CN205388568U - Organic pollutant's of survey aquatic device - Google Patents
Organic pollutant's of survey aquatic device Download PDFInfo
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- CN205388568U CN205388568U CN201520962506.0U CN201520962506U CN205388568U CN 205388568 U CN205388568 U CN 205388568U CN 201520962506 U CN201520962506 U CN 201520962506U CN 205388568 U CN205388568 U CN 205388568U
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Abstract
The utility model belongs to the technical field of chemical analysis detects, a organic pollutant's of survey aquatic device is disclosed. The device is including filter, water pump, water sample enrichment enrichment facility, a spectrophotometer and computer, filter and water pump are through a water piping connection, water sample enrichment enrichment facility passes through the peristaltic pump and the second water pipe is connected with the filter, acquires and filters good water sample, the water sample of water sample enrichment enrichment facility after with the enrichment concentration is carried to a spectrophotometer through advancing the appearance pipe, the computer is connected with a spectrophotometer, and obtain spectral data and carry out a series of preliminary treatment with spectral data, then substitution mathematic model model to obtain the testing result. Installing functional unit such as set water sampling, filtration, concentration, on -line measuring and data processing, adopting the control of the computer automation overall situation, realized organic pollutant on -line measuring's function, the that more outstanding is the organic pollutant while on -line measuring that can realize more than 15 kinds.
Description
Technical field
This utility model belongs to the technical field of chemical analysis detection, more particularly, to the device of a kind of organic pollution measured in water.
Background technology
Toxic organic pollutant is primarily referred to as the organic pollution materials with bio-toxicity, biological and the mankind are not only had obvious toxicity by them, causing acute and chronic poisoning, some noxious substance can also cause cancer, monster and cytogenetics gene mutation, i.e. " three cause " effect.In recent years, high speed development along with modern chemical industry, create a lot of toxic organic pollutant, these pollutant can pass through rainwash, precipitation etc. and enter water body, and the Drinking Water source of south most area is surface water, once the water source being not affected by effective monitoring enters water system, the health of drinking water crowd will be brought great harm, it is therefore necessary to the toxic organic pollutant in water body is carried out on-line monitoring.
Traditional assay method of toxic organic pollutant mainly has gas chromatography, combined gas chromatography mass spectrometry and liquid chromatography etc..These analysis methods need to keep instrument to have carrier gas or mobile phase to pass through in analysis process always, and environmental requirement is harsh, and sample analysis time is longer, is not appropriate for for field monitoring and on-line monitoring.It addition, these methods are difficult to carry out the detection of multiple different physicochemical properties component simultaneously, precision and the accuracy of testing result are very poor.
Summary of the invention
The technical problems to be solved in the utility model is in that to overcome the defect of prior art, the device of a kind of organic pollution measured in water is provided, Some Organic Pollutants in described device energy on-line checking water sample, it is achieved sample extraction, filtration, concentration and detection integration and the completing of automatization.
This utility model is achieved through the following technical solutions:
The device of a kind of organic pollution measured in water, including filter, water pump, water sample enrichment enrichment facility, the first spectrophotometer and computer；Described filter and water pump are connected by the first water pipe, filter on-line filtration water sample；Described water sample enrichment enrichment facility is connected with filter by peristaltic pump and the second water pipe, obtains the water sample filtered；Water sample after enrichment concentration is delivered to the first spectrophotometer by sample feeding pipe by described water sample enrichment enrichment facility；Described computer and the first spectrophotometer connect, and obtain spectroscopic data and are acted upon obtaining testing result.
The functional parts such as this utility model set water sampling, filtration, concentration, on-line checking and data process, adopt the computer automation overall situation to control, it is achieved that the function of organic pollution on-line checking.
Further, described filter is cross-flow filter or dead-end filter.In order to realize the effect keeping filtering for a long time, it is prevented that foreign material blocking filter in water, it is preferable that described filter is selected from cross-flow filter.The aperture of described filter is 0.8um～1.5um.Described filter is provided with filter membrane.
In order to accurately carry out detection by quantitative, further, the device of the organic pollution in described mensuration water is additionally provided with water sample quantifier, and described water sample quantifier connects filter, and the water sample after metering leads to water sample enrichment enrichment facility.Preferably, described water sample quantifier is volume gauger, mass metrology device or online flow gauge etc..
In order to detect the organic pollution of trace in water, further, described water sample enrichment enrichment facility is solid-phase extraction device or liquid liquid extraction plant.Preferably, described water sample enrichment enrichment facility is solid-phase extraction device.
Further, described water sample enrichment enrichment facility includes reagent bottle, dosing pump, solid-phase extraction column, Nitrogen evaporator, concentration tube.
In order to realize detecting other indexs needing not move through concentration, such as COD, TOC, NO3 -Deng, further, the device of the organic pollution in described mensuration water is additionally provided with the second spectrophotometer, and described second spectrophotometer is connected with filter and computer.Water sample through filtering is sent into the second spectrophotometer and is detected, and the spectral information obtained is sent in computer and carried out data process.
Further, described first, second spectrophotometer is respectively selected from ultraviolet-uisible spectrophotometer, ultraviolet spectrophotometer, visible spectrophotometer, infrared spectrophotometer, atomic absorption spectrophotometer.Preferably, described spectrophotometric is calculated as ultraviolet-uisible spectrophotometer.
Further, between described water sample enrichment enrichment facility and the first spectrophotometer, between filter and the second spectrophotometer, it is provided with froth breaker.
Further, the device of the organic pollution in described mensuration water is additionally provided with the rinser of the pipelines such as water pipe, filter, the water sample enrichment device such as enrichment facility, spectrophotometer.
Further, described rinser includes reagent bottle, the second dosing pump, cleans pipeline, three-way valve.Described second dosing pump, three-way valve are connected with computer, control consumption and the ratio of various reagent, described cleaning pipeline connects reagent bottle, the second dosing pump and three-way valve, and described three-way valve will clean pipeline and be connected with described second water pipe, be passed into by reagent in described second water pipe.
Preferably, described three-way valve is selected from Pneumatic three-way valve, electric T-shaped valve or hydraulic dynamic three-way valve.
In order to overcome the temperature impact on testing result of ambient temperature, detection water sample, further, described device is additionally provided with climatic chamber, and described climatic chamber is connected with computer；Described water sample enrichment enrichment facility, water sample quantifier, the first spectrophotometer, the second spectrophotometer and computer installation are in described climatic chamber.
Further, described device is additionally provided with the temperature sensor of detection TWS, and described temperature sensor is connected with computer；Described temperature sensor is arranged at the first spectrophotometer and/or the second spectrophotometer.
The method adopting the organic pollution measured in water of said apparatus, comprises the following steps:
S1., after water sample is filtered, passes into water sample enrichment enrichment facility and concentrate, obtain test solution to be measured；
S2. adopt the first spectrophotometer that test solution to be measured in S1 is measured, obtain sample spectrum diagram；
S3. the sample spectrum diagram in S2 is carried out Pretreated spectra by computer, selected characteristic wave band, and by the computing of mathematical model, carry out Data correction in conjunction with the temperature of climatic chamber and/or the accumulative access times of the temperature of temperature sensor, water sample enrichment enrichment facility, obtain the content of toxic organic pollutant；
Described toxic organic pollutant be G-30027, carbaryl, parathion, 2,4-chlorophenesic acid, 2,4,6-trichlorophenol, 2,4,6,-T, Pentachorophenol, phenol, phthalic acid (2-ethylhexyl) ester, dibutyl phthalate, benzene, toluene, ethylbenzene, meta-xylene, naphthalene, aniline.
Preferably, in described S1, water sample enrichment concentration adopts automatic solid-phase extractor, detailed process is as follows: successively with dichloromethane, ethyl acetate, methanol and ultra-pure water activated solid extraction column, water sampling is by solid-phase extraction column, to be enriched with the dry solid-phase extraction column of final vacuum nitrogen blowing apparatus, afterwards with ethyl acetate and eluent methylene chloride solid-phase extraction column, eluent is collected in concentration tube, finally closely dry with Nitrogen evaporator concentrate eluant, add acetonitrile solution, obtain test solution to be measured.
Preferably, Pretreated spectra described in S3 includes spectrogram carries out Noise Elimination from Wavelet Transform, first derivative process, multiplicative scatter correction, standard normal conversion, average centralization process.
Preferably, characteristic wave bands described in S3 is 200nm～800nm.
Preferably, described mathematical model is set up by following steps:
S31. choosing at least 2 water samples of different dry point, each water sample obtains ground control concentrated solution and sample concentration liquid through the process of described S1；
S32. the random reference material adding all described toxic organic pollutants in sample concentration liquid, obtains mark-on sample to be measured, and in described mark-on sample to be measured, the concentration range of toxic organic pollutant is 0.20 μ g/L～700 μ g/L；Background concentrated solution adds the acetonitrile solution of the reference material equivalent with toxic organic pollutant and obtains Background Samples to be measured；
S33. the method according to described S2, adopts the first spectrophotometer centering Background Samples to be measured and mark-on sample to be measured to be measured, obtains sample spectrum diagram；With acetonitrile solution for reference liquid；
S34. according to the Pretreated spectra in described S3, sample spectrum diagram being processed, selected characteristic wave band, in mark-on sample to be measured, the concentration of each toxic organic pollutant is for Y (y1、y2、y3、…、y15) variable, with characteristic wave bands for X (x1、x2、x3、…、xn) variable, adopt partial least-squares regressive analysis, multiple linear regression analysis, support vector machine or artificial neural network analysis to carry out data fitting, obtain described mathematical model.
Preferably, the ethane nitrile content of described acetonitrile solution is the aqueous solution of 85%.
Compared with prior art, this utility model has the advantages that
The functional parts such as the apparatus and method set water sampling of the organic pollution in mensuration water described in the utility model, filtration, concentration, on-line checking and data process, the computer automation overall situation is adopted to control, achieving the function of organic pollution on-line checking, described device is effectively improved sensitivity and the accuracy of detection by physical means such as filtration, concentration, froth breakings.The on-line checking while that more prominent being the organic pollution that can realize more than 15 kinds.
Accompanying drawing explanation
Fig. 1 is the block diagram of the device of the organic pollution measured in water of embodiment 1；
Fig. 2 is the block diagram of the device of the organic pollution measured in water of embodiment 2.
Detailed description of the invention
This utility model is further illustrated below in conjunction with specific embodiment.Unless stated otherwise, the raw material that adopts in this utility model embodiment, equipment and method are the conventional commercial raw material in this area, conventional use of equipment and method.
Embodiment 1
The device of a kind of organic pollution measured in water, including filter 1, water pump 2, water sample enrichment enrichment facility the 3, first spectrophotometer 4 and computer 5；Filter 1 and water pump 2 are connected by the first water pipe 6, filter 1 on-line filtration water sample；Water sample enrichment enrichment facility 3 is connected with filter 1 by peristaltic pump 7 and the second water pipe 8, obtains the water sample filtered；Water sample after enrichment concentration is delivered to the first spectrophotometer 4 by sample feeding pipe 9 by water sample enrichment enrichment facility 3；Computer 5 is connected with the first spectrophotometer 4, obtains spectroscopic data and to process acquisition testing result.
Filter 1 is cross-flow filter.The aperture of filter is 0.8um.Filter 1 is provided with glass fiber filter.
The device of the organic pollution measured in water of the present embodiment is additionally provided with water sample quantifier 10.Water sample quantifier 10 connects filter 1, and the water sample after metering leads to water sample enrichment enrichment facility 3.Water sample quantifier 10 is online flow gauge.
Water sample enrichment enrichment facility 3 is solid-phase extraction device.Water sample enrichment enrichment facility 3 includes reagent bottle, dosing pump, solid-phase extraction column, Nitrogen evaporator, concentration tube.
First spectrophotometer 4 is ultraviolet-uisible spectrophotometer.
It is provided with froth breaker 11 between water sample enrichment enrichment facility 3 and the first spectrophotometer 4.
The present embodiment is additionally provided with the rinser 12 of the devices such as the pipelines such as water pipe, filter 1, water sample enrichment enrichment facility 3, spectrophotometer.
Rinser 12 includes reagent bottle the 121, second dosing pump 122, cleans pipeline 123, three-way valve 124.Second dosing pump 122, three-way valve 124 are connected with computer 5, control consumption and the ratio of various reagent.Clean pipeline 123 and connect reagent bottle the 121, second dosing pump 122 and three-way valve 124.Cleaning pipeline 123 is connected by three-way valve 124 with the second water pipe 8, is passed into by reagent in described second water pipe 8.
The present embodiment is additionally provided with the temperature sensor of detection TWS.Temperature sensor is arranged in the first spectrophotometer, and is connected with computer.
A kind of method of organic pollution measured in water adopting said apparatus, comprises the following steps:
S1. water sample is after filter 1 filters, and passes into water sample enrichment enrichment facility 3 and concentrates, obtains test solution to be measured；
S2. adopt the first spectrophotometer 4 that test solution to be measured in S1 is measured, obtain sample spectrum diagram；
S3. the sample spectrum diagram in S2 is carried out Pretreated spectra, selected characteristic wave band by computer 5, and by the computing of mathematical model, obtains the content of toxic organic pollutant；
In the present embodiment toxic organic pollutant be G-30027, carbaryl, parathion, 2,4-chlorophenesic acid, 2,4,6-trichlorophenol, 2,4,6,-T, Pentachorophenol, phenol, phthalic acid (2-ethylhexyl) ester, dibutyl phthalate, benzene, toluene, ethylbenzene, meta-xylene, naphthalene, aniline.
Specifically, in S1, water sampling is after filtering, water sample enrichment concentration adopts automatic solid-phase extractor, detailed process is as follows: use 5mL dichloromethane successively, 5mL ethyl acetate, 10mL methanol and 10mL ultra-pure water activation HLB solid-phase extraction column, take 1000mL water sample and pass through solid-phase extraction column with 10mL min-1 flow velocity, it is enriched with the dry solid-phase extraction column 50min of final vacuum nitrogen blowing apparatus, afterwards with 3ml ethyl acetate and 3mL eluent methylene chloride solid-phase extraction column, eluent is collected in concentration tube, last at 35 DEG C, closely dry with Nitrogen evaporator concentrate eluant, add the aqueous solution containing 85% acetonitrile of 10mL, obtain test solution to be measured.
Pretreated spectra described in S3 includes that spectrogram carries out Noise Elimination from Wavelet Transform, first derivative processes, average centralization processes.
Characteristic wave bands described in S3 is 200nm～400nm.
In S3, mathematical model is set up by following steps:
S31. choosing at least 2 water samples of different dry point, each water sample obtains ground control concentrated solution and sample concentration liquid through the process of described S1；
S32. the random reference material adding all (15 kinds) described toxic organic pollutants in sample concentration liquid, obtains mark-on sample to be measured, and in described mark-on sample to be measured, the concentration range of toxic organic pollutant is 0.20 μ g/L～700 μ g/L；Background concentrated solution adds the acetonitrile solution of the reference material equivalent with toxic organic pollutant and obtains Background Samples to be measured；
S33. the method according to described S2, adopts the first spectrophotometer centering Background Samples to be measured and mark-on sample to be measured to be measured, obtains sample spectrum diagram；With acetonitrile solution for reference liquid；
S34. according to the Pretreated spectra in described S3, sample spectrum diagram being processed, selected characteristic wave band, in mark-on sample to be measured, the concentration of each toxic organic pollutant is for Y (y1、y2、y3、…、y15) variable, with characteristic wave bands for X (x1、x2、x3、…、xn) variable, adopt partial least-squares regressive analysis, multiple linear regression analysis, support vector machine or artificial neural network analysis to carry out data fitting, obtain described mathematical model.
Specifically, S31. 2L water sample is respectively taken in 12 tidal level points, totally 12 water samples, each water sample is after the solid-phase extraction device enrichment concentration through water sample enrichment enrichment facility of described S1 is 20mL, being divided into 8 samples that 2.5mL is unit, wherein each tidal level point respectively takes 1 for ground control, totally 12 ground control concentrated solutions, other 7 water samples are used for sample mark-on, totally 84 sample concentration liquid.
S32. 15 kinds of toxic organic pollutants of random addition in 84 water samples, obtain mark-on sample to be measured.The concentration change scope of these organic pollutions is in Table 1.
The organic pollution concentration change scope added in table 1 sample concentration liquid
| Object | Minima (μ g/L) | Maximum (μ g/L) |
| G-30027 | 0.22 | 8.04 |
| Carbaryl | 0.30 | 38.0 |
| Parathion | 0.35 | 9.08 |
| 2,4 dichloro phenol | 0.33 | 91.1 |
| 2,4,6-trichlorophenol, 2,4,6,-T | 0.33 | 155 |
| Pentachorophenol | 0.40 | 9.75 |
| Phenol | 0.30 | 10.2 |
| Phthalic acid (2-ethylhexyl) ester | 0.35 | 34.7 |
| Dibutyl phthalate | 0.31 | 28.8 |
| Benzene | 0.81 | 191 |
| Toluene | 0.91 | 700 |
| Ethylbenzene | 0.39 | 300 |
| Meta-xylene | 0.68 | 500 |
| Naphthalene | 0.31 | 200 |
| Aniline | 0.30 | 100 |
S33. the method according to described S2, adopts the first spectrophotometer centering Background Samples to be measured and mark-on sample to be measured to be measured, there are 96 sample spectrum diagrams；With the ethane nitrile content of acetonitrile solution be 85% aqueous solution for reference liquid.
Water sample background value measures
Volatile organic matter (benzene, toluene, ethylbenzene, meta-xylene and naphthalene): with the GC-MS detection being equipped with HP-5MS chromatographic column (30m × 250mm × 0.25 μm), He is carrier gas, and constant flow rate is 1.3mL min-1, linear velocity 42cm sec-1；Injection port 180 DEG C, ion source (EI source) temperature 230 DEG C, electron energy: 70eV；Temperature programming under SIM pattern: initial temperature 35 DEG C retains 1min, 4 DEG C of min-1Rise to 100 DEG C, then rise to 230 DEG C with 30 DEG C of min-1, retain 5min, Splitless injecting-Sample 1 μ L.
Semi-volatile organic matter (other organic pollution): with the GC-MS detection being equipped with DB-624 chromatographic column (30m × 250mm × 0.25 μm), He is carrier gas, and constant flow rate is 1.3mL min-1, linear velocity 42cm sec-1；Injection port 300 DEG C, ion source (EI source) temperature 300 DEG C, electron energy: 70eV；Temperature programming under SIM pattern: initial temperature 60 DEG C retains 1min, 15 DEG C of min-1Rise to 110 DEG C and retain 1min, 20 DEG C of min-1Rise to 180 DEG C, 2 DEG C of min-1Rise to 203 DEG C, 5 DEG C of min-1Rise to 250 DEG C, 2 DEG C of min-1Rise to 310 DEG C and retain 2min, Splitless injecting-Sample 1 μ L.
Show through GC-MS testing result: the water sample of 12 tidal level points is all not detected by described 15 kinds of toxic organic pollutants.
Embodiment 2
The present embodiment is similar to embodiment 1, is different in that:
In order to realize detecting other indexs needing not move through concentration, such as COD, TOC, NO3 -Deng, the device of the organic pollution measured in water of the present embodiment is additionally provided with the second spectrophotometer 13, and the second spectrophotometer 13 is connected with filter 1 and computer 5.Water sample through filtering is sent into the second spectrophotometer 13 and is detected, and the spectral information obtained is sent in computer 5 and carried out data process, obtains required desired value.
Second spectrophotometer 13 is ultraviolet-uisible spectrophotometer.It is provided with froth breaker 11 between filter 1 and the second spectrophotometer 13.
The device of the present embodiment is additionally provided with climatic chamber, and is connected with computer；Water sample enrichment enrichment facility, water sample quantifier, the first spectrophotometer, the second spectrophotometer and computer installation are in described climatic chamber, and are connected with computer.
Claims (11)
1. the device of the organic pollution measured in water, it is characterised in that include water pipe, filter, water pump, water sample enrichment enrichment facility, the first spectrophotometer and computer；Described filter and water pump are connected by the first water pipe, filter on-line filtration water sample；Described water sample enrichment enrichment facility is connected with filter by peristaltic pump and the second water pipe, obtains the water sample filtered；Water sample after enrichment concentration is delivered to the first spectrophotometer by sample feeding pipe by described water sample enrichment enrichment facility；Described computer and the first spectrophotometer connect, and obtain spectroscopic data and are acted upon obtaining testing result.
2. measure the device of organic pollution in water according to claim 1, it is characterised in that described filter is cross-flow filter or dead-end filter.
3. measure the device of organic pollution in water according to claim 1, it is characterised in that being additionally provided with water sample quantifier, described water sample quantifier connects filter, and the water sample after metering leads to water sample enrichment enrichment facility.
4. measure the device of organic pollution in water according to claim 3, it is characterised in that being additionally provided with the second spectrophotometer, described second spectrophotometer is connected with filter and computer.
5. measure the device of organic pollution in water according to claim 4, it is characterised in that described device is additionally provided with climatic chamber, and described climatic chamber is connected with computer；Described water sample enrichment enrichment facility, water sample quantifier, the first spectrophotometer, the second spectrophotometer and computer installation are in described climatic chamber.
6. the device of the organic pollution in mensuration water according to claim 4 ~ 5 any one, it is characterised in that described device is additionally provided with the temperature sensor of detection TWS, and described temperature sensor is connected with computer；Described temperature sensor is arranged at the first spectrophotometer and/or the second spectrophotometer.
7. measure the device of organic pollution in water according to claim 6, it is characterized in that, described first, second spectrophotometer is respectively selected from ultraviolet-uisible spectrophotometer, ultraviolet spectrophotometer, visible spectrophotometer, infrared spectrophotometer, atomic absorption spectrophotometer.
8. measure the device of organic pollution in water according to claim 1, it is characterised in that described water sample enrichment enrichment facility includes reagent bottle, dosing pump, solid-phase extraction column, Nitrogen evaporator, concentration tube.
9. measure the device of organic pollution in water according to claim 6, it is characterised in that between described water sample enrichment enrichment facility and the first spectrophotometer, between filter and the second spectrophotometer, be provided with froth breaker.
10. measure the device of organic pollution in water according to claim 1, it is characterised in that be additionally provided with water pipe, filter, water sample enrichment enrichment facility, spectrophotometric rinser.
11. the device of the organic pollution measured according to claim 10 in water, it is characterised in that described rinser includes reagent bottle, the second dosing pump, cleans pipeline, three-way valve；Described second dosing pump, three-way valve are connected with computer, control consumption and the ratio of various reagent, described cleaning pipeline connects reagent bottle, the second dosing pump and three-way valve, and described three-way valve will clean pipeline and be connected with described second water pipe, be passed into by reagent in described second water pipe.
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| CN201520962506.0U CN205388568U (en) | 2015-11-27 | 2015-11-27 | Organic pollutant's of survey aquatic device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105334173A (en) * | 2015-11-27 | 2016-02-17 | 珠江流域水环境监测中心 | Device and method for determining organic pollutants in water |
| WO2018068185A1 (en) * | 2016-10-10 | 2018-04-19 | 深圳市比特原子科技有限公司 | Water quality detection device and detection method therefor |
| CN109298156A (en) * | 2018-11-27 | 2019-02-01 | 昆山三泽仪器有限公司 | A kind of quality of river water multi-parameter on-line monitoring circulation device |
-
2015
- 2015-11-27 CN CN201520962506.0U patent/CN205388568U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105334173A (en) * | 2015-11-27 | 2016-02-17 | 珠江流域水环境监测中心 | Device and method for determining organic pollutants in water |
| CN105334173B (en) * | 2015-11-27 | 2018-02-09 | 珠江流域水环境监测中心 | A kind of apparatus and method of organic pollution in measure water |
| WO2018068185A1 (en) * | 2016-10-10 | 2018-04-19 | 深圳市比特原子科技有限公司 | Water quality detection device and detection method therefor |
| CN109298156A (en) * | 2018-11-27 | 2019-02-01 | 昆山三泽仪器有限公司 | A kind of quality of river water multi-parameter on-line monitoring circulation device |
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