CN101614669A - The method and the detecting device of methyl alcohol and methyl tert-butyl ether in the nano catalytic luminescence detection gasoline - Google Patents
The method and the detecting device of methyl alcohol and methyl tert-butyl ether in the nano catalytic luminescence detection gasoline Download PDFInfo
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- CN101614669A CN101614669A CN200910012960A CN200910012960A CN101614669A CN 101614669 A CN101614669 A CN 101614669A CN 200910012960 A CN200910012960 A CN 200910012960A CN 200910012960 A CN200910012960 A CN 200910012960A CN 101614669 A CN101614669 A CN 101614669A
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Abstract
The present invention discloses method and the detecting device that a kind of nano catalytic luminescence detects methyl alcohol and methyl tert-butyl ether in the gasoline, be to detect with the nano catalytic luminescence device, used nano material is a tin ash, the detection wavelength is 400～460nm, 120～300 ℃ of heating-up temperature scopes, flow rate of carrier gas 1～40ml/min.The light signal that detects and the concentration of methyl alcohol and methyl tert-butyl ether are linear, can realize that content to methyl alcohol in the gasoline and methyl tert-butyl ether carries out the while fast, accurately detect, overcome and analyzed with gas chromatograph that existing instrument and equipment costs an arm and a leg, analysis time long and the shortcoming of poor accuracy.Have simple in structure, easy operating, (several ten thousand yuan) with low cost, selectivity is strong, operating cost is few, long service life, highly sensitive and high repeatability and other advantages.
Description
Technical field:
The present invention relates to a kind of method and checkout equipment that detects methyl alcohol and methyl tert-butyl ether in the gasoline, especially a kind of simple in structure, easy operating is done carrier gas with air, does not need chemical reagent and H
2, high-purity gas carrier gas such as He, cost is low, highly sensitive, the nano catalytic luminescence of favorable reproducibility, long service life detects methyl alcohol and methyl tert-butyl ether in the gasoline method and detecting device.
Background technology:
Gasoline is formed very complicated, and it is individual that the component of having known reaches hundreds of, even thousands of.General ethanol petrol is to add ethanol (for example E10 gasoline promptly adds 9.5%～10.5% (V/V) ethanol) in gasoline at present, because methyl alcohol is relatively cheap, therefore also often is added in the blended gasoline.Methyl alcohol toxicity is bigger, mainly acts on nervous system, has tangible anesthetic action.Main impaired organ is central nervous system, optic nerve and retina after the acute methanol poisoning, regular meeting occur dizziness, headache, dizzy, weak, lurch, have a sleepless night, phenomenons such as apathy, clouding of consciousness; The serious acute methanol poisoning eyesight can occur and sharply descend, even loses the sight of both eyes, at last can be dead because of respiratory failure.Therefore, the methanol content in the blended gasoline must satisfy standard-required, otherwise is judged to be non-conformity article.Because methyl tert-butyl ether (being MTBE) can significantly improve the octane value of unleaded gasoline, therefore also often be added in the blended gasoline, but because methyl tert-butyl ether is in the nature difficult degradation, the hidden danger that has polluted underground water, therefore its addition is also limited by strictness, otherwise be considered as violating environmental regulation, be judged to be non-conformity article.At present, according in check such as the U.S. ASTMD 6839-2002 standard gasoline when methyl alcohol and methyl tertbutyl ether content, all be to adopt multidimensional gas chromatograph (as the M3 reformulated gasoline analyser of AC company).Not only instrument and equipment cost an arm and a leg (more than 120 ten thousand yuan), analysis time long (about 75 minutes), and separation process complexity, influenced factor are many, even under identical separation condition to also often there being unknown peak to occur in the gasoline sample analytic process of different process, the chromatographic peak broadening causes bigger quantitative error, the accuracy that influence is measured.
Existing nano-material surface-catalyzed luminescent detecting device is that the diameter that will scribble nano material is that to place diameter be that 12～20mm, length are in the quartz ampoule of 100～150mm to 4～7mm electric ceramic rod, diagonally opposing corner is provided with injection port, drain on quartz ampoule, corresponding optical filter or grating, the photosignal conversion equipment (near ultraviolet sensitive spectroscopy measurement type Weak-luminescence measuring instrument, photomultiplier etc.) of being provided with nano material outside quartz ampoule.During measurement, the electric ceramic rod heats nano material, sampling systems such as pneumatic pump enter quartz ampoule with carrier gas from injection port with sample, the nano-material surface of flowing through is discharged from drain, the nano-material surface-catalyzed light that sends is behind optical filter or grating removal parasitic light, become the electric signal that is adapted to data processing units such as microcomputer through the photosignal conversion equipment again, carry out check and analysis.Nano material in the existing nano-material surface-catalyzed luminescent detecting device adopts alundum (Al, zinc paste, iron oxide etc. usually, be used for quantitative test ethanol, trimethylamine etc. and food hormone medicine residue detection etc., have simple in structure, easy operating, (several ten thousand yuan) cheap for manufacturing cost, selectivity is strong, operating cost is few, long service life, highly sensitive and high repeatability and other advantages.But up to now also not about detect methyl alcohol and the method for methyl tert-butyl ether and the relevant report of detecting device in the gasoline simultaneously with nano-material surface-catalyzed luminescent.
Summary of the invention:
The present invention is in order to solve the above-mentioned technical matters of existing in prior technology, a kind of simple in structure, easy operating to be provided, do carrier gas with air, not needing chemical reagent and H
2, high-purity gas carrier gas such as He, cost is low, highly sensitive, the nano catalytic luminescence of favorable reproducibility, long service life detects methyl alcohol and methyl tert-butyl ether in the gasoline method and detecting device.
Technical solution of the present invention is: the method for methyl alcohol and methyl tert-butyl ether in a kind of nano catalytic luminescence detection gasoline, it is characterized in that it being to detect with the nano catalytic luminescence reactor, used nano material is a tin ash, the detection wavelength is 400～460nm, 120～300 ℃ of heating-up temperature scopes, flow rate of carrier gas 1～40ml/min.
The method detecting device of methyl alcohol and methyl tert-butyl ether in a kind of detection of nano catalytic luminescence according to claim 1 gasoline, optical filter or grating 1, photosignal conversion equipment 2 and nano material 3 are arranged, described nano material 3 is a tin ash, and the wavelength of described optical filter or grating is 400～460nm.
Be provided with housing 4, be built-in with heating element 5 and quartz capillary 6 at housing 4, described nano material 3 is coated in the inwall of quartz capillary 6 and leaves transparent surface 7; Transparent surface 7 is oppositely arranged with optical filter or grating 1, and the two ends of quartz capillary 6 join with sample introduction pipe 8, blow-down pipe 9 respectively.
Be equipped with photo-conduction cell 10 between described transparent surface 7 and optical filter or the grating 1.
The diameter of the middle part of described quartz capillary 6 has rounding off face 11 less than two ends between middle part and the two ends, described nano material 3 is coated in the middle part.
Described sample introduction pipe 8, blow-down pipe 9 are kapillary, are plugged in the two ends of quartz capillary 6.
Described photo-conduction cell 10 is an optical fiber.
The diameter of the middle part of described quartz capillary 6 is 0.1～0.75mm.
The present invention is set at tin ash with the nano material in the nano catalytic luminescence detecting device, the concentration of light signal that is detected and methyl alcohol and methyl tert-butyl ether is linear, can realize that content to methyl alcohol in the gasoline and methyl tert-butyl ether carries out the while fast, accurately detect, overcome and analyzed with gas chromatograph that existing instrument and equipment costs an arm and a leg, analysis time long and the shortcoming of poor accuracy.Have simple in structure, easy operating, (several ten thousand yuan) with low cost, selectivity is strong, operating cost is few, long service life, highly sensitive and high repeatability and other advantages.
Description of drawings:
Fig. 1 is the structural representation of the embodiment of the invention 2.
Fig. 2 is the structural representation of the embodiment of the invention 3.
Embodiment:
Embodiment 1:
Select existing nano-material surface-catalyzed luminescent detecting device for use, but the detecting device nano material is a tin ash, detecting device is 400～460nm with the wavelength of optical filter or grating, it is 440～460nm that methyl alcohol detects wavelength, the detection wavelength of methyl tert-butyl ether is 400～425, the heating-up temperature scope is 120～300 ℃ during detection, and flow rate of carrier gas is 1～40ml/min, range of linearity 100ug～300mg/mL.
Experimental example 1: with 93
#Unleaded gasoline is a sample, and the content of the methyl alcohol of measuring with the method for embodiment 1 is 0.09% (V/V), and the detected value of multidimensional gas chromatographic is 0.08% (V/V); The content of the methyl tert-butyl ether of measuring is 0.65% (V/V), the detected value 0.62% (V/V) of multidimensional gas chromatographic.
Embodiment 2:
As shown in Figure 1: material and fixed form are arranged all with the optical filter or the grating 1 of prior art, photosignal conversion equipment 2, with the wavelength of prior art different is optical filter or grating 1 is 400～460nm, be provided with housing 4, be built-in with heating element 5 and quartz capillary 6 at housing 4, heating element 5 and quartz capillary 6 can be used any of prior art, and heating element 5 can join with temperature-control circuit, makes the temperature factor that influences catalytic luminescence accurately controlled.Scribble nano material 3 at quartz capillary 6 inwalls, nano material 3 adopts tin ash.Must reserve the part blank when being coated with nano material 3, promptly transparent surface 7, leave some space as on the downside that 3 of nano materials is coated in quartz capillary 6 inwalls or the part on upper side.Transparent surface 7 is oppositely arranged with optical filter or grating 1, and the two ends of quartz capillary 6 join with sample introduction pipe 8, blow-down pipe 9 respectively.
Detection method is with embodiment 1.
Embodiment 3:
As shown in Figure 2:
Basic structure as different from Example 1, for fear of the loss of light signal and the interference of parasitic light, is equipped with photo-conduction cell 10 with embodiment 1 between described transparent surface 7 and optical filter or grating 1.The diameter of the middle part of described quartz capillary 6 is less than two ends, and the diameter of middle part is 0.1～0.75mm, and rounding off face 11 is arranged between middle part and the two ends, and described nano material 3 is coated in the middle part.For ease of being connected of quartz capillary 6 and sample introduction pipe 8, blow-down pipe 9, dismounting, described sample introduction pipe 8, blow-down pipe 9 preferably are kapillary, the polyimide coating of kapillary outside just can guarantee closely to be plugged in the two ends of quartz capillary 5, and described photo-conduction cell 10 is an optical fiber.
Detection method is with embodiment 1.
Experimental example 2: with 97
#Unleaded gasoline is a sample, and the content of the methyl alcohol that present embodiment 2,3 is measured is 0.04% (V/V), and the detected value of multidimensional gas chromatographic is 0.03% (V/V); The content of the methyl tert-butyl ether of measuring is 5.28% (V/V), the detected value 5.01% (V/V) of multidimensional gas chromatographic.
Claims (8)
1. a nano catalytic luminescence detects the method for methyl alcohol and methyl tert-butyl ether in the gasoline, it is characterized in that it being to detect with the nano catalytic luminescence detecting device, used nano material is a tin ash, the detection wavelength is 400～460nm, 120～300 ℃ of heating-up temperature scopes, flow rate of carrier gas 1～40ml/min.
One kind according to claim 1 nano catalytic luminescence detect the method detecting device of methyl alcohol and methyl tert-butyl ether in the gasoline, optical filter or grating (1), photosignal conversion equipment (2) and nano material (3) are arranged, it is characterized in that: described nano material (3) is tin ash, and the wavelength of described optical filter or grating is 400～460nm.
3. the method detecting device of methyl alcohol and methyl tert-butyl ether in the nano catalytic luminescence detection gasoline according to claim 2, it is characterized in that: be provided with housing (4), be built-in with heating element (5) and quartz capillary (6) at housing (4), described nano material (3) is coated in the inwall of quartz capillary (6) and leaves transparent surface (7); Transparent surface (7) is oppositely arranged with optical filter or grating (1), and the two ends of quartz capillary (6) join with sample introduction pipe (8), blow-down pipe (9) respectively.
4. the method detecting device of methyl alcohol and methyl tert-butyl ether is characterized in that: be equipped with photo-conduction cell (10) between described transparent surface (7) and optical filter or the grating (1) in the nano catalytic luminescence detection gasoline according to claim 3.
5. detect the method detecting device of methyl alcohol and methyl tert-butyl ether in the gasoline according to claim 3 or 4 described nano catalytic luminescences, it is characterized in that: the diameter of the middle part of described quartz capillary (6) is less than two ends, rounding off face (11) is arranged between middle part and the two ends, and described nano material (3) is coated in the middle part.
6. the method detecting device of methyl alcohol and methyl tert-butyl ether in the nano catalytic luminescence detection gasoline according to claim 5, it is characterized in that: described sample introduction pipe (8), blow-down pipe (9) are kapillary, are plugged in the two ends of quartz capillary (6).
7. the method detecting device of methyl alcohol and methyl tert-butyl ether in the nano catalytic luminescence detection gasoline according to claim 2, it is characterized in that: described photo-conduction cell (10) is an optical fiber.
8. the method detecting device of methyl alcohol and methyl tert-butyl ether in the nano catalytic luminescence detection gasoline according to claim 3, it is characterized in that: the diameter of the middle part of described quartz capillary (6) is 0.1～0.75mm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101793836A (en) * | 2010-03-18 | 2010-08-04 | 中华人民共和国辽宁出入境检验检疫局 | Method for simultaneously detecting methanol and ethanol in gasoline by using photoelectric double signals and detector thereof |
| CN101799424A (en) * | 2010-03-18 | 2010-08-11 | 中华人民共和国辽宁出入境检验检疫局 | Method for simultaneously detecting ethanol and MTBE (methyl tert-butyl ether) in gasoline by photoelectric double-signal and detector |
| CN102127433A (en) * | 2010-12-31 | 2011-07-20 | 中华人民共和国辽宁出入境检验检疫局 | Tin dioxide nano-rod material for nanocatalysis luminescent sensor and preparation method thereof |
| CN103163123A (en) * | 2013-02-22 | 2013-06-19 | 北京联合大学生物化学工程学院 | Catalysis sensitive material for methanol |
Family Cites Families (2)
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| CN1188692C (en) * | 2002-01-29 | 2005-02-09 | 清华大学 | Luminous gas-sensitive sensor based on nanomaterial and process for film-forming of nanomaterial |
| CN1246688C (en) * | 2003-12-23 | 2006-03-22 | 清华大学 | Method for detecting organic molecule in solution by nano material catalytic light emitting and detector |
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2009
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101793836A (en) * | 2010-03-18 | 2010-08-04 | 中华人民共和国辽宁出入境检验检疫局 | Method for simultaneously detecting methanol and ethanol in gasoline by using photoelectric double signals and detector thereof |
| CN101799424A (en) * | 2010-03-18 | 2010-08-11 | 中华人民共和国辽宁出入境检验检疫局 | Method for simultaneously detecting ethanol and MTBE (methyl tert-butyl ether) in gasoline by photoelectric double-signal and detector |
| CN101799424B (en) * | 2010-03-18 | 2011-09-21 | 中华人民共和国辽宁出入境检验检疫局 | Method for simultaneously detecting ethanol and MTBE (methyl tert-butyl ether) in gasoline by photoelectric double-signal and detector |
| CN101793836B (en) * | 2010-03-18 | 2011-09-21 | 中华人民共和国辽宁出入境检验检疫局 | Method for simultaneously detecting methanol and ethanol in gasoline by using photoelectric double signals and detector thereof |
| CN102127433A (en) * | 2010-12-31 | 2011-07-20 | 中华人民共和国辽宁出入境检验检疫局 | Tin dioxide nano-rod material for nanocatalysis luminescent sensor and preparation method thereof |
| CN102127433B (en) * | 2010-12-31 | 2013-12-25 | 中华人民共和国辽宁出入境检验检疫局 | Tin dioxide nano-rod material for nanocatalysis luminescent sensor and preparation method thereof |
| CN103163123A (en) * | 2013-02-22 | 2013-06-19 | 北京联合大学生物化学工程学院 | Catalysis sensitive material for methanol |
| CN103163123B (en) * | 2013-02-22 | 2015-05-20 | 北京联合大学生物化学工程学院 | Catalysis sensitive material for methanol |
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