CN203053930U - Pyrolysis gas chromatography and mass spectrum double-detection device - Google Patents
Pyrolysis gas chromatography and mass spectrum double-detection device Download PDFInfo
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- CN203053930U CN203053930U CN 201220684334 CN201220684334U CN203053930U CN 203053930 U CN203053930 U CN 203053930U CN 201220684334 CN201220684334 CN 201220684334 CN 201220684334 U CN201220684334 U CN 201220684334U CN 203053930 U CN203053930 U CN 203053930U
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Abstract
The utility model discloses a pyrolysis gas chromatography and mass spectrum double-detection device, which consists of a heat pyrolysis device, a gas chromatograph, a capillary chromatographic column, two circuits of distribution controllers, a capillary damping pipe a, a capillary damping pipe b, a flame brightness detector and a quadrupole-rod mass spectrum detector. Only few samples are directly tested without being pretreated, the qualitative analysis for all response components of the entire sample can be completed through one-time feeding, not only can the high-sensitivity response and analysis confirmation for sulfur-contained or phosphorus compound be guaranteed, but also simplicity, rapidness and sensitivity in analysis can be realized, few samples are needed for the analysis, the result is accurate and reliable, the information is complete, and convenience in popularization to use can be realized.
Description
Technical field
The utility model relates to a kind of pick-up unit, is specifically related to the two pick-up units of a kind of pyrolysis gas chromatograph and mass spectrum, belongs to the gas chromatographic analysis technique field.
Background technology
Mass spectrum is combined the high resolving power of gas chromatography and the strong structure identification capacity of mass detector as the gas chromatography combined with mass spectrometry device of gas chromatography detector, become and solve volatility and separates strong instrument with evaluation with the half volatile complex mixture.Heat cracker can be handled the macromolecule sample of the various forms that comprise insoluble three-dimensional crosslinking structure, heat cracker is installed in the front end of gas chromatography as the gas chromatograph pretreating device, only need micro-example just can analyze, it uses also accidental report of document, but relate to the main body of analyzing macromolecular material mostly, other applied analyses are still not extensive.
The flame photometric detector (FPD) of gas chromatography (FPD) is a kind of sulphur or phosphorus organic compound to be had high selectivity, highly sensitive specific detectors.Sample is when rich hydrogen flame combustion, and organic phosphorus compound mainly is to launch the light that wavelength is 526nm with the form of HPO group fragment, and sulfocompound is then with S
2The form of molecule is launched the characteristic light that wavelength is 394nm.Photomultiplier converts light signal to electric signal, amplifies through little electric current and notes down.The sensitivity of this type of detecting device can reach tens to hundreds of coulomb/gram, and minimum detectable quantity can reach 10
-11Gram.Simultaneously, this detecting device can reach 10 to the ratio of the response of organophosphorus, organic sulfur and the response of hydrocarbon
4, therefore can get rid of the interference of a large amount of solvent peaks and hydro carbons, be very beneficial for the analysis of trace phosphorus, sulphur, be the main tool that detects organophosphorus pesticide and sulfocompound.
Want the unknown component in the qualitative analysis complex sample, as during the sulfur-bearing compounding ingredient that needs to contain in the qualitative analysis rubber, need at first carry out just can analyzing after the sample pre-treatments.Especially under the situation that sulphur or phosphorus compound content are not high, need the FPD of advanced promoting the circulation of qi phase chromatogram to detect to confirm the retention time of sulfur-bearing or phosphorus compound when sample solution after the processing is analyzed, afterwards more again sample introduction carry out gas chromatography mass spectrometry and detect for the second time to infer and confirm its structure.Troublesome operation such as this kind method relates to sample pre-treatments, changes chromatographic column outlet detecting device, mass spectrum is started shooting again take time and effort, and are unfavorable for the maintenance of instrument and equipment.
The utility model content
The utility model purpose
The purpose of this utility model provides a kind of pyrolysis gas chromatograph and the two pick-up units of mass spectrum.The utility model is applicable to the gas chromatography of undressed micro-example and mass spectrally detects simultaneously, has single injected sampling and realize highly sensitive response and analysis confirmation to unknown sulfur-bearing or phosphorus compound in the qualitative analysis of response full constituent.
Technical scheme
For achieving the above object, the utility model provides a kind of pyrolysis gas chromatograph and the two pick-up units of mass spectrum, is made of heat cracker, gas chromatograph, capillary chromatographic column, two-way shunt controller, a capillary damper tube, b capillary damper tube, flame photometric detector (FPD) and quadrupole rod mass detector.Heat cracker is positioned at the front end of gas chromatograph, the capillary chromatographic column end of gas chromatograph is connected with the two-way shunt controller, connect gas chromatography detector and level Four bar mass detector respectively by the capillary damper tube, reach the purpose that single injected sampling is realized chromatography of gases and mass spectrum double check.
Heat cracker is one of heated filament type, Curie point type and pipe furnace type, micro-solid and fluid sample needn't handle can be under high temperature and low temperature direct injected, simple and efficient; The capillary damper tube is uncoated capillary column, and the pressure of its different inner diameters and length and two-way shunt controller has determined to detect the ratio of gas shunting jointly; Gas chromatography detector adopts flame photometric detector (FPD), uses respectively when surveying sulphur or phosphorus pattern, to the sulfur-bearing in the sample or the response of phosphorus compound rapid sensitive; Can infer compound structure according to the mass spectrogram of level Four bar mass detector with reference to the spectrum storehouse.
Complicated micro-example direct injected in the utility model, hot cracked device is after heating under the temperature of setting, blending ingredients enters capillary chromatographic column with the injection port of carrier gas by gas chromatograph to be separated, each component after the separation enters the capillary damper tube respectively in proportion by the two-way shunt controller that is divided into two that control pressurer system is arranged, component through damper tube enters FPD detecting device and level Four bar mass detector respectively, two detecting devices detect and draw spectrogram simultaneously, and each component retention time is corresponding.
Beneficial effect
The beneficial effect of the two pick-up units of the utility model pyrolysis gas chromatograph and mass spectrum is: the utility model is single injected sampling at short notice, in the full constituent qualitative analysis of finishing the whole sample response, high sensitivity response and analysis confirmation to sulfur-bearing or phosphorus compound have been realized, improved the sensitivity of analysis efficiency and instrument, greatly reduce cost, easy to utilize; The cooperation of thermal cracker make especially analyze sensitive, fast, sample is micro-, usually need not any pre-treatment, direct injection analysis, make operation fast and convenient, reduce the human factor influence simultaneously, make the result more accurately and reliably, simultaneously because there is not the participation of solvent, the mass spectrum collection does not need the solvent delay program, thereby obtains more sample message.The utility model is applicable to the demand of a plurality of application qualitative analyses such as rubber, plastics and compounding ingredient.
Description of drawings
The structural representation of the two pick-up units of Fig. 1 pyrolysis gas chromatograph and mass spectrum;
Number in the figure: 1 is heat cracker, and 2 is gas chromatograph, and 3 is capillary chromatographic column, and 4 is the two-way shunt controller, and 5 is a capillary damper tube, and 6 is b capillary damper tube, and 7 is flame photometric detector (FPD), and 8 is the quadrupole rod mass detector.
The two pyrograms that detect of Fig. 2 vulcanization accelerator TMTM; Last figure is mass spectrogram, and figure below is the FPD spectrogram.
Embodiment
Below in conjunction with accompanying drawing in detail embodiment of the present utility model is described in detail, but following examples are only for ease of illustrating one of purposes of this device, and unrestricted protection domain of the present utility model, scope of the present utility model proposes in claims:
With reference to Fig. 1: the two pick-up units of the utility model pyrolysis gas chromatograph and mass spectrum, by heat cracker (1), gas chromatograph (2), capillary chromatographic column (3), two-way shunt controller (4), a capillary damper tube (5), b capillary damper tube (6), flame photometric detector (FPD) (7) and quadrupole rod mass detector (8) formation.Sample enters capillary chromatographic column (3) with carrier gas after putting into heat cracker (1) enters gas chromatograph (2) by heating injection port, component after the separation enters by behind the two-way shunt controller (4) that is divided into two that control pressurer system is arranged, being divided into two-way enters flame photometric detector (FPD) (7) and enters level Four bar mass detector (8) through b capillary damper tube (6) through (a) capillary damper tube (5) respectively, draw two chromatograms simultaneously, it is corresponding to respond each component retention time, has realized gas chromatography and mass spectral detection simultaneously.
Operation embodiment 1: be used for the analysis of rubber materials sulfur-bearing compounding ingredient.
The rubber of trace is put into 200 ℃ of heat crackers with vulcanization accelerator TMTM, the gas that heat volatilizes enters capillary chromatographic column behind injection port separates, after component after the separation enters the two-way shunt controller of set pressure 3.5psi, enter the flame photometric detector (FPD) surveyed under the sulphur pattern and enter level Four bar mass detector through the capillary damper tube of internal diameter 0.18 μ m length 2.7m through the capillary damper tube of internal diameter 0.18 μ m length 1.2m respectively, 50 ℃ of following segregation ratios of initial temperature are about 1:1.3, draw two chromatograms simultaneously, see Fig. 2.By being composed the peak more by force, from left to right three among the mass spectrogram retrieval analysis basic confirmation FPD figure of corresponding retention time are respectively carbon disulphide, tetramethyl thiourea, tetramethylthiuram monosulfide, think preceding two pyrolysis products that component is this promoter, the 3rd component is the original molecule of this promoter.This analysis result can be used as reference frame when analyzing rubber sulfur-bearing compounding ingredient.
Claims (5)
1. two pick-up units of a pyrolysis gas chromatograph and mass spectrum, it is characterized in that it is made of heat cracker (1), gas chromatograph (2), capillary chromatographic column (3), two-way shunt controller (4), a capillary damper tube (5), b capillary damper tube (6), flame photometric detector (FPD) (7) and quadrupole rod mass detector (8).
2. two pick-up units of pyrolysis gas chromatograph according to claim 1 and mass spectrum, it is characterized in that: heat cracker (1) is one of heated filament type, Curie point type and pipe furnace type.
3. two pick-up units of pyrolysis gas chromatograph according to claim 1 and mass spectrum, it is characterized in that: capillary damper tube (5,6) be uncoated capillary column, the pressure of its different inner diameters and length and two-way shunt controller can be adjusted, to adapt to the requirement that detects gas shunting ratio.
4. the two pick-up units of pyrolysis gas chromatograph according to claim 1 and mass spectrum is characterized in that: gas chromatography detector employing flame photometric detector (FPD) (FPD) (7).
5. two pick-up units of pyrolysis gas chromatograph according to claim 1 and mass spectrum, it is characterized in that: heat cracker (1) is positioned at gas chromatograph (2) front end, capillary chromatographic column (3) back connects two-way shunt controller (4) and is connected with level Four bar mass detector with gas chromatography FPD detecting device (7) respectively through capillary damper tube (5,6).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220684334 CN203053930U (en) | 2012-12-13 | 2012-12-13 | Pyrolysis gas chromatography and mass spectrum double-detection device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220684334 CN203053930U (en) | 2012-12-13 | 2012-12-13 | Pyrolysis gas chromatography and mass spectrum double-detection device |
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| Publication Number | Publication Date |
|---|---|
| CN203053930U true CN203053930U (en) | 2013-07-10 |
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|---|---|---|---|
| CN 201220684334 Expired - Lifetime CN203053930U (en) | 2012-12-13 | 2012-12-13 | Pyrolysis gas chromatography and mass spectrum double-detection device |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458986A (en) * | 2014-10-29 | 2015-03-25 | 中国科学院广州地球化学研究所 | Gas chromatography multichannel sample introduction system and realized atmosphere detection method thereof |
| CN106596745A (en) * | 2015-10-16 | 2017-04-26 | 中国石油化工股份有限公司 | Method for analyzing products for removing alkene |
| CN106596746A (en) * | 2015-10-16 | 2017-04-26 | 中国石油化工股份有限公司 | Comprehensive two-dimensional analysis method of light circulation oil |
| CN111213054A (en) * | 2018-02-23 | 2020-05-29 | 株式会社Lg化学 | High-speed processing gas chromatography system for additive analysis and analysis method using same |
-
2012
- 2012-12-13 CN CN 201220684334 patent/CN203053930U/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458986A (en) * | 2014-10-29 | 2015-03-25 | 中国科学院广州地球化学研究所 | Gas chromatography multichannel sample introduction system and realized atmosphere detection method thereof |
| CN106596745A (en) * | 2015-10-16 | 2017-04-26 | 中国石油化工股份有限公司 | Method for analyzing products for removing alkene |
| CN106596746A (en) * | 2015-10-16 | 2017-04-26 | 中国石油化工股份有限公司 | Comprehensive two-dimensional analysis method of light circulation oil |
| CN111213054A (en) * | 2018-02-23 | 2020-05-29 | 株式会社Lg化学 | High-speed processing gas chromatography system for additive analysis and analysis method using same |
| US11835498B2 (en) | 2018-02-23 | 2023-12-05 | Lg Chem, Ltd. | High throughput gas-chromatography system for additive analysis, and analysis method using same |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term |
Granted publication date: 20130710 |
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| CX01 | Expiry of patent term |