CN101266208A - Material for near infrared spectra rapid detection for low concentration gaseous organic pollutant - Google Patents
Material for near infrared spectra rapid detection for low concentration gaseous organic pollutant Download PDFInfo
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- CN101266208A CN101266208A CN 200710034531 CN200710034531A CN101266208A CN 101266208 A CN101266208 A CN 101266208A CN 200710034531 CN200710034531 CN 200710034531 CN 200710034531 A CN200710034531 A CN 200710034531A CN 101266208 A CN101266208 A CN 101266208A
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Abstract
The invention discloses a material for quickly detecting gaseous organic pollutant at low concentration using near infrared light, comprising at least two porous material, wherein the first material at least comprises one of the carbon containing compound and silica gel; and the second material at least comprises one of the metal oxide, metal hydrooxide, metal halide, metal sulfide, metal sulphate, metal carbonate, metal phosphate, metal borate, metal silicate and the blending ratio (mass%) of the material is: 30-80 of first material, 20-70 of second material. The invention has double function of high efficiency enriching the gaseous organic matter and diffusely reflecting and disposably and accurately obtains the concentration of all the pollutant by matching the near infra-red spectrometer or portable near infra-red spectrometer.
Description
Technical field
The invention belongs to the auxiliary material of chemical substance quantitative test instrument, be specifically related to a kind of material that is used near infrared spectra rapid detection for low concentration gaseous organic pollutant.
Background technology
Retain in factory, workshop even office, the airborne organic contaminant of family (as benzene, dimethylbenzene, formaldehyde etc.) healthhazard has been well-known.Therefore, exploitation is a kind of can really accomplish quick, online, easy, nearly all organic contaminant and can have social effect and economic worth widely undoubtedly by portable mobile instrument in the quantitative test gas simultaneously.
Have a lot of technology and equipments can both detect the gaseous organic substance of low concentration at present, commonly used have chemical analysis, chromatogram, ultraviolet-visible spectrum, a mid and far infrared spectrum etc.But they respectively have its deficiency.Chemical method operation is loaded down with trivial details, consuming time, can't real time on-line monitoring; A lot of organism there is no absorption on ultraviolet-visible spectrum; Though most organism all have mid and far infrared spectrum, conditional request height to external world when spectrum is collected, instrument need cooled with liquid nitrogen and heaviness, it is portable mobile to be unsuitable for; Comparatively speaking, chromatograph is effective organism analytical approach, but also heavy, valency is high, analysiss is consuming time, the need professional, and can't carry out on-line real time monitoring truly.
The requirement that the near infrared technology basic symbols of development in recent years is closed and stated.Except that methane, phenixin etc. a few, most organism are absorption near infrared ray all, and this has established versatility for near-infrared analysis; Different with mid and far infrared, need not liquid nitrogen during near-infrared analysis and instrument is light, can satisfy portable mobile condition fully; Near infrared spectrogram acquisition time short (generally being less than 3 minutes), by computer technology efficiently in the present age, just can analysis spectrogram in a few minutes, and disposablely provide all organic quantitative concentrations in the gas to be checked; Instrumentation is simple, need not the professional; At last, the nir instrument price also is lower than chromatogram and mid and far infrared instrument, and is suitable with ultraviolet-visible spectrometer.
Certainly, near infrared also has its deficiency.The one, different organic near-infrared spectras overlap, and no characteristic absorption peak need be handled the concentration that can draw separately with Chemical Measurement; The 2nd, organism is generally not high in the absorbance of near-infrared band, can't directly detect the gaseous organic substance of low concentration (10000-10ppm).The latter causes current near infrared technology only to be applied to liquid state, solid just and is not used for the main cause of gaseous organic substance.Therefore, synthetic a kind of can enrichment gaseous state light concentration organic pollutant, efficient diffuse reflection near infrared ray again, and the Material Used that can repeat to regenerate just becomes the key of near infrared detection gaseous state light concentration organic pollutant.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of material that is used near infrared spectra rapid detection for low concentration gaseous organic pollutant is provided.With this material and emission with accept the supporting use of near infrared quantitative test instrument, can obtain the testing result of low concentration gaseous organic pollutant easily and fast, exactly.
The present invention seeks to be achieved through the following technical solutions:
The material that is used near infrared spectra rapid detection for low concentration gaseous organic pollutant is made up of two kinds of porous masses at least, and wherein first kind of material is at least a kind of in carbon compound, the silica gel; Second kind of material is at least a kind of in metal oxide, metal hydroxides, metal halide, metal sulfide, metal sulfate, metal carbonate, metal phosphate, metal borate, the metal silicate.
The proportioning of described material (quality %) is: first kind of material 30-80, second kind of material 20-70.
Described carbon compound has activated charcoal, activated charcoal carbon fiber, fullerene, graphite, carbon black preferably.
Described metal (element) has magnesium, calcium, barium, titanium, zirconium, molybdenum, tungsten, zinc, cadmium, aluminium, tin, lead, antimony, bismuth preferably.
Described material specific surface area is more than or equal to 10 meters squared per gram.
Material of the present invention can adopt conventional synthetic method preparation, as hydro-thermal method, coprecipitation, sol-gel process or solid-phase synthesis commonly used.
The detection principle of material of the present invention: material of the present invention has efficiently concentrating gaseous organic substance, the efficient near infrared dual-use function of diffuse reflection.First during detection with the organic contaminant in the material enrichment of the present invention gas to be measured, this material is placed the luminotron front end of near infrared spectrometer, near infrared ray with the near infrared spectrometer emission shines this material, because this material has the characteristic near infrared ray reflective, the near infrared spectrum that has comprised organic contaminant information by diffuse reflection in spectrometer, and be recorded, microcomputer through investing spectrometer carries out the Chemical Measurement processing again, just can quick disposable each pollutant content data separately that obtains.
Material of the present invention can be repeatedly used after regeneration.Renovation process can be with 100-300 degree centigrade heated dry air (heated dry air is produced by common electric heater unit), to remove last time by the organism of enrichment; Another kind of renovation process is after described material is washed with dippings such as phenixin or carbon disulphide, to regenerate through heated dry air again.
Because material of the present invention has efficiently concentrating gaseous organic substance, the efficient near infrared dual-use function of diffuse reflection, with it and near infrared spectrometer or the supporting use of portable near infrared spectrometer, can the disposable concentration that obtains nearly all pollutant quickly and accurately.This material has enlarged the usable range of infrared spectrometer, has broken through present infrared technique and can only be applied to liquid state, solid and can not be used for the limitation that gaseous organic pollutant detects.And material of the present invention can repeatedly reuse behind simple fast rapid regeneration.Carry out gaseous organic pollutant with material of the present invention and detect, method is easy, the detection efficiency height, and the result is accurate, can detect online (generally being less than 10 minutes) fast the gaseous organic pollutant of nearly all low concentration (sensing range 10000-10ppm).The development of material of the present invention provides a kind of online, quick, easy, general, inexpensive, light movably means for monitoring factory, workshop, office, family's airborne nearly all light concentration organic pollutant (as benzene, dimethylbenzene, formaldehyde etc.).
Embodiment
Embodiment 1
The HCl that gets 245ml4mol/l adds 300ml water, and other gets 10g eight water basic zirconium chlorides and dissolves in the above-mentioned HCl solution.Get 50g water glass (sodium oxide molybdena 8.7%, monox 27.0%) again and add 1000ml water.Under high degree of agitation, water glass is added in the hydrochloric acid, stop to stir after the beginning gelling.Soaked 2 hours with 1mol/lHCl, the 1mol/lHCl liquid that more renews repeats 3 times.Wash gel with water, until no chlorion.Drying is 4 hours under 150 degree, and roasting is 2 hours under 550 degree.Comprise the about 13g of silica gel, the about 3.5g of zirconium dioxide in the product, specific surface area is 50 meters squared per gram.Downcut thickness and be right cylinder about 5mm as gauge material and near infrared spectrometer or the supporting use of portable near infrared spectrometer.
The gained material is placed the luminotron front end of near infrared spectrometer, near infrared ray with the near infrared spectrometer emission shines this material, measures 20 air samples that all contain benzene (concentration range is 12.4-120.5ppm), o-xylene (concentration range is 23.0-87.8ppm), three kinds of pollutants of formaldehyde (concentration range is 11.3-213.7ppm).Carry out Chemical Measurement by the microcomputer that invests spectrometer and handle, its result's maximum relative error is respectively: benzene is 3.32%, and o-xylene is 2.87%, and formaldehyde is 4.55%.
The gained material can continue to use after regenerating with heated dry air (180 degree).Perhaps, regenerate through heated dry air again with after the dipping washings such as phenixin or carbon disulphide.
Embodiment 2
(concentration is 11.2g/l) adds the 0.1g carboxymethyl cellulose in the aluminum sulfate solution of 1000ml, fully stirring and dissolving.And then wherein add 30g325 purpose cocoanut active charcoal.Under fully stirring, slowly splash into about 10% sodium hydroxide solution, till the pH of solution is 7-8.Filter, washing is till the sulfate radical-free ion.Filter cake was being calcined 2 hours under 420 degree under the nitrogen protection, and the gained product is material of the present invention.Comprise the about 30g of activated charcoal, aluminium oxide 10g in the product, specific surface area is 100 meters squared per gram, and cutting-out thickness is that the right cylinder about 10mm is standby.
Measure ten air samples that all contain benzene (concentration range is 10.3-555.5ppm), chlorobenzene (concentration range is 43.1-267.3ppm), three kinds of pollutants of formaldehyde (concentration range is 24.3-100.9ppm) with the gained material by the method for embodiment 1.Its result's maximum relative error is respectively: benzene is 1.82%, and chlorobenzene is 1.07%, and formaldehyde is 2.11%.
Embodiment 3
(concentration is counted 15g/l with diboron trioxide) adds the 0.1g carboxymethyl cellulose in the borax soln of 1000ml, fully stirring and dissolving.And then wherein add 30g325 purpose NACF.Under fully stirring, slowly splash into about 10% white vitriol solution, till the pH of solution is 7-8.Filter, washing is till the sulfate radical-free ion.Filter cake was being calcined 2 hours under 700 degree under the nitrogen protection.Comprise the about 30g of NACF, Firebrake ZB 34g in the product, specific surface area is 150 meters squared per gram, and cutting-out thickness is that the right cylinder about 5mm is standby.
Measure ten air samples that all contain ethanol (concentration range is 22.3-585.7ppm), chlorobenzene (concentration range is 143.5-211.0ppm), three kinds of pollutants of acetone (concentration range is 35.3-212.7ppm) with the gained material by embodiment 1 identical method.Its result's maximum relative error is respectively: ethanol is 5.30%, and chlorobenzene is 5.22%, and acetone is 1.89%.
Embodiment 4
The macro porous silica gel of 10g bulk is placed lead nitrate solution (in massicot 100-150g/l), flooded 24 hours, take out solid, 400 degree were calcined 1 hour down; In lead nitrate solution, flood calcining again, three times like this after the product cooling again.Contain the about 10g of silica gel, massicot 2.8g in the end product, specific surface area is 280 meters squared per gram, and cutting-out thickness is that the right cylinder about 5mm is standby.
Embodiment 5
10g crosses the magnesium oxide powder of 325 mesh sieves and expanded graphite that 10g crosses 325 mesh sieves in mortar fully behind the mixing, splashes into 10ml water glass (sodium oxide molybdena about 1%, monox 3%) again under the situation of stirring and evenly mixing.With the pressure compressing tablet of 5Mpa, calcined 1 hour down by 400 degree on sheeter for this potpourri.Cutting-out thickness is that the right cylinder about 5mm is standby.
Claims (4)
1. a material that is used near infrared spectra rapid detection for low concentration gaseous organic pollutant is characterized in that being made up of two kinds of porous masses at least, and wherein first kind of material is at least a kind of in carbon compound, the silica gel; Second kind of material is at least a kind of in metal oxide, metal hydroxides, metal halide, metal sulfide, metal sulfate, metal carbonate, metal phosphate, metal borate, the metal silicate;
The proportioning of described material (quality %) is: first kind of material 30-80, second kind of material 20-70.
2. according to the described material that is used near infrared spectra rapid detection for low concentration gaseous organic pollutant of claim 1, it is characterized in that described carbon compound is activated charcoal, activated charcoal carbon fiber, fullerene, graphite, carbon black.
3. according to the described material that is used near infrared spectra rapid detection for low concentration gaseous organic pollutant of claim 1, it is characterized in that described metallic element is magnesium, calcium, barium, titanium, zirconium, molybdenum, tungsten, zinc, cadmium, aluminium, tin, lead, antimony, bismuth.
4. according to the described material that is used near infrared spectra rapid detection for low concentration gaseous organic pollutant one of in the claim 1 to 3, it is characterized in that described material specific surface area is more than or equal to 10 meters squared per gram.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200710034531 CN101266208A (en) | 2007-03-14 | 2007-03-14 | Material for near infrared spectra rapid detection for low concentration gaseous organic pollutant |
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| CN 200710034531 CN101266208A (en) | 2007-03-14 | 2007-03-14 | Material for near infrared spectra rapid detection for low concentration gaseous organic pollutant |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101660999B (en) * | 2009-09-11 | 2011-01-19 | 华东理工大学 | Micro near-infrared spectral analytical method based on enrichment of integrated material |
| CN105223166A (en) * | 2015-11-18 | 2016-01-06 | 天津工业大学 | A kind of based on contents of many kinds of heavy metal ion Simultaneously test method in the water of film enrichment-near infrared spectrum |
| CN106908533A (en) * | 2016-12-14 | 2017-06-30 | 宁海德宝立新材料有限公司 | A kind of application of metal oxide |
| CN113933257A (en) * | 2021-11-03 | 2022-01-14 | 德之昭科技(苏州)有限公司 | Detection apparatus for TVOC in air |
| CN113933257B (en) * | 2021-11-03 | 2024-06-07 | 德之昭科技(苏州)有限公司 | Detection device for TVOC in air |
-
2007
- 2007-03-14 CN CN 200710034531 patent/CN101266208A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101660999B (en) * | 2009-09-11 | 2011-01-19 | 华东理工大学 | Micro near-infrared spectral analytical method based on enrichment of integrated material |
| CN105223166A (en) * | 2015-11-18 | 2016-01-06 | 天津工业大学 | A kind of based on contents of many kinds of heavy metal ion Simultaneously test method in the water of film enrichment-near infrared spectrum |
| CN106908533A (en) * | 2016-12-14 | 2017-06-30 | 宁海德宝立新材料有限公司 | A kind of application of metal oxide |
| CN106908533B (en) * | 2016-12-14 | 2019-11-12 | 宁海德宝立新材料有限公司 | A kind of application of metal oxide |
| CN113933257A (en) * | 2021-11-03 | 2022-01-14 | 德之昭科技(苏州)有限公司 | Detection apparatus for TVOC in air |
| CN113933257B (en) * | 2021-11-03 | 2024-06-07 | 德之昭科技(苏州)有限公司 | Detection device for TVOC in air |
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Open date: 20080917 |