CN101713762A - Method for identifying and detecting halogenated hydrocarbons - Google Patents
Method for identifying and detecting halogenated hydrocarbons Download PDFInfo
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- CN101713762A CN101713762A CN200810013549A CN200810013549A CN101713762A CN 101713762 A CN101713762 A CN 101713762A CN 200810013549 A CN200810013549 A CN 200810013549A CN 200810013549 A CN200810013549 A CN 200810013549A CN 101713762 A CN101713762 A CN 101713762A
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Abstract
The invention relates to a method for identifying and detecting halogenated hydrocarbons, which is characterized by using vacuum ultraviolet as the ionization source of ion mobility spectrometry, adopting the mode of positive-negative ion switching, adopting the principle of photo ionization in the positive ion mode and adopting the principle of photo-electric reflection in the negative ion mode. Being used for detecting halogenated hydrocarbons, the method can widen the type of the compounds measured by the ion mobility spectrometry, greatly improve the capabilities of the ion mobility spectrometry in rapidly identifying and analyzing the samples and simultaneously improve the sensitivity of the ion mobility spectrometry to the compounds with ionization energy lower than that of the vacuum ultraviolet in the negative ion mode.
Description
Technical field
The invention belongs to the analysis of halogenated hydrocarbon compound, specially refer to a kind of new method that halogenated hydrocarbon compound is discerned and detected, this method can be widened the classes of compounds that ion mobility spectrometry is measured, greatly improve quick identification and the analytic ability of ion mobility spectrometry, the sensitivity that improves ion mobility spectrometry simultaneously to sample.
Background technology
The alkyl halide compounds is a ubiquitous volatile organic contaminant in the urban atmosphere as phenixin, triclene and zellon, also is the object of numerous scholar's research.They mainly discharge from mankind's activity, as the raw material of industry, solvent, extractant and clean-out system etc., have emission source widely in the city.Triclene (Trichloroethylene for example, write a Chinese character in simplified form TCE) be a kind of fine solvent, it also is the substitute of benzene and gasoline, can be used as metal cleaner, electroplate the preceding detersive of paint, the degreasing agent of metal, the extractant of fat, oil, paraffin wax, agricultural chemical insecticide, and medicine and organic chemical industry's raw material; And zellon (tetrachIoroethyIene; PerchIoroethyIene writes a Chinese character in simplified form PCE) then mainly as the dry cleaning agent of fabric, also as degreasing washing agent, drying agent, paint stripper, pest repellant and the common solvent of metal, organic synthesis intermediate etc.The extensive use of halogenated hydrocarbon compound such as TCE and PCE has made them become pollutant common in workshop, workshop, surface water and the underground water, and wherein triclene belongs to the property accumulated anesthetic, and central nervous system is had the strong inhibition effect; Though the toxicity of zellon is little than triclene, nervous centralis, lung, skin, digestive system, liver and kidney etc. to human body after its steam suction contacts with skin damage.And halogenated hydrocarbons has crucial influence to the atmospheric envelope chemistry, particularly to the consumption of stratospheric ozone, reaches 40 years as the life-span of phenixin in atmospheric envelope, is to consume the ozone controlled substance.Therefore, the 129 kinds of priority pollutants that they are put into all that American National Environmental Protection Agency 1976 announces and " blacklist " of China's environmental characteristic pollutant, halogenated hydrocarbon compound must cause people's great attention to the harm that environment caused, and efficiently apace they is detected and discern extremely urgent.
The method of traditional detection halogenated hydrocarbons mainly is the gas chromatographic detection method.This traditional detection method needs loaded down with trivial details sample collecting and pre-treatment program, wastes time and energy, and can not be implemented in line analysis, and detection sensitivity not high enough (ppm magnitude).In the last few years, ion mobility spectrometry was because advantage such as its high sensitivity, express-analysis, portability and be used to the on-line analysis of industry and environment more and more.Eighties of last century seventies, scientists just is used for ion mobility spectrometry the detection of hydrocarbons.Because it is the electron affinity of halogenated hydrocarbon material is than higher, and the proton affinity is lower, therefore traditional
63The Ni ion mobility spectrometry all is to measure halogenated hydrocarbons under negative ion mode.But the mobility ratio at the mobility of halogenated hydrocarbons and reagent ion peak is more approaching, and all only occurs the migration spectrum peak of halide ion in the migration spectrogram of most halogenated hydrocarbon material, so all cpds is difficult to well be separated and detects.
Here the applicant proposes a kind of new method that halogenated hydrocarbon compound is discerned and detected, this method utilizes ultraviolet source to be equipped with wire netting or becket as ionization source, mix the positive and negative ion handover control system of external circuit, can under two kinds of patterns of positive and negative ion, detect halogenated hydrocarbons, widen the classes of compounds that ion mobility spectrometry is measured, greatly improve quick identification and the analytic ability of ion mobility spectrometry, improve ion mobility spectrometry is lower than the compound of ultraviolet light ionization energy to those ionization energy under negative ion mode sensitivity simultaneously sample.
Summary of the invention
The purpose of this invention is to provide a kind of new method that halogenated hydrocarbon compound is discerned and detected.The present invention utilizes ultraviolet source to be equipped with wire netting or the becket ionization source as ion mobility spectrometry, the pattern that adopts negative ions to switch, and positive ion mode utilizes the principle of photoionization, and negative ion mode utilizes the principle of photoelectric reflection.This method is used for the detection of halogenated hydrocarbon compound, can widen the classes of compounds that ion mobility spectrometry is measured, greatly improve quick identification and the analytic ability of ion mobility spectrometry, improve the detection sensitivity of ion mobility spectrometry simultaneously some compound to sample.
For achieving the above object, technical scheme of the present invention is as follows:
A kind of identification and the method that detects halogenated hydrocarbon compound is characterized in that:
It utilizes ultraviolet source to be equipped with wire netting or becket as ionization source, and described wire netting or becket place in the zone that ultraviolet light shone that ultraviolet source sends, and ionization source can be used in migration spectrum or the mass spectrum;
On the high and low pressure connection terminal of the connection terminal of migration tube or tof tube and ultraviolet source, apply positive and negative high pressure, the positive-negative polarity of the connection terminal by adjusting migration tube or tof tube and ultraviolet source, realized the detection of positive ion mode or negative ion mode, thereby widen the kind of ion mobility spectrometry or mass-spectrometer measurement compound, greatly improve ion mobility spectrometry or mass spectrum quick identification and analytic ability sample.
Described migration tube or tof tube can be respectively more than 1 or 1,
When migration tube or tof tube are respectively 1, be equipped with the detection that the positive and negative ion handover control system is realized positive and negative ion with a migration tube or tof tube;
When migration tube or tof tube are respectively 1 when above, on different migration tubes or tof tube respectively with addition of ionization source, the positive-negative polarity of the connection terminal by adjusting different migration tubes or tof tube and ultraviolet source, thus realize the detection of positive ion mode or negative ion mode.
Described positive and negative ion handover control system is made up of the conventional positive and negative commutation circuit of series connection on the direct supply, and the positive and negative ion handover control system links to each other with the high and low pressure connection terminal of ultraviolet source and the connection terminal of migration tube or tof tube by lead respectively.
When migration tube or tof tube are respectively 1 when above, on different migration tubes or tof tube with addition of different ionization sources, form different test set, and the test set that each migration tube or tof tube and ionization source form is mixed the positive and negative ion handover control system of an external circuit respectively, can realize the detection of positive and negative ion pattern between different test set simultaneously.
Described ultraviolet source is the equipment that vacuum UV lamp, diode, xenon lamp, mercury lamp or ultraviolet laser etc. can produce ultraviolet light; The material of metal grid mesh or becket is metal and the alloys of various electron work functons less than ultraviolet source ionization energy.
The external diameter of described metal grid mesh is more than or equal to the aperture of ultraviolet light; The internal diameter of becket is equal to or less than the aperture of ultraviolet light; The distance of metal grid mesh or becket and ultraviolet source is 0～L, and L is the light path of ultraviolet light, and the more little effect of distance is good more.
Ionization source and ion mobility spectrometry coupling that described ultraviolet source, wire netting or becket are formed are formed ultraviolet light photo when the source ion migration is composed, and it mainly comprises following components usually: ionization source, reaction zone, ion gate, migration tube, signals collecting and disposal system and positive and negative ion handover control system; Its process that is used for detecting halogenated hydrocarbons is: the ion gate that the sample ions that ionization obtains under the ionization source positive and negative ion pattern is opened by pulse enters migration tube, difference according to its mobility in migration tube obtains separating, enter Faraday cylinder at last, received and detection system reception and detection by signal.
Advantage of the present invention:
Ultraviolet source is equipped with wire netting or the becket ionization source as ion mobility spectrometry, the pattern that adopts negative ions to switch is measured halogenated hydrocarbons, can widen the classes of compounds that ion mobility spectrometry is measured, greatly improve quick identification and the analytic ability of ion mobility spectrometry, improve the detection sensitivity that ion mobility spectrometry does not have some compound simultaneously sample.
Compare with traditional gas chromatography, this method need not loaded down with trivial details sample pre-treatments program, detection speed fast (tens ms), and sensitivity higher (several to dozens of ppb), the instrument volume is small and exquisite, can realize the real-time online analysis; Compare with the radioactive source ion mobility spectrometry, this method can avoid using radioactive source, just, negative ion mode all can detect down, just can access it for ionization energy less than the compound of ultraviolet light, migration spectrogram under the negative ion mode, then only can obtain migration spectrogram under its negative ion mode for ionization energy greater than the compound of ultraviolet light, thereby improved quick identification and the analytic ability of migration spectrum to sample, simultaneously for the compound of ionization energy less than used ultraviolet light ionization energy, the photoionization reaction also can take place at negative ion mode in it, the a large amount of electronics that obtains also can react with determinand, thereby has improved the detection sensitivity of ion mobility spectrometry to these compounds greatly.
Description of drawings
The present invention is further detailed explanation below in conjunction with drawings and Examples:
Fig. 1 is a ultraviolet light ionization source positive and negative ion measured ion migration simultaneously spectrum synoptic diagram.
Fig. 2 is a positive and negative ion handover control system circuit theory synoptic diagram.
Fig. 3 is the migration spectrogram under the TCE positive and negative ion pattern.
Fig. 4 is CCl
4Detection spectrogram under the negative ion mode.
Embodiment
In order to realize that halogenated hydrocarbon compound is carried out quick identification and detection, the present invention's ionization source of ultraviolet source as ion mobility spectrometry.Ionization source structure as shown in the figure, it mainly comprises following components: ultraviolet source 1, becket (2a) or metal grid mesh (2b) and support column 3.Ultraviolet source can be the equipment that vacuum UV lamp, diode, xenon lamp, ultraviolet laser etc. can produce ultraviolet light, is example here with the vacuum UV lamp; The material of metal grid mesh or becket is mainly metal and the alloy of various electron work functons less than ultraviolet source ionization energy, as gold, silver, stainless steel etc., the internal diameter of becket is equal to or slightly less than the diameter of ultraviolet aperture, and the external diameter of metal grid mesh is more than or equal to the diameter of ultraviolet aperture; Support column uses nonmetallic materials, as processable ceramic, teflon etc.Metal grid mesh or becket are placed between vacuum UV lamp and the support column, are close to light source.
Under the positive ion mode, vacuum-ultraviolet light irradiation sample, the sample that ionization energy is littler than the ionization energy of ultraviolet light (as triclene, zellon, trichloro-benzenes etc.) can absorb photon, and the photoionization reaction shown in equation 1 takes place, and makes sample obtain ionization;
M+hv→M
++e (1)
Under the negative ion mode, the vacuum ultraviolet light radioglold belongs to the interior ring of aperture plate or becket, produces photoelectric effect, launches photoelectron.Photoelectron can and example reaction, make sample ionization; Photoelectron also can obtain reagent ion CO by a series of reaction with carrier gas simultaneously
3 -(H
2O)
n, CO
3 -(H
2O)
nCan reaction shown in equation 2 take place with halogenated hydrocarbon compound M, make compound obtain ionization.
CO
3 -(H
2O)
n+M→M
-+CO
2+nH
2O+(1/2)O
2 (2)
Simultaneously for the compound of those ionization energy less than ultraviolet light, the reaction that it also can take place under negative ion mode shown in equation 1 obtains a large amount of electronics, these electronics also can and example reaction, make sample obtain ionization, thereby improve the detection sensitivity of compound greatly.
During work, triclene, these ionization energy of zellon all can be ionized under the positive and negative ion pattern less than the material of ultraviolet light, obtain it and detect spectrogram, and for phenixin, these ionization energy of methenyl choloride material greater than ultraviolet light, it only can be ionized under negative ion mode, obtain its negative ion migration spectrogram, thereby realize separating and identification of triclene, zellon and phenixin, methenyl choloride, also solved the interference that these compounds of phenixin detect triclene simultaneously; In addition, photoionization also can take place in triclene and zellon under negative ion mode, thereby produces a large amount of photoelectrons, and photoelectron reacts with triclene or zellon again, make their ionization, thereby improved the detection sensitivity of ion mobility spectrometry greatly these compounds.
With ultraviolet light ionization source recited above and conventional ion mobility spectrometry coupling, ionization source as ion mobility spectrometry, be equipped with by on the direct supply with addition of the positive and negative ion commutation circuit of forming by the positive and negative commutation circuit of routine, form ultraviolet light photo from source ion migration spectrum, its structure as shown in Figure 1, this instrument mainly comprises following components: ultraviolet source 1, metal grid mesh or becket 2, support column 3, reaction zone 4, ion gate 5, migration tube 6, sample carrier gas 7, make-up gas? 8, signal receive and detection system 9 and positive and negative ion control switching circuit 15; Wherein: 10 is Faraday cylinder, and 11 is amplifier, and 12 is A/D converter, and 13 is pressurized air, and 14 is data handling system (as oscillograph).The concrete principle schematic of positive and negative ion control switching circuit 15 as shown in Figure 2, it mainly contains high pressure independent current source 16, high- voltage relay 19,20,21,22 and high- voltage output end 17 and 18 and forms.When high- voltage relay 19 and 22 conductings, high-voltage output end 17 output positive high voltages, and when high- voltage relay 20 and 21 conductings, high-voltage output end 18 is exported positive high voltages, thus realized the switching of the positive and negative polarity of circuit.
Utilize this ultraviolet light photo to detect halogenated hydrocarbon compound from source ion migration spectrum, the process of test sample is: just/and ion gate that the sample ions that obtains under the negative ion mode is opened by pulse enters the migration area, difference according to its mobility in the migration area obtains separating, enter Faraday cylinder at last, received and detection system reception and detection by signal.
Fig. 2-3 has provided some experiment spectrograms the present invention has been given and explanation.Except special proposition, the experiment condition of these spectrograms is: migration tube length is 11.0cm, migration electric field intensity is 216V/cm, the ion gate time of opening the door is 0.2ms, cycle is 40ms, float gas and sample carrier gas and be the pressurized air of handling through silica gel, activated charcoal and molecular sieve, wherein moisture content is lower than 10ppm.Float gas velocity 600sccm, flow rate of carrier gas 400sccm, experimental temperature remains on room temperature, places a copper ring between vacuum UV lamp and the support column, and the copper ring internal diameter is 6mm, and thickness is 0.2mm.
Fig. 2 has provided the detection spectrogram under the TCE positive and negative ion pattern.RIP represents the reagent ion peak among the figure, here is CO
3 -(H
2O)
nAs can be seen from the figure, TCE all can well be detected under the positive and negative ion pattern.Under positive ion mode, it has four characteristic peaks, and its transit time is respectively 18.49ms, 19.69ms, 20.63ms and 23.33ms, and under negative ion mode, it is except having Cl
-Characteristic peak (18.61ms) outside, it also has its oneself characteristic peak, transit time is 22.50ms, thereby can well separate with the reagent ion peak.
That Fig. 3 provides is CCl
4Detection spectrogram under the negative ion mode.As can be seen from the figure, CCl
4Under negative ion mode, has Cl
-Characteristic peak (18.69ms).Because CCl
4Ionization energy greater than the ionization energy of ultraviolet light, its under positive ion mode, can not be ionized can, can not get its spectrogram.Like this, it distinguishes with regard to energy and TCE, also can eliminate it simultaneously to detecting the interference of TCE.
Its experiment condition is identical with above-mentioned Fig. 2-3 experiment experiment condition that spectrogram adopted; Record the detection that this ultraviolet light photo is composed phenixin from the source ion migration under negative ion mode in the experiment and be limited to 4.3 * 10
-9G is limited to 5.0 * 10 to the detection of zellon
-11G, thereby as can be seen because the ionization energy of phenixin, zellon is 11.47eV and 9.326eV, the former is than ionization energy (10.6eV) height of ultraviolet light, the latter is lower than the ionization energy of ultraviolet light, therefore photoionization can not take place in phenixin, photoionization then can take place in zellon, produces a large amount of electronics, thereby improves the detection sensitivity of ion mobility spectrometry to it greatly.
Claims (7)
1. identification and the method that detects halogenated hydrocarbon compound is characterized in that:
It utilizes ultraviolet source to be equipped with wire netting or becket as ionization source, and described wire netting or becket place in the zone that ultraviolet light shone that ultraviolet source sends, and ionization source can be used in migration spectrum or the mass spectrum;
On the high and low pressure connection terminal of the connection terminal of migration tube or tof tube and ultraviolet source, apply positive and negative high pressure, the positive-negative polarity of the connection terminal by adjusting migration tube or tof tube and ultraviolet source, realized the detection of positive ion mode or negative ion mode, thereby widen the kind of ion mobility spectrometry or mass-spectrometer measurement compound, greatly improve ion mobility spectrometry or mass spectrum quick identification and analytic ability sample;
Utilize the principle of photoionization to make sample ionization under the described ionization source positive ion mode, next photoemission and the photochemically reactive principle utilized of negative ion mode makes sample ionization.
2. method according to claim 1 is characterized in that: described migration tube or tof tube can be respectively more than 1 or 1,
When migration tube or tof tube are respectively 1, be equipped with the detection that the positive and negative ion handover control system is realized positive and negative ion with a migration tube or tof tube;
When migration tube or tof tube are respectively 1 when above, on different migration tubes or tof tube respectively with addition of ionization source, the positive-negative polarity of the connection terminal by adjusting different migration tubes or tof tube and ultraviolet source, thus realize the detection of positive ion mode or negative ion mode.
3. method according to claim 2, it is characterized in that: described positive and negative ion handover control system is made up of the conventional positive and negative commutation circuit of series connection on the direct supply, and the positive and negative ion handover control system links to each other with the high and low pressure connection terminal of ultraviolet source and the connection terminal of migration tube or tof tube by lead respectively.
4. method according to claim 2, it is characterized in that: when migration tube or tof tube are respectively 1 when above, on different migration tubes or tof tube with addition of different ionization sources, form different test set, and the test set that each migration tube or tof tube and ionization source form is mixed the positive and negative ion handover control system of an external circuit respectively, can realize the detection of positive and negative ion pattern between different test set simultaneously.
5. method according to claim 1 is characterized in that: described ultraviolet source is vacuum UV lamp, diode, xenon lamp, mercury lamp or ultraviolet laser; The material of metal grid mesh or becket is metal and the alloys of various electron work functons less than ultraviolet source ionization energy.
6. method according to claim 1 is characterized in that: the external diameter of described metal grid mesh is more than or equal to the aperture of ultraviolet light; The internal diameter of becket is equal to or less than the aperture of ultraviolet light; The distance of metal grid mesh or becket and ultraviolet source is 0～L, and L is the light path of ultraviolet light, and the more little effect of distance is good more.
7. method according to claim 1 is characterized in that:
Ionization source and ion mobility spectrometry coupling that described ultraviolet source, wire netting or becket are formed are formed ultraviolet light photo when the source ion migration is composed, and it mainly comprises following components usually: ionization source, reaction zone, ion gate, migration tube, signals collecting and disposal system and positive and negative ion handover control system; Its process that is used for detecting halogenated hydrocarbons is: the ion gate that the sample ions that ionization obtains under the ionization source positive and negative ion pattern is opened by pulse enters migration tube, difference according to its mobility in migration tube obtains separating, enter Faraday cylinder at last, received and detection system reception and detection by signal.
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Application publication date: 20100526 |