CN113640247A - On-site dark current acquisition method based on near infrared spectrum technology - Google Patents

On-site dark current acquisition method based on near infrared spectrum technology Download PDF

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CN113640247A
CN113640247A CN202111086591.5A CN202111086591A CN113640247A CN 113640247 A CN113640247 A CN 113640247A CN 202111086591 A CN202111086591 A CN 202111086591A CN 113640247 A CN113640247 A CN 113640247A
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spectrometer
reference plate
sample
lens
dark current
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杨增玲
梁浩
韩鲁佳
范雅彭
李守学
黄圆萍
廖科科
史卓林
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China Agricultural University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/359Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01JMEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/02Details
    • G01J3/0205Optical elements not provided otherwise, e.g. optical manifolds, diffusers, windows
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01JMEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28Investigating the spectrum
    • G01J3/42Absorption spectrometry; Double beam spectrometry; Flicker spectrometry; Reflection spectrometry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/27Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration

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Abstract

The invention relates to a field dark current acquisition method based on a near infrared spectrum technology, which comprises the following steps: and under the condition of ensuring that the light source of the spectrometer is closed, the reference plate is tightly attached to the lens of the spectrometer, so that dark current collection is completed. The reference plate is made of polytetrafluoroethylene with the reflectivity of more than 99%. The reference plate is tightly attached to the spectrometer lens, namely the reference plate and the spectrometer lens are in a zero optical path. The invention is suitable for the condition that the change of the field illumination condition is obvious, but the invention is suitable for the condition that the change of the illumination condition is not obvious, has good universality and is suitable for all attached diffuse reflection spectrometers.

Description

On-site dark current acquisition method based on near infrared spectrum technology
Technical Field
The invention relates to a field dark current acquisition method based on a near infrared spectrum technology, and relates to the technical field of micro near infrared spectrum acquisition.
Background
The micro near-infrared spectrometer is widely applied to the fields of agriculture, food, petrifaction, traditional Chinese medicine and the like due to the advantages of high integration level, good portability, high price, simple field application and the like.
However, when the micro near-infrared spectrometer is popularized and applied on the spot, the signal acquisition of the near-infrared spectrometer is seriously interfered by noises such as external environments (stray light, temperature, humidity and the like), and particularly, the stray light is difficult to avoid in the environment during the on-site use process, so that the spectrometer is difficult to acquire a stable dark current signal, and finally, the accurate absorbance value of a sample is difficult to acquire.
When a near-infrared spectrometer is used in a laboratory, the spectrometer is required to collect the dark current of the spectrometer on the premise of turning off a light source, and the laboratory environment is in a relatively stable state. However, in the field use of the micro spectrometer, since the light in the environment is constantly changing, the stray light is often the main reason that the dark current cannot be collected in a standardized manner.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a method for collecting dark current in a field based on near infrared spectroscopy, which can stably collect dark current and avoid the influence of ambient light.
The invention also aims to provide an absorbance test method based on the near infrared spectrum technology.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a field dark current collecting method based on a near infrared spectrum technology, which comprises the following steps: and under the condition of ensuring that the light source of the spectrometer is closed, the reference plate is tightly attached to the lens of the spectrometer, so that dark current collection is completed.
In the field dark current acquisition method, the reference plate is made of polytetrafluoroethylene with the reflectivity of more than 99%.
The field dark current acquisition method is characterized in that the reference plate is tightly attached to the lens of the spectrometer, namely the reference plate and the lens of the spectrometer are in a zero optical path.
In a second aspect, the present invention further provides an absorbance testing method based on the near infrared spectrum technology, including:
starting a spectrometer and preheating;
setting acquisition parameters of a spectrometer;
turning off a light source of the spectrometer, tightly attaching a reference plate to a lens of the spectrometer, and collecting a dark current energy value;
turning on a light source of the spectrometer, tightly attaching a reference plate on a lens of the spectrometer, and collecting the energy value of the reference plate;
turning on a light source of the spectrograph, placing a sample to be detected in a sample cup, enabling the sample cup to be tightly attached to a lens of the spectrograph, and collecting an energy value of the sample;
and calculating the absorbance of the sample to be detected.
In the absorbance test method, the reference plate is made of polytetrafluoroethylene material with the reflectivity of more than 99%.
The absorbance test method further comprises the following step of calculating the absorbance of a sample to be tested by the following formula:
Figure BDA0003265768200000021
wherein ABS refers to sample absorbance, REF refers to reference plate energy value, DARK refers to DARK current energy value of spectrometer, and SMP refers to sample energy value.
According to the absorbance test method, the sample cup is made of quartz materials, and the quartz materials are subjected to hydroxyl removal process treatment to remove hydroxyl infrared absorption.
The absorbance test method further comprises the step of tightly attaching the reference plate to the lens of the spectrometer, namely that the optical path between the reference plate and the lens of the spectrometer is zero.
In the absorbance test method, further, the sample cup is tightly attached to the lens of the spectrometer, namely the sample cup is not in clearance with the lens of the spectrometer.
Due to the adoption of the technical scheme, the invention has the following advantages:
1. the reference plate is tightly attached to the lens of the spectrometer under the condition that the light source of the spectrometer is closed, so that dark current collection is completed, and a polytetrafluoroethylene reference plate with the reflectivity of more than 99% is adopted, so that standardized dark current is conveniently collected, the influence of ambient stray light on the method is reduced, and the standardization degree is high;
2. the design method is simple, avoids using a black dark box, simplifies the whole structure and is convenient for acquiring signals on site;
in conclusion, the method is suitable for the condition that the change of the field illumination condition is obvious, but the method is also suitable for the condition that the change of the illumination condition is not obvious, and the universality is good; the problem of inconsistent dark current collected on site can be effectively solved, the application effect is good, and the method is suitable for all attached diffuse reflection spectrometers.
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Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Like reference numerals refer to like parts throughout the drawings. In the drawings:
fig. 1 is parameters collected in different environments for a solid state spectrometer in an embodiment of the present invention, where (a) is a dark current collected in different environments by the spectrometer, (b) is a reference energy collected in different environments by the spectrometer, (c) is a sample energy collected in different environments by the spectrometer, and (d) is an absorbance of a sample collected in different environments by the spectrometer;
fig. 2 shows parameters collected by the liquid spectrometer under different environments in the embodiment of the present invention, (a) shows dark current collected by the spectrometer under different environments, (b) shows reference energy collected by the spectrometer under different environments, (c) shows sample energy collected by the spectrometer under different environments, and (d) shows sample absorbance collected by the spectrometer under different environments;
FIG. 3 shows dark current collected by a spectrometer covered with a reference plate for 29 consecutive days in an example of the present invention.
Detailed Description
Exemplary embodiments of the present invention will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the invention are shown in the drawings, it should be understood that the invention can be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
It is to be understood that the terminology used herein is for the purpose of describing particular example embodiments only, and is not intended to be limiting. As used herein, the singular forms "a", "an" and "the" may be intended to include the plural forms as well, unless the context clearly indicates otherwise. The terms "comprises," "comprising," "including," and "having" are inclusive and therefore specify the presence of stated features, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, steps, operations, elements, components, and/or groups thereof. The method steps, processes, and operations described herein are not to be construed as necessarily requiring their performance in the particular order described or illustrated, unless specifically identified as an order of performance. It should also be understood that additional or alternative steps may be used.
For convenience of description, spatially relative terms, such as "inner", "outer", "lower", "upper", and the like, may be used herein to describe one element or feature's relationship to another element or feature as illustrated in the figures. Such spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures.
Typically, the absorbance of a sample is calculated by the following equation:
Figure BDA0003265768200000041
wherein ABS refers to sample absorbance, REF refers to reference plate energy value, DARK refers to DARK current energy value of spectrometer, and SMP refers to sample energy value.
It can be seen from the above formula that the absorbance is mainly affected by the reference plate energy value, the dark current energy value and the sample energy value. Generally, the energy value of the reference plate is the energy value of 100% reflected back to the detector from the light source, the dark current value is the photoelectric energy received by the detector when the excitation light source of the spectrometer is not turned on, and the energy value of the sample reflected back to the detector, which all determine the absorbance value of a certain sample. The absorbance of the sample is correlated with the concentration of the sample, i.e., the absorbance of the sample by the spectrometer is also known as the amount of the sample component.
The following description will explain, by way of specific examples, that the difference in absorbance of the same sample in different environments is caused by the difference in dark current.
Example 1: measuring the condition of a solid sample
Aiming at the same solid sample, under the condition that a light source of the spectrometer is closed, dark current of the spectrometer is respectively collected towards an indoor greenhouse, the sky, the sun and a reference plate, then a reference energy value and an energy value of the sample are collected, and finally the absorbance of the final sample is calculated.
For the solid sample, it can be seen in fig. 1(a) that, in general, the energy values of dark current are greatly different for different environments of indoor greenhouses, sky, sun and reference plates, wherein the highest value of dark current generated against the sun can reach 17354, and the lowest value of dark current generated against the reference plate can reach 5320. As shown in fig. 1(b), the energy value of the reference plate was not significantly different under different environments, and was always kept in a stable state, with a maximum value of about 62463. It can be seen from fig. 1(c) that the energy values of the samples were substantially not significantly different under the four different environments, with a maximum around 47650. FIG. 1(d) shows the absorbance difference of the final sample, and obviously, the absorbance of the sample obtained facing the sun is obviously different from that of the other three environments, the difference is mainly reflected in that the peak signals of 1128nm and 1178nm are enhanced, and a peak appears at 990 nm.
From the above results of the solid samples, it can be seen that the final absorbance difference of the same solid sample is mainly caused by the non-uniform dark current collection.
Example 2: measuring the condition of a liquid sample
Aiming at the same liquid sample, under the condition that a light source of the spectrometer is closed, dark current of the spectrometer is respectively collected towards an indoor greenhouse, the sky, the sun and a reference plate, then a reference energy value and an energy value of the sample are collected, and finally the absorbance of the final sample is calculated.
For the liquid sample, it can be seen from fig. 2(a) that the energy value of the dark current is very different for different environments of the indoor greenhouse, sky, sun and the reference plate in general, wherein the highest dark current is generated towards the sun, the maximum value of which can reach 13739, and the lowest dark current is generated towards the reference plate, the maximum value of which is 5322. As can be seen from fig. 2(b), the energy value of the reference plate has no significant difference under different environments, and is always kept in a stable state, and the maximum value is about 62249. Fig. 2(c) shows that the energy values of the samples are substantially not significantly different under four different environments, with a maximum value around 13900, where the slight decrease in the highest value is mainly due to the non-uniformity of the liquid sample and the slight difference in energy values. FIG. 2(d) shows the absorbance difference of the final sample, and clearly, the absorbance of the sample obtained facing the sun is significantly different from that of the other three environments, and the absorbance maximum of 5 is reached in the four wavelength ranges of 950-.
From the above results, it can be seen that the final significant absorbance difference of the sample for the same liquid sample is also caused by the non-uniform dark current collection of the spectrometer.
When the spectrometer is applied on site, the energy value of the reference plate is a substance with extremely stable optical performance, and the energy value of the reference plate is basically unchanged under the premise that the setting parameters of the spectrometer are fixed, while the dark current is generally greatly influenced by ambient light, so that the control of the dark current is very important. The micro spectrometer is usually contacted with a sample when collecting spectral information, so that on one hand, a consistent sampling optical path can be ensured, and meanwhile, stray light is reduced from entering a detector.
According to the on-site dark current acquisition method for the near infrared spectrum technology, provided by the embodiment of the invention, under the condition that the light source is ensured to be turned off, the reference plate is tightly attached to the lens of the spectrometer to finish dark current acquisition, so that stray light is effectively prevented from entering, and the dark current acquisition under the same condition is ensured.
After the dark current is collected, a spectrometer light source is started to collect energy values of a reference plate and a sample, and based on the dark current collecting method, the embodiment of the invention also provides a method for testing absorbance, which comprises the following steps:
s1, connecting the spectrometer with a computer, starting the spectrometer, preheating for more than half an hour, and ensuring the operation stability of the spectrometer;
s2, setting acquisition parameters of the spectrometer, including parameters such as wavelength range, resolution, integration time, repetition times and PGA;
s3, turning off a light source of the spectrometer, tightly attaching a reference plate on a lens of the spectrometer to ensure no gap (zero optical path), and collecting dark current energy signals, wherein the reference plate is made of polytetrafluoroethylene materials with reflectivity of more than 99%;
s4, turning on a light source of the spectrometer, tightly attaching the reference plate to a lens of the spectrometer, and collecting an energy signal of the reference plate;
s5, turning on a light source of the spectrometer, placing a sample in a sample cup, enabling the sample cup to be tightly attached to a lens of the spectrometer, ensuring no gap (zero optical path), and collecting an energy signal of the sample, wherein the sample cup is made of quartz (JSG 3), and all quartz materials are subjected to hydroxyl removal process treatment, so that hydroxyl infrared absorption is removed, and irrelevant signal interference is reduced;
and S6, completing one complete signal acquisition, and calculating the Absorbance (Absorbance) of the sample according to a formula.
To verify the stability of the method of the present invention, dark current of the spectrometer covered with the reference plate was collected in the field environment for 29 consecutive days, and the results are shown in fig. 3. The dark current of the spectrometer is stabilized at 5300, so that the method is practical, simple and easy to operate, and can be used as a method for stably collecting the dark current.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: it is to be understood that modifications may be made to the above-described arrangements in the embodiments or equivalents may be substituted for some of the features of the embodiments without departing from the spirit or scope of the present invention.

Claims (9)

1. A field dark current acquisition method based on near infrared spectrum technology is characterized by comprising the following steps: and under the condition of ensuring that the light source of the spectrometer is closed, the reference plate is tightly attached to the lens of the spectrometer, so that dark current collection is completed.
2. The method of claim 1, wherein the reference plate is made of polytetrafluoroethylene with a reflectivity of 99% or more.
3. The on-site dark current collection method according to claim 1, wherein the reference plate is closely attached to the spectrometer lens, that is, the reference plate and the spectrometer lens are in a zero optical path.
4. An absorbance test method based on near infrared spectrum technology is characterized by comprising the following steps:
starting a spectrometer and preheating;
setting acquisition parameters of a spectrometer;
turning off a light source of the spectrometer, tightly attaching a reference plate to a lens of the spectrometer, and collecting a dark current energy value;
turning on a light source of the spectrometer, tightly attaching a reference plate on a lens of the spectrometer, and collecting the energy value of the reference plate;
turning on a light source of the spectrograph, placing a sample to be detected in a sample cup, enabling the sample cup to be tightly attached to a lens of the spectrograph, and collecting an energy value of the sample;
and calculating the absorbance of the sample to be detected.
5. The method for measuring absorbance according to claim 4, wherein the reference plate is made of polytetrafluoroethylene having a reflectance of 99% or more.
6. The method for measuring absorbance according to claim 4, wherein the absorbance of the sample to be measured is calculated by the following formula:
Figure FDA0003265768190000011
wherein ABS refers to sample absorbance, REF refers to reference plate energy value, DARK refers to DARK current energy value of spectrometer, and SMP refers to sample energy value.
7. The method of claim 4, wherein the sample cup is made of quartz, and the quartz is subjected to a hydroxyl radical removal process to remove infrared absorption of hydroxyl radicals.
8. The absorbance test method according to any one of claims 4 to 7 based on near infrared spectroscopy, wherein the reference plate is closely attached to the spectrometer lens, i.e. the optical path between the reference plate and the spectrometer lens is zero.
9. The absorbance test method according to any one of claims 4 to 7 based on near infrared spectroscopy, wherein the close contact between the sample cup and the lens of the spectrometer means that there is no gap between the sample cup and the lens of the spectrometer.
CN202111086591.5A 2021-09-16 2021-09-16 On-site dark current acquisition method based on near infrared spectrum technology Pending CN113640247A (en)

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Application publication date: 20211112

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