CN202676677U - On-line detection device for spray extraction of volatile organic matters in water - Google Patents

On-line detection device for spray extraction of volatile organic matters in water Download PDF

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Publication number
CN202676677U
CN202676677U CN 201220370676 CN201220370676U CN202676677U CN 202676677 U CN202676677 U CN 202676677U CN 201220370676 CN201220370676 CN 201220370676 CN 201220370676 U CN201220370676 U CN 201220370676U CN 202676677 U CN202676677 U CN 202676677U
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China
Prior art keywords
volatile organic
organic matter
spray
jet chamber
interface
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Withdrawn - After Issue
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CN 201220370676
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Chinese (zh)
Inventor
沈成银
王宏志
刘升
黄超群
江海河
储焰南
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Hefei Institutes of Physical Science of CAS
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Hefei Institutes of Physical Science of CAS
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Abstract

An on-line detection device for spray extraction of volatile organic matters in water comprises a peristaltic pump, a sample inlet capillary, a spray room, a volatile organic matter on-line detection mass spectrum, a constant temperature cavity, a to-be-detected liquid interface, a carrier gas interface, a spray needle, a gas detection opening and a waste liquid guide outlet, wherein the sample inlet capillary, the spray room, the to-be-detected liquid interface and the spray needle are positioned in the constant temperature cavity; the spray room is communicated with the to-be-detected liquid interface, the carrier gas interface, the spray needle, the gas detection opening and the waste liquid guide outlet; the to-be-detected liquid interface is positioned on the left side of the spray room; the spray needle is positioned in the spray room; one end of the spray needle is connected with the to-be-detected liquid interface and the other end of the spray needle is suspended in the spray room; the carrier gas is positioned on the left side above the spray room; the waste liquid guide outlet is positioned on the right side under the spray room; the gas detection opening is positioned on the right side above the spray room; and the sample inlet capillary is connected with the to-be-detected liquid interface. The on-line detection device for spray extraction of the volatile organic matters in water can realize efficient extraction of the volatile organic matters in water and can also realize on-line high-sensitivity detection.

Description

The on-line measuring device that the volatile organic matter spraying is extracted in a kind of water
Technical field
The utility model belongs to the analyzing and testing field, is specifically related to the on-line measuring device that the volatile organic matter spraying is extracted in a kind of water.
Background technology
Volatile organic matter is the large important pollutant of class of one in the water body; have persistence, animal migration; and carcinogenic, teratogenesis, mutagenic characteristic; so online detection of volatile organic matter particularly paid attention at field of environment protection in the water; in addition, in the water volatile organic matter online detect in fields such as the biomedical research such as body fluid metabolic analysis, cell cultivation process analysis and chemical preparations significant equally.
The volatile organic matter extracting method has Solid-Phase Extraction, Solid-phase Microextraction, liquid-liquid extraction, headspace technique (containing Puffing and trapping), film sampling system, dynamic gas extraction method, direct liquid introduction method etc. in the water at present, and the volatile organic matter that is extracted can utilize the organism detection techniques such as chromatogram or chromatogram mass spectrum to detect.Wherein front four kinds of organism extracting method are off-line enrichment sampling method, do not satisfy online detection demand, though rear three kinds can be at the line drawing volatile organic matter, but not only sensitivity is low for the film sampling system, response speed is slow, and memory effect causes cross pollution, the required sample size of dynamic gas extraction method is large, and the direct liquid introduction method purges gasification by the carrier gas of heating to testing liquid, and a large amount of carrier gas that pass into have diluting effect to the target organism.
The utility model content
Technology of the present utility model is dealt with problems: overcome the deficiency that volatile organic matter detects at line drawing in the existing water, the on-line measuring device that the volatile organic matter spraying is extracted in a kind of water is provided, can realize volatile organic matter in a small amount of water sample is carried out high efficiency extraction, and realize online highly sensitive detection.
The utility model technical solution: the on-line measuring device that the volatile organic matter spraying is extracted in a kind of water comprises that peristaltic pump, sample introduction kapillary, jet chamber, volatile organic matter detect mass spectrum, constant temperature chamber, testing liquid interface, carrier gas interface, spray needle, gas detection mouth and waste liquid export mouth online; Described sample introduction kapillary, jet chamber, testing liquid interface and spray needle are positioned at the constant temperature chamber; Mouth detects with testing liquid interface, carrier gas interface, spray needle, gas respectively in described jet chamber and the waste liquid export mouth communicates; The testing liquid interface is positioned at the left side, jet chamber, spray needle is positioned at the jet chamber, spray needle one end links to each other with liquid interface to be measured, the other end is suspended in the jet chamber, the carrier gas interface is positioned at left side, top, jet chamber, the waste liquid export mouth is positioned at right side, below, jet chamber, and gas detects mouth and is positioned at right side, top, jet chamber; Described sample introduction kapillary 2 links to each other with the testing liquid interface; Peristaltic pump links to each other with the sample introduction kapillary, and volatile organic matter detects online mass spectrum and links to each other with gas detection mouth.
Described sample introduction capillary inner diameter can be at 0.1mm ~ 1mm, and length can at 0.1m ~ 5m, can be metal or quartzy material.
Described waste liquid export mouth designs for U-shaped.
Described spray needle internal diameter is 0.01mm ~ 1mm, can be one or more.
Described jet chamber is funnel-form.
It is in room temperature to the 100 ℃ scope that sample introduction kapillary, jet chamber, testing liquid interface and spray needle temperature can be regulated in described constant temperature chamber.
The carrier gas that described carrier gas interface passes into can be drying nitrogen or air, and flow detects online mass spectrum sample introduction flow with volatile organic matter and equates, in 5ml/min ~ 500ml/min scope.
The course of work of the present utility model is as follows: water sample to be measured enters the sample introduction kapillary through peristaltic pump pumps, in the constant temperature chamber, be heated to constant temperature chamber design temperature (room temperature to 100 ℃ scope), pass into afterwards the testing liquid interface, liquid to be measured is sprayed to the jet chamber by the spray needle of hollow, the volatile organic matter that separate out on vaporific drop surface detects mouth by gas and enters volatile organic matter to detect online mass spectrum detected, and waste liquid flows out the jet chamber along the waste liquid export mouth.
The utility model advantage compared with prior art is:
(1) the utility model can be realized volatile organic matter in a small amount of water sample is carried out efficiently at line drawing, thereby realizes online highly sensitive detection.Because the volatile organic matter in the liquid can spread in the gas towards periphery according to concentration gradient, behind the gas-liquid concentration distribution that reaches the Henry's law regulation, then realize concentration mobile equilibrium, fluid temperature raises then can improve the distribution ratio coefficient.According to this principle, the utility model with water sample to be measured heating after by one or how to extract wherein organism with spray needle to jet chamber's spraying, spraying forms endlessly droplet, greatly improve liquid surface area, thereby efficiently organism in line drawing water is realized the mass spectral:mass spectrographic highly sensitive detection of the online detection of volatile organic matter.
(2) the utility model produces droplet by spraying and extracts target substance, compares dynamic gas and carries device, and extraction efficiency is higher, and required sample still less; Compare direct liquid introduction method principle different, the utility model has avoided in the direct liquid introduction method a large amount of carrier gas to separating out organic dilution, and therefore the required sample size of spraying of the present utility model is few, without a large amount of carrier gases dilute sample gas, funnelform jet chamber dead volume is little, has improved response speed.
Description of drawings
Fig. 1 is the on-line measuring device schematic diagram that the volatile organic matter spraying is extracted in a kind of water of the present utility model.
Embodiment
As shown in Figure 1, the on-line measuring device embodiment that the volatile organic matter spraying is extracted in a kind of water of the present utility model comprises: peristaltic pump 1, sample introduction kapillary 2, jet chamber 3, volatile organic matter detect mass spectrum 4, constant temperature chamber 5, testing liquid interface 6, carrier gas interface 7, spray needle 8, gas detection mouth 9 and waste liquid export mouth 10 online; Described sample introduction kapillary 2, jet chamber 3, testing liquid interface 6 and spray needle 8 are positioned at constant temperature chamber 5; Mouth 9 detects with testing liquid interface 6, carrier gas interface 7, spray needle 8, gas in described jet chamber 3 and waste liquid export mouth 10 communicates; Testing liquid interface 6 is positioned at 3 left sides, jet chamber, spray needle 8 is positioned at jet chamber 3, spray needle 8 one ends link to each other with liquid interface 6 to be measured, the other end is suspended on jet chamber 3, carrier gas interface 7 is positioned at left side, 3 tops, jet chamber, waste liquid export mouth 10 is positioned at right side, 3 below, jet chamber, and gas detects mouth 9 and is positioned at right side, 3 top, jet chamber; Sample introduction kapillary 2 links to each other with testing liquid interface 6; Peristaltic pump 1 links to each other with sample introduction kapillary 2, and volatile organic matter detects online mass spectrum 4 and links to each other with gas detection mouth 9; Jet chamber 3 is designed to " funnel " shape according to the shape of spraying diffusion, and " bell mouth " direction is identical with spray direction.
The utility model work is: before detecting water sample to be measured, survey first blank water sample, clean on the one hand inside surface and the waste liquid export mouth 10 of jet chamber 3, obtain on the one hand the background signal that the utility model device detects the blank water sample.When detecting water sample to be measured, water sample to be measured extracts through peristaltic pump 1 and enters sample introduction kapillary 2, in constant temperature chamber 5, be rapidly heated to constant temperature chamber design temperature (normally from room temperature to 100 ℃ scope) in the flow process, pass into afterwards testing liquid interface 6, liquid to be measured forms vaporific at spray needle 8 heads of hollow.According to Henry's law, the volatile organic matter of drop inside can enter in the ambient gas according to specific gas-liquid distribution ratio.Nitrogen or other carrier gas detect Mass Spectrometer Method 4 online according to volatile organic matter gas consumption enters jet chamber 3 by carrier gas injection port 7.The volatile organic matter of separating out is followed carrier gas to be inhaled into volatile organic matter by gas detection mouth 9 and is detected online Mass Spectrometer Method 4, and waste liquid then flows out jet chambers along waste liquid export mouth 10.After water sample detection to be measured is finished, survey blank water sample purging system, blank water sample can be released waste liquid and derive the interior waste liquid of pipe U-shaped pipe simultaneously, reduces the impact on next test sample again.
In order to obtain different heating effects and pressure result, sample introduction kapillary 2 internal diameters can be at 0.1mm~1mm, and length can be at 0.1m ~ 5m, and the kapillary material can be metal or quartz.Because it is bad that the waste liquid interface is processed, volatile organic matter may flow back to the jet chamber testing sample is produced interference, so waste liquid export mouth 10 designs (referring to Fig. 1) for U-shaped.According to the variable concentrations sensing range, spray needle 8 internal diameters are 0.01mm ~ 1mm, can be one or more, and many spray needles can obtain better extraction effect.Because under the high-temperature condition, gas extraction efficient is higher in the water, and under the high temperature, the volatile organic matter that extracts is difficult for being adsorbed in the inside surface of jet chamber 3, is room temperature to 100 ℃ scope so constant temperature chamber 5 can be regulated sample introduction kapillary 2, jet chamber 3, testing liquid interface 6 and spray needle 8 temperature according to actual needs.In order to reduce dead volume, improve response speed, jet chamber 3 is designed to funnel-form according to spray shapes.The carrier gas that the carrier gas interface passes into can be drying nitrogen or air, and flow detects online mass spectrum sample introduction flow with volatile organic matter and equates, in 5ml/min ~ 500ml/min scope, avoids large flow carrier gas to the dilution of gas to be measured, improves and detects effect.

Claims (7)

1. the on-line measuring device that the volatile organic matter spraying is extracted in the water is characterized in that comprising: peristaltic pump (1), sample introduction kapillary (2), jet chamber (3), volatile organic matter detect online mass spectrum (4), constant temperature chamber (5), testing liquid interface (6), carrier gas interface (7), spray needle (8), gas and detect mouthful (9) and a waste liquid export mouth (10); Described sample introduction kapillary (2), jet chamber (3), testing liquid interface (6) and spray needle (8) are positioned at constant temperature chamber (5); Mouthful (9) are detected with testing liquid interface (6), carrier gas interface (7), spray needle (8), gas respectively by described jet chamber (3) and waste liquid export mouth (10) communicates; Testing liquid interface (6) is positioned at left side, jet chamber (3), spray needle (8) is positioned at jet chamber (3), spray needle (8) one ends link to each other with liquid interface to be measured (6), the other end is suspended in the jet chamber (3), carrier gas interface (7) is positioned at left side, top, jet chamber (3), waste liquid export mouth (10) is positioned at right side, below, jet chamber (3), and gas detects mouthful (9) and is positioned at right side, top, jet chamber (3); Described sample introduction kapillary (2) links to each other with testing liquid interface (6); Peristaltic pump (1) links to each other with sample introduction kapillary (2), and volatile organic matter detects online mass spectrum (4) and links to each other with gas detection mouthful (9).
2. the on-line measuring device that the volatile organic matter spraying is extracted in the water according to claim 1, it is characterized in that: described sample introduction kapillary (2) internal diameter is 0.1mm ~ 1mm, length is 0.1m ~ 5m, and the material of sample introduction kapillary (2) is metal or quartzy material.
3. the on-line measuring device that the volatile organic matter spraying is extracted in a kind of water according to claim 1, it is characterized in that: described waste liquid export mouth (10) is U-shaped.
4. the on-line measuring device that the volatile organic matter spraying is extracted in a kind of water according to claim 1 is characterized in that: described spray needle (8) is one or more formation, and every internal diameter is 0.01mm ~ 1mm.
5. the on-line measuring device that the volatile organic matter spraying is extracted in a kind of water according to claim 1 is characterized in that: described jet chamber (3) are funnel-form.
6. the on-line measuring device that volatile organic matter spraying is extracted in a kind of water according to claim 1 is characterized in that: the temperature range in described constant temperature chamber (5) is from room temperature to 100 ℃.
7. the on-line measuring device that the volatile organic matter spraying is extracted in a kind of water according to claim 1, it is characterized in that: the carrier gas that described carrier gas interface (7) passes into is drying nitrogen or air, flow detects online mass spectrum (4) sample introduction flow with volatile organic matter and equates, scope is 5ml/min ~ 500ml/min.
CN 201220370676 2012-07-27 2012-07-27 On-line detection device for spray extraction of volatile organic matters in water Withdrawn - After Issue CN202676677U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102788855A (en) * 2012-07-27 2012-11-21 中国科学院合肥物质科学研究院 On-line detection device and detection method for atomizing extraction for volatile organic matters in water
CN104330481A (en) * 2014-10-17 2015-02-04 上海应用技术学院 Device and method for measuring organic matters entrained in water phase in solvent extraction process

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102788855A (en) * 2012-07-27 2012-11-21 中国科学院合肥物质科学研究院 On-line detection device and detection method for atomizing extraction for volatile organic matters in water
CN102788855B (en) * 2012-07-27 2014-08-06 中国科学院合肥物质科学研究院 On-line detection device and detection method for atomizing extraction for volatile organic matters in water
CN104330481A (en) * 2014-10-17 2015-02-04 上海应用技术学院 Device and method for measuring organic matters entrained in water phase in solvent extraction process

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