CN102866224B - Gas chromatographic detection method for determining carbon-containing compound based on carbon atomic emission spectroscopy - Google Patents
Gas chromatographic detection method for determining carbon-containing compound based on carbon atomic emission spectroscopy Download PDFInfo
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- CN102866224B CN102866224B CN201210344012.7A CN201210344012A CN102866224B CN 102866224 B CN102866224 B CN 102866224B CN 201210344012 A CN201210344012 A CN 201210344012A CN 102866224 B CN102866224 B CN 102866224B
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Abstract
The invention discloses a gas chromatographic detection method for determining a carbon-containing compound based on carbon atomic emission spectroscopy. A dielectric barrier discharge (DBD) device is used as an atomizer and an excitation source of a carbon element in the carbon-containing compound, 193.0nm is selected as a detection wavelength, a charge-coupled device is used for quantitative detection, and detection sensitivity is improved by adopting an auxiliary heating method. The method has the characteristics of high selectivity, high analysis speed, high stability and the like for the detection of the carbon element.
Description
Technical field
The invention belongs to gas chromatographic detection new technology in analytical chemistry, relate to a kind of gas-chromatography detection method carbon to high selectivity.
Background technology
In gas chromatograph, detecting device is the important composition parts of detection method.At present, tens kinds of known gas chromatography detectors, wherein modal thermal conductivity detector (TCD) (TCD), flame ionization ditector (FID), nitrogen phosphorous detector (NPD), electron capture detector (ECD), the flame photometric detector (FPD) (FPD) etc. of comprising.These detecting devices are used as different gas-chromatography detection methods because of its different detection principles.TCD has the principle of different thermal conductivities based on difference analysis component and carrier gas, be a kind of general non-destructive concentration detector, can be applicable in theory the detection of any component, but sensitivity is lower; FID is based on detecting object at hydrogen flame intermediate ion, and the ion of generation is mobile under electric field action to be formed ion current and be detected, and it detects target is combustible organism, but for aphlogistic objects such as carbon dioxide without responding; NPD is for measuring nitrogenous and phosphorous organic compound, and ECD is for analyzing the large compound of some electronegativity such as halogen compounds, palycyclic aromatic, and FPD is mainly used in measuring sulfur-bearing, phosphorus-containing compound.At present, not yet there is pair carbon to there is optionally gas-chromatography detection method report.
Dielectric barrier discharge (Dielectric Barrier Discharge, DBD) is to have insulating medium to insert a kind of nonequilibrium state gas discharge of discharge space.DBD has many good qualities, and comprises that working temperature is low, energy consumption is little, apparatus structure is simple, can under atmospheric pressure work etc.At present, DBD is widely used in surface modification and pollutant processing etc. industrial.In analytical chemistry, DBD has been used as atomizer and ion gun.As, the people such as Miclea are using DBD as atomizer, for laser atomic absorption spectrum (Miclea, M.; Kunze, K.; Musa, G.; Franzke, J.; Niemax, K.Spectrochim.Acta Part B, 2001,56,37-43); Patent (ZL-200510086518.2) has designed a kind of atomizer based on DBD, can be used for producing the atomization of the elements such as the arsenic, selenium, tin, antimony of hydride; Patent (ZL-200610011548.1) has designed a kind of chemical ioning method and mass ion source based on DBD, can detect for organism with mass detector coupling.DBD also has report in the literature as the detection method of gas chromatography, and the laser Atomic Absorption Spectrometer based on DBD is used as gas chromatography detector by the people such as Kunze, for detection (Kunze, the K. of halogen-containing analyte gas; Miclea, M.; Franzke, J.; Niemax, K.Spectrochim.Acta Part B, 2003,58,1435-1443); The people such as Li find that DBD can excite the molecular emission spectrometry of halogenated hydrocarbons, and detect halogenated hydrocarbons (Li, W. used as the detecting device of gas chromatography; Zheng, C.; Fan, G.; Tang, L.; Xu, K.; Lv, Y.; Hou, X.Anal.Chem.2011,83,5050-5055).DBD device as atomizer only for easy atomizing element, as elements such as mercury, arsenic, selenium, tin, antimony; Can only excite for organism the molecular emission spectrometry that its energy requirement is lower, as halogenated hydrocarbons; Do not have DBD for exciting the report of carbon atomic emission spectrum at present.
Summary of the invention
The object of the invention is to adopt the auxiliary DBD plasma exciatiaon carbon atom emission spectrum of heating, and developed into carbon is had to high selectivity, high stability and highly sensitive gas-chromatography detection method, for the gas chromatographic detection of carbon compound.
Technical scheme
The present invention using dielectric barrier discharge device as carbon compound in atomizer and the excitaton source of carbon, detecting device using charge-coupled image sensor as carbon atom emission spectrum, dielectric barrier discharge device adopts hollow quartz ampoule as insulating medium, be wound around copper wire as external electrode in quartz ampoule outside, the inner copper wire that inserts is as interior electrode, heated for controlling temperature equipment is installed on the quartz ampoule of dielectric barrier discharge device, pass into argon gas as discharge gas, use transformer to regulate the voltage of internal and external electrode, using carbon compound as detecting thing, select the specific atoms emission line of 193.0nm carbon quantitatively to detect, its detecting step is:
(1) sample enters from gas chromatograph injection port, after separating, enters into dielectric barrier discharge device from discharge gas import;
(2) dielectric barrier discharge device internal and external electrode Control of Voltage is at 1.84～3.25kV;
Discharge gas argon gas through discharge gas mouth with 300～900mL min
-1enter;
(4) by controlling the voltage of electrical heating wire, control medium discharge-blocking device temperature is 25～300 DEG C;
(5) sample enters after the dielectric barrier discharge device of heating, produces the free atom of carbon in dielectric barrier discharge plasma Atomization;
(6) the free atom of carbon excites through dielectric barrier discharge plasma, produces the characteristic atomic spectral line of emission of the 193.0nm of carbon, detects through charge-coupled image sensor, realizes the quantitative test of carbon compound.
Gas chromatography detector based on dielectric barrier discharge of the present invention, as shown in Figure 1, its structure is made up of dielectric barrier discharge plasma excitation apparatus, heating and temperature controlling device, optical detection apparatus.
Carbon compound of the present invention, refers to the carbon compound that can gasify in gas chromatography.The optimum temperature of dielectric barrier discharge device is 200～300 DEG C, and the inside and outside optimum electrode voltage of dielectric barrier discharge device is 2.54～3.25kV, and best argon gas flow velocity is 300～600mL min
-1.
Invention effect
The present invention, compared with existing gas-chromatography detection method, mainly contains following characteristics/advantage: (1) adopts DBD plasma device to excite and obtains carbon atom emission spectrum; (2) DBD plasma device is heated and assisted, improve the stability of detection method, and strengthen the sensitivity of its detection; (3) select 193.0nm carbon specific atoms emission line, disturb less, highly sensitive; (4) analyze quick, easy; (5) detection method only needs argon gas as discharge gas, and argon gas consumption is little, environmental protection; (6) measurement range is wide, is applicable to organic and inorganic carbon compound.
Brief description of the drawings
The gas chromatographic detection device schematic diagram of Fig. 1 heats auxiliary-DBD plasma-atomic emission spectrum.1: copper external electrode; 2: copper inner electrode; 3: sealing plug; 4: quartz ampoule; 5: discharge gas import; 6: heating and temperature controlling device; 7: charge-coupled detector(CCD); 8: discharge gas outlet.Wherein, the length of quartz ampoule 4 is 50mm, and internal diameter is 3.0mm, and external diameter is 5.0mm; The copper wire for outside (diameter is 1.0mm) of quartz ampoule is closely wound around one section of about 25mm as copper external electrode 1; Insert a copper wire (diameter is 1.5mm, and length is 30mm) in inside as copper inner electrode 2; In the left side of quartz ampoule with high temperature resistant silica gel as sealing plug 3; Quartz ampoule left and right two ends 7.5mm respectively has a leg respectively as discharge gas entrance 5 and outlet 8, also uses high temperature resistant silica gel as sealing plug 3 simultaneously; Heating and temperature controlling device 6, comprises resistance heater, temperature controller, by the Control of Voltage heating-up temperature of regulating resistance silk heating arrangement; Be sealing plug 3 at the right-hand member of quartz ampoule, ensure that the characteristic emission spectrum of detection object is successfully collected, in quartz ampoule, material does not pollute charge-coupled detector(CCD) 7 simultaneously; Detect the atomic emission line of carbon in object by charge-coupled detector(CCD) 7 records.
Fig. 2 this method is the atomic emissions spectrogram at 193.0nm place for carbon compound and Non-carbonized compound.In figure, horizontal ordinate is wavelength, and unit is nm; Ordinate is signal response intensity; 15 kinds of materials are respectively: 1, blank, 2, hydrogen peroxide, 3, water, 4, ammoniacal liquor, 5, carbon dioxide, 6, methane, 7, formaldehyde, 8, methyl alcohol, 9, ether, 10, acetonitrile, 11, acetone, 12, normal butyl alcohol, 13, ethyl acetate, 14, normal hexane, 15, tert-butylamine.
The impact of sparking voltage on 7 kinds of carbon compound sensitivity in Fig. 3 this method.Condition of work is: sampling volume: 1 μ L, argon gas flow velocity: 300mL min
-1, heating-up temperature: 300 DEG C.In figure, horizontal ordinate is sparking voltage, and unit is kV; Ordinate is peak area; 7 kinds of materials are respectively: 1, formaldehyde, 2, ethyl acetate, 3, methyl alcohol, 4, ethanol, 5, n-propanol, 6, normal butyl alcohol, 7, n-amyl alcohol.
The impact of argon gas flow velocity on 7 kinds of carbon compound sensitivity in Fig. 4 this method.Condition of work is: sampling volume: 1 μ L, sparking voltage: 2.95kV, heating-up temperature: 300 DEG C.In figure, horizontal ordinate is argon gas flow velocity, and unit is mL min
-1; Ordinate is peak area; 7 kinds of materials are respectively: 1, formaldehyde, 2, ethyl acetate, 3, methyl alcohol, 4, ethanol, 5, n-propanol, 6, normal butyl alcohol, 7, n-amyl alcohol.
The impact of heating-up temperature on 7 kinds of carbon compound sensitivity in Fig. 5 this method.Condition of work is: sampling volume: 1 μ L, sparking voltage: 2.95kV, argon gas flow velocity: 300mL min
-1.In figure, horizontal ordinate is temperature, and unit is DEG C; Ordinate is peak area; 7 kinds of materials are respectively: 1, formaldehyde, 2, ethyl acetate, 3, methyl alcohol, 4, ethanol, 5, n-propanol, 6, normal butyl alcohol, 7, n-amyl alcohol.
Fig. 6 this method is measured the standard model of 4 kinds of liquid carbon-containing components and the gas chromatogram of beer sample in beer.In figure, horizontal ordinate is retention time, and unit is second; Ordinate is signal response intensity; Figure A is standard model, and figure B is beer sample; 4 kinds of components are respectively: 1, and formaldehyde; 2, ethyl acetate; 3, methyl alcohol; 4, ethanol.
Fig. 7 this method is measured the gas chromatogram of 3 kinds of gas carbonaceous component standard models.In figure, horizontal ordinate is retention time, and unit is second; Ordinate is signal response intensity; 3 kinds of components are respectively: 1, CO; 2, CH
4; 3, CO
2.
Embodiment
Embodiment mono-:
The present embodiment is selected common various volatile organic and inorganic carbon compound sample, detect the carbon characteristic atomic spectral line of emission that is positioned at 193.0nm place that it produces after DBD, and by contrasting with the non-carbon compound sample such as ammoniacal liquor, water and hydrogen peroxide, confirm the detectability of the present invention to carbon compound.Concrete operation steps is: (1) sample enters from gas chromatograph injection port, after separating, enters into DBD device from discharge gas import; (2) DBD device internal and external electrode Control of Voltage is at 2.95kV; Discharge gas argon gas through discharge gas mouth with 400mL min
-1enter; (4) by controlling the voltage of electrical heating wire, controlling DBD unit temp is 300 DEG C; (5) sample enters after the DBD device of heating, produces the free atom of carbon in DBD plasma Atomization; (6) the free atom of carbon, through DBD plasma exciatiaon, produces the characteristic atomic spectral line of emission of the 193.0nm of carbon, detects through charge-coupled image sensor, realizes the quantitative test of carbon compound.The various carbon compounds of analyzing comprise tert-butylamine, normal hexane, ethyl acetate, normal butyl alcohol, acetone, acetonitrile, ether, methyl alcohol, formaldehyde, methane and carbon dioxide etc., and its atomic emission line under 193.0nm is shown in accompanying drawing 2.
Embodiment bis-:
The present embodiment is investigated the impact of internal and external electrode voltage on carbon compound detection sensitivity in DBD device.With reference to the operation steps of embodiment mono-, taking formaldehyde, ethyl acetate, methyl alcohol, ethanol, n-propanol, normal butyl alcohol and n-amyl alcohol as tested object, the test specification of internal and external electrode voltage is 1.84～3.25kV.The experimental result of the present embodiment is shown in accompanying drawing 3, determines that thus best exciting voltage of the present invention is 2.54～3.25kV.
Embodiment tri-:
The present embodiment is investigated the impact of discharge gas argon gas flow velocity on carbon compound detection sensitivity in DBD device.With reference to the operation steps of embodiment mono-, taking formaldehyde, ethyl acetate, methyl alcohol, ethanol, n-propanol, normal butyl alcohol and n-amyl alcohol as tested object, the test specification of argon gas flow velocity is 300～900mL min
-1.The experimental result of the present embodiment is shown in accompanying drawing 4, determines that thus best argon gas flow velocity of the present invention is 300～600mL min
-1.
Embodiment tetra-:
The impact of the temperature of heating and temperature controlling device on carbon compound detection sensitivity in the present embodiment investigation DBD device.With reference to the operation steps of embodiment mono-, taking formaldehyde, ethyl acetate, methyl alcohol, ethanol, n-propanol, normal butyl alcohol and n-amyl alcohol as tested object, the test specification of DBD unit temp is 25～300 DEG C.The experimental result of the present embodiment is shown in accompanying drawing 5, determines that thus optimum working temperature of the present invention is 200～300 DEG C.
Embodiment five:
The content of low-carbon (LC) aldehydes, ester class and alcohols material is one of important indicator of evaluating drinks sample quality.The present embodiment is analyzed the liquid component of carbon containing in beer sample, and the analyte of selection comprises formaldehyde, ethyl acetate, methyl alcohol and ethanol.Sample is from gas chromatograph sampling, and sampling volume is 0.02 μ L; The exciting voltage of internal and external electrode is 2.95kV, and the flow velocity of discharge gas argon gas is 400mL min
-1, regulating the temperature of heating arrangement is 300 DEG C.This method is successfully applied to the mensuration of formaldehyde, ethyl acetate, methyl alcohol and ethanol in beer class sample, and the chromatogram of standard model and beer sample is shown in accompanying drawing 6.Wherein the index such as the relative standard deviation of 4 kinds of carbon compounds (RSD) and detection limit (LOD) is in table 1.
Table 1 this method is measured the detection limit of 4 kinds of carbon compounds
Embodiment six:
The quantitative detection of carbonaceous gas is the major issue facing in analytical work, relates to the aspects such as oil gas, garbage disposal, chemical catalysis, organic synthesis.The present embodiment is analyzed the gaseous sample of carbon containing, and the analyte of selection comprises CO
2, CH
4and CO.Sample is from gas chromatograph sampling, and sampling volume is 0.50mL; The exciting voltage of internal and external electrode is 2.95kV, and the flow velocity of discharge gas argon gas is 400mL min
-1, regulating the temperature of heating arrangement is 300 DEG C.This method is successfully applied to CO
2, CH
4with the detection of CO3 kind mixed gas, the chromatogram of its detected components standard substance is shown in accompanying drawing 7.Wherein the index such as the relative standard deviation of 3 kinds of gas carbon compounds (RSD) and detection limit (LOD) is in table 2.
Table 2 this method is measured the detection limit of 3 kinds of carbon compounds
Claims (4)
1. the gas-chromatography detection method based on carbon atom emission spectrometry carbon compound, atomizer and the excitaton source of carbon in it is characterized in that using dielectric barrier discharge device as carbon compound, dielectric barrier discharge device adopts hollow quartz ampoule as insulating medium, be wound around copper wire as external electrode in quartz ampoule outside, the inner copper wire that inserts is as interior electrode, heated for controlling temperature equipment is installed on the quartz ampoule of dielectric barrier discharge device, pass into argon gas as discharge gas, use transformer to regulate the voltage of internal and external electrode; Detecting device using charge-coupled image sensor as carbon atom emission spectrum, using carbon compound as detecting thing, selects the specific atoms emission line of 193.0 nm carbon quantitatively to detect, and its detecting step is:
(1) sample enters from gas chromatograph injection port, after separating, enters into dielectric barrier discharge device from discharge gas import;
(2) dielectric barrier discharge device internal and external electrode Control of Voltage is at 1.84 ~ 3.25 kV;
(3) discharge gas argon gas through discharge gas mouth with 300 ~ 900 mL min
-1enter;
(4) by controlling the voltage of electrical heating wire, regulating dielectric barrier discharge unit temp is 25 ~ 300 DEG C;
(5) sample enters after the dielectric barrier discharge device of heating, produces the free atom of carbon in dielectric barrier discharge plasma Atomization;
(6) free atom of carbon excites through dielectric barrier discharge plasma, produces the characteristic atomic spectral line of emission of 193.0 nm of carbon, detects through charge-coupled image sensor, realizes the quantitative test of carbon compound.
2. the internal and external electrode voltage that in accordance with the method for claim 1, it is characterized in that dielectric barrier discharge device is 2.54 ~ 3.25 kV.
3. in accordance with the method for claim 1, it is characterized in that argon gas flow velocity is 300 ~ 600 mL min
-1.
4. the temperature that in accordance with the method for claim 1, it is characterized in that dielectric barrier discharge device is 200 ~ 300 DEG C.
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| CN110146487B (en) * | 2019-06-11 | 2022-01-04 | 中国热带农业科学院分析测试中心 | In-situ determination of total SO in food2Method (2) |
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