CN-121978065-A - In-situ substance component detection equipment and method based on fluorescence spectrum

CN121978065ACN 121978065 ACN121978065 ACN 121978065ACN-121978065-A

Abstract

The invention discloses an in-situ substance component detection device and method based on fluorescence spectrum, which aim at the problems that the existing spectrum detection device relies on manual sampling to carry out off-line detection, not only has poor aging and can not dynamically track the substance change process in real time, but also adopts an APL two-wire system power supply and communication module and a time-sharing multi-wavelength laser light source to circularly excite the fluorescence characteristics of different substances in mixed liquid according to a preset sequence by replacing the traditional grating with a quantum dot array spectrum sensor; and the detection window is directly contacted with the liquid medium to resist the working condition of high temperature and high pressure, so that the in-situ on-line installation of equipment in an industrial pipeline or a reactor is realized, and sampling and sample pretreatment are not required.

Inventors

Guo Xiangxia
CHEN QINGFENG
YANG KEWEI
GUAN YUJIE
HU MENGJIE
ZHONG XIAOBO

Assignees

浙江中控自动化仪表有限公司

Dates

Publication Date: 20260505
Application Date: 20251231

Claims (8)

1. An in-situ species composition detection apparatus based on fluorescence spectroscopy, comprising: A pressure housing, in which the following modules are integrated and which are connected to each other by means of an APL two-wire bus for cooperation: The power supply module is used for simultaneously supplying power to the light source module and the spectrum module through the APL two-wire bus and internally provided with a capacitor energy storage unit so as to maintain stable voltage during peak power consumption of the light source module; The communication module is connected to the APL two-wire system bus of the power supply module and is used for realizing wavelength switching control of the light source module, full spectrum data acquisition of the spectrum module and full duplex data transmission through an APL industrial communication protocol; the light source module consists of a plurality of laser light sources with specific wavelengths, and emits laser in a time-sharing mode according to a switching instruction of the communication module, and the laser is transmitted to the detection window through the light guide structure to excite the liquid medium to generate a fluorescent signal; The spectrum module adopts a quantum dot array spectrum sensor and is used for receiving fluorescent signals transmitted by the light guide structure and converting the fluorescent signals into full spectrum data, and the full spectrum data is uploaded in real time through the communication module; The detection window is fixedly arranged at the end part of the pressure-resistant shell, is directly immersed into a liquid medium in an industrial pipeline or a reactor, and is used for realizing physical isolation and optical coupling of an optical path and a measured environment.
2. The fluorescence spectrum-based in-situ species composition detection apparatus as claimed in claim 1 wherein the laser light source has wavelengths including 355nm, 405nm and 532nm, respectively corresponding to fluorescence excitation peaks of different species.
3. The fluorescence spectrum-based in-situ substance component detection apparatus according to claim 2, wherein each laser light source is independently operated in a cyclic time-sharing manner under the synchronous timing control of the communication module, the 355nm laser light source is used for exciting the fluorescence characteristic of ethanol, the 405nm laser light source is used for exciting the fluorescence characteristic of caproic acid, the 532nm laser light source is used for exciting the fluorescence characteristic of ethyl caproate, and the fluorescence signals generated by the excitation of each wavelength are transmitted to the spectrum module through the light guide structure.
4. The fluorescence spectrum-based in situ species composition detection apparatus as claimed in claim 1 wherein said APL two-wire power and communication timing control is configured to: In the detection stage, the power supply equipment periodically transmits detection signals on the twisted pair, and when the power receiving equipment is not electrified, the circuit is in a non-voltage state, and the power supply equipment recognizes the access of the power receiving equipment through the impedance of a detection loop; In the grading stage, after the power supply equipment detects effective power receiving equipment, a grading signal is sent to determine the power grade of the power receiving equipment, then a power supply switch is closed to output stable voltage, and the power receiving equipment enters a wake-up and initialization state after obtaining the voltage; in the link establishment stage, a physical layer chip in the powered device starts and continuously transmits link pulses to attempt to establish a link with the power supply device, and the two parties complete full duplex initialization through auto-negotiation, and enter a normal communication ready state after the establishment is successful; In the data communication stage, in each period, the power supply equipment provides constant current power supply for the power receiving equipment through the same pair of cables, and meanwhile, full duplex data signals are overlapped on a power supply line in a burst time slot of 1ms at the end of the period, so that physical layer multiplexing of power supply and communication is realized; In the periodical detection embedding stage, in the data communication process, the power supply equipment inserts detection signals periodically to monitor the state of the power receiving equipment, and the power receiving equipment feeds back response pulses after receiving the detection signals, so that the continuous stability of a link is ensured.
5. The fluorescence spectrum-based in-situ substance component detection apparatus according to claim 4, wherein in the data communication phase, when the light source module of the power receiving apparatus generates peak power consumption at the moment of excitation, the capacitor energy storage unit built in the power receiving apparatus instantaneously discharges to compensate the current gap, so as to ensure that the APL bus voltage fluctuation is smaller than a threshold value.
6. The fluorescence spectrum-based in-situ substance component detection apparatus according to claim 4, wherein in the link establishment phase, full duplex communication is implemented between the powered apparatus and the power supply apparatus by using an echo cancellation technique, a downlink control command and uplink spectrum data are separated in a frequency domain, signal collision is avoided, and the communication module sends a TTL level synchronization pulse at a starting moment of each period, and triggers the light source module to start a new round of wavelength switching.
7. The fluorescence spectrum-based in-situ species composition detection apparatus of claim 1, wherein the light guide structure is disposed between the light source module, the spectrum module, and the detection window, comprising: the light guide column is used for directionally transmitting laser and fluorescent signals in a limited space, an incident end of the light guide column is coupled to the light source module and the spectrum module, and an emergent end of the light guide column is coupled to the detection window; the optical filter is arranged in the light path of the light guide column, is a dichroic optical filter and is used for transmitting laser with specific wavelength in the excitation light path and reflecting fluorescent signals, and transmitting the fluorescent signals in the receiving light path and blocking laser leakage; The lens group is arranged at two ends of the light guide column and comprises a collimating lens and a focusing lens, the collimating lens is used for collimating divergent laser beams emitted by the light source module into parallel light, and the focusing lens is used for focusing returned fluorescent signals to a photosurface of the spectrum module.
8. A method for quantitative analysis of components of a multicomponent substance in situ based on fluorescence spectra, using an apparatus as claimed in any one of claims 1 to 7, comprising the steps of: a time-sharing multi-wavelength excitation step, namely switching laser light sources with different wavelengths according to a preset sequence through a light source module, and exciting fluorescent characteristics of each target substance in the mixed liquid; a full spectrum acquisition step, namely receiving fluorescent signals generated in the time-sharing multi-wavelength excitation step through a quantum dot array spectrum sensor, and generating full spectrum data covering a 350 nm-1070 nm range; A data preprocessing step, namely carrying out noise reduction, baseline correction and normalization processing on the full spectrum data, and eliminating environmental interference; A component analysis step, namely carrying out real-time analysis on the processed full spectrum data by utilizing a pre-stored chemometric model, carrying out nonlinear mapping inversion on the spectrum intensity and the substance concentration, and calculating a real-time concentration value of each target component; And a data transmission step, namely transmitting the calculated concentration data to an external control system in real time through an APL communication module.

Description

In-situ substance component detection equipment and method based on fluorescence spectrum Technical Field The invention belongs to the technical field of spectrum detection, and particularly relates to in-situ substance component detection equipment and method based on fluorescence spectrum. Background The existing spectrum detection equipment depends on large-scale optical elements such as gratings, has huge volume and is difficult to integrate into industrial pipelines, so that the existing spectrum detection equipment often needs to rely on manual sampling for offline detection, has poor aging, cannot dynamically track the material change process in real time, has high labor cost and easily pollutes samples, and meanwhile, has complicated offline multicomponent detection flow, often needs to perform preseparation, depends on manual detection experience and has inaccuracy. Disclosure of Invention The invention aims to provide in-situ substance component detection equipment based on fluorescence spectrum, which can be installed in an industrial pipeline to detect in-situ substance components in real time. In order to solve the problems, the technical scheme of the invention is as follows: An in situ species composition detection apparatus based on fluorescence spectroscopy, comprising: A pressure housing, in which the following modules are integrated and which are connected to each other by means of an APL two-wire bus for cooperation: The power supply module is used for simultaneously supplying power to the light source module and the spectrum module through the APL two-wire bus and internally provided with a capacitor energy storage unit so as to maintain stable voltage during peak power consumption of the light source module; The communication module is connected to the APL two-wire system bus of the power supply module and is used for realizing wavelength switching control of the light source module, full spectrum data acquisition of the spectrum module and full duplex data transmission through an APL industrial communication protocol; the light source module consists of a plurality of laser light sources with specific wavelengths, and emits laser in a time-sharing mode according to a switching instruction of the communication module, and the laser is transmitted to the detection window through the light guide structure to excite the liquid medium to generate a fluorescent signal; The spectrum module adopts a quantum dot array spectrum sensor and is used for receiving fluorescent signals transmitted by the light guide structure and converting the fluorescent signals into full spectrum data, and the full spectrum data is uploaded in real time through the communication module; The detection window is fixedly arranged at the end part of the pressure-resistant shell, is directly immersed into a liquid medium in an industrial pipeline or a reactor, and is used for realizing physical isolation and optical coupling of an optical path and a measured environment. According to an embodiment of the present invention, the wavelength of the laser light source includes 355nm, 405nm and 532nm, which respectively correspond to fluorescence excitation peaks of different substances. According to an embodiment of the invention, each laser light source circularly and time-sharing independently works under the synchronous time sequence control of the communication module, the 355nm laser light source is used for exciting the fluorescent characteristic of ethanol, the 405nm laser light source is used for exciting the fluorescent characteristic of caproic acid, the 532nm laser light source is used for exciting the fluorescent characteristic of ethyl caproate, and fluorescent signals generated by the excitation of each wavelength are transmitted to the spectrum module through the light guide structure. According to an embodiment of the present invention, the APL two-wire power supply and communication timing control is configured to: In the detection stage, the power supply equipment periodically transmits detection signals on the twisted pair, and when the power receiving equipment is not electrified, the circuit is in a non-voltage state, and the power supply equipment recognizes the access of the power receiving equipment through the impedance of a detection loop; In the grading stage, after the power supply equipment detects effective power receiving equipment, a grading signal is sent to determine the power grade of the power receiving equipment, then a power supply switch is closed to output stable voltage, and the power receiving equipment enters a wake-up and initialization state after obtaining the voltage; in the link establishment stage, a physical layer chip in the powered device starts and continuously transmits link pulses to attempt to establish a link with the power supply device, and the two parties complete full duplex initialization through auto-negotiation, and enter a normal communication ready state afte