CN107764805A - A kind of device and method of on-line quick detection ethyl acetate - Google Patents
A kind of device and method of on-line quick detection ethyl acetate Download PDFInfo
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- CN107764805A CN107764805A CN201710951711.0A CN201710951711A CN107764805A CN 107764805 A CN107764805 A CN 107764805A CN 201710951711 A CN201710951711 A CN 201710951711A CN 107764805 A CN107764805 A CN 107764805A
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- ethyl acetate
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- filtering piece
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/76—Chemiluminescence; Bioluminescence
- G01N21/766—Chemiluminescence; Bioluminescence of gases
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/27—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration
Abstract
The present invention relates to on-line quick detection field, especially a kind of device and method of on-line quick detection ethyl acetate, the device includes ethyl acetate gas sensor, Weak light investigating instrument and temperature controller；The ethyl acetate gas sensor includes chemiluminescence reactor, optically filtering piece and photomultiplier with air inlet/outlet, and described chemiluminescence reactor scribbles a nanometer GeO by the surface of quartz glass tube and inserted therein2Ceramic electric heating rod composition；Using ethyl acetate gas, oxyluminescence characteristic designs ethyl acetate gas sensor to the present invention on a preset condition based, and use the spectral signal that the sensor Detection wavelength is 425nm, so as to detect the ethyl acetate gas concentration in tested gas, have the advantages that it is simple, quick, stably, it is accurate, can be widely used in industrial production real-time online detection and environmental monitoring.
Description
Technical field
The present invention relates to on-line quick detection field, the device of especially a kind of on-line quick detection ethyl acetate and side
Method.
Background technology
Ethyl acetate is a kind of colourless, volatile, inflammable and with fruit sample aromatic odor liquid, to air-sensitive,
Moisture can be absorbed and be dissolved in water, can be miscible with chloroform, ethanol, acetone and ether, there is excellent dissolubility, quick-drying, be one
The very important Organic Chemicals of kind and fabulous industrial solvent, are widely used in acetate fiber, ethyl cellulose, chlorination rubber
In the production process of glue, vinyl, acetate fiber resin, synthetic rubber, coating and paint etc..But ethyl acetate can be through
Respiratory tract is sucked and absorbed through skin, endangers eye, nose, throat, respiratory tract, can cause cough, uncomfortable in chest, expiratory dyspnea, dizzy, pharynx
Laryngalgia, stomachache, diarrhoea, dermatitis etc., Long Term Contact ethyl acetate can cause the opacity of the cornea, secondary anemia, leukocytosis etc..When
When ethyl acetate concentration is 400ppm in air, human eye, nose, throat irritation symptom can be caused；There is anesthesia to make people during high concentration
With continuing largely to suck, respiratory paralysis can be caused.Ethyl acetate is accidental to cause allergy.Ethyl acetate is also widely used for medicine
Solvent extraction in field of medicament production process.And ethyl acetate is three class solvents, pharmacopoeia of each country provides ethyl acetate in medicine
Residual content must not exceed 0.5% in product, it is necessary to residual solvent control be carried out to the medicine to dispatch from the factory, by GMP or other quality marks
Quasi- limitation uses.In addition, ethyl acetate is the main flavor of wine, be Spirit and assembled alcoholic drinks main technical requirements it
One, it is one of the conventional method of sanitary inspection and index to determine ethyl acetate content therein.Therefore extensively should in ethyl acetate
With while, its existing hidden danger and drawback are like the shadow following the person, and the detection of ethyl acetate also increasingly receives much concern.
Instrument analytical method currently used for determining ethyl acetate gas is mainly gas chromatography and liquid chromatography, gas
Although phase chromatography and liquid chromatography with higher selectivity and sensitivity, equipment instrument is huge, system complex, behaviour
Bother, it is more difficult to realize real-time, on-line checking.Using portable detector made of gas chromatography, although also having very high
Selectivity and sensitivity, but continuous detection can not be realized.And gas sensor small volume, simple to operate and response quickly etc.
The advantages of, meet the real-time, requirement of on-line checking.According to our understanding and investigation, there is no at present on detecting acetic acid second
The sensor of ester gas.Therefore, a kind of detection method of simple, quick, stable ethyl acetate gas concentration and the implementation party
The research and development of the sensor of method, have great importance for the effective detection of ethyl acetate.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of device and method of on-line quick detection ethyl acetate.This
The purpose of invention has two, and one is to provide a kind of device of on-line quick detection ethyl acetate, and the device has that selectivity is good, makes
With long lifespan and be easy in real time, on-line checking the advantages that, another object is to provide a kind of simple, quick, stable ethyl acetate
The detection method of gas concentration.
The technical scheme is that：
A kind of device of on-line quick detection ethyl acetate, the device include ethyl acetate gas sensor, Weak-luminescence
Measuring instrument and temperature controller；The ethyl acetate gas sensor includes chemiluminescence reactor, light with air inlet/outlet
Learn filter plate and photomultiplier, described chemiluminescence reactor scribble nanometer by the surface of quartz glass tube and inserted therein
GeO2Ceramic electric heating rod composition, described optically filtering piece is located at the outside of quartz glass tube, the optically filtering piece
Smooth surface is parallel with ceramic electric heating rod, and its detection wavelength is 425nm, and described photomultiplier is coaxial simultaneously with optically filtering piece
String is located at the shady face of optically filtering piece；The temperature controller is by gathering the ceramic electric heating rod in ethyl acetate sensor
Surface temperature feedback control ceramic electric heating rod power output, make quartz glass tube surface keep constant temperature；The acetic acid
The optical signal of optically filtering piece outflow in ethyl ester gas sensor is re-fed into described after photomultiplier is transformed into electric signal
Weak light investigating instrument be amplified and handle.
A kind of method of on-line quick detection ethyl acetate, the described method comprises the following steps：
Step 1：It is 10-1200mg/m by ethyl acetate gas concentration3Gaseous sample with 250mL/min flow velocity stream
A nanometer GeO is scribbled through the surface that temperature is 275 DEG C2Ceramic electric heating rod appearance, produce chemiluminescence, to each gas sample
The wavelength that product are sent is that 425nm lightwave signal is detected, then by the lightwave signal intensity and acetic acid of gained gaseous sample
Ethyl ester gas concentration carries out linear regression processing, obtains the linear equation of ethyl acetate gas concentration and lightwave signal intensity；
Step 2：Using the same procedure detection under test gas institute of the lightwave signal intensity of detection gas sample in step 1
The wavelength sent is 425nm lightwave signal intensity, the linear equation lightwave signal intensity level substituted into obtained by step 1,
The ethyl acetate concentration under test gas is calculated.
Beneficial effects of the present invention are：Using ethyl acetate gas, oxyluminescence characteristic designs the present invention on a preset condition based
Ethyl acetate gas sensor, and using the spectral signal that the sensor Detection wavelength is 425nm, so as to detect in tested gas
Ethyl acetate gas concentration, have the advantages that it is simple, quick, stably, it is accurate, can be widely used in industrial production it is real-time
Line detects and environmental monitoring.
Brief description of the drawings
Fig. 1 is the structural representation of apparatus of the present invention；
Fig. 2 is the intensity profile of light emission figure that ethyl acetate gas aoxidizes luminescence-producing reaction under the different flow rate of carrier gas of the present invention；
Fig. 3 is that ethyl acetate gas aoxidizes the luminous intensity of luminescence-producing reaction and the curve of signal to noise ratio under different temperatures of the present invention
Figure；
Fig. 4 is the chemiluminescence intensity and wavelength and the relation curve of signal to noise ratio and wavelength of ethyl acetate gas of the present invention
Figure；
Fig. 5 is the chemiluminescence response curve of the ethyl acetate gas of various concentrations of the present invention；
Fig. 6 is the comparison figure of gas with various response signal intensity of the present invention；
Fig. 7 is ethyl acetate concentration of the present invention and the working curve diagram of chemiluminescence intensity relation.
In figure, 1, ceramic electric heating rod；2nd, quartz glass tube；3rd, optically filtering piece；4th, photomultiplier；5th, temperature control
Device；6th, Weak light investigating instrument.
Embodiment
The embodiment of the present invention is described further below in conjunction with the accompanying drawings：
Embodiment 1：
As shown in figure 1, a kind of device of on-line quick detection ethyl acetate, the device includes ethyl acetate gas sensing
Device, Weak light investigating instrument 6 and temperature controller 5；The ethyl acetate gas sensor includes the chemistry with air inlet/outlet
Luminescence-producing reaction room, optically filtering piece 3 and photomultiplier 4, described chemiluminescence reactor is by quartz glass tube 2 and is inserted in it
Interior surface scribbles a nanometer GeO2Ceramic electric heating rod 1 form, described optically filtering piece 3 is located at the outer of quartz glass tube 2
Side, the smooth surface of the optically filtering piece 3 is parallel with ceramic electric heating rod 1, and its detection wavelength is 425nm, and described photoelectricity is again
Increase that pipe 4 is coaxial with optically filtering piece 3 and string is located at the shady face of optically filtering piece 3；The temperature controller 5 is by gathering acetic acid
The power output of the surface temperature feedback control ceramic electric heating rod 1 of ceramic electric heating rod 1 in ethyl ester sensor, makes quartzy glass
The surface of glass pipe 2 keeps constant temperature；The optical signal that optically filtering piece 3 in the ethyl acetate gas sensor is spread out of is through photoelectricity times
Increase pipe 4 and be transformed into and described Weak light investigating instrument 6 is re-fed into after electric signal is amplified and handles.
Embodiment 2：
As shown in figure 1, a kind of method of on-line quick detection ethyl acetate, the described method comprises the following steps：
It is 10-1200mg/m by ethyl acetate gas concentration3Gaseous sample using 250mL/min flow velocity flow through temperature as
275 DEG C of surface scribbles a nanometer GeO2Ceramic electric heating rod 1 appearance, produce chemiluminescence, each gaseous sample is sent
Wavelength be 425nm lightwave signal detected, then by the lightwave signal intensity and ethyl acetate gas of gained gaseous sample
Bulk concentration carries out linear regression processing, obtains the linear equation of ethyl acetate gas concentration and lightwave signal intensity；Using step
The light wave that the wavelength that the same procedure detection under test gas of the lightwave signal intensity of detection gas sample is sent in one is 425nm
Signal intensity, the linear equation lightwave signal intensity level substituted into obtained by step 1, is calculated the second under test gas
Acetoacetic ester concentration.
Embodiment 3：
As shown in Fig. 2 it is 275 DEG C by ceramic heating bar surface temperature control, then with air pump in 120-390mL/min
In the range of it is different in flow rate by concentration be 20mg/m3Ethyl acetate gas be sent into quartz glass tube in, finally by Weak-luminescence
Measuring instrument records lower corresponding luminous intensity different in flow rate, as a result as shown in Figure 2；As shown in Figure 2, flow velocity is in 120-
In the range of 250mL/min, luminous intensity increases with the increase of flow velocity；Flow velocity is in the range of 250-390mL/min, luminous intensity
Increase with flow velocity and reduce；And flow velocity is in 250mL/min, luminous intensity reaches maximum, therefore is selected as determining acetic acid
The optimum flow rate of ethyl ester.
Embodiment 4：
As shown in figure 3, the ceramic heat rod surface temperature in reative cell first is set as into 275 DEG C, then with air pump with
Concentration is 20mg/m by 250mL/min constant flow rate3Ethyl acetate gas be sent into quartz glass tube in, then progressively will pottery
Porcelain heating rod surface temperature is increased to 336 DEG C, finally as luminous strong corresponding to Weak light investigating instrument records different temperatures
Degree, temperature range as a result as shown in Figure 3 are 224-336 DEG C of intensity curves；Using air as background gas, then with same
Method measure the heat radiated noise intensity of system, above-mentioned luminous signal intensity is calculated into noise compared with heat radiated noise intensity
Than obtaining the signal to noise ratio curve that temperature range as shown in Figure 3 is 224-336 DEG C.By two curves compared to visible, relatively low anti-
When answering temperature, as temperature raises, luminous intensity and signal to noise ratio all gradually increase, but when exceeding certain temperature, luminous intensity shows
Writing reduces, because heat radiation background signal can acutely increase with the increase of reaction temperature, causes real luminous strong
Degree acutely reduces, so as to cause signal to noise ratio to be significantly reduced.When reaction temperature is adjusted to 275 DEG C, signal to noise ratio has maximum, therefore
275 DEG C of optimal reaction temperatures for detection ethyl acetate of selection.
Embodiment 5：
As shown in figure 4, chemiluminescence is a kind of material light radiation phenomenon adjoint in chemical reaction process is carried out, it is different
Substance reaction there is certain emission spectrum scope, and the characteristic frequency with a peak of luminous intensity.In order to detect acetic acid
The optically filtering piece of ethyl acetate gas sensor is replaced with wavelength by the characteristic frequency of ethyl ester gas oxidation reaction, the present embodiment
Scope is 350-555nm 9 kinds of interference filter elements, ceramic heat rod surface temperature then is set as into 275 DEG C, then use air pump
Using 250mL/min constant flow rate by concentration as 20mg/m3Ethyl acetate gas be sent into quartz glass tube in, obtain such as Fig. 4
Shown wave-length coverage is 350-555nm intensity curves and heat radiation signal to noise ratio curve.By two curves compared to visible,
In wavelength in the range of 350-555nm, luminous intensity and signal to noise ratio are as wavelength increases first increases and then decreases, when wavelength is
Signal to noise ratio is maximum during 425nm, therefore selects 425nm wavelength as measurement wavelength.
Embodiment 6：
As shown in figure 5, ceramic heat rod surface temperature is first set as 275 DEG C, then with air pump with 250mL/min perseverance
Concentration is 12mg/m by constant current speed3、20mg/m3、32mg/m3Ethyl acetate gas be respectively fed in quartz glass tube, obtain as
Curve 1,2 and 3 shown in Fig. 5.As shown in figure 5, luminous signal increases and increased with ethyl acetate concentration, but curve shape is phase
As.It is passed through after ethyl acetate gas about 3.0s and maximum occurs, luminous signal can decays back baseline in 5s from maximum
Value, shows that the sensor has fast-response to ethyl acetate gas.
Embodiment 7：
As shown in fig. 6, in order to investigate the selectivity of ethyl acetate gas sensor of the present invention, the present embodiment uses acetic acid second
Ester gas sensor has carried out substantial amounts of comparative experiments, and specific experiment method is as described below：Ceramic heat rod surface temperature is set
It is set to 275 DEG C, then with air pump concentration is 20mg/m3Ethyl acetate, ethyl mercaptan, acetone, methanol, ethanol, normal propyl alcohol, first
The gases such as aldehyde, acetaldehyde, chloroform, tetrachloromethane, n-hexane, acetic acid, benzene, toluene, paraxylene are respectively with 250mL/min's
Constant flow rate is sent into quartz glass tube, and the luminous intensity of each gas is as shown in Figure 6.Fig. 6 shows, only ethyl acetate, second sulphur
Alcohol and acetone produce certain luminous intensity, respectively 2452,245 and 123, and luminous intensity phase caused by ethyl mercaptan and acetone
There was only the 9.99% and 5.02% of ethyl acetate luminous intensity for ethyl acetate.In addition, methanol, ethanol, normal propyl alcohol, first
The common gas such as aldehyde, acetaldehyde, chloroform, tetrachloromethane, n-hexane, acetic acid, benzene, toluene, paraxylene are without generation hair
Optical phenomenon, show that inventive sensor has splendid selectivity to ethyl acetate.
Embodiment 8：
As shown in fig. 7, first compound concentration be 10,20,32,100,300,800,1200mg/m3Ethyl acetate gas
Series of samples, ceramic heat rod surface temperature is then set as 275 DEG C, with 250mL/min constant flow rate respectively each
Sample is sent into quartz glass tube, obtains the luminous intensity that the lightwave signal that each sample is sent is 425nm, they are corresponded to respectively
It is abscissa and using luminous intensity as a point in the rectangular coordinate system of ordinate using concentration, is 10-1200mg/m in concentration3
In the range of gaseous sample corresponding to point dispersion it is relatively small, by these point carry out linear regression processings obtain such as Fig. 7
Shown coefficient correlation is r=0.9965 straight line, and the linear equation is I=389.6c-3871, and wherein I is luminous intensity, c
For ethyl acetate gas concentration.The ethyl acetate gas sensor range of linearity of the present invention is 10-1200mg/m3, detection is limited to
3.0mg/m3。
Embodiment 9：
In order to verify ethyl acetate gas sensor of the present invention to ethyl acetate accurate with detection during other gas coexistences
Exactness, while be the raw material of industrial synthesizing ethyl acetate based on ethanol and acetic acid, and benzene and formaldehyde are common room airs
Pollutant, the present embodiment carry out the rate of recovery analysis of ethyl acetate from two gaseous samples manually prepared.Wherein sample 1 is
Ethyl acetate, ethanol and acetic acid containing concentration known；Sample 2 is the ethyl acetate containing concentration known, benzene and formaldehyde.The present embodiment
Comprise the following steps that it is described：
It it is first 275 DEG C by ceramic heating bar surface temperature control, with air pump respectively two gaseous samples, with 250mL/
Min constant flow rate is sent into quartz glass tube, and the luminous intensity of each sample is recorded by Weak light investigating instrument, then
The luminous intensity values I of each mixed gas sample is substituted into the linear equation obtained by embodiment 8 respectively, calculates each mixing
The concentration c of ethyl acetate in gaseous sample, as a result as shown in table 1.As a result show that the rate of recovery is relatively satisfactory, show acetic acid second of the present invention
Ester gas sensor has applications well value in workshop and room air monitoring.
The Synthesis Diethyl ether sample analysis result of table 1
Embodiment 10：
In order to verify the application value of ethyl acetate gas sensor of the present invention, using ethyl acetate gas sensing of the present invention
Device and GC-MS are analyzed 3 environmental samples simultaneously, and result is compared.Concrete operation step is as follows：Using air
Sampling pump, the air of neighbouring 3 different locis of collection storage ethyl acetate reagent, sampling flow rate pump are 100mL/min, during use
Between be 8min, then extract 1mL samples, analyzed respectively using ethyl acetate gas sensor of the present invention and GC-MS, with
GC-MS measured results are actual value, calculate the relative error of ethyl acetate gas sensor testing result of the present invention, as a result such as table
Shown in 2.As a result it is -4.5% to+5.9% to show relative error, and two methods acquired results have higher matching degree, enter one
Step shows that this ethyl acetate gas sensor of the present invention has better application value.
Table 2 uses ethyl acetate gas sensor of the present invention and GC-MS analysis environments sample results
Merely illustrating the principles of the invention described in above-described embodiment and specification and most preferred embodiment, this is not being departed from
On the premise of spirit and scope, various changes and modifications of the present invention are possible, and these changes and improvements both fall within requirement and protected
In the scope of the invention of shield.
Claims (2)
- A kind of 1. device of on-line quick detection ethyl acetate, it is characterised in that the device include ethyl acetate gas sensor, Weak light investigating instrument and temperature controller；It is anti-that the ethyl acetate gas sensor includes the chemiluminescence with air inlet/outlet Room, optically filtering piece and photomultiplier are answered, described chemiluminescence reactor is by quartz glass tube and the surface of inserted therein Scribble a nanometer GeO2Ceramic electric heating rod composition, described optically filtering piece is located at the outside of quartz glass tube, the optics The smooth surface of filter plate is parallel with ceramic electric heating rod, and its detection wavelength is 425nm, described photomultiplier and optically filtering Piece is coaxially and string is located at the shady face of optically filtering piece；The temperature controller is by gathering the ceramics in ethyl acetate sensor The power output of the surface temperature feedback control ceramic electric heating rod of electrically heated rod, the surface of quartz glass tube is set to keep constant temperature； In the ethyl acetate gas sensor optically filtering piece outflow optical signal after photomultiplier is transformed into electric signal again Described Weak light investigating instrument is sent into be amplified and handle.
- A kind of 2. method of on-line quick detection ethyl acetate, it is characterised in that the described method comprises the following steps：Step 1：It is 10-1200mg/m by ethyl acetate gas concentration3Gaseous sample temperature is flowed through with 250mL/min flow velocity A nanometer GeO is scribbled for 275 DEG C of surfaces2Ceramic electric heating rod appearance, produce chemiluminescence, each gaseous sample is sent Wavelength be 425nm lightwave signal detected, then by the lightwave signal intensity and ethyl acetate gas of gained gaseous sample Bulk concentration carries out linear regression processing, obtains the linear equation of ethyl acetate gas concentration and lightwave signal intensity；Step 2：Sent using the same procedure detection under test gas of the lightwave signal intensity of detection gas sample in step 1 Wavelength be 425nm lightwave signal intensity, by the lightwave signal intensity level substitute into step 1 obtained by linear equation, calculate Obtain the ethyl acetate concentration under test gas.
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| CN107764805B (en) | 2021-01-29 |
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