CN107101996B - A kind of real-time online dynamic detection system of pentachlorophenol degradation intermediate - Google Patents
A kind of real-time online dynamic detection system of pentachlorophenol degradation intermediate Download PDFInfo
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Abstract
The invention discloses a kind of real-time online dynamic detection systems of pentachlorophenol degradation intermediate.It includes excitation light source, pentachlorophenol degradation reaction container, chemical oxidation reagent container, chemiluminescence detection pond, photomultiplier tube and signal analyzer host；Pentachlorophenol degradation reaction container and chemical oxidation reagent container are connected with chemiluminescence detection pond；Photomultiplier tube is used to the optical signal generated in chemical detection pond being converted to electric signal；Photomultiplier tube is connected with signal analyzer host, and signal analyzer host is connected with computer terminal.Using real-time online dynamic detection system of the present invention detect when, can on-line determination, it is easy to operate, it does not need to separate sample offline, then the processes such as upper machine testing, therefore finding speed is fast, working efficiency is improved, rapid screening and assessment suitable for catalysis material for pentachlorophenol ability of degrading；The system can also track the dynamic change of TrCBQ-OH and TCBQ online, by dynamic information, track its generation and degradation process.
Description
Technical field
The present invention relates to a kind of real-time online dynamic detection systems of pentachlorophenol degradation intermediate.
Background technique
Pentachlorophenol is a kind of common chlorinated aromatic organic pollutant, due to the antibacterial, desinsection, fire-retardant etc. with wide spectrum
Effect is widely used as the anti-corrosion and disinfection of the products such as industrial and agricultural production raw material and timber, coating.It can by volatilization,
The approach such as container leakage, discharge of wastewater enter environment, seriously polluted atmosphere, soil, underground water and surface water.These persistence
Organic matter just can lead to biomutation in the reconditioning of ultra trace.Therefore, the pentachlorophenol pollutant removed in environment is to work as
One of the main task of modern environmental problem.Light (catalysis) degradation technique is due to having the characteristics that hypotoxicity, oxidability are strong, in chlorine
Phenolic comp ' ds pollution degradation and improvement aspect have obtained extensive concern.But in photocatalysis treatment, most researchs are thought to drop at present
The chlorophenols of solution determines the palliating degradation degree of entire reaction process, only focuses on the degradation efficiency of chlorophenols and influences degradation effect
The external condition of rate, however often after the concentration of former degradation material is met the requirements, the bigger intermediate production of toxicity may be generated
Object, this just causes bigger harm to environment and human health.Therefore, research control pentachlorophenol contaminant degradation dynamic process and
The generation of its high toxicity intermediate is the premise and key that can degradation technique carry out practical application.
Under the conditions of different photocatalysis, the degradation process and approach of pentachlorophenol are not quite similar, Antonopoulou et al.
[Environ.Sci.Pollut.Res., 2015,22,9438] reports nitrogen/Fluorin doped TiO2Photocatalytic degradation pentachlorophenol process
In, in condition of different pH, it may occur that its different degradation pathway；And the generation of wherein mesosome and poisonous effect are evaluated, recognize
Its dechlorination product TCBQ is mainly derived from for the risk of toxicity in PCP degradation process.And Mills and Hoffmann
[Environ.Sci.Technol., 1993,27,1681] points out pentachlorophenol in TiO2In photocatalytic system, main intermediate production
Object is p- tetrachloroquinone and four chlorohydroquinones；But itself the study found that its illumination each PCP early period dechlorination molecular number be 1.8, dropping
Four chloro thing of solution initial stage is not unique dechlorination intermediate, is likely present de- 2 or 3 chloros benzoquinones intermediate, Preliminary Study
Speculate that the low chloro intermediate of this high toxicity is TrCBQ-OH.But at present for the research of pentachlorophenol photocatalytic degradation reaction process
Means mainly have high performance liquid chromatography, mass spectrography etc., these are required to addition selective probe and are captured, then at some
Between point be sampled, separate, measuring, have sensitivity it is low, it is cumbersome it is time-consuming, online dynamic analysis in situ can not be carried out, can not be right
Pentachloro- phenolic comp ' ds pollution degradation toxic intermediate generating process provides enough online verifying means in situ, to its photocatalytic degradation
The generation of toxic intermediate and knowledge of regularity are not enough.Therefore, a kind of real-time online dynamic detection system is established, toxicity chlorine is used for
It is necessary for research pentachlorophenol degradation process, mechanism and its risk of toxicity for the dynamic monitoring of benzoquinones substance.
Summary of the invention
The object of the present invention is to provide a kind of real-time online dynamic detection system of pentachlorophenol degradation intermediate, the present invention will
It flows chemoluminescence method and is applied to photocatalysis field, combined by the way that chemical photic device will be flowed with photocatalytic reaction device,
Realize that carrying out real-time online dynamic to the TrCBQ-OH and TCBQ generated in pentachlorophenol degradation process examines by chemical luminous system
It surveys；Real-time online dynamic detection system of the present invention can also be used in assessment and the pentachlorophenol biodegrading process of various pentachlorophenol biodegrading process
Condition optimizing and pentachlorophenol degradation process in the generation of TrCBQ-OH and TCBQ and the research of degradation behavior.
Present invention firstly provides a kind of real-time online dynamic testing methods of pentachlorophenol degradation intermediate, including walk as follows
It is rapid:
Under photocatalysis or the catalysis of photochemical catalyst, pentachlorophenol degradation generates intermediate；Using flowing chemoluminescence method inspection
The chemiluminescence signal of the redox reaction product of the intermediate and chemical oxidation reagent is surveyed, that is, realizes and degrades to pentachlorophenol
The real-time online dynamic detection of intermediate；
The intermediate is trichlorine hydroxyl -1,4- benzoquinones (TrCBQ-OH) and four chloro- 1,4- benzoquinones (TCBQ).
In the present invention, the flowing chemoluminescence method is referred to: the centre that pentachlorophenol and its light (catalysis) reaction are generated
Body is continuously transmitted to sensing chamber and mixes generation chemiluminescence reaction with chemical oxidation reagent, generated by flow device
Luminous signal, while the optical signal received is converted by electric signal by photomultiplier tube, after enhanced processing, pass through number
It is shown on computer screen according to line transmission；And the generation and disappearance process of the direct reaction intermediate of variation of signal, therefore there is behaviour
Make the advantages that simple, finding speed is fast, high sensitivity, specificity are good, real-time online, be suitable for the degradation feature of pentachlorophenol: five
Chlorophenols photocatalytic degradation intermediate species are various, and the toxic intermediate TrCBQ-OH and TCBQ generated in reaction has concentration
It is low, the service life is shorter, and be easy hydrolysis and conversion etc., the present invention by flow chemiluminescence analysis method be applied to pollution object light urge
The research field for changing degradation process establishes pentachlorophenol photocatalytic degradation flowing chemiluminescence system for pentachlorophenol degradation process
The dynamic of Poisoning intermediate generates and tracking.
In above-mentioned real-time online dynamic testing method, the chemical oxidation reagent can for hydrogen peroxide or hydrogen peroxide with
The mixed liquor of buffer solution, the molar concentration of hydrogen peroxide can be 0.01~0.5M in the mixed liquor, concretely 0.1M.
In above-mentioned real-time online dynamic testing method, in ultraviolet light (such as from mercury lamp, deuterium lamp or ultraviolet LED) or can
It degrades under the catalysis of light-exposed (such as from xenon lamp or LED light source) pentachlorophenol.
In above-mentioned real-time online dynamic testing method, photocatalysis material in the prior art is can be used in the photochemical catalyst
Material, such as titanium dioxide, zinc oxide.
In above-mentioned real-time online dynamic testing method, electricity is converted for the chemiluminescence signal using photomultiplier tube
Signal is transmitted to computer terminal after enhanced processing and is analyzed.
Based on chemiluminescence analysis method, the real-time online that the present invention still further provides a kind of phenol degradation intermediate is dynamic
State detection system, it includes excitation light source, pentachlorophenol degradation reaction container, chemical oxidation reagent container, chemiluminescence detection
Pond, photomultiplier tube and signal analyzer host；
The pentachlorophenol degradation reaction container and the chemical oxidation reagent container with the chemiluminescence detection
Pond is connected；
The photomultiplier tube is used to the optical signal generated in the chemical detection pond being converted to electric signal；
The photomultiplier tube is connected with signal analyzer host, the signal analyzer host and a computer terminal phase
Connection.
In above-mentioned real-time online dynamic detection system, the pentachlorophenol degradation reaction container and the chemiluminescence detection
It is equipped with peristaltic pump between pond, is pumped into the mixed of pentachlorophenol or pentachlorophenol and photochemical catalyst into the chemiluminescence detection pond with quantitative
Close liquid；
Peristaltic pump is equipped between the chemical oxidation reagent container and the detection cell, with quantitative to the chemistry
Chemical oxidation reagent is pumped into luminescence detecting pool.
In above-mentioned real-time online dynamic detection system, the excitation light source is ultraviolet lamp source (such as mercury lamp, deuterium lamp, ultraviolet
) or visible light source (such as xenon lamp, LED light source) LED.
Real-time online dynamic detection system of the present invention being capable of simple, quick, sensitive measurement pentachlorophenol degradation process toxicity
The generation and conversion of intermediate TrCBQ-OH and TCBQ, and then light reflex system quickly sieves the degradation capability of chlorinated phenol
It looks into and assesses.
Real-time online dynamic detection system of the present invention can also in real time, on-line determination pentachlorophenol degradation process, may be implemented
Generation and decaying behavior to toxic intermediate TrCBQ-OH and TCBQ carry out real-time online track determining, are become by luminous signal
The dynamic information of change is studied pentachlorophenol degradation process and mechanism, is verified through the specific embodiment of the invention, photocatalysis pH value of solution
The generation type of two kinds of intermediates can be influenced with pentachlorophenol initial concentration, generate the multidate informations such as concentration and time of occurrence.
Real-time online dynamic detection system of the present invention can also be used in the assessment and pentachlorophenol drop of various pentachlorophenol biodegrading process
The condition optimizing of solution method.
Real-time online dynamic detection system of the present invention can quantitative detection TrCBQ-OH and TCBQ.
The present invention has the advantage that compared with the conventional method
1) real-time online dynamic detection system structure of the present invention is simple and at low cost, is easy to business promotion.
2) high sensitivity of real-time online dynamic testing method of the present invention, specificity are good, overcome among light-catalyzed reaction
Bulk concentration is low, needs the problems such as sample pre-treatments.
3) using real-time online dynamic detection system of the present invention detection when, can on-line determination, it is easy to operate, do not need to sample
Product are separated offline, then the processes such as upper machine testing, therefore finding speed is fast, improves work efficiency, and is suitable for photocatalysis
Rapid screening and assessment of the material for pentachlorophenol ability of degrading.
4) when detecting using real-time online dynamic detection system of the present invention, it can be realized online the real time measure, it can be online
The dynamic change for tracking TrCBQ-OH and TCBQ tracks its generation and degradation process by dynamic information.
Detailed description of the invention
Fig. 1 is the schematic diagram of the real-time online dynamic detection system of pentachlorophenol of the present invention degradation intermediate.
It is respectively marked in figure as follows:
1 simulating sun light source, 2 pentachlorophenol degradation reaction containers, 3 chemical oxidation reagent containers, 4,5 peristaltic pumps, 6 chemistry
Luminescence detecting pool, 7 photomultiplier tubes, 8 signal analyzer hosts, 9 computer terminals.
Fig. 2 is that the chemiluminescence that pentachlorophenol Photocatalytic Degradation Process high toxicity intermediate TrCBQ-OH and TCBQ are generated shines
Intensity changes with time and its compares with mass spectrometry method, hair when wherein Fig. 2 (a) and Fig. 2 (b) is respectively undegraded and degradation
Optical signal changes with time, the mass signal value of TrCBQ-OH and TCBQ during Fig. 2 (c) pentachlorophenol catalytic degradation.
Fig. 3 is present system for measuring the obtained standard curve of TrCBQ-OH, wherein corresponding to curve a-g
The concentration of TrCBQ-OH standard solution is respectively as follows: 0 μM, 1 μM, 2 μM, 5 μM, 8 μM, 10 μM and 20 μM.
Fig. 4 is present system for measuring the obtained standard curve of TCBQ, and wherein TCBQ corresponding to curve a-g is marked
The concentration of quasi- solution is respectively as follows: 0 μM, 0.5 μM, 1 μM, 2 μM, 5 μM, 10 μM and 20 μM.
Fig. 5 is used in the different initially pH systems of dynamic measurement generated in pentachlorophenol degradation process for present system
The chemiluminescence luminous intensity of TrCBQ-OH and TCBQ changes with time, and the initial pH that wherein Fig. 5 (A) is indicated is 10, Fig. 5
(B) it is 3 that the initial pH indicated, which is the initial pH that the initial pH that 7, Fig. 5 (C) is indicated is 5, Fig. 5 (D) expression,.
Fig. 6 is generated in degradation process when present system is used to dynamically measure different initial pentachlorophenol concentration
The chemiluminescence luminous intensity of TrCBQ-OH and TCBQ changes with time, and the pentachlorophenol initial concentration that wherein Fig. 6 (A) is indicated is
30 μM, the pentachlorophenol initial concentration that Fig. 6 (B) is indicated is 20 μM, and the pentachlorophenol initial concentration that Fig. 6 (C) is indicated is 10 μM.
Specific embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Fig. 1 is pentachlorophenol Photocatalytic Degradation Process toxic intermediate TrCBQ-OH and TCBQ real-time online provided by the invention
The structural schematic diagram of dynamic detection system, it includes simulating sun light source 1, pentachlorophenol photocatalytic degradation reaction vessel 2, chemical oxidation
Reagent container 3, peristaltic pump 4 and 5, chemiluminescence detection pond 6, photomultiplier tube 7, signal analyzer host 8 and computer are whole
End 9.Mercury lamp, xenon lamp, deuterium lamp or LED may be selected in simulating sun light source 1, for make pentachlorophenol light degradation generate TrCBQ-OH and
TCBQ, or for exciting photochemical catalyst, photocatalyst for degrading pentachlorophenol is made to generate TrCBQ-OH and TCBQ.Pentachlorophenol degradation is anti-
Answer container 2 for holding pentachlorophenol solution or pentachlorophenol and photochemical catalyst mixed solution to be degraded, pentachlorophenol degradation reaction
Container 2 is connected with chemiluminescence detection pond 6, and a peristaltic pump 4 is equipped between them, is used to provide power.Chemical oxidation
Reagent container 3 carries out redox reaction for holding chemical oxidation reagent, with TrCBQ-OH and TCBQ, generates light letter
Number, to be detected.Chemical oxidation reagent container 3 is connected with chemiluminescence detection pond 6, and one is equipped between them
Peristaltic pump 5, is used to provide power.Photomultiplier tube 7 is used to the optical signal generated in chemiluminescence detection pond 6 being converted to telecommunications
Number, it is then transmit to signal analyzer host 8, signal analyzer host 8 is connected with computer terminal 9, will test result progress
Display.
With pentachlorophenol/TiO2For photocatalytic system, illustrate the present embodiment Real-time and Dynamic Detection system measurement pentachlorophenol light
The specific implementation process of the toxic intermediate TrCBQ-OH and TCBQ that are generated during catalytic degradation:
As shown in Figure 1, first by finely dispersed TiO2Particle and certain density pentachlorophenol solution are transferred to pentachlorophenol
In photocatalytic degradation device, it is protected from light stirring and reaches the attached balance of absorption-desorption in 30 minutes.Chemical illuminating reagent is transferred to chemical hair
In light reagent container 3.When testing progress, light source 1 is opened, pentachlorophenol is made to carry out Photocatalytic Degradation Process and is generated
TrCBQ-OH and TCBQ.Start flow device peristaltic pump 4 and peristaltic pump 5 simultaneously, by pentachlorophenol/TiO2Mixed solution (TiO2It is dense
Degree is 0.2g/L), chemical oxidation reagent (H2O2With the mixed liquor of buffer solution, wherein H2O2Concentration be 0.1M) pass through pipeline
It is transmitted to the progress biochemical reaction of hybrid concurrency in chemiluminescence detection pond 6, generates chemiluminescence signal.Meanwhile being located at chemistry
The optical signal received is converted into electric signal by the photomultiplier tube 7 of 6 lower section of luminescence detecting pool, after enhanced processing, is passed through
Data line is transferred on the display of computer terminal 7.When light source is not opened, pentachlorophenol cannot be degraded, without TrCBQ-OH
Almost very low signal with the generation of TCBQ, therefore display screen display is background noise (Fig. 2 (a)).Conversely, when light source is opened
Qi Shi, pentachlorophenol is in photochemical catalyst TiO2Under catalysis, degrade, the intermediate TrCBQ-OH and TCBQ of generation detection cell with
Oxidants hydrogen peroxide mixing occurs redox reaction and generates chemiluminescence signal (Fig. 2 (b)), to realize to pentachloro-
Phenol is degraded the dynamic in-situ measurement of intermediate TrCBQ-OH and TCBQ, and with the progress of pentachlorophenol Photocatalytic Degradation Process,
The generation and conversion of intermediate TrCBQ-OH and TCBQ can successively occur, thus show screen display chemiluminescence signal be with
The photocatalytic degradation time gradually rise, reduce, increasing again, reducing again and to obtain dynamic-change information.This chemiluminescence signal difference
The dynamic that represent TrCBQ-OH (first glow peak) and TCBQ (second glow peak) is generated, generated, decaying and its conversion
Process.Mass spectroscopy signal value (such as Fig. 2 (c)) in this chemiluminescence signal and pentachlorophenol Photocatalytic Degradation Process has very
Good correlation.
Light source 1 is closed, pentachlorophenol solution is replaced with TrCBQ-OH standard solution and TCBQ standard solution respectively, can be used for
The quantitative detection of TrCBQ-OH and TCBQ standard solution, testing result difference are as shown in Figure 3 and Figure 4.
In Fig. 3 the concentration of TrCBQ-OH standard solution corresponding to curve a-g be respectively as follows: 0 μM, 1 μM, 2 μM, 5 μM, 8 μM,
10 μM and 20 μM.
The concentration of TCBQ standard solution corresponding to curve a-g is respectively as follows: 0 μM, 0.5 μM, 1 μM, 2 μM, 5 μM, 10 in Fig. 4
μM and 20 μM.
Had in 0.15 μM to 20 μM concentration range by TrCBQ-OH and TCBQ it can be seen from Fig. 3 and Fig. 4 good
Linear relationship, about 0.05 μM of detection limit.
Using real-time online dynamic detection system of the present invention, (different pH and difference five have been investigated in different photocatalytic systems
Chlorophenol concentration), the dynamic of high toxicity intermediate TrCBQ-OH and TCBQ generate and conversion in the Photocatalytic Degradation Process of pentachlorophenol
Process.
Fig. 5 is used in the different initially pH systems of dynamic measurement generated in pentachlorophenol degradation process for present system
TrCBQ-OH and TCBQ, the initial pH=10 that wherein Fig. 5 (A) is indicated；The initial pH=7 that Fig. 5 (B) is indicated；What Fig. 5 (C) was indicated
Initial pH=5；The initial pH=3 that Fig. 5 (D) is indicated.
It is generated in degradation process when Fig. 6 is that present system is used to dynamically measure different initial pentachlorophenol concentration
TrCBQ-OH and TCBQ, pentachlorophenol initial concentration=30 μM that wherein Fig. 6 (A) is indicated；The pentachlorophenol that Fig. 6 (B) is indicated is initially dense
=20 μM of degree；Pentachlorophenol initial concentration=10 μM that Fig. 6 (C) is indicated.
Photocatalysis pH value of solution and pentachlorophenol initial concentration can influence two kinds of intermediates it can be seen from Fig. 5 and Fig. 6
It generates type, generate the multidate informations such as concentration and time of occurrence.Illustrate that pentachlorophenol photocatalysis may be implemented using present system
The online tracking of degradation process toxic intermediate TrCBQ-OH and TCBQ and dynamic change, and then be the pentachloro- of research toxicity guidance
Phenol degradation process and mechanism provide support.
The invention is equally applicable to pentachlorophenol degradation process risk of toxicity under the conditions of different catalysis materials and photocatalysis
Rapid screening and assessment.
Claims (1)
1. a kind of real-time online dynamic testing method of pentachlorophenol degradation intermediate, includes the following steps:
Under photocatalysis and the catalysis of photochemical catalyst, pentachlorophenol degradation generates intermediate；Institute is detected using flowing chemoluminescence method
The chemiluminescence signal of the redox reaction product of intermediate and chemical oxidation reagent is stated, that is, is realized intermediate to pentachlorophenol degradation
The real-time online dynamic detection of body；
The intermediate is trichlorine hydroxyl -1,4- benzoquinones and four chloro- 1,4- benzoquinones；
The chemical oxidation reagent is the mixed liquor of hydrogen peroxide and buffer solution；
It degrades under the catalysis of ultraviolet light or visible light the pentachlorophenol；
Electric signal is converted for the chemiluminescence signal using photomultiplier tube, be transmitted to after enhanced processing computer terminal into
Row analysis.
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| CN102809559A (en) * | 2012-08-21 | 2012-12-05 | 中国科学院生态环境研究中心 | Method for detecting halogenated aromatic organic matter |
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| CN102809559A (en) * | 2012-08-21 | 2012-12-05 | 中国科学院生态环境研究中心 | Method for detecting halogenated aromatic organic matter |
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