CN102393390B - Method for identifying organic matter by using single cataluminescence sensor - Google Patents
Method for identifying organic matter by using single cataluminescence sensor Download PDFInfo
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- CN102393390B CN102393390B CN 201110274797 CN201110274797A CN102393390B CN 102393390 B CN102393390 B CN 102393390B CN 201110274797 CN201110274797 CN 201110274797 CN 201110274797 A CN201110274797 A CN 201110274797A CN 102393390 B CN102393390 B CN 102393390B
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Abstract
The invention relates to a method for identifying organic matter by using a single cataluminescence sensor, which comprises the following steps of: respectively establishing a standard spectrum of each organic matter standard sample; acquiring a spectrum of an organic matter sample to be measured by using the same method for establishing the standard spectrum; comparing the obtained spectrum with the standard spectrum one by one; if the spectrum is the same as the standard spectrum, determining the organic matter standard sample corresponding to the standard spectrum to be the organic matter sample to be measured: feeding the organic matter standard sample into a quartz glass tube from an inlet or outlet of the quartz glass tube of the cataluminescence sensor; sealing the inlet and the outlet of the quartz glass tube of the cataluminescence sensor, heating and carrying out a cataluminescence reaction until the reaction is ended; meanwhile, amplifying an electrical signal output by the cataluminescence sensor and carrying out A/D (Analogue/Digital) conversion to obtain a curve that the luminance intensity of the organic matter standard sample changes along with time in the luminance reaction process; and saving the curve in a memory to obtain the standard spectrum of the organic matter standard sample.
Description
Technical field
The present invention relates to utilize the chemiluminescence means to test or the technical field of analysis of material, be specifically related to the discrimination method of organic substance.
Background technology
Ultraviolet spectrum, gas chromatography, high performance liquid chromatography and chromatogram mass spectrum the instrument analytical method such as are used in conjunction and are widely used in industrial and commercial quality inspection and environmental monitoring field.These analytical approachs all have advantage separately, but the more difficult on-the site analysis requirement of satisfying real-time online.
The catalytic luminescence sensor is little owing to having a volume, response rapidly, but the advantage of on-line analysis has been widely used in analysis field.Optical filter and photomultiplier that existing catalytic luminescence sensor is 400～600nm by the quartz glass tube with import and outlet, ceramic electroheating tube, detection wavelength form, wherein, the surface of described ceramic electroheating tube scribbles catalyzer and is inserted in quartz glass tube; Described optical filter is located at the outside of quartz glass tube, and sensitive surface is parallel with ceramic electroheating tube; Coaxial and string is located at the shady face of optical filter to described photomultiplier with optical filter.During detection, described ceramic electroheating tube heats its surperficial catalyzer, pneumatic pump enters quartz glass tube with carrier gas from import with sample, discharge from outlet on the flow through surface of the ceramic electroheating tube that scribbles catalyzer, light wave that this process produces is detected the lightwave signal of specific wavelength by optical filter, this signal just obtains the gas concentration in testing sample after the Weak-luminescence pick-up unit is processed.This shows, existing catalytic luminescence sensor can only carry out quantitative test to certain specific gas, and can not carry out qualitative analysis to unknown gas, and a kind of sensor of catalyzer can only carry out quantitative test to a kind of gas.Given this, the sensor array based on multiple nano material (being catalyzer) begins development.the array that this sensor array is comprised of the catalytic luminescence sensor of different catalysts in fact, produce the light signal of a plurality of varying strengths when utilizing specific blend gas (standard items) to flow through the array that described catalytic luminescence sensor forms, and adopt CCD image sensor (Charge Coupled Device) that the light signal that picks up is transformed into electric signal, again by data processing equipment (as the analog to digital converter chip, computing machine) convert " fingerprint " collection of illustrative plates to and record as standard diagram, then unknown gas (sample) is compared by spectrum and standard diagram that described display sensor produces, and then identification unknown gas.As the existing report that can identify the sensor array of the organic gass such as trimethylamine, sulfuretted hydrogen and ethanol (referring to Na N, Zhang S C, Wang S, Zhang X R.A catalytic nanomaterial-based optical chemo-sensor array [J] .J.Am.Chem.Soc.2006,128 (45): 14420-14421).But, still there is following deficiency in above-mentioned sensor array: the array that (1) described sensor array is comprised of the catalytic luminescence sensor of different catalysts, therefore not only complicated, and each catalytic luminescence sensor of described array is a labile factor, and one of them catalytic luminescence sensor causes the signal drift all can affect whole recognition effect with increasing the labile factor that produces service time; (2) because same gas different catalytic luminescence light intensities that sensor sends in described sensor array are different, therefore must adopt the imageing sensor as CCD one class that light signal is transformed into electric signal.Therefore it is desired setting up the single catalytic luminescence sensor identification of a kind of use organic.
Summary of the invention
In view of there is above-mentioned deficiency in prior art, the technical problem to be solved in the present invention is to provide the organic method of the single catalytic luminescence sensor of a kind of use identification, and the method has advantages of simple, the easy to operate and effect stability of equipment.
In the prior art, no matter adopt the quantitative test that single catalytic luminescence sensor carries out known gas or adopt sensor array to carry out qualitative analysis to the determinand of the unknown, the method that adopts is all to make gas to be measured cross the catalytic luminescence sensor with the carrier gas continuous stream, the resulting radiation intensity value that flows through the light that the catalytic luminescence sensor produces in a flash in just known gas or unknown gas.Therefore to carry out to the determinand of the unknown the sensor array that qualitative analysis just must use the catalytic luminescence sensor by different catalysts to form.The inventor is in the middle discovery that studies for a long period of time, when the gas with various of equal volume is carried out the catalytic luminescence reaction in the quartz glass tube of same catalytic luminescence sensor, not only the time length of course of reaction is different, and the rule that changes at the light radiation intensity that course of reaction produces is different.Based on above-mentioned new discovery, the technical scheme that the present invention addresses the above problem is as follows:
The organic method of the single catalytic luminescence sensor identification of a kind of use, the method is comprised of following steps:
(1) set up respectively according to the following steps the standard diagram of each organism standard items:
(1.1) the organism standard items are inserted in quartz glass tube from the import or export of the quartz glass tube of catalytic luminescence sensor;
(1.2) with quartz glass tube import and the exit seal of catalytic luminescence sensor, and heating is carried out catalytic luminescence reaction to reaction and is finished; Simultaneously,
(1.3) wavelength of the catalytic luminescence sensor being exported is that the electric signal of the light wave of 400-490nm amplifies, the A/D conversion just obtains machine thing standard items time dependent curve of luminous intensity in the luminescence-producing reaction process, this curve is deposited in the standard diagram that namely gets these organism standard items in storer;
(2) obtain according to the following steps the spectrum of organic matter samples to be measured:
(2.1) organic matter samples is inserted in quartz glass tube from the import or export of the quartz glass tube of catalytic luminescence sensor;
(2.2) with quartz glass tube import and the exit seal of catalytic luminescence sensor, and heating is carried out catalytic luminescence reaction to reaction and is finished; Simultaneously,
(2.3) wavelength of the catalytic luminescence sensor being exported is that the electric signal of the light wave of 400-490nm amplifies, the A/D conversion just obtains machine thing standard items time dependent curve of luminous intensity in the luminescence-producing reaction process, namely gets the spectrum of this organic matter samples;
The standard diagram of each organism standard items that the spectrum of the organic matter samples that (3) step (2) is obtained and step (1) are set up compares one by one, spectrum person identical with standard diagram, the corresponding organism standard items of this standard diagram are organic matter samples to be measured;
Insert machine thing standard items in quartz glass tube described in above-mentioned steps (1.1) and step (2.1) in method that organic matter samples is inserted in quartz glass tube be:
When described machine thing standard items and organic matter samples are gas, adopt syringe to extract described gas and be in the quartz glass tube of 1/5～1/10 injection catalytic luminescence sensor by the volume ratio of described gas and quartz glass inner air tube;
When described machine thing standard items and organic matter samples are liquid, adopt syringe to draw described liquid and be 1/1000～1/2000 to be injected on the surface of the ceramic electroheating tube that scribbles catalyzer in the quartz glass tube of catalytic luminescence sensor by the volume ratio of described liquid and quartz glass inner air tube;
The temperature of reaction of the catalytic luminescence reaction described in above-mentioned steps (1.2) and (2.2) is:
When described machine thing standard items and organic matter samples were gas, temperature of reaction was 200～290 ℃;
When described machine thing standard items and organic matter samples were liquid, temperature of reaction was 300～400 ℃.
The organic method of identification of the present invention, wherein, the preferred range of the temperature of reaction of described catalytic luminescence reaction is:
When described machine thing standard items and organic matter samples were gas, temperature of reaction was 250 ± 10 ℃;
When described machine thing standard items were liquid, temperature of reaction was 350 ± 10 ℃.
The organic method of identification of the present invention, wherein said organism can be monomeric compounds, can be also the potpourris that the various of monomer compound forms.
The organic method of identification of the present invention, wherein said catalytic luminescence sensor are a kind of common sensors, and its structure is as described in the second nature section in the application's background technology.The organic method of identification of the present invention, wherein, the detection wavelength of the optical filter of described catalytic luminescence sensor is generally 400～600nm, this wavelength on the shape of luminescence response curve without impact, but according to the inventor's experience, wavelength during greater than 490nm background signal increase, give the instability of bringing mensuration, therefore the better range of choice of the detection wavelength of optical filter is 400-490nm, optimal selection 425nm; The catalyzer that the surface of the ceramic electroheating tube of described catalytic luminescence sensor is coated with is to determine its sensitivity and optionally.Catalytic luminescence sensor catalyzer used is different, but the most frequently used catalyzer is all metal nanoparticle, as the nano-MgO that detects the steams such as parenteral solution, vinyl acetate such as Ceftriaxone Sodium, the nanometer SrCO that detects the steams such as acetaldehyde, ethyl acetate
3, detect the nanometer ZrO of the parenteral solutions such as oral liquid, Ceftriaxone Sodium such as the positive air water of ageratum
2, detect the nano-TiO of the steams such as ethanol, acetone
2Deng, all can use in the method.The organic method of identification of the present invention, wherein the wavelength with the output of catalytic luminescence sensor is the device that electric signal amplifies, A/D changes and records of the light wave of 400-490nm, it can be Weak-luminescence pick-up unit in common Weak-luminescence detector, as the Weak-luminescence pick-up unit in the Weak-luminescence detector of Institute of Biophysics, Academia Sinica's development, can be also the equipment of other similar functions.
owing to being not quite similar in serviceable life of the catalytic luminescence sensor of different catalysts, and the catalytic luminescence sensor kind that the general user buys is also limited, if therefore the standard diagram of described organism standard items is the standard diagram of the resulting organism standard items of catalytic luminescence sensor of a certain catalyzer, so when the user at hand the catalytic luminescence sensor failure or just cannot detect when there is no the catalytic luminescence sensor of corresponding catalyzer, especially when the user does not know the precision reduction of catalytic luminescence sensor at hand or lost efficacy, resulting result is just inaccurate.In addition, also accidentally exist the collection of illustrative plates difference on a kind of catalyzer of two kinds of materials not obvious, but on another kind of catalyzer collection of illustrative plates difference phenomenon clearly.In order to address the above problem, standard diagram of the present invention preferably uses the standard diagram of the same organism standard items that the catalytic luminescence sensor of two or more different catalysts obtains respectively.
The present invention uses single catalytic luminescence sensor namely to realize organic identification, therefore has following beneficial effect than prior art:
(1) sensor that uses is the catalytic luminescence sensor of routine, and the sensor array cost that uses than existing methods significantly reduces;
(2) easy and simple to handle, volume is little, operating cost is low, can be widely used in industrial and commercial quality inspection and environmental monitoring;
(3) a kind of conventional catalytic luminescence sensor of catalyzer can be completed organic identification, so accuracy of judgement, and reliable and stable;
(4) opened up a kind of new purposes for existing Weak-luminescence detector.
Description of drawings
Fig. 1 is the schematic diagram of the Weak-luminescence detector of Institute of Biophysics, Academia Sinica's development.
Fig. 2 is the spectrogram of Yinqiao detoxification liquid and vinyl acetate catalytic luminescence reaction under condition of different temperatures.
Fig. 3 is for adopting the surface to scribble nanometer ZrO
2The standard diagram of the fluid organic material standard items set up as the ceramic heating pipe in the catalytic luminescence sensor of ceramic heating pipe.
The standard diagram of Fig. 4 fluid organic material standard items that to be the employing surface ceramic heating pipe that scribbles nano-MgO set up as the ceramic heating pipe in the catalytic luminescence sensor.
The standard diagram of Fig. 5 gas organism standard items that to be the employing surface ceramic heating pipe that scribbles nano-MgO set up as the ceramic heating pipe in the catalytic luminescence sensor.
Fig. 6 is for adopting the surface to scribble nanometer SrCO
3The standard diagram of the gas organism standard items set up as the ceramic heating pipe in the catalytic luminescence sensor of ceramic heating pipe.
The spectrogram of Fig. 7 aldehydes gas that to be the employing surface ceramic heating pipe that scribbles nano-MgO obtain as the ceramic heating pipe in the catalytic luminescence sensor.
Fig. 8 is for adopting the surface to scribble nanometer SrCO
3The spectrogram of the cease of ethyl-acetate gas that obtains as the ceramic heating pipe in the catalytic luminescence sensor of ceramic heating pipe.
Fig. 9 is for adopting the surface to scribble nanometer ZrO
2The spectrogram of the amino acids oral-liquor that obtains as the ceramic heating pipe in the catalytic luminescence sensor of ceramic heating pipe.
The spectrogram of Figure 10 amino acids oral-liquor that to be the employing surface ceramic heating pipe that scribbles nano-MgO obtain as the ceramic heating pipe in the catalytic luminescence sensor.
Figure 11 is for adopting the surface to scribble nanometer ZrO
2The spectrogram of the Benzylpenicillin sodium salt parenteral solution that obtains as the ceramic heating pipe in the catalytic luminescence sensor of ceramic heating pipe.
The spectrogram of Figure 12 Benzylpenicillin sodium salt parenteral solution that to be the employing surface ceramic heating pipe that scribbles nano-MgO obtain as the ceramic heating pipe in the catalytic luminescence sensor.
Embodiment
The instrument that following embodiment uses is the Weak-luminescence detector of Institute of Biophysics, Academia Sinica's development, this instrument is comprised of catalytic luminescence sensor 7, Weak-luminescence pick-up unit 8 and temperature controller 9 three parts, and wherein catalytic luminescence sensor 7 forms (referring to Fig. 1) by quartz glass tube 1, ceramic heating pipe 2, optical filter 3 and the photomultiplier 4 that the two ends in the dotted line frame are respectively equipped with gas feed 5 and gas vent 6.In quartz glass tube 1 in the catalytic luminescence sensor 7 of this Weak-luminescence detector, except ceramic heating pipe 2 shared space, the spatial volume of reaction chamber is 10ml.In order to complete following experiment, the inventor has purchased 3 surfaces and has scribbled respectively nano-MgO, nanometer SrCO
3With nanometer ZrO
2Ceramic heating pipe 2 standby.
Example 1 (choice of experimental conditions of catalytic luminescence reaction)
1, experiment equipment: the Weak-luminescence detector, wherein, the ceramic heating pipe 2 in catalytic luminescence sensor 7 is respectively the surface and scribbles nanometer ZrO
2With nanometer SrCO
3Ceramic heating pipe; The detection wavelength of filter plate 3 is 425nm.
2, laboratory sample: Yinqiao detoxification liquid and vinyl acetate.
3, experimental technique:
(1) referring to seeing Fig. 1, the experimental procedure that Yinqiao detoxification liquid catalytic luminescence reaction experiment condition is selected is as described below:
(1.1) select the surface to scribble nanometer ZrO
2Ceramic heating pipe as the ceramic heating pipe 2 in catalytic luminescence sensor 7, draw 10 μ l Yinqiao detoxification liquid with injector for medical purpose and scribble nanometer ZrO from import 5 notes of the quartz glass tube 1 of catalytic luminescence sensor 7 to the surface in quartz glass tube 1
2Ceramic heating pipe 2 on;
(1.2) quartz glass tube 1 import of catalytic luminescence sensor 7 is used teflon seal with exporting, heating is carried out the catalytic luminescence reaction to reacting end under 300 ℃; Simultaneously,
(1.3) wavelength of by Weak-luminescence pick-up unit 8, catalytic luminescence sensor 7 being exported is that the electric signal of the light wave of 425nm amplifies, the A/D conversion just obtains Yinqiao detoxification liquid time dependent curve of luminous intensity in the luminescence-producing reaction process, namely gets Yinqiao detoxification liquid at the spectrum of 300 ℃ of lower catalytic luminescences reactions.
Setting respectively the catalytic luminescence reaction is 350 ℃ and 400 ℃ again, repeats above-mentioned experimental procedure (1.1)～(1.3) and just obtains Yinqiao detoxification liquid at the spectrum of 350 ℃ and 400 ℃ lower catalytic luminescence reactions.
(2) referring to seeing Fig. 1, the experimental procedure that vinyl acetate catalytic luminescence reaction experiment condition is selected is as described below:
(2.1) select the surface to scribble nanometer SrCO
3Ceramic heating pipe as the ceramic heating pipe 2 in catalytic luminescence sensor 7, with injector for medical purpose draw 1ml vinyl acetate steam from import 5 notes of the quartz glass tube 1 of catalytic luminescence sensor 7 in quartz glass tube 1;
(2.2) quartz glass tube 1 import of catalytic luminescence sensor 7 is used teflon seal with exporting, heating is carried out the catalytic luminescence reaction to reacting end under 200 ℃; Simultaneously,
(2.3) wavelength of by Weak-luminescence pick-up unit 8, catalytic luminescence sensor 7 being exported is that the electric signal of the light wave of 425nm amplifies, the A/D conversion just obtains vinyl acetate time dependent curve of luminous intensity in the luminescence-producing reaction process, namely gets vinyl acetate at the spectrum of 200 ℃ of lower catalytic luminescences reactions.
Setting respectively the catalytic luminescence reaction is 250 ℃ and 290 ℃ again, repeats above-mentioned experimental procedure (2.1)～(2.3) and just obtains vinyl acetate at the spectrum of 250 ℃ and 290 ℃ lower catalytic luminescence reactions.
Above-mentioned Yinqiao detoxification liquid and vinyl acetate catalytic luminescence under condition of different temperatures reacts spectrogram as shown in Figure 2.As seen from Figure 2, temperature is very large on the impact of measurement result, measures temperature low, reacts abundant not, and appearance time is longer, and peak intensity is relatively little; Measure excess Temperature, reaction is carried out too soon, and appearance time is too short, gets together in the peak, and characteristic is not strong.Therefore, the optimum temperature of measuring fluid organic material is 350 ℃, and optional temperature range is 350 ± 10 ℃, and the organic optimum temperature of mensurated gas composition is 250 ℃, and optional temperature range is 250 ± 10 ℃.
Example 2 (foundation of the standard diagram of organism standard items)
1, experiment equipment: the Weak-luminescence detector, wherein, the ceramic heating pipe 2 in catalytic luminescence sensor 7 is respectively the surface and scribbles nano-MgO, nanometer ZrO
2With nanometer SrCO
3Ceramic heating pipe; The detection wavelength of filter plate 3 is 425nm.
2, organism standard items:
(1) gas organism standard items: ether, vinyl acetate, acetaldehyde and ethyl acetate.
(2) fluid organic material standard items: shuanghuanglian mixture, shuanghuanglian koufuye, Yinqiao detoxification liquid, amino acids oral-liquor, HuoXiangZhengQiShui, gentamicine sulphate injection, Benzylpenicillin sodium salt parenteral solution, chloramphenicol inj, analgin injection, ceftriaxone inj, Polyinosinic injection, Cefazolin sodium injection and Cefradine parenteral solution.
3, experimental technique:
(1) referring to seeing Fig. 1, adopt the surface to scribble nanometer ZrO
2Ceramic heating pipe set up the step of standard diagram of fluid organic material standard items as the ceramic heating pipe 2 in catalytic luminescence sensor 7 as described below:
(1.1) draw 10 μ l HuoXiangZhengQiShuis with injector for medical purpose and scribble nanometer ZrO from import 5 notes of the quartz glass tube 1 of catalytic luminescence sensor 7 to the surface in quartz glass tube 1
2Ceramic heating pipe 2 on;
(1.2) quartz glass tube 1 import of catalytic luminescence sensor 7 is used teflon seal with exporting, heating is carried out the catalytic luminescence reaction to reacting end under 350 ℃; Simultaneously,
(1.3) wavelength of by Weak-luminescence pick-up unit 8, catalytic luminescence sensor 7 being exported is that the electric signal of the light wave of 425nm amplifies, the A/D conversion just obtains HuoXiangZhengQiShui time dependent curve of luminous intensity in the luminescence-producing reaction process, this curve is deposited in the standard diagram that namely gets HuoXiangZhengQiShui in storer.
Select respectively all the other fluid organic material standard items, repeat the standard diagram (referring to Fig. 3) that above-mentioned experimental procedure (1.1)～(1.3) just obtain shuanghuanglian mixture, shuanghuanglian koufuye, Yinqiao detoxification liquid, amino acids oral-liquor, gentamicine sulphate injection, Benzylpenicillin sodium salt parenteral solution, chloramphenicol inj, analgin injection, ceftriaxone inj, Polyinosinic injection, Cefazolin sodium injection and Cefradine parenteral solution.
(2) referring to seeing Fig. 1, the ceramic heating pipe that adopts the surface to scribble nano-MgO is set up the step of standard diagram of fluid organic material standard items as the ceramic heating pipe 2 in catalytic luminescence sensor 7 as described below:
(2.1) scribble on the ceramic heating pipe 2 of nano-MgO to the surface in quartz glass tube 1 with outlet 6 notes of injector for medical purpose absorption 10 μ l HuoXiangZhengQiShuis from the quartz glass tube 1 of catalytic luminescence sensor 7;
(2.2) quartz glass tube 1 import of catalytic luminescence sensor 7 is used teflon seal with exporting, heating is carried out the catalytic luminescence reaction to reacting end under 350 ℃; Simultaneously,
(2.3) wavelength of by Weak-luminescence pick-up unit 8, catalytic luminescence sensor 7 being exported is that the electric signal of the light wave of 425nm amplifies, the A/D conversion just obtains HuoXiangZhengQiShui time dependent curve of luminous intensity in the luminescence-producing reaction process, this curve is deposited in the standard diagram that namely gets HuoXiangZhengQiShui in storer.
Select respectively all the other fluid organic material standard items, repeat the standard diagram (referring to Fig. 4) that above-mentioned experimental procedure (2.1)～(2.3) just obtain shuanghuanglian mixture, shuanghuanglian koufuye, Yinqiao detoxification liquid, amino acids oral-liquor, gentamicine sulphate injection, Benzylpenicillin sodium salt parenteral solution, chloramphenicol inj, analgin injection, ceftriaxone inj, Polyinosinic injection, Cefazolin sodium injection and Cefradine parenteral solution.
(3) referring to seeing Fig. 1, the ceramic heating pipe that adopts the surface to scribble nano-MgO is set up the step of standard diagram of gas organism standard items as the ceramic heating pipe 2 in catalytic luminescence sensor 7 as described below:
(3.1) with injector for medical purpose extract the 1ml ether fume from import 5 notes of the quartz glass tube 1 of catalytic luminescence sensor 7 in quartz glass tube 1;
(3.2) quartz glass tube 1 import of catalytic luminescence sensor 7 is used teflon seal with exporting, heating is carried out the catalytic luminescence reaction to reacting end under 250 ℃; Simultaneously,
(3.3) wavelength of by Weak-luminescence pick-up unit 8, catalytic luminescence sensor 7 being exported is that the electric signal of the light wave of 425nm amplifies, the A/D conversion just obtains ether time dependent curve of luminous intensity in the luminescence-producing reaction process, this curve is deposited in the standard diagram that namely gets ether in storer.
Select respectively all the other fluid organic material standard items, repeat the standard diagram (referring to Fig. 5) that above-mentioned experimental procedure (3.1)～(3.3) just obtain vinyl acetate, acetaldehyde and ethyl acetate.
(4) referring to seeing Fig. 1, adopt the surface to scribble nanometer SrCO
3Ceramic heating pipe set up the step of standard diagram of gas organism standard items as the ceramic heating pipe 2 in catalytic luminescence sensor 7 as described below:
(4.1) with injector for medical purpose extract the 1ml ether fume from import 5 notes of the quartz glass tube 1 of catalytic luminescence sensor 7 in quartz glass tube 1;
(4.2) quartz glass tube 1 import of catalytic luminescence sensor 7 is used teflon seal with exporting, heating is carried out the catalytic luminescence reaction to reacting end under 250 ℃; Simultaneously,
(4.3) wavelength of by Weak-luminescence pick-up unit 8, catalytic luminescence sensor 7 being exported is that the electric signal of the light wave of 425nm amplifies, the A/D conversion just obtains ether time dependent curve of luminous intensity in the luminescence-producing reaction process, this curve is deposited in the standard diagram that namely gets ether in storer.
Select respectively all the other fluid organic material standard items, repeat the standard diagram (referring to Fig. 6) that above-mentioned experimental procedure (4.1)～(4.3) just obtain vinyl acetate, acetaldehyde and ethyl acetate.
Example 3 (organic identification):
The experiment equipment that this example is used is same as Example 2.
(1) the organic identification of gas
Extract 1ml gas A and gas B with injector for medical purpose respectively, obtain the spectrum of gas A by the method that the ceramic heating pipe that adopts the surface to scribble nano-MgO in example 2 is set up the standard diagram of gas organism standard items as the ceramic heating pipe 2 in catalytic luminescence sensor 7, then scribble nanometer SrCO by employing surface in example 2
3The ceramic heating pipe method of setting up the standard diagram of gas organism standard items as the ceramic heating pipe 2 in catalytic luminescence sensor 7 obtain the spectrum of gas B, wherein, the spectrogram of gas A as shown in Figure 7, the spectrogram of gas B is as shown in Figure 8.With each the width trace analysis in Fig. 7 and Fig. 5, spectrum is identical with the standard diagram of acetaldehyde in Fig. 5 as shown in Figure 7, then each the width trace analysis in Fig. 8 and Fig. 6, and spectrum is identical with the standard diagram of ethyl acetate in Fig. 6 as shown in Figure 8.Therefore judgement, gas A is acetaldehyde, gas B is ethyl acetate.
In order to verify the above results, re-use the gas chromatograph that Agilent company produces above-mentioned gas A and gas B are carried out qualitative analysis, result is also, and gas A is acetaldehyde, and gas B is ethyl acetate.
(2) identification of fluid organic material
Draw 10 μ l liquid A and liquid B with injector for medical purpose respectively, then carry out following detection:
(2.1) first by adopting the surface to scribble nanometer ZrO in example 2
2The ceramic heating pipe method of setting up the standard diagram of fluid organic material standard items as the ceramic heating pipe 2 in catalytic luminescence sensor 7 obtain the spectrum of liquid A, the method of setting up the standard diagram of fluid organic material standard items by the ceramic heating pipe that adopts the surface to scribble nano-MgO in example 2 as the ceramic heating pipe 2 in catalytic luminescence sensor 7 is again obtained the spectrum of liquid A, and the spectrogram of the catalytic luminescence sensor gained spectrum of two kinds of different catalysts respectively as shown in Figure 9 and Figure 10.With each the width trace analysis in Fig. 9 and Fig. 3, spectrum is identical with the standard diagram of amino acids oral-liquor in Fig. 3 as shown in Figure 9, then each the width trace analysis in Figure 10 and Fig. 4, and spectrum is identical with the standard diagram of amino acids oral-liquor in Fig. 4 as shown in Figure 10.Therefore judgement, liquid A is amino acids oral-liquor.
(2.2) first by adopting the surface to scribble nanometer ZrO in example 2
2The ceramic heating pipe method of setting up the standard diagram of fluid organic material standard items as the ceramic heating pipe 2 in catalytic luminescence sensor 7 obtain the spectrum of liquid B, the method of setting up the standard diagram of fluid organic material standard items by the ceramic heating pipe that adopts the surface to scribble nano-MgO in example 2 as the ceramic heating pipe 2 in catalytic luminescence sensor 7 is again obtained the spectrum of liquid B, and the spectrogram of the catalytic luminescence sensor gained spectrum of two kinds of different catalysts is respectively as Figure 11 and shown in Figure 12.With each the width trace analysis in Figure 11 and Fig. 3, spectrum is identical with the standard diagram of Benzylpenicillin sodium salt parenteral solution in Fig. 3 as shown in Figure 11, each width trace analysis in Figure 12 and Fig. 4 again, spectrum is identical with the standard diagram of Benzylpenicillin sodium salt parenteral solution in Fig. 4 as shown in Figure 12.Therefore judgement, liquid B is the Benzylpenicillin sodium salt parenteral solution.
(2.3) in order to verify the above results, re-use the gas chromatograph that Agilent company produces aforesaid liquid A and liquid B are carried out qualitative analysis, result is also, and liquid A is amino acids oral-liquor, and liquid B is the Benzylpenicillin sodium salt parenteral solution.
Claims (3)
1. one kind is used the organic method of single catalytic luminescence sensor identification, and the method is comprised of following steps:
(1) set up respectively according to the following steps the standard diagram of each organism standard items:
(1.1) the organism standard items are inserted in quartz glass tube from the import or export of the quartz glass tube of catalytic luminescence sensor;
(1.2) with quartz glass tube import and the exit seal of catalytic luminescence sensor, and heating is carried out catalytic luminescence reaction to reaction and is finished; Simultaneously,
(1.3) wavelength of the catalytic luminescence sensor being exported is that the electric signal of the light wave of 400-490nm amplifies, the A/D conversion just obtains organism standard items time dependent curve of luminous intensity in the luminescence-producing reaction process, this curve is deposited in the standard diagram that namely gets these organism standard items in storer;
(2) obtain according to the following steps the spectrum of organic matter samples to be measured:
(2.1) organic matter samples is inserted in quartz glass tube from the import or export of the quartz glass tube of catalytic luminescence sensor;
(2.2) with quartz glass tube import and the exit seal of catalytic luminescence sensor, and heating is carried out catalytic luminescence reaction to reaction and is finished; Simultaneously,
(2.3) wavelength of the catalytic luminescence sensor being exported is that the electric signal of the light wave of 400-490nm amplifies, the A/D conversion just obtains organism standard items time dependent curve of luminous intensity in the luminescence-producing reaction process, namely gets the spectrum of this organic matter samples;
The standard diagram of each organism standard items that the spectrum of the organic matter samples that (3) step (2) is obtained and step (1) are set up compares one by one, spectrum person identical with standard diagram, the corresponding organism standard items of this standard diagram are organic matter samples to be measured;
Insert the organism standard items in quartz glass tube described in above-mentioned steps (1.1) and step (2.1) in method that organic matter samples is inserted in quartz glass tube be:
When described organism standard items and organic matter samples are gas, adopt syringe to extract described gas and be in the quartz glass tube of 1/5～1/10 injection catalytic luminescence sensor by the volume ratio of described gas and quartz glass inner air tube;
When described organism standard items and organic matter samples are liquid, adopt syringe to draw described liquid and be 1/1000～1/2000 to be injected on the surface of the ceramic electroheating tube that scribbles catalyzer in the quartz glass tube of catalytic luminescence sensor by the volume ratio of described liquid and quartz glass inner air tube;
The temperature of reaction of the catalytic luminescence reaction described in above-mentioned steps (1.2) and (2.2) is:
When described organism standard items and organic matter samples were gas, temperature of reaction was 200～290 ℃;
When described organism standard items and organic matter samples were liquid, temperature of reaction was 300～400 ℃.
2. the single catalytic luminescence sensor of a kind of use according to claim 1 is identified organic method, it is characterized in that, described standard diagram is the standard diagram that uses the same organism standard items that the catalytic luminescence sensor of two or more different catalysts obtains respectively.
3. the organic method of the single catalytic luminescence sensor identification of a kind of use according to claim 1 and 2, is characterized in that, the temperature of reaction of described catalytic luminescence reaction is:
When described organism standard items and organic matter samples were gas, temperature of reaction was 250 ± 10 ℃;
When described organism standard items were liquid, temperature of reaction was 350 ± 10 ℃.
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| CN101571484A (en) * | 2009-06-11 | 2009-11-04 | 刘名扬 | Nano-material surface-catalyzed luminescent micro-sensor |
| CN101858867A (en) * | 2009-04-08 | 2010-10-13 | 清华大学 | Method and sensor for nano material enrichment and in-situ chemical luminescence detection |
| CN102072896A (en) * | 2010-10-29 | 2011-05-25 | 清华大学 | Device and method for identifying protein based on catalyzed light emission on surface of nano material |
| CN102175667A (en) * | 2010-12-26 | 2011-09-07 | 广州大学 | Nanometer material for detecting acrolein gas, and preparation method and application thereof |
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| CN101858867A (en) * | 2009-04-08 | 2010-10-13 | 清华大学 | Method and sensor for nano material enrichment and in-situ chemical luminescence detection |
| CN101571484A (en) * | 2009-06-11 | 2009-11-04 | 刘名扬 | Nano-material surface-catalyzed luminescent micro-sensor |
| CN102072896A (en) * | 2010-10-29 | 2011-05-25 | 清华大学 | Device and method for identifying protein based on catalyzed light emission on surface of nano material |
| CN102175667A (en) * | 2010-12-26 | 2011-09-07 | 广州大学 | Nanometer material for detecting acrolein gas, and preparation method and application thereof |
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