prior art;
under the action of the pump 3, the sample in the sample bottle 1 sequentially flows through the pump 3, the two bubble detection units 5-6 and the liquid core waveguide 7 and finally enters the waste liquid bottle 8;
the calculation unit is used for obtaining the full-wave-band absorbance A of the liquid to be detected in the transmission pipeline 2;
n is the initial intensity of the measuring light emitted by the light source, N 0 The intensity of the measuring light received by the detector, D the diameter of the transmission pipeline 2, T the time required for each bubble in the liquid to be detected to pass through any bubble detection unit, T the time required for each bubble in the liquid to be detected to pass through the two bubble detection units 5-6, and l the distance between the two bubble detection units 5-6;
r is the radius of the capillary of the liquid core waveguide 7, zeta is the refractive index of the measuring light in the liquid to be measured, v is the kinematic viscosity of the liquid to be measured, rho is the density of the liquid to be measured, T p Is the temperature, R, of the liquid to be measured e Is the radius of curvature of the bubble and λ is the wavelength of the measuring light.
The absorbance detection method provided by the embodiment of the invention comprises the following steps:
under the action of the pump 3, the sample in the sample bottle 1 sequentially flows through the pump 3, the two bubble detection units 5-6 and the liquid core waveguide 7 and finally enters the waste liquid bottle 8;
two bubble detection units 5-6 sequentially arranged on the transmission pipeline 2 detect parameters of bubbles in the liquid to be detected, and the specific mode is that a light receiving module receives light which is emitted by a light emitting module and penetrates through the liquid to be detected in the transmission pipeline 2, converts the light into an electric signal and sends the electric signal to an analysis module; the analysis module obtains bubble information according to the change of the electric signal, wherein the bubble information comprises parameters T and T; the parameter T is the time difference between the 2 nth change and the (2 n-1) th change of the electric signal in the same bubble detection unit, n is a positive integer, the parameter T is the time difference between the (2 m-1) th change of the electric signal in the downstream bubble detection unit and the 2m th change of the electric signal in the upstream bubble detection unit, and m is a positive integer;
the ultraviolet visible light source emits polychromatic measuring light, the polychromatic measuring light is then incident into a capillary of the liquid core waveguide 7 through the optical fiber 10, the measuring light which is emitted out of the liquid core waveguide 7 is incident into a grating (or a prism) for light splitting through the optical fiber 10, the linear array detector receives the light, and the light is finally sent to an analysis unit, wherein the analysis unit is the prior art;
the calculation unit obtains the full-spectrum absorbance of the liquid to be measured according to the parametersN is the initial intensity of the measuring light emitted by the light source, N 0 The intensity of the measuring light received by the detector, D is the diameter of the transmission pipeline 2, T is the time required for each bubble in the liquid to be detected to pass through any bubble detection unit, T is the time required for each bubble in the liquid to be detected to pass through two bubble detection units 5-6, and l is the distance between the two bubble detection units 5-6;
r is the radius of the capillary of the liquid core waveguide 7, zeta is the refractive index of the measuring light in the liquid to be measured, v is the kinematic viscosity of the liquid to be measured, rho is the density of the liquid to be measured, and T is p Is the temperature, R, of the liquid to be measured e Is the radius of curvature of the bubble and λ is the wavelength of the measuring light.
The experimental result shows that the error is reduced by the corrected absorbance in the following table;
through carrying out a correction control experiment on ultrapure water, the experimental result is shown in the following table, and compared with a detection method which is subjected to degassing treatment and untreated treatment, the absorbance detection device and method disclosed by the invention can reduce the error.
Claims (8)
1. The absorbance detection device comprises a pump and a transmission pipeline; characterized in that, the absorbance detection device further comprises:
the two bubble detection units are sequentially arranged on the transmission pipeline and are respectively used for detecting bubbles in the liquid to be detected in the transmission pipeline;
the liquid to be detected enters the transmission pipeline and the liquid core waveguide; the measuring light emitted by the light source enters the liquid core waveguide, and the detector is used for receiving the measuring light emitted from the liquid core waveguide;
a calculation unit for obtaining the absorbance of the liquid to be measured by using the parameters of the bubble, the transmission pipeline and the liquid core waveguide and the measuring lightN is the initial intensity of the measuring light emitted by the light source, N 0 The intensity of the measuring light received by the detector, D the diameter of the transmission pipeline, T the time required for each bubble in the liquid to be detected to pass through any bubble detection unit, T the time required for each bubble in the liquid to be detected to pass through two bubble detection units, and l the distance between the two bubble detection units;
,,,r is the radius of the liquid core waveguide capillary, zeta is the refractive index of the measuring light in the liquid to be measured, v is the kinematic viscosity of the liquid to be measured, rho is the density of the liquid to be measured, and T is p Is the temperature, R, of the liquid to be measured e Is the radius of curvature of the bubble and λ is the wavelength of the measuring light.
2. The absorbance detection device according to claim 1, wherein the pump and the liquid core waveguide are respectively disposed upstream and downstream of the two bubble detection units.
3. The absorbance detection device according to claim 1, wherein the bubble detection unit includes:
the light receiving module is used for receiving the light which is emitted by the light emitting module and penetrates through the liquid to be detected in the transmission pipeline, converting the light into an electric signal and sending the electric signal to the analysis module;
and the analysis module acquires bubble information according to the change of the electric signal, wherein the bubble information comprises parameters T and T.
4. The absorbance detection device according to claim 3, wherein the parameter T is a time difference between the 2 n-th change and the (2 n-1) -th change of the electric signal in the same bubble detecting unit, n is a positive integer, the parameter T is a time difference between the (2 m-1) -th change of the electric signal in the downstream bubble detecting unit and the 2 m-th change of the electric signal in the upstream bubble detecting unit, and m is a positive integer.
5. The absorbance detection device according to claim 1, further comprising:
and the light splitting unit is used for spatially separating the polychromatic light emitted from the liquid core waveguide and is received by the detector.
6. An absorbance detection method, comprising:
the liquid to be measured enters the transmission pipeline and the liquid core waveguide;
two bubble detection units which are sequentially arranged on the transmission pipeline detect the parameters of bubbles in the liquid to be detected;
measuring light emitted by the light source enters the liquid core waveguide, passes through the liquid core waveguide and is received by the detector, and a signal is output to the computing unit;
the calculation unit obtains the absorbance of the liquid to be measured by using the parameters of the bubbles, the parameters of the transmission pipeline and the output signalN is the initial intensity of the measuring light emitted by the light source, N 0 The intensity of the measuring light received by the detector, D the diameter of the transmission pipeline, T the time required for each bubble in the liquid to be detected to pass through any bubble detection unit, T the time required for each bubble in the liquid to be detected to pass through two bubble detection units, and l the distance between the two bubble detection units;
,,,r is the radius of the liquid core waveguide capillary, zeta is the refractive index of the measuring light in the liquid to be measured, v is the kinematic viscosity of the liquid to be measured, and rho isDensity, T, of the liquid to be measured p Is the temperature, R, of the liquid to be measured e Is the radius of curvature of the bubble and λ is the wavelength of the measuring light.
7. The method for detecting absorbance according to claim 6, wherein the parameter of the bubble is obtained by:
the light receiving module receives the light which is emitted by the light emitting module and passes through the liquid to be detected in the transmission pipeline, converts the light into an electric signal and sends the electric signal to the analysis module;
and the analysis module obtains bubble information according to the change of the electric signal, wherein the bubble information comprises parameters T and T.
8. The absorbance detection method according to claim 7, wherein the parameter T is a time difference between the 2 n-th change and the (2 n-1) -th change of the electric signal in the same bubble detecting unit, n is a positive integer, the parameter T is a time difference between the (2 m-1) -th change of the electric signal in the downstream bubble detecting unit and the 2 m-th change of the electric signal in the upstream bubble detecting unit, and m is a positive integer.
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