CN112285044A - Online differential ultraviolet-visible spectrum detector for organic matters in water and organic matter detection method - Google Patents
Online differential ultraviolet-visible spectrum detector for organic matters in water and organic matter detection method Download PDFInfo
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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Abstract
An online differential ultraviolet-visible spectrum detector for organic matters in a water body and an organic matter detection method. The invention discloses an instrument for monitoring differential ultraviolet-visible light absorption spectrum of an organic matter on line and an algorithm for extracting a spectrum fingerprint spectrum by utilizing the change difference of light absorption characteristics of main components in the organic matter in the water chemical reaction process. The specific instrument functional units include: light source, light path system, detector, reference cell, sample cell and pH control adjustment unit. The method has the advantages of high sensitivity, convenient operation and wide application, and is suitable for online water quality monitoring of various water bodies such as rivers, lakes (reservoirs), oceans, drinking water, sewage (waste water) and the like.
Description
The technical field is as follows:
the invention belongs to the technical field of environmental protection and environmental monitoring, relates to a water quality monitoring instrument, and particularly relates to an instrument for quantitatively acquiring differential ultraviolet-visible absorption spectrum information of organic matter components in a water body.
Background art:
organic Matters (AOM) in the water body mainly come from animal and plant rottenness, algae reproduction and metabolism residues and pollutants discharged by human activities, cause water quality problems such as color, smell, dissolved oxygen concentration, eutrophication and the like, are also the largest carbon reservoir of the earth, and play a key role in global C circulation and N, P, heavy metal, POPs and other substance circulation. TOC, COD and UV of conventional water quality monitoring items254Etc. only reflect the total amount of organic pollutants, but not the source, components and behavior characteristics of the organic pollutants in the environmental processA significant difference in the difference.
The AOM contains a small amount of N, S, P-containing groups except carboxyl, phenol and cycloaliphatic structures, and most of the groups have ultraviolet-visible light absorption characteristics. The ultraviolet-visible spectrum technology has high sensitivity, simple equipment and convenient operation, and is widely applied to water quality detection including AOM monitoring. Currently, the existing online ultraviolet-visible light monitoring methods mainly comprise two types: the first is a single wavelength mode, and the concentration of AOM is indicated by measuring the absorption value at 254nm and other wavelengths; the second is continuous wavelength scanning within the range of 200-700nm, but because of the complex composition of AOM and the superposition interference of various light groups, the ultraviolet-visible absorption spectrum (UV) intensity is exponentially reduced along with the wavelength, and no obvious characteristic peak exists. Using Slope, E only3:E5The parameters indicate limited information such as the concentration of AOM, aromatic group content and molecular size.
The invention content is as follows:
in order to solve the problems in the prior art, the invention discloses an online differential ultraviolet-visible spectrum detector for organic matters in a water body and a differential ultraviolet-visible absorption spectrum information extraction method for components of organic matter components.
In order to achieve the above object, the present invention specifically adopts the following technical solutions.
An online differential ultraviolet-visible spectrum detector for organic matters in water comprises a spectrometer optical path system and a water path system; the method is characterized in that:
in the light path system, a light source is divided into two paths through an optical fiber and a light splitter, the two paths of light sources respectively penetrate through a reference cell and a sample cell and then are collected and transmitted to a detector, and a detection result is displayed through a display module after signal processing of the detector;
the waterway system comprises a water body sample container and an injection pump system, and the water body sample is injected into the sample pool through a peristaltic pump;
the injection pump system is at least provided with four injection channels which are respectively connected with four liquid storage tanks of acid, alkali, deionized water and cleaning agent, and can inject the liquid in the corresponding liquid storage tanks into the sample cell according to the requirements through different injection channels.
The present invention further includes the following preferred embodiments.
The reference cell and the sample cell are cylindrical or other containers made of quartz materials, the reference cell contains a reference solution or only injects air, and the sample cell injects a sample to be measured.
The light path length of the reference cell and the sample cell is 1-10 cm.
The waste liquid collecting container is connected to a liquid outlet of the sample pool through a peristaltic pump.
In an alkali liquid storage tank, preparing NaOH or KOH solution with the concentration of 0.01-2mol/L, wherein the specific concentration is set according to the following mode:
when the alkali liquor in the alkali liquor storage tank is injected into the sample cell to make the sample reach the target pH value, the dilution ratio of the sample is not higher than 1%.
In an acid storage tank, preparing H with the concentration of 0.01-2mol/L2SO4、HNO3、HCl、HClO4The specific concentration of any one of the solutions is set as follows:
when the acid liquid in the acid liquid storage tank is injected into the sample cell to enable the sample to reach the target pH value, the dilution ratio of the sample is not higher than 1%.
The acid and base reservoirs may be configured to hold other redox, complexing/chelating reagents that react with the organic species.
2L of deionized water is prepared in the deionized water storage tank;
in the cleaning agent storage tank, the cleaning agent is 5% potassium permanganate solution or aqua regia.
The application also discloses a method for detecting organic matters in the water body based on the online differential ultraviolet-visible spectrum detector, which comprises the following steps:
s1: sucking a sample to be detected into a sample cell, scanning within the wavelength range of 200-600nm, and recording a scanning spectrum;
s2: adding acid or alkali solution or other chemical reagents into the sample cell through an injection pump system, scanning within the wavelength range of 200-600nm after reaction components are stable, and recording the scanning spectrum of the light source passing through the sample cell under a plurality of set reaction conditions;
s3: and analyzing the spectrogram to obtain component spectrum information of the organic matters in the water body.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention is different from the conventional water quality monitoring items of TOC, COD and UV254Etc. only reflect the total amount of organic contaminants. When the total amount is monitored, the change of the organic matter in the ultraviolet-visible spectrum before and after the water chemical reaction process, namely the difference ultraviolet-visible spectrum, is obtained by setting the water chemical reaction, the obvious difference of the source, the component and the behavior characteristic of the organic matter in the environmental process is reflected, and the method has wide application prospect in the field of water quality on-line monitoring and early warning.
Drawings
FIG. 1 is a schematic structural diagram of an online differential ultraviolet-visible spectrum detector for organic matters in water bodies according to the invention;
FIG. 2 is a graph showing the difference in UV-visible absorption spectra of solutions at different pH values measured using a UV-visible spectrometer;
fig. 3 is a result of analyzing the differential spectrum signal in fig. 1.
It can be seen that the spectrum signal of the alkalization process consists of six Gaussian characteristic peaks, which reflect AOM component and characteristic information fingerprints.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. The embodiments described herein are only some embodiments of the invention, and not all embodiments. All other embodiments obtained by a person skilled in the art without any inventive step based on the spirit of the present invention are within the scope of the present invention.
(I) an online differential ultraviolet-visible spectrum detector for organic substances in water (see figure 1)
An online differential ultraviolet-visible spectrum detector for organic matters in water comprises a spectrometer optical path system and a water path system (as shown in figure 1).
(1) The spectrometer light path system comprises a light source, an optical fiber, a light splitter, a reference cell, a sample cell, a detector and data processing and display. Specifically speaking:
1) light source: xenon lamp, deuterium lamp, tungsten lamp, LED lamp, etc.
2) Fiber and splitter: the light source is divided into two paths to the reference cell and the sample cell, and the light rays penetrating through the reference cell and the sample cell are collected and transmitted to the detector.
3) Reference cell and sample cell: the reference cell is a cylindrical container made of quartz or other containers in shapes and respectively filled with a reference solution and a sample to be detected, wherein the reference cell can also be air. The optical path length of the reference cell and the sample cell is usually 1-10 cm, and can be adjusted according to specific conditions.
4) A detector: array diode detector, ultraviolet-visible spectrometer.
5) Data processing and display: the signals of the detectors corresponding to the reference cell and the sample cell are processed, displayed on a screen and stored.
The spectrometer optical path system needs to meet the following requirements: stray light of an ultraviolet-visible spectrometer is less than or equal to 0.01 percent of T; the precision of the photometer is +/-0.01A; the repeatability of the photometer is less than 0.005A; baseline drift < 0.005A/h. The device has the function of continuous wavelength scanning within the wavelength range of 200-600nm (the wavelength range can be expanded as required), can perform continuous wavelength scanning on a sample to acquire more information, and can also perform specific waveband or wavelength mode detection as required.
(2) The waterway system includes: water sample, peristaltic pump, filter, liquid storage pot, syringe pump. Specifically speaking:
1) water sampling: the sample to be detected can be manually sampled or can be automatically sampled by pumping.
2) A filter: the filter element and the filter membrane are used for intercepting the particles with large particle size, and the particles can be selected and matched.
3) A peristaltic pump: the sample is input into the sample cell and can be used as the liquid drainage of the sample cell at the same time.
4) Syringe pump system: and (3) accurately injecting the liquid in the liquid storage tank into the sample cell according to the requirement, wherein the channel is not less than 4.
5) A liquid storage tank: main reserved acid, alkali, deionized water, cleaning agent, waste liquid and other reagents capable of reacting with organic matter
(II) monitoring analysis operation method
The application also discloses a method for detecting organic matters in the water body based on the online differential ultraviolet-visible spectrum detector, which comprises the following steps:
s1: and (3) sucking the sample to be detected into the sample cell, scanning within the wavelength range of 200-600nm, and recording the scanning spectrum.
S2: adding acid or alkali solution or other reagents capable of reacting with organic matters into the sample cell through an injection pump system, scanning within the wavelength range of 200-600nm after the reaction is stable, and recording the scanning spectrum of a light source under the condition of passing through a plurality of water chemical reactions; referring to fig. 2, the uv-vis absorption spectra of the solutions were different at different pH as detected by uv-vis spectroscopy.
S3: and analyzing the spectrogram to obtain component spectrum information of the organic matters in the water body.
Example 1: a method for realizing water body monitoring based on the water body organic matter detector comprises the following steps:
step 1: preparing NaOH, KOH and other solutions with the concentration of 0.01-2 mol/L. The method is determined according to specific conditions, and the guide principle is that the dilution ratio of the sample when the target pH is reached is not higher than 1%.
Step 2: h with the concentration of 0.01-2mol/L is prepared2SO4、HNO3、HCl、HClO4And (3) solution. The method is determined according to specific conditions, and the guide principle is that the dilution ratio of the sample when the target pH is reached is not higher than 1%.
Other redox reagents and complexing/chelating reagents which can react with organic matters can be also configured in the acid and alkali liquid storage tanks.
And step 3: 2L of deionized water was prepared.
And 4, step 4: preparing a cleaning agent, and preparing a 5% potassium permanganate solution or aqua regia.
And 5: preheating a light path system and a water path system of the water organic matter detector, cleaning a pipeline, a sample pool and a reference pool, adding deionized water into the sample pool and the reference pool, and calibrating the baseline stability of the spectrometer.
Step 6: and (4) scanning and spectrum detecting the sample.
6.1 the sample to be tested is sucked into the sample cell, scanning is carried out in the wavelength range of 200-600nm, and the scanning spectrum is recorded (if single wavelength mode detection is carried out, single wavelength detection analysis is carried out, and the light absorption value is recorded, which is not repeated below).
6.2 adding a certain amount (the dilution ratio of the sample is not higher than 1%) of acid or alkali solution in the step 1 or the step 2 or other redox reagent and complexing/chelating reagent which can react with organic matters into the sample cell, after the reaction components (usually 1-120 minutes), scanning within the wavelength range of 200-600nm, and recording the scanning spectrum.
6.3 analyzing the spectrogram to obtain the components of the organic matters in the water body.
The method for analyzing the spectrogram adopted by the invention is disclosed in the previous patent application (CN201810131185.8) of the present application.
Referring to fig. 3, the ultraviolet-visible absorption spectrum fingerprint spectrum of the organic matter is calculated by extracting and analyzing data of signals measured by a spectrometer; the method specifically comprises the following steps:
(1) calculating the spectral effect (difference spectrum) by the following method:
ΔAλ＝Aλ,i-Aλ,ref (1)
wherein, Delta AλIs the difference spectrum before and after the sample reaction, Aλ,iIs the absorbance value at a specific pH (or reaction condition), wavelength lambda; a. theλ,refIs the absorption spectrum of the sample before reaction of the AOM;
(2) spectral feature peak analysis
Analyzing a spectrum effect map to obtain material components and microstructure information contained in the spectrum effect map and a fingerprint map, and firstly converting the spectrum wavelength into a spectrum with photon energy E (eV) (taking electron voltage as a unit and eV) as a horizontal coordinate by using a formula (2).
The spectral effect spectrum is analyzed by six Gaussian peaks, and each peak can be determined by the position of the peak (E)0,i) Peak width (W)i) And E ═ E0,iPeak height of (A)0,i) For complete definition, the differential spectrum is modeled by the following equation (3):
wherein λ (nm) is the wavelength, Δ A (E) is the difference in the intensity of light absorbed at photon energy E, E, E0,iMeaning the photon energy intensity and the central photon energy of the i-peak, respectively.
(3) Quantitative index of organic matter characteristics
Specific parameters can be used to quantitatively describe the components and reactivity of the organic matter.
Using Δ A (λ)pH3-7Indicating the total amount of carboxyl groups, i.e. the difference in absorption spectra at pH3 and pH 7;
using Δ A (λ)pH7-11Index the total amount of phenolic groups, i.e. the difference in absorption spectra at pH7 and pH 11;
describing the activity of the AOM by using an index in a wavelength range of 325-420 nm; the activity of the carboxyl group is described by using an index in the wavelength range of 240-275 nm. The spectral parameter calculation adopts the formulas 4-6.
ΔAλ＝Aλ,i-Aλ,ref (1)
Δln Aλ＝ln Aλ,i-ln Aλ,ref (4)
ΔAλIs the difference spectrum before and after the sample reaction, Aλ,iIs the absorbance value at a specific pH (or reaction condition), wavelength lambda; a. theλ,refIs the absorption spectrum of the sample before reaction of the AOM; lnAλ,iAnd lnAλ,refIs the logarithm of the absorbance values at the wavelength lambda at the target pH and the reference pH.
Is logarithmic of absorption spectrum at wavelength lambda1To lambda2Slope of the interval, λ1-to-λ2Means wavelength λ 1 to wavelength λ 2.
Respectively means that the absorption spectrum is logarithmized at a wavelength lambda1To lambda2Change of slope of interval, logarithm of absorption spectrum at target pH value and reference pH value, and wavelength lambda1To lambda2The slope of the interval.
And 7: and (3) after the detection is finished, discharging the liquid in the sample pool to a waste liquid tank, and cleaning the sample pool by using the cleaning agent prepared in the step (4) and the step (3) and deionized water respectively.
To reduce errors, the experimental operating conditions need to be precisely controlled. The method mainly comprises the following steps: (1) in the experiment, the solution concentration and the sample amount error are controlled within the range of 5 percent; (2) the pH has obvious influence on the spectral detection precision, the pH fluctuation is controlled within +/-0.1, and the pH can be regulated and controlled by adding a buffer solution or a proper amount of acid and alkali solution; (3) the experiment requires that the formation of precipitates is avoided, which affects the spectroscopic measurements.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the above embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which is to be covered by the claims.
Claims (8)
1. An online differential ultraviolet-visible spectrum detector for organic matters in water comprises a spectrometer optical path system and a water path system; the method is characterized in that:
in the light path system, a light source is divided into two paths through an optical fiber and a light splitter, the two paths of light sources respectively penetrate through a reference cell and a sample cell and then are collected and transmitted to a detector, and a detection result is displayed through a display module after signal processing of the detector;
the waterway system comprises a water body sample container and an injection pump system, and the water body sample is injected into the sample pool through a peristaltic pump;
the injection pump system is at least provided with four injection channels which are respectively connected with four liquid storage tanks of acid, alkali, deionized water and cleaning agent, and can inject the liquid in the corresponding liquid storage tanks into the sample cell according to the requirements through different injection channels.
2. The online differential ultraviolet-visible spectrum detector for organic matters in water bodies according to claim 1, characterized in that:
the reference cell and the sample cell are cylindrical or other containers made of quartz materials, the reference cell contains a reference solution or only injects air, and the sample cell injects a sample to be measured.
3. The online differential ultraviolet-visible spectrum detector for organic matters in water bodies according to claim 2, characterized in that:
the light path length of the reference cell and the sample cell is 1-10 cm.
The waste liquid collecting container is connected to a liquid outlet of the sample pool through a peristaltic pump.
4. The online differential ultraviolet-visible spectrum detector for organic matters in water bodies according to claim 1, characterized in that:
in an alkali liquid storage tank, preparing NaOH or KOH solution with the concentration of 0.01-2mol/L, wherein the specific concentration is set according to the following mode:
when the alkali liquor in the alkali liquor storage tank is injected into the sample cell to make the sample reach the target pH value, the dilution ratio of the sample is not higher than 1%.
5. The online detector for organic matters in water bodies according to claim 1 or 4, which is characterized in that:
in an acid storage tank, preparing H with the concentration of 0.01-2mol/L2SO4、HNO3、HCl、HClO4The specific concentration of any one of the solutions is set as follows:
when the acid liquid in the acid liquid storage tank is injected into the sample cell to enable the sample to reach the target pH value, the dilution ratio of the sample is not higher than 1%.
6. The online differential ultraviolet-visible spectrum detector for organic matters in water bodies according to claim 1 or 4, characterized in that:
the acid and base reservoirs may be configured to hold other redox, complexing/chelating reagents that react with the organic species.
7. The online differential ultraviolet-visible spectrum detector for organic matters in water bodies according to claim 1, characterized in that:
2L of deionized water is prepared in the deionized water storage tank;
in the cleaning agent storage tank, the cleaning agent is 5% potassium permanganate solution or aqua regia.
8. The method for detecting the organic matters in the water body based on the online detector of claims 1 to 7 is characterized by comprising the following steps of:
s1: sucking a sample to be detected into a sample cell, scanning within the wavelength range of 200-600nm, and recording a scanning spectrum;
s2: adding acid or alkali solution or other chemical reagents into the sample cell through an injection pump system, scanning within the wavelength range of 200-600nm after reaction components are stable, and recording the scanning spectrum of the light source passing through the sample cell under a plurality of set reaction conditions;
s3: and analyzing the spectrogram to obtain component spectrum information of the organic matters in the water body.
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