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Full two dimension gas phase chromatography modulator

A two-dimensional gas chromatography and modulator technology, applied in instruments, scientific instruments, measuring devices, etc., can solve the problems of poor modulation effect of low-boiling point substances, affecting the stability of furnace temperature, non-repetitive retention time, etc., and achieve equipment investment. and low operating cost, easy availability and low energy loss

Inactive Publication Date: 2005-10-19
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantages are: since the temperature of the modulator must be 100°C higher than the furnace temperature, the analysis temperature is limited by the maximum operating temperature of the thick liquid film modulation tube, and its modulation effect on low boiling point substances is not good
Both use large amounts of CO 2 (~40ml / min), the Joule-Thompson effect at the time of spraying obtains cooling capacity, and the lowest temperature of cold spraying can reach -50°C, but a large amount of CO must be consumed 2 , its pollution and emissions are non-negligible problems
[0009] The comprehensive two-dimensional gas chromatographic modulators currently developed and adopted are all designed in the furnace of the gas chromatograph, although a large number of insulation materials or vacuum facilities are used to strictly insulate the cold source transmission pipeline to minimize cold At the same time, the heat emitted by the heating parts (generally 100°C higher than the furnace temperature, or 350°C at a constant temperature) affects the stability of the furnace temperature, resulting in non-repetition of the retention time

Method used

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  • Full two dimension gas phase chromatography modulator
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  • Full two dimension gas phase chromatography modulator

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Example 1. Injection peak broadening σ of external modulator l

[0042] The peak broadening of the modulator injection is an important indicator for evaluating the performance of the modulator. As mentioned above, column 2 is a fast analysis column, and the separation needs to be completed within one cycle (1-10 seconds), so as not to overlap with the separation of the second cycle. Therefore, the broadening of the injection peak will directly lead to the broadening of the second dimension peak, which will eventually affect the separation ability of the second dimension.

[0043]The total peak broadening (σ t ) consists of three parts [Document 5]:

[0044] σ t 2 = σ l 2 + σ c 2 + σ d 2 - - - 1

[004...

Embodiment 2

[0066] Example 2. External modulator is used for comprehensive two-dimensional gas chromatography analysis of triphenyl and C 7 、C 8 、C 10

[0067] Test conditions: The comprehensive two-dimensional spectrum processing adopts the self-compiled software GCXGC workstation;

[0068] Analysis conditions:

[0069] Chromatographic column: column 1 DB-530m×0.25mm×0.5μm (J&W, USA)

[0070] Column 2 DB-1701 1.75m×0.10mm×0.10μm (J&W, USA)

[0071] Vaporization chamber: 280°C; Hydrogen flame detector: 250°C;

[0072] Split ratio 30:1; carrier gas: helium constant flow (198kPa);

[0073] Column temperature: 35°C(1)→15°C / min→250°C;

[0074] Sample: Triphenyl and C 7 、C 8 、C 10 ;

[0075] Modulating tube: 1m×0.25mm empty capillary column; auxiliary heater: 30°C higher than the furnace temperature;

[0076] Cold bath: water / ice 0°C; CO 2 The pressure is 7.0Mpa; nozzle 3.

[0077] Pulse period 6.5 seconds; All the other are with embodiment 1;

[0078] Modulated tripheny...

Embodiment 3

[0079] Example 3. An external modulator is used for comprehensive two-dimensional gas chromatography analysis of light diesel oil (catalytic cracking diesel oil from refinery of Sinopec Shanghai Gaoqiao Branch Company)

[0080] Test condition: same as embodiment 2

[0081] Analysis conditions: sample: catalytic cracking diesel oil;

[0082] Carrier gas: Helium constant flow (150kPa);

[0083] Column temperature: 35°C(1)→5°C / min→270°C;

[0084] Auxiliary heater: rises synchronously with the furnace temperature;

[0085] Modulating tube: 2m×0.175mm empty capillary column;

[0086] Cold bath: water / ethanol / dry ice -7°C; CO 2 The pressure is 3.5Mpa; nozzle 5.

[0087] Pulse period 5.8 seconds; All the other are with embodiment 2;

[0088] The comprehensive two-dimensional chromatographic separation chart of catalytic cracking diesel oil after modulation Image 6 , whose enlarged comprehensive two-dimensional chroma...

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Abstract

The present invention relates to gas chromatography analysis and is especially a kind of full two-dimensional gas chromatography modulator. There are modulating pipe form with annular hollow column through winding by two turns, the first and the second chromatographic column connected to ends of the modulating pipe separately, chromatographic furnace heat insulating layer on the top board, through which the modulating pipe passes with the pipe top extending beyond the heat insulating layer; vertical hot nozzle connected to heat source and blowing to the modulating pipe to form one section of modulating part; and cold nozzle connected to CO2 cold source to blow the modulating part. The present invention has less cold loss, no influence on the temperature inside the furnace and ensured preservation time reproducibility.

Description

technical field [0001] The invention relates to gas chromatographic analysis, in particular to a comprehensive two-dimensional gas chromatographic modulator. Background technique [0002] From the design of the first modulator by Liu and Phillips in 1991 to the present [2.Z.Y.Liu, J.B.Phillips, J.Chromatogr.Sci.1991, 29, 227.], comprehensive two-dimensional gas chromatography has developed rapidly and has been Scientists at home and abroad pay more and more attention [Document 1.Dalluge J., Beens J., Brinkman U.A.Th.J.Chromatogr.A, 1000(2003) 69-108]. It combines two chromatographic columns with different and independent separation mechanisms in series through a specially designed modulator to form a two-dimensional gas chromatograph. Comprehensive two-dimensional gas chromatography (GCxGC) differs from conventional two-dimensional chromatography in that components eluting from the first dimension (first column) are collected at low temperature (cold trapping) or with a thi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/80
Inventor 叶芬孔宏伟许国旺
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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