CN218726969U - Cold trap for gas focusing peak shape - Google Patents
Cold trap for gas focusing peak shape Download PDFInfo
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- CN218726969U CN218726969U CN202222730976.7U CN202222730976U CN218726969U CN 218726969 U CN218726969 U CN 218726969U CN 202222730976 U CN202222730976 U CN 202222730976U CN 218726969 U CN218726969 U CN 218726969U
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Abstract
The application relates to a cold trap for gas focusing peak shape, which belongs to the technical field of volatile organic compound gas analysis and is mainly applied to gas chromatography-mass spectrometry sample introduction pretreatment instrument equipment. The problems of reduced response of peaks, overlapping of peak shapes and the like when the related technology is used for sampling high and low concentration volatile organic compound gas samples. According to the gas focusing peak-shaped cold trap, a gas sample is firstly introduced into a compound channel of the gas focusing peak-shaped cold trap, and the sample is frozen by using a freezing medium in a freezing chamber. The compound channel is arranged in the temperature rising channel, after freezing is finished, the frozen sample is rapidly heated through the temperature rising channel, volatile organic compounds in the compound channel are analyzed out in a short time and transferred to a chromatographic column in the gas chromatography, all volatile organic compounds are desorbed, and the gas chromatography-mass spectrometer has the advantages of high peak shape, high peak, complete separation, no tailing and high data effectiveness.
Description
Technical Field
The application relates to the technical field of volatile organic compound gas analysis, in particular to a cold trap for gas focusing peak shape.
Background
The gas chromatography-mass spectrometry combined technology utilizes the excellent separability of gas chromatography and the high selectivity of mass spectrometry identification, and can realize the qualitative and quantitative determination of complex mixed organic matters. Currently, when a gas chromatography-mass spectrometry (GC-MS) instrument samples high and low concentration volatile organic compound gas, the following sampling methods are mainly used: the injection device comprises an injector, a screw needle, a quantitative tube, an injector, a high-pressure rotary valve, a main pump or an auxiliary pump for sample injection, a solid adsorption method for sample injection and the like. Wherein, the injector, the screw needle and the quantitative tube are saved most, the laboratory is adopted more, and the factory is used more by the main pump or the auxiliary pump for sample introduction.
However, when a gas chromatography-mass spectrometry (GC-MS) instrument is used to sample high and low concentration volatile organic compound gas samples at the same time, the samples will diffuse under the conditions of rapid temperature rise, short flow, fixed zero dead volume and high flow rate, so that the response of the earlier peaks is weakened, and the peaks overlap.
SUMMERY OF THE UTILITY MODEL
In order to improve the problems of reduced response and overlapping of peak shapes of early peaks caused by diffusion of gas samples, the application provides a cold trap for gas focusing peak shapes.
The application provides a be used for gaseous focusing peak shape cold trap, adopts following technical scheme.
The utility model provides a be used for gaseous focusing peak shape cold trap, includes the cold trap shell, the inside freezing chamber who is used for the holding freezing medium that is provided with of cold trap shell, be provided with in the freezing chamber and be used for high, low concentration volatile organic compound gaseous compound channel of circulating and be used for supplying the intensification passageway that preheating medium passed through, compound passageway set up in inside the intensification passageway, it can be right to freeze the chamber compound passageway with the intensification passageway cools down simultaneously.
By adopting the technical scheme, before a gas chromatography-mass spectrometry (GC-MS) instrument simultaneously samples high and low concentration volatile organic compound gas samples, firstly, the high and low concentration volatile organic compound gas is introduced into a compound channel of the gas focusing peak-shaped cold trap, and the samples are frozen by using a freezing medium in a freezing chamber. The compound channel is arranged in the temperature rising channel, after freezing is finished, the frozen sample is rapidly heated through the temperature rising channel, volatile organic compounds in the compound channel are analyzed out in a short time and transferred to a chromatographic column in a gas chromatograph, all the volatile organic compounds are desorbed, and by utilizing the characteristics of the volatile organic compounds, the peak shape in the gas chromatograph-mass spectrometer is high, sharp, complete in separation, not trailing and high in data validity, so that the problems that the response of an earlier peak is weakened and the peak shapes are overlapped due to the fact that a gas sample is diffused are solved.
Optionally, the system further comprises a heat conducting pipe, a heat uniform distribution pipe arranged in the heat conducting pipe, and a compound pipe arranged in the heat uniform distribution pipe, wherein the compound channel is formed in the compound pipe, and the warming channel is formed between the heat uniform distribution pipe and the heat conducting pipe.
Through adopting above-mentioned technical scheme, heat equipartition pipe is coaxial to be set up in the heat conduction pipe, and the compound pipe is coaxial to be set up in heat equipartition intraductally to realize that compound passageway diameter is unanimous, and the interval that the passageway that heaies up apart from in the compound passageway is even, guarantees that the passageway that heaies up heats the in-process that freezes in the compound passageway rapidly, and frozen compound is heated evenly, and the peak shape of resolving out is more stable.
Optionally, the interior of the compound tube is coated with a thin film silanized coating for adsorbing polar volatile organic compounds.
By adopting the technical scheme, the thin film silanization coating is coated inside the compound tube, so that the stability and the capacity of the adsorption of the polar volatile organic compound are improved, and the saturation threshold of the gas focusing peak-shaped cold trap is improved.
Optionally, the compound pipe, the heat equipartition pipe and the heat conduction pipe constitute cold trap pipeline jointly, cold trap pipeline has wear to locate cold trap shell and the extension portion that stretches out and the portion of receiving cold that sets up in order to reduce occupation volume of returning the ring, the portion of receiving cold set up in the freezing chamber and with the extension portion intercommunication.
Through adopting above-mentioned technical scheme, through returning the cold portion to encircle the setting to reduce the shared space of cold portion in the cold trap shell. Meanwhile, if the angle of the compound pipe in the cold trap pipeline is less than 90 degrees, the thin film silanization coating is damaged, and the desorption of the volatile organic compound is not facilitated.
Optionally, the cold trap shell includes a cold trap bottom shell and a cold trap upper cover covering the cold trap bottom shell, and a through hole for introducing a freezing medium is provided on the opposite side of the side wall of the cold trap bottom shell.
Through adopting above-mentioned technical scheme, cold-trap upper cover can seal the lid and cover in the cold-trap drain pan to make the cold-trap shell be convenient for the dismouting to maintain. Through set up the through-hole at the lateral wall offside of cold-trap drain pan, be convenient for let in freezing medium in the freezing chamber.
Optionally, a heat insulation bottom plate for isolating heat transfer is fixedly arranged on the side surface of the cold trap bottom shell, which is far away from the cold trap upper cover.
Through adopting above-mentioned technical scheme, keep away from the fixed temperature-insulated bottom plate that sets up in the side at cold trap upper cover place at the cold trap drain pan, separate the installation basis of cold trap shell and cold trap shell through the temperature-insulated bottom plate to improve the in-process that cools down to the cold trap shell, the influence of temperature beyond the cold trap shell to the cold trap shell.
Optionally, the heat conducting pipe is composed of a copper pipe beneficial to conducting heat, and the heat uniform distribution pipe is composed of a polytetrafluoroethylene pipe with uniform temperature conduction.
By adopting the technical scheme, the heat conduction pipe is composed of the copper pipe, so that the cold trap pipeline can quickly absorb the heat of the internal organic compound gas sample in the process of freezing the organic compound gas sample; the heat distributing pipe is composed of polytetrafluoroethylene pipes, and is beneficial to the fact that in the process that the frozen sample is rapidly heated through the temperature rising channel, heat of the outer peripheral wall of the heat distributing pipe can be more uniformly conducted into the compound pipe, so that the frozen compound is convenient to heat uniformly, and the analyzed peak shape is more stable.
Optionally, a temperature probe for monitoring the temperature in the compound tube is arranged between the compound tube and the heat quantity distribution tube.
By adopting the technical scheme, the specific temperature of low temperature and high temperature needs to be strictly controlled in the process of processing the volatile organic compound gas sample by the gas focusing peak-shaped cold trap, and the temperature probe is used for monitoring the temperature in the compound tube, so that the gas focusing peak-shaped cold trap is ensured to have a more stable temperature control mode.
In summary, the present application includes at least one of the following beneficial technical effects:
1. after a sample passes through the gas focusing peak-shaped cold trap, the sample has high peak shape, is sharp, is completely separated, is not trailing and has high data validity in a gas chromatography-mass spectrometer. Before a gas chromatography-mass spectrometry (GC-MS) instrument simultaneously samples high and low concentration volatile organic compound gas samples, firstly introducing the high and low concentration volatile organic compound gas into a compound tube of the gas focusing peak-shaped cold trap, and freezing the samples by using a freezing medium in a freezing chamber, so that the gas phase volatile organic compound gas samples are consolidated and concentrated into a solid phase. And a thin film silanization coating is coated inside the compound tube, so that the stability and the capacity of the adsorption of the polar volatile organic compound are improved, and the saturation threshold of the gas focusing peak-shaped cold trap is improved. Because the compound pipe sets up between heat equipartition pipe and heat conduction pipe, after freezing, heat the sample that freezes through heat equipartition pipe rapidly, the volatile organic compound of short time in with the compound passageway is resolved out and is shifted to the chromatographic column in the gas chromatogram, desorbs out whole volatile organic compound.
2. The cold trap housing is smaller in volume. The cold receiving part is arranged in a loop, so that the space occupied by the cold receiving part in the cold trap shell is reduced. Meanwhile, if the angle of the compound pipe in the cold trap pipeline is less than 90 degrees, the thin film silanization coating is damaged, and the desorption of the volatile organic compound is not facilitated.
3. And controlling the temperature stably. The temperature probe is arranged between the compound tube and the heat uniform distribution tube and used for monitoring the temperature in the compound tube, so that the gas focusing peak-shaped cold trap is ensured to have a more stable temperature control mode.
Drawings
FIG. 1 is a schematic cross-sectional view of a gas focusing peak cold trap in an embodiment of the present application;
fig. 2 is a structural sectional view of a cold trap pipe in an embodiment of the present application.
Description of reference numerals:
310. a cold trap housing; 311. a freezing chamber; 312. a cold trap bottom shell; 3121. an annular seal groove; 313. covering the cold trap; 314. a heat insulation bottom plate; 320. a cold trap pipe; 321. a heat conducting tube; 322. heat quantity is uniformly distributed; 323. a compound tube; 324. an extension portion; 325. a cold receiving part.
Detailed Description
The present application is described in further detail below with reference to the attached drawings.
The embodiment of the application discloses a cold trap for a gas focusing peak.
Referring to fig. 1, a cold trap for gas focusing peak shape includes a cold trap housing 310 and a cold trap pipe 320, the cold trap pipe 320 being partially located inside the cold trap housing 310. Specifically, cold trap housing 310 includes a cold trap bottom shell 312 and a cold trap top cover 313. The cold trap bottom casing 312 is substantially a hollow rectangular parallelepiped structure with an upper opening, and a cold trap upper cover 313 covers the open end face of the cold trap bottom casing 312 in a sealing manner, so that a freezing chamber 311 is formed inside the cold trap bottom casing 312. In order to improve the sealing performance between the cold trap bottom shell 312 and the cold trap upper cover 313, an annular sealing groove 3121 is formed on the opening end surface of the cold trap bottom shell 312, and an annular sealing gasket (not shown) is installed in the annular sealing groove 3121. The cold trap upper cover 313 is pressed on the opening end face of the cold trap bottom shell 312 through bolts arranged on the edge and tightly abuts against the annular sealing gasket, so that sealing between the cold trap bottom shell 312 and the cold trap upper cover 313 is guaranteed.
Referring to fig. 1, through holes for introducing a freezing medium, in this embodiment, partially vaporized liquid nitrogen, are formed on opposite sides of the sidewall of the bottom shell 312 of the cold trap. In order to separate cold trap housing 310 from the installation foundation of cold trap housing 310, a thermal insulation bottom plate 314 is fixedly arranged on the side of cold trap bottom shell 312 away from cold trap upper cover 313, and the contour of thermal insulation bottom plate 314 is larger than the projection of cold trap bottom shell 312 on thermal insulation bottom plate 314, so that the influence of the temperature outside cold trap housing 310 on cold trap housing 310 is improved in the process of cooling cold trap housing 310. In this embodiment, the thermal insulating base plate 314 is made of bakelite.
Referring to fig. 2, the cold trap pipe 320 is formed by coaxially sheathing a heat conducting pipe 321, a heat evenly distributing pipe 322, and a compound pipe 323. The heat quantity distributing pipe 322 is coaxially arranged in the heat quantity conducting pipe 321, and the compound pipe 323 is coaxially arranged in the heat quantity distributing pipe 322, so that the uniform distance between the heat quantity distributing pipe 322 and the compound pipe 323 is realized. A compound passage is formed in the compound pipe 323, and a temperature rising passage is formed between the heat uniforming pipe 322 and the heat conducting pipe 321. The compound channel is used for the circulation of high and low concentration volatile organic compound gas, and the heating channel is used for the passing of a preheating medium. Specifically, the preheating medium is preheated nitrogen. Preheated gas is introduced between the heat distribution pipe 322 and the heat conduction pipe 321, so that the heat distribution pipe 322 is uniformly heated.
Referring to fig. 1, the cold trap pipe 320 has an outer extension 324 penetrating the cold trap housing 310 and protruding therefrom, and a cold receiving portion 325 annularly arranged to reduce an occupied volume, the cold receiving portion 325 being disposed in the freezing chamber 311 and communicating with the outer extension 324. In the present embodiment, the cooled portion 325 is disposed in a loop of a substantially "U" shape, thereby reducing the space occupied by the cooled portion 325 within the cold trap housing 310. In other embodiments, the cooled portion 325 can be arranged in a multi-turn spiral loop as needed to increase the length of the cold trap conduit 320 within the freezing chamber 311 and increase the freezing effect.
The specific structure of the cold trap pipe 320 will be described in detail below according to the implementation principle of the gas focusing peak type cold trap. The cold trap pipeline 320 is formed by coaxially sleeving a heat conduction pipe 321, a heat uniform distribution pipe 322 and a compound pipe 323. Before a gas chromatography-mass spectrometry (GC-MS) instrument simultaneously samples high-concentration volatile organic compound gas and low-concentration volatile organic compound gas, firstly, the high-concentration volatile organic compound gas and the low-concentration volatile organic compound gas are introduced into a compound pipe 323 of the gas focusing peak-shaped cold trap, and a freezing medium in a freezing chamber 311 is used for freezing the samples, so that the gas phase volatile organic compound gas samples are consolidated and concentrated into a solid phase.
Because the compound pipe 323 is arranged between the heat distribution pipe 322 and the heat conduction pipe 321, after freezing is finished, preheated gas is introduced between the heat distribution pipe 322 and the heat conduction pipe 321, the frozen sample is rapidly heated through the heat distribution pipe 322, volatile organic compounds in a compound channel are analyzed in a short time and transferred to a chromatographic column in gas chromatography, all volatile organic compounds are desorbed, and by utilizing the characteristics of the volatile organic compounds, the peak shape in a gas chromatography-mass spectrometer is high, sharp, complete in separation, not trailing and high in data effectiveness. Because the specific temperature of low temperature and high temperature needs to be strictly controlled in the process of processing the volatile organic compound gas sample by the gas focusing peak cold trap, the temperature probe is used for monitoring the temperature in the compound pipe 323, and therefore the gas focusing peak cold trap is ensured to have a more stable temperature control mode.
The temperature control method of the gas focusing peak-shaped cold trap comprises the following steps:
the freezing temperature is 0 to-196 ℃ (standard-180 ℃);
freezing time is 0-20 minutes (standard 15 minutes);
heating desorption time is 0-3600 seconds (standard 30 seconds);
the cleaning time is 0-3600 seconds (standard 240 seconds), the cleaning time is to desorb all required volatile organic compounds, and the impurities are cleaned and discharged out of the gas focusing peak-shaped cold trap;
the cold/hot constant temperature range is 0 to 50 degrees (standard 5 degrees);
the cold/hot constant temperature time is 0-3600 seconds (standard 10 seconds).
Referring to fig. 1, in order to increase the saturation threshold of the gas focusing peak type cold trap, the interior of the compound tube 323 is coated with a thin film silanized coating for adsorbing polar volatile organic compounds, thereby increasing stability and capacity for polar volatile organic compound adsorption. Polarity refers to a covalent bond or the non-uniformity of charge distribution in one covalent molecule. If the charge distribution is not uniform, the bond or molecule is said to be polar. Meanwhile, if the angle of the compound pipe 323 in the cold trap pipe 320 is less than 90 degrees, the thin film silanized coating is damaged, and the desorption of the volatile organic compound is not facilitated. The compound tube 323 is therefore arranged in a "U" loop, thereby ensuring that the angle of the bend at each bend of the compound tube 323 is evenly distributed and greater than 90 degrees.
In this embodiment, the compound pipe 323 is a column pipe with an outer diameter of 0.7mm, and the heat conducting pipe 321 is a 1/4 "inch copper pipe, which is beneficial for the cold trap pipe 320 to absorb the heat of the organic compound gas sample in the cold trap pipe during the process of freezing the organic compound gas sample; the heat uniform distribution pipe 322 is composed of 1/8 inch polytetrafluoroethylene pipes, and is a good electric insulating material due to the fact that the polytetrafluoroethylene pipes are nonpolar, heat-resistant and do not absorb water, and the heat uniform distribution pipe is beneficial to being capable of conducting heat of the peripheral wall of the heat uniform distribution pipe 322 into the compound pipe 323 more uniformly in the process of heating the frozen sample rapidly through the temperature rising channel, so that the frozen compound is heated uniformly, and the resolved peak shape is more stable.
The above are preferred embodiments of the present application, and the scope of protection of the present application is not limited thereby. Wherein like parts are designated by like reference numerals. It should be noted that as used in the foregoing description, the terms "front," "back," "left," "right," "upper" and "lower" refer to directions in the drawings, and the terms "inner" and "outer" refer to directions toward and away from, respectively, the geometric center of a particular component. Therefore, the method comprises the following steps: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (8)
1. The utility model provides a be used for gaseous focusing peak shape cold trap which characterized in that, includes cold trap shell (310), cold trap shell (310) inside is provided with freezing chamber (311) that is used for holding freezing medium, be provided with in freezing chamber (311) and be used for the compound passageway of high, low concentration volatile organic compound gas circulation and be used for supplying the intensification passageway that preheating medium passed through, the compound passageway set up in it is inside to heat up the passageway, freezing chamber (311) can be right the compound passageway with heat up the passageway and cool down simultaneously.
2. A gas focusing peak cold trap according to claim 1, further comprising a heat conducting pipe (321), a heat uniforming pipe (322) disposed inside the heat conducting pipe (321), and a compound pipe (323) disposed inside the heat uniforming pipe (322), wherein the compound passage is formed inside the compound pipe (323), and the warming passage is formed between the heat uniforming pipe (322) and the heat conducting pipe (321).
3. A cold trap for gas focusing peak according to claim 2 characterized in that the inside of the compound tube (323) is coated with a thin film silanized coating for adsorbing polar volatile organic compounds.
4. A cold trap for peak gas focusing according to claim 2, characterized in that the compound pipe (323), the heat distributing pipe (322) and the heat conducting pipe (321) together constitute a cold trap pipe (320), the cold trap pipe (320) has an outer extension (324) penetrating the cold trap housing (310) and protruding out and a cooled part (325) arranged back to the ring to reduce the occupied volume, the cooled part (325) is arranged in the freezing chamber (311) and communicates with the outer extension (324).
5. A cold trap for gas focusing peak according to claim 1, characterized in that the cold trap housing (310) comprises a cold trap bottom shell (312) and a cold trap upper cover (313) covering the cold trap bottom shell (312) by a sealing cover, and the side wall of the cold trap bottom shell (312) is provided with a through hole for passing freezing medium.
6. A cold trap with gas focusing peak according to claim 5, characterized in that the side of the bottom shell (312) of the cold trap far from the upper cover (313) of the cold trap is fixedly provided with a thermal insulation bottom plate (314) for isolating heat transfer.
7. A cold trap for gas focusing peak according to claim 2, characterized in that the heat conducting pipe (321) is made of copper pipe for conducting heat, and the heat distributing pipe (322) is made of teflon pipe with uniform temperature conduction.
8. A cold trap for gas focusing peak according to claim 2, characterized in that a temperature probe for monitoring the temperature inside the compound tube (323) is arranged between the compound tube (323) and the heat quantity distribution tube (322).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222730976.7U CN218726969U (en) | 2022-10-15 | 2022-10-15 | Cold trap for gas focusing peak shape |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222730976.7U CN218726969U (en) | 2022-10-15 | 2022-10-15 | Cold trap for gas focusing peak shape |
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| Publication Number | Publication Date |
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| CN218726969U true CN218726969U (en) | 2023-03-24 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202222730976.7U Active CN218726969U (en) | 2022-10-15 | 2022-10-15 | Cold trap for gas focusing peak shape |
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| CN (1) | CN218726969U (en) |
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- 2022-10-15 CN CN202222730976.7U patent/CN218726969U/en active Active
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