CN100476409C - Method for measuring total organic carbon in water body by chemiluminescence in ozone oxidizing process - Google Patents
Method for measuring total organic carbon in water body by chemiluminescence in ozone oxidizing process Download PDFInfo
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- CN100476409C CN100476409C CNB2005100446013A CN200510044601A CN100476409C CN 100476409 C CN100476409 C CN 100476409C CN B2005100446013 A CNB2005100446013 A CN B2005100446013A CN 200510044601 A CN200510044601 A CN 200510044601A CN 100476409 C CN100476409 C CN 100476409C
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Abstract
This invention relates to one method to test water total organic carbon, which comprises the following steps: a, sending ozone into TOC reacting room and then into water sample reaction room after filtering and isolator; b, the sample going through heating device and flowing into sample reaction room of TOC reactor through flow pump; c, the ozone and sample reacting in the room to generating optical signals; d, collecting and amplifying the signals sent by the electron-multiplier phototube in the TOC reactor and converting into electrical signals into micro computer process system and after signal processing and comparing data with standard relative curve for displaying and printing and outputting test data.
Description
Technical field
The invention belongs to the environmental chemistry monitoring technical field, specifically utilize the method for chemiluminescence principle measurement water body total organic carbon (TOC) in the ozone oxidation process.
Background technology
Total organic carbon, English name are Total Organic Carbon, are abbreviated as TOC.The method of present domestic measurement total organic carbon (TOC) is still carried out on based on the laboratory platform substantially, and the principle of employing mainly contains following several (1). and high temperature catalytic combustion-NDIR (Non-Dispersive Infrared) is surveyed (NDIR), i.e. high-temperature oxidation; (2). use oxygenant oxidations such as persulfate-NDIR (Non-Dispersive Infrared) and survey (NDIR), i.e. wet oxidation; (3). ultraviolet (UV)-persulfate oxidation-NDIR (Non-Dispersive Infrared) is surveyed (NDIR), i.e. ultraviolet ray adds analytical approachs such as wet method oxidation.
(1). high temperature catalytic combustion oxidation-NDIR (Non-Dispersive Infrared) is surveyed (NDIR) measuring principle and is: will-quantitatively water sample injects the quartz ampoule in the high temperature furnace, under 900-950 ℃ of temperature, with platinum and three cobalt oxides or chrome green is catalyzer, make the organic compound combustion cracking be converted into carbon dioxide, utilize NDIR (Non-Dispersive Infrared) to survey (NDIR) principle then and measure CO with infrared ray gas analyzer
2Content, thereby the content of total organic carbon (TOC) in definite water sample.
(2). wet oxidation (persulfate)-NDIR (Non-Dispersive Infrared) is surveyed (NDIR) measuring principle and is: potassium persulfate is an oxygenant, in course of reaction, will be in conjunction with high temperature and high pressure, with this understanding, potassium persulfate oxidation organic carbon material, generate carbon dioxide, the carbon dioxide that is generated imports the NDIR (Non-Dispersive Infrared) detecting device equally, by detecting device carbon dioxide is measured, concentration (3) ultraviolet (UV)-persulfate oxidation-NDIR (Non-Dispersive Infrared) detection (NDIR) method that can obtain TOC is basic identical with (2), just add the irradiation of ultraviolet (UV) line, the cooxidant oxidation.
Said method exists following defective in various degree: 1, must finish in the laboratory, application can not be in real time on-the-spot, and scope is restricted.2, analyze longer duration, need 1 hour at least.3, analytic process is numerous and diverse, and condition harshness, energy consumption are big, requires high to experimenter's technical merit.4, must use chemical reagent, produce secondary pollution, be unfavorable for environmental protection.
Though in recent years, along with electronic technology, new material, new technology, the development of new optical device, especially computer technology makes rapid progress, adopting the automatical analysis pattern is the corresponding appearance of instrument on basis, but because the technical difficulty of some realization aspect is too big, though this instrument has been broken away from some shortcomings of lab analysis, but the pattern from on-the-spot real-time working also has a segment distance, big as reagent consumption, on-the-spot, the real time execution cycle is short, poor stability, sensitivity and resolution are low, Deng the defective that is difficult to overcome, truly do not realize the pattern of on-the-spot real-time continuous work.
Summary of the invention
The invention provides a kind of method of utilizing chemiluminescence in the ozone oxidation process to measure the water body total organic carbon, it can solve must finishing in the laboratory that prior art exists, and range of application is limited, and produces problem such as pollution.
In order to reach the purpose that solves the problems of the technologies described above, technical scheme of the present invention is that a kind of method of utilizing chemiluminescence measurement water body total organic carbon in the ozone oxidation process is characterized in that may further comprise the steps:
(1). utilize ozone generator to produce ozone, it is sent into the Ozone chamber of TOC reaction chamber, isolator enters in the water sample reaction chamber after filtration;
(2). detected water sample is through heating apparatus, after the intensification, by the water sample reaction chamber of flow pump input TOC reaction chamber;
(3). ozone and water sample carry out hybrid reaction at the water sample reaction chamber, make between ozone and the water sample fully to mix, and produce light signal;
(4). utilize the photomultiplier of TOC reaction chamber to gather amplification to reacting the light signal that is sent, and convert electric signal to and send into the microcomputer data handling system, to the signal after handling quantize, after the time series Integral Processing, according to the correlation curve contrast of data and standard method TOC value afterwards demonstration, printout detected value.
In the present invention, also have following technical characterictic, described ozone flow is 100-200ml/min, and concentration is 2-4mg/l.
In the present invention, also have following technical characterictic, water sample is through heating, and temperature range is 40 ± 5 ℃.
In the present invention, also have following technical characterictic, described filtration isolator adopts porosint-teflon, and ozone gas is emerged from the micropore of porous material surface, in the detected water sample around being mixed into.
In the present invention, also have following technical characterictic, the light signal that reaction is sent is faint chemiluminescence signal, and wavelength coverage is at 185-850nm.
In the present invention, also have following technical characterictic, photomultiplier adopts Japanese shore pine PhotosensorModules H5784Series.
In the present invention, also have following technical characterictic, the ozone transfer pipeline in the TOC reaction chamber, waste water are got rid of pipeline and are adopted poly-PTFE, and reaction chamber adopts stainless steel material.
In the present invention, also have following technical characterictic, the microcomputer data handling system is by control and the signal Processing of software programming realization to system.
Water body total organic carbon of the present invention (TOC) in-site measurement technology, it is the important component part in the environmental monitoring system, it is a using ozone oxidation chemistry principle of luminosity, utilize chemiluminescence time series integral mode to handle, be that using ozone reacts as strong oxidizer and pollution organism, by the low-light photoelectric conversion technique light signal that produces in the course of reaction is detected and to pick up, after amplification, quantification, time series Integral Processing, with standard method contrast water-outlet body total organic carbon (TOC) content.
The contrast of method of the present invention and existing several method is as follows:
| The contrast feature | Classic method (laboratory) | Day island proper Tianjin | U.S.'s Hash | The present invention |
| Measurement range mg/l | Lower limit 0.15 | 0.2-20000 | 0.2～20000 | 0.1-20000 |
| Whether sample is handled | Need | Need | Need | Do not need |
| Measuring Time/each | 4-6 |
1 |
1 hour | (less than 10 minutes) continuously |
| Whether need reaction reagent | Need | Need | Need | Do not need |
| Have or not noxious material to form | Have | Have | Have | No |
| Environment for use | Only for the laboratory | The laboratory | The laboratory | On-the-spot |
| Working method | Burning | Combustion catalysis | Combustion catalysis | Chemiluminescence |
| Measuring accuracy % | 20-30 | 20 | 15 | 10 |
By last table contrast as can be seen, every contrast of method of the present invention all has tangible advantage and significant effect.
Ozone and water body carry out hybrid reaction at reaction chamber, in order to guarantee fully to mix between ozone and the water sample, filter isolator and adopt porosint-teflon, ozone gas is emerged from the micropore of porous material surface, in the detected water sample around being mixed into, porosint-teflon application target is to increase the gas-liquid area that contacts, and strengthens mass transfer power, mix fully, reaction efficiency is strengthened.Be the control reaction time, the continual and steady of reversal valve control ozone pressure and concentration is set.
Reaction chamber is carried out corrosion-resistant design, because ozone and a large amount of testing samples have highly corrosive, so ozone transfer pipeline, waste water are got rid of pipeline and adopted poly-PTFE, reaction chamber adopts stainless steel material.
Utilize photomultiplier that the light signal that sent of reaction is gathered amplification, and convert electric signal to and send into the microcomputer data handling system, to the signal of gathering quantize, the time series Integral Processing, show with the standard method contrast, printout.
The faint optical signal that reaction chamber produces is through the optical lens cumulative, import photomultiplier, light signal is electric signal output through the photomultiplier treatment conversion, the output electric signal is changed through the feeble signal amplifying circuit, being amplified to the certain voltage amplitude send the A/D ALT-CH alternate channel of data processing section to quantize the time series Integral Processing.
Photomultiplier of the present invention adopts Japanese shore pine Photosensor Modules H5784Series.
Utilize the microcomputer data handling system, by control and the signal Processing of software programming realization to system.
Aspect data processing, adopt instrument and reference material can cause that to optical system gain, sample turbidity etc. the factor of systematic error carries out the data correction processing.
Demarcate and on-the-spot test through the laboratory, obtain the signal correction coefficient of different water bodys, set up the correction factor database.According to the corresponding relation of the TOC value of signal time sequence integration data and standard method, the total organic carbon (TOC) that can the measure detected water sample line output of going forward side by side shows.
Ozone generating-device of the present invention is that the dry after filtration back of air is pulled the trigger by high pressure, produces high-concentrated ozone.
The present invention utilizes the method for chemiluminescence principle measurement water body total organic carbon (TOC) in the ozone oxidation process, need not add reagent, do not produce secondary pollution, can test water body total organic carbon (TOC) accurately, continuously, fast, can be at the medium-term and long-term reliably working of rugged environment.
Description of drawings
Below in conjunction with drawings and Examples the present invention is described in detail.
Fig. 1 utilizes method of the present invention to measure the process flow diagram of TOC;
Fig. 2 is the structural representation of TOC reaction chamber.
In Fig. 2,1. photomultiplier; 2. detection window; 3. water sample reaction chamber; 4. moisture outlet; 5. reaction chamber cap; 6. water inlet; 7. filtration isolator; 8. ozone air intake opening; 9. Ozone chamber; 10. reversal valve joint; 11.TOC reaction chamber.
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
As shown in Figure 1: in measuring process, system's Control Flow pump carries out water sample by predetermined flow to be carried, and water sample is transported to reaction chamber by filtration unit and attemperating unit.The purpose of filtration unit is to guarantee that water sample does not have floating material and low concentration suspension.Temperature control module is to guarantee that microorganisms in water in oxidizing process, bioluminescence can not occur.
Ozone generating-device is made up of air strainer, instrument air dryer, pneumatic pump and controlling and driving part thereof, controllable high-voltage generator, ozone generation ionization chamber etc.Ozone generation ionization chamber is sent into by pneumatic pump in the dry after filtration back of air, is excited the generation high-concentrated ozone by high voltage here, sends into reaction chamber., adopt control principle here, control the voltage output of adjustable high pressure generator, and cooperate control, guarantee that ozoniferous concentration and flow satisfy the requirement of this method pneumatic pump.
Referring to Fig. 2, the TOC reaction chamber is used mark 11 chief representatives.TOC reaction chamber 11 mainly is made of institutes such as photomultiplier 1, detection window 2, water sample reaction chamber 3, filtration isolator 7 and Ozone chambers 9.
The effect of filtering isolator 7 is not only to isolate the water sample whereabouts but also can make ozone enter water sample reaction chamber 3.
In order to guarantee fully to mix between ozone and the water sample, filter isolator 7 and adopt porosint-teflon, ozone gas is emerged from the micropore of porous material surface, in the detected water sample around being mixed into, porosint-teflon application target is to increase the gas-liquid area that contacts, strengthen mass transfer power, mix fully, reaction efficiency is strengthened.
In measuring process, water sample is sent into water sample reaction chamber 3, and ozone from Ozone chamber 9 after filtration isolator 7 enter water sample reaction chamber 3, ozone and water sample react rapidly, optics pickup apparatus-the photomultiplier of the optical signals reaction chamber sidewall that produces (Japanese shore pine Photosensor ModulesH5784 Series) is gathered amplification, and converts electric signal to and send into the microcomputer data handling system; Utilize the microcomputer data handling system, realize signal is handled, behind the time series integration,, measure the total organic carbon (TOC) of water sample, and output shows according to the correlation curve of data behind the integration and standard TOC by software programming.
(1). utilize ozone generator to produce ozone, ozone flow 100ml/min, concentration is 2mg/l, and it is sent into the Ozone chamber 9 of TOC reaction chamber, isolator 7 enters in the water sample reaction chamber 3 after filtration;
(2). detected water sample after filtration, heating apparatus, be warming up to 40 ℃, by the water sample reaction chamber 3 of flow pump input TOC reaction chamber;
(3). ozone and water sample carry out hybrid reaction at water sample reaction chamber 3, make between ozone and the water sample fully to mix, and produce light signal;
(4). the light signal that utilizes 1 pair on the photomultiplier reaction of TOC reaction chamber to be sent is gathered amplification, and convert electric signal to and send into the microcomputer data handling system, to the signal after handling quantize, after the time series Integral Processing, according to the correlation curve contrast of data and standard method TOC value afterwards demonstration, printout detected value.
(1). utilize ozone generator to produce ozone, ozone flow 200ml/min, concentration is 4mg/l, and it is sent into the Ozone chamber 9 of TOC reaction chamber, isolator 7 enters in the water sample reaction chamber 3 after filtration;
(2). detected water sample after filtration, heating apparatus, be warming up to 45 ℃, by the water sample reaction chamber 3 of flow pump input TOC reaction chamber;
(3). ozone and water sample carry out hybrid reaction at water sample reaction chamber 3, make between ozone and the water sample fully to mix, and produce light signal;
(4). the light signal that utilizes 1 pair on the photomultiplier reaction of TOC reaction chamber to be sent is gathered amplification, and convert electric signal to and send into the microcomputer data handling system, to the signal after handling quantize, after the time series Integral Processing, according to the correlation curve contrast of data and standard method TOC value afterwards demonstration, printout detected value.
(1). utilize ozone generator to produce ozone, ozone flow 150ml/min, concentration is 3mg/l, and it is sent into the Ozone chamber 9 of TOC reaction chamber, isolator 7 enters in the water sample reaction chamber 3 after filtration;
(2). detected water sample after filtration, heating apparatus, be warming up to 35 ℃, by the water sample reaction chamber 3 of flow pump input TOC reaction chamber;
(3). ozone and water sample carry out hybrid reaction at water sample reaction chamber 3, make between ozone and the water sample fully to mix, and produce light signal;
(4). the light signal that utilizes 1 pair on the photomultiplier reaction of TOC reaction chamber to be sent is gathered amplification, and convert electric signal to and send into the microcomputer data handling system, to the signal after handling quantize, after the time series Integral Processing, according to the correlation curve contrast of data and standard method TOC value afterwards demonstration, printout detected value.
(1). utilize ozone generator to produce ozone, ozone flow 170ml/min, concentration is 3.2mg/l, and it is sent into the Ozone chamber 9 of TOC reaction chamber, isolator 7 enters in the water sample reaction chamber 3 after filtration;
(2). detected water sample after filtration, heating apparatus, be warming up to 39 ℃, by the water sample reaction chamber 3 of flow pump input TOC reaction chamber;
(3). ozone and water sample carry out hybrid reaction at water sample reaction chamber 3, make between ozone and the water sample fully to mix, and produce light signal;
(4). the light signal that utilizes 1 pair on the photomultiplier reaction of TOC reaction chamber to be sent is gathered amplification, and convert electric signal to and send into the microcomputer data handling system, to the signal after handling quantize, after the time series Integral Processing, according to the correlation curve contrast of data and standard method TOC value afterwards demonstration, printout detected value.
(1). utilize ozone generator to produce ozone, ozone flow 130ml/min, concentration is 2.8mg/l, and it is sent into the Ozone chamber 9 of TOC reaction chamber, isolator 7 enters in the water sample reaction chamber 3 after filtration;
(2). detected water sample after filtration, heating apparatus, be warming up to 42 ℃, by the water sample reaction chamber 3 of flow pump input TOC reaction chamber;
(3). ozone and water sample carry out hybrid reaction at water sample reaction chamber 3, make between ozone and the water sample fully to mix, and produce light signal;
(4). the light signal that utilizes 1 pair on the photomultiplier reaction of TOC reaction chamber to be sent is gathered amplification, and convert electric signal to and send into the microcomputer data handling system, to the signal after handling quantize, after the time series Integral Processing, according to the correlation curve contrast of data and standard method TOC value afterwards demonstration, printout detected value.
In the above-described embodiments, the light signal that reaction is sent is faint chemiluminescence signal, and wavelength coverage is at 185-850nm.
After testing, from the bathing beach, several sea areas sampling such as harbour, off-lying sea, be divided into two parts.Portion detects in Shandong Province's ocean monitoring technologytechnologies key lab, and portion is monitored with method of the present invention.
Being compared as follows of this method and national marine monitoring standard (HY003.4-91) measured TOC value:
Experiment shows that both methods have good corresponding relation, and consequently the TOC deviation is smaller or equal to 10%.
Claims (8)
1. method of utilizing chemiluminescence in the ozone oxidation process to measure the water body total organic carbon is characterized in that may further comprise the steps:
(1). utilize ozone generator to produce ozone, it is sent into the Ozone chamber of TOC reaction chamber, isolator enters in the water sample reaction chamber after filtration;
(2). detected water sample is through heating apparatus, after the intensification, by the water sample reaction chamber of flow pump input TOC reaction chamber;
(3). ozone and water sample carry out hybrid reaction at the water sample reaction chamber, make between ozone and the water sample fully to mix, and produce light signal;
(4). utilize the photomultiplier of TOC reaction chamber to gather amplification to reacting the light signal that is sent, and convert electric signal to and send into the microcomputer data handling system, to the signal after handling quantize with the time series Integral Processing after, according to the correlation curve contrast demonstration printout afterwards detected value of data and standard method TOC value.
2. according to the method for the measurement water body total organic carbon of claim 1, it is characterized in that the ozone flow is 100-200ml/min, concentration is 2-4mg/1.
3. according to the method for the measurement water body total organic carbon of claim 1 or 2, it is characterized in that water sample is through heating, temperature range is 40 ± 5 ℃.
4. according to the method for the measurement water body total organic carbon of claim 3, it is characterized in that, described filtration isolator porosint, promptly teflon is emerged ozone gas from the micropore of porous material surface, in the detected water sample around being mixed into.
5. according to the method for the measurement water body total organic carbon of claim 1, it is characterized in that the light signal that reaction is sent is faint chemiluminescence signal, wavelength coverage is at 185-850nm.
6. according to the method for the measurement water body total organic carbon of claim 5, it is characterized in that photomultiplier adopts Japanese shore pine Photosensor Modules H5784 Series.
7. according to the method for the measurement water body total organic carbon of claim 4, it is characterized in that ozone transfer pipeline in the TOC reaction chamber and waste water are got rid of pipeline and adopted poly-PTFE, reaction chamber adopts stainless steel material.
8. according to the measurement water body total organic carbon method of claim 6, it is characterized in that the microcomputer data handling system is by control and the signal Processing of software programming realization to system.
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