CN105675832A - Apparatus and method for measuring total organic carbon (TOC) - Google Patents
Apparatus and method for measuring total organic carbon (TOC) Download PDFInfo
- Publication number
- CN105675832A CN105675832A CN201510891903.8A CN201510891903A CN105675832A CN 105675832 A CN105675832 A CN 105675832A CN 201510891903 A CN201510891903 A CN 201510891903A CN 105675832 A CN105675832 A CN 105675832A
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- water
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
- G01N33/1826—Water organic contamination in water
- G01N33/1846—Total carbon analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
- G01N33/1806—Water biological or chemical oxygen demand (BOD or COD)
Abstract
The invention provides an apparatus and method for measuring total organic carbon in sea water, high-chlorine and -salt wastewater, surface water, underground water, drinking water, domestic sewage and industrial wastewater, wherein the apparatus mainly includes a multi-position valve, a combined oxidization reactor, a gas-liquid separator, a halogen remover, a membrane filter, a multi-channel detector, and a data processing and display apparatus. The apparatus can be used for measuring the total organic carbon in water for measurement in laboratories, on-line measurement and emergent portable in-site measurement.
Description
Technical field
The present invention relates to a kind of water quality analyzer device, it is a kind of device measuring total organic carbon in water specifically.
Background technology
Organic pollutant in current water is growing on and on, and organic contamination is the main problem of water pollution, and our life be unable to do without water, and therefore we more and more pay attention to the monitoring problem for water and sewage. Total organic carbon TOC (Totalorganiccarbon) is the summation of the carbon content of the organic substance in water, and the principal element in organism is represented by the amount of carbon, and TOC can reflect that organism is to the pollution level of water body completely.
The organic content in water body (federal industrial standards D-2579) mainly detects with TOC index in the present U.S., Japan also lists Japanese Industrial Standards (JISK0102) in TOC index, China also using its one of index as water quality detection, lists GB in. " in sewage drainage standard GB8978-1996 " and " drinking water sanitary standard GB5749-2006 ".
The external general price of water quality TOC analyser is very expensive, and universal at home also have certain difficulty; On the other hand, from independent intellectual property right angle, in several years of future, China should progressively formulate oneself TOC standard method of analysis and corresponding technical specifications and agreement. Our research provides solid theoretical basis and experiment basis will to evaluation method from now on and technical protocol, and provides the detecting instrument of low cost and instruments design theoretical.
The measuring method of current TOC mainly adopts combustion oxidation method and wet oxidation process, and namely first is CO the oxidation operation in water2, then measure CO2Gas gross. Combustion oxidation method is divided into 900-950 DEG C of catalyticcombustion oxidation style and 680 DEG C of catalytic oxidations; Wet oxidation process can be divided into persulphate catalytic oxidation and ultraviolet catalytic oxidation style; CO2Mensuration adopt non-dispersive infrared method and conductometric titration.
In the development of surveying instrument, development and production have the various types of TOC analysers comprising and realizing continuous on-line monitoring both at home and abroad. Different by principle of work, combustion oxidation-NDIR method can be divided into; Heating-persulfate oxidation-NDIR method; UV photochemical catalysis-persulfate oxidation-NDIR method, ion selective electrode (ISE) method, conductometric titration, vapor-phase chromatography etc. Wherein, combustion oxidation-NDIR method only needs disposable conversion, and flow process is simple, for extensively adopting both at home and abroad.
Imported product, although its detection method is ripe, accuracy of detection height, but there is the problem such as complex structure, price height, combustion oxidation method and wet oxidation process heating 40-50 minute, cooling 40-50 minute, the time is long, and power consumption is high, and volume is big.The instrument detection TOC that actual needs one batch of structure is simple, cost is lower. Use just as ammeter is the same with water meter. This demand is very huge, develops new detection method and detecting instrument is very important for this reason.
Single mode of oxidizing oxidation organic pollutant can not realize complete oxidation, it is necessary to combination, the mode of oxidizing of associating.
In actual use, although infrared detector (NDIR) is widely used, but, NDIR is big by temperature, humidity effect, affects measurement accuracy, it is necessary to have replacement or auxiliary detector.
Summary of the invention
For the deficiencies in the prior art, it is an object of the invention to provide the determinator of total organic carbon in a kind of seawater, high chlorine high-salt wastewater, the surface water, underground water, tap water, sanitary sewage, trade effluent and method, can be used for experimental determination, on-line determination, emergent portable field mensuration.
In mensuration water provided by the invention, the device of chlorion and total organic carbon, mainly comprises multi-position valve, combination oxidation reactor, gas-liquid separator, halogen remover, film filter, double-channel detector, data processing and display unit.
Foregoing device, it is preferable that scheme be, when for scene meet an urgent need portable mensuration time, CO2 removal cleaner can be installed before quantitative sampling device.
Foregoing device, it is preferable that scheme be that described multi-position valve can be 2 logical valves, 3 logical valves, 6 logical valves, 10 logical valves etc.
Foregoing device, preferred scheme is, described combination oxidation reactor can be made with the material such as platinum, quartz, and combination oxidation reactor adopts Ultraviolet Oxidation device, ozone oxidation device, microwave oxidizer, hydrogen peroxide combination mode of oxidizing oxidation Organic substance in water; Wherein, microwave oxidizer can adopt light wave oxidizer, ultrasound oxidation technology device, carbon fiber oxidizer, electrically heated to replace, and cocatalyst has titanium dioxide, cupric oxide, platinum; Use high purity oxygen gas, high pure air, rare gas element, nitrogen as carrier gas.
Foregoing device, it is preferable that scheme be, described multichannel detector, it is possible to be 1,2,3,4,5 kind of detector, such as infrared detector (NDIR) and electrical conductivity detector; Wherein, infrared detector (NDIR), electrical conductivity detector can adopt plasma atomic emission spectrometer, laser gas analyzer, hydrogen flameionization method flame ionization ditector, coulomb analyser, ultraviolet spectroscopy and carry out optical signal gathering by photomultiplier and amplify, and the detector (chemoluminescence method detector) converting the analysis process system of electrical signal to replaces.
Foregoing device, it is preferable that scheme be that the device of total organic carbon in described mensuration water, realizes the needs of control automatically with software programming and micro-chip, PLC, data collecting card, stepper-motor, servomotor; May be used for solid matter such as soil, solid waste, solid article etc., gas, after being manipulated so water sample, measures the concentration of total organic carbon (TOC).
Present invention also offers the method that the device described in utilization measures total organic carbon in water, step is:
The mensuration of TOC concentration: a testing sample part enters acidification reactor, acidification reactor adds acid solution (such as phosphoric acid solution), inorganic carbon such as sodium carbonate, sodium bicarbonate and acid-respons is made to decomposite carbonic acid gas, detector measures gas concentration lwevel, with organic carbon concentration in minusing calculation sample, or the carbonic acid gas that inorganic carbon is produced directly discharges.
Na2CO3+2H+→2Na++H2O+CO2↑
NaHCO3+H+→Na++H2O+CO2↑
Testing sample another part enters combination oxidation reactor, make total organic carbon generation oxidizing reaction in sample, produce carbonic acid gas, by gas-liquid separator, after film filter, enter detector and measure gas concentration lwevel, extrapolating organic carbon concentration in sample according to gas concentration lwevel, organic carbon concentration stores in a database, shows at upper computer (display screen) simultaneously, or by network, it is transferred to remote display.
Total organic carbon oxidizing reaction formula is:
CnHn+O2→CO2+H2O
Organic carbon concentration (TOC) and chemical oxygen demand (COD) (COD) concentration show simultaneously
One is that COD is the oxygen (O consumed theoretically2), representing oxygen-consumption, TOC represents oxygen-consumption, then COD=K*TOC with carbon (C), because C+O2=CO2, so K=32/12=2.67.
Two is the linear regression theory using organic carbon concentration (TOC) and chemical oxygen demand (COD) (COD), according to Y=a+bX, measure the series concentration of TOC and COD respectively, extrapolate the concentration of chemical oxygen demand (COD) (COD), accomplish to show organic carbon concentration (TOC) and chemical oxygen demand (COD) (COD) concentration over the display simultaneously;
Accompanying drawing explanation
In order to be illustrated more clearly in the present invention, simply introduce the accompanying drawing used required in the present invention is done one below, apparently, accompanying drawing in the following describes is some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, it is also possible to obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the structural representation that embodiment 1 measures total organic carbon device in water
Fig. 2 is the structural representation that embodiment 2 measures total organic carbon device in water
Fig. 3 is the structural representation measuring the combination oxidation reactor device of total organic carbon in water
Fig. 4 is another kind of structural representation measuring the combination oxidation reactor device of total organic carbon in water
Wherein, 1, multi-position valve; 2, oxidation reactor is combined; 2-1, water sample import to be measured; 2-2, hydrogen peroxide import; 2-3 Ultraviolet Oxidation device; 2-4, ozone import; 2-5, ozone reaction room; 2-6, microwave oxidizer; 2-7, ozone equilibrium device; 2-8, pneumatic outlet; 3, gas-liquid separator; 4, film filter; 5-1, NDIR infrared detector; 5-2, electrical conductivity detector; 5-3, UV-detector; 6, data handler; 7, indicating meter; 8, network data transmission device; 9, acidification reactor; 10, acid solution;
Embodiment
The technical scheme of the present invention is described in detail below in conjunction with embodiment and accompanying drawing, but protection domain is not by this restriction.
Embodiment 1 measures the device of total organic carbon in water, accompanying drawing 1, Fig. 3:
The mensuration of TOC concentration: a testing sample part enters 9. acidification reactors, 9. acidification reactors add 10. acid solutions (such as phosphoric acid solution), inorganic carbon such as sodium carbonate, sodium bicarbonate and acid-respons is made to decomposite carbonic acid gas, detector 5-1 or 5-2 measures gas concentration lwevel, with organic carbon concentration in minusing calculation sample, or the carbonic acid gas that inorganic carbon is produced directly discharges.
Na2CO3+2H+→2Na++H2O+CO2↑
NaHCO3+H+→Na++H2O+CO2↑
Testing sample another part enters 2, combines oxidation reactor, make total organic carbon generation oxidizing reaction in sample, produce carbonic acid gas, by 3. gas-liquid separators, 4. after film filter, enter detector 5-1 or 5-2 and measure gas concentration lwevel, in 6. data handlers, organic carbon concentration in sample is extrapolated according to gas concentration lwevel, organic carbon concentration is stored in database or file, show in 7. indicating meters simultaneously, or by 8. network data transmission devices, it is transferred to remote display.
Total organic carbon oxidizing reaction formula is:
CnHn+O2→CO2+H2O
Organic carbon concentration (TOC) and chemical oxygen demand (COD) (COD) concentration show simultaneously
One is that COD is the oxygen (O consumed theoretically2), representing oxygen-consumption, TOC represents oxygen-consumption, then COD=K*TOC with carbon (C), because C+O2=CO2, so K=32/12=2.67.
Two is the linear regression theory using organic carbon concentration (TOC) and chemical oxygen demand (COD) (COD), according to Y=a+bX, measure the series concentration of TOC and COD respectively, extrapolate the concentration of chemical oxygen demand (COD) (COD), accomplish to show organic carbon concentration (TOC) and chemical oxygen demand (COD) (COD) concentration over the display simultaneously;
Embodiment 2 uses UV-detector directly to measure the concentration of total organic carbon in water, accompanying drawing 2, Fig. 3:
Embodiments of the invention 2 utilize the organism contained in sewage that the principle of the absorption of ultraviolet is carried out TOC detection, the absorption of ultraviolet is met Law of Lambert-Beer by the organism contained in sewage, is also exactly that the concentration containing organism in sewage is directly proportional to its absorbancy. the optical density of the ultraviolet light of different wavelength is different by different organism, according to organism to the ultraviolet absorbancy of different wave length, several bigger ultra-violet bands of the absorbancy of each organism can be chosen as detection wave band, owing to the absorbancy of organism and the concentration of organism at each selected wave band place meets Law of Lambert-Beer, so carrying out UV scanning in a certain selected wave band, the numerical value obtained after the numerical integration then absorbancy in scanning wave band carried out is same with the total concn of the organism producing to absorb in this wave band meets Law of Lambert-Beer. according to sewage integrated value to the absorbancy that UV-light produces in certain selected wave band, calculate TOC value.
Water sample to be measured directly enters 5-3 UV-detector and carries out Single wavelength or multi-wavelength scanning, the ultraviolet beam being transmitted through sample pool is carried out light-splitting processing, owing to organism is at UV spectrum district absorption special spectrum, according to relation between characteristic wavelength place absorbancy and TOC content, determine TOC value, in 6. data handlers, calculate organic carbon concentration in sample, organic carbon concentration is stored in database or file, show in 7. indicating meters simultaneously, or by 8. network data transmission devices, it is transferred to remote display.
Organic carbon concentration (TOC) and chemical oxygen demand (COD) (COD) concentration show simultaneously
One is that COD is the oxygen (O consumed theoretically2), representing oxygen-consumption, TOC represents oxygen-consumption, then COD=K*TOC with carbon (C), because C+O2=CO2, so K=32/12=2.67.
Two is the linear regression theory using organic carbon concentration (TOC) and chemical oxygen demand (COD) (COD), according to Y=a+bX, measure the series concentration of TOC and COD respectively, extrapolate the concentration of chemical oxygen demand (COD) (COD), accomplish to show organic carbon concentration (TOC) and chemical oxygen demand (COD) (COD) concentration over the display simultaneously;
2-3. Ultraviolet Oxidation device in figure 3, is mounted in the outside of 2-6, microwave oxidizer, and 2-3. Ultraviolet Oxidation device puts into 2-6, microwave oxidizer inside in the diagram.
Claims (10)
1. seawater, high chlorine high-salt wastewater, the surface water, underground water, tap water, sanitary sewage, the determinator of total organic carbon in trade effluent, it is characterized in that, mainly comprise multi-position valve, combination oxidation reactor, gas-liquid separator, halogen remover, film filter, multichannel detector; Data processing and display unit, can be used for experimental determination, on-line determination, emergent portable field mensuration.
2. device according to claim 1, is characterized in that, described multi-position valve can be 2 logical valves, 3 logical valves, 6 logical valves, 10 logical valves etc.
3. device according to claim 1, it is characterized in that, described combination oxidation reactor can be made with materials such as platinum, quartz, stainless steels, and combination oxidation reactor adopts Ultraviolet Oxidation device, ozone oxidation device, microwave oxidizer, hydrogen peroxide combination mode of oxidizing oxidation Organic substance in water; Wherein, microwave oxidizer can adopt light wave oxidizer, ultrasound oxidation technology device, carbon fiber oxidizer, electrically heated to replace; Use high purity oxygen gas, high pure air, rare gas element, nitrogen as carrier gas.
4. device according to claim 1, it is characterized in that, described combination oxidation reactor, different according to Organic substance in water matter content, it is possible to adopt the one of Ultraviolet Oxidation device, ozone oxidation device, microwave oxidizer, hydrogen peroxide combination mode of oxidizing, two kinds, three kinds, four kinds mode of oxidizing to carry out oxidizing reaction respectively.
5. device according to claim 1, it is characterized in that, described combination oxidation reactor, it is possible to use the assisted oxidation such as titanium dioxide, persulphate, platinum, cupric oxide, hydrogen peroxide or the Fenton class oxygenant that is made up of ferrous iron and hydrogen peroxide, does not produce secondary pollution.
6. device according to claim 1, is characterized in that, when for scene meet an urgent need portable mensuration time, CO2 removal cleaner can be installed before quantitative sampling device.
7. device according to claim 1, is characterized in that, described multichannel detector, it is possible to be 1,2,3,4,5 kind of detector, such as infrared detector (NDIR) and electrical conductivity detector; Wherein, infrared detector (NDIR), electrical conductivity detector can adopt plasma atomic emission spectrometer, laser gas analyzer, hydrogen flameionization method flame ionization ditector, coulomb analyser, ultraviolet spectroscopy and carry out optical signal gathering by photomultiplier and amplify, and the detector (chemoluminescence method detector) converting the analysis process system of electrical signal to replaces.
8. device according to claim 1, is characterized in that, described combination oxidation reactor, and Ultraviolet Oxidation device can be arranged on the outside of microwave oxidizer, and it is inner that Ultraviolet Oxidation device can also put into microwave oxidizer.
9. device according to claim 1, is characterized in that, water sample to be measured according to organism UV spectrum district absorb special spectrum, it is possible to use UV-detector directly measures the concentration of total organic carbon in water.
10. device according to claim 1, it is characterized in that, the device of total organic carbon in described mensuration water, it is possible to for solid matter if soil, solid waste, solid article etc. and gas are after being manipulated so water sample, measures the concentration of total organic carbon (TOC).
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106226131A (en) * | 2016-09-19 | 2016-12-14 | 中国石油大学(华东) | The sampling system of a kind of volatile organic matter in sewage and the method for sampling thereof |
| CN106770201A (en) * | 2016-12-08 | 2017-05-31 | 北京国电龙源环保工程有限公司 | The method that low concentration organic amine in waste water and waste liquid is determined using plasma emission spectrum |
| CN107983123A (en) * | 2017-12-29 | 2018-05-04 | 浙江省海洋水产养殖研究所 | Air filtering dust-removing laboratory |
| CN108414645A (en) * | 2018-04-19 | 2018-08-17 | 南京大学 | A kind of size exclusion chromatograph combination type Nitrogen detector and application process |
| CN109612794A (en) * | 2018-12-06 | 2019-04-12 | 同济大学 | The separation and quantitative approach of different preservation state organic matters in a kind of hydrocarbon source rock |
| CN109946197A (en) * | 2019-03-21 | 2019-06-28 | 重庆地质矿产研究院 | Shale organic carbon determination method |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106226131A (en) * | 2016-09-19 | 2016-12-14 | 中国石油大学(华东) | The sampling system of a kind of volatile organic matter in sewage and the method for sampling thereof |
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| CN106770201A (en) * | 2016-12-08 | 2017-05-31 | 北京国电龙源环保工程有限公司 | The method that low concentration organic amine in waste water and waste liquid is determined using plasma emission spectrum |
| CN107983123A (en) * | 2017-12-29 | 2018-05-04 | 浙江省海洋水产养殖研究所 | Air filtering dust-removing laboratory |
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| CN108414645A (en) * | 2018-04-19 | 2018-08-17 | 南京大学 | A kind of size exclusion chromatograph combination type Nitrogen detector and application process |
| WO2019201086A1 (en) * | 2018-04-19 | 2019-10-24 | 南京大学 | Size exclusion chromatography-combined nitrogen detector and application method |
| CN108414645B (en) * | 2018-04-19 | 2023-05-23 | 南京大学 | Volume exclusion chromatography combined nitrogen detector and application method |
| CN109612794A (en) * | 2018-12-06 | 2019-04-12 | 同济大学 | The separation and quantitative approach of different preservation state organic matters in a kind of hydrocarbon source rock |
| CN109612794B (en) * | 2018-12-06 | 2021-05-11 | 同济大学 | Method for separating and quantifying organic matters in different occurrence states in hydrocarbon source rock |
| CN109946197A (en) * | 2019-03-21 | 2019-06-28 | 重庆地质矿产研究院 | Shale organic carbon determination method |
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Application publication date: 20160615 |