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Full two dimension gas phase chromatography modulator

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

Inactive Publication Date: 2007-08-15
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. Sample injection peak broadening σ of external modulator i

[0042] Modulator injection peak broadening is an important indicator for evaluating the performance of the modulator. As mentioned above, column 2 is a fast analytical column and needs to be separated within one cycle (1-10 seconds) to avoid overlapping with the separation of the second cycle. Therefore, the broadening of the injection peak will directly lead to the broadening of the second-dimensional peak, and ultimately affect the second-dimensional separation ability.

[0043] The total peak broadening of the second-dimensional analysis component (σ i ) Consists of three parts [Reference 5]:

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

Embodiment 2

[0067] Example 2. External modulator used for comprehensive two-dimensional gas chromatography to analyze triphenyl and C 7 , C 8 , C 10

[0068] Test conditions: The self-edited software GCXGC workstation is used to process the full two-dimensional spectrum;

[0069] Analysis conditions:

[0070] Chromatographic column: column 1 DB-5 30m×0.25mm×0.5μm (J&W, USA)

[0071] Column 2 DB-17011.75m×0.10mm×0.10μm (J&W, USA)

[0072] Vaporization chamber: 280°C; hydrogen flame detector: 250°C;

[0073] Split ratio 30:1; carrier gas: constant flow of helium (198kPa);

[0074] Column temperature: 35℃(1)→15℃ / min→250℃;

[0075] Sample: Triphenyl and C 7 , C 8 , C 10 ;

[0076] Modulation tube: 1m×0.25mm empty capillary column; auxiliary heater: 30℃ higher than furnace temperature;

[0077] Cold bath: water / ice 0℃; CO 2 The pressure is 7.0Mpa; the nozzle is 3.

[0078] The pulse period is 6.5 seconds; the rest are the same as in embodiment 1;

[0079] After modulation, triphenyl and C 7 , C 8...

Embodiment 3

[0080] Example 3. External modulator used for comprehensive two-dimensional gas chromatography analysis of light diesel oil (Sinopec Shanghai Gaoqiao Branch Refinery Catalytic Cracking Diesel)

[0081] Test conditions: same as Example 2

[0082] Analysis conditions: sample: catalytic cracking diesel;

[0083] Carrier gas: constant flow of helium (150kPa);

[0084] Column temperature: 35℃(1)→5℃ / min→270℃;

[0085] Auxiliary heater: synchronized with furnace temperature rise;

[0086] Modulation tube: 2m×0.175mm empty capillary column;

[0087] Cold bath: water / ethanol / dry ice -7℃; CO 2 The pressure is 3.5Mpa; nozzle 5.

[0088] The pulse period is 5.8 seconds; the rest is the same as in embodiment 2;

[0089] The comprehensive two-dimensional chromatographic separation diagram of the modified catalytic cracking diesel is shown in Figure 5, and the enlarged comprehensive two-dimensional chromatographic separation diagram is shown in Figure 6. The comprehensive two-dimensional chromat...

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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 [Literature 2. ZYLiu, JBPhillips, J. Chromatogr. Sci. 1991, 29, 227.], comprehensive two-dimensional gas chromatography has achieved rapid development and has been Scientists at home and abroad are paying more and more attention [Document 1.Dalluge J., Beens J., Brinkman UATh.J. Chromatogr.A.1000(2003)69-108]. It combines two chromatographic columns with different separation mechanisms but independent of each other in series through a specially designed modulator to form a two-dimensional gas chromatograph. Comprehensive two-dimensional gas chromatography (GC×GC) is different from conventional two-dimensional chromatography. The components flowing out from the first dimension (the first column) are processed at low...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/80G01N30/46
Inventor 叶芬孔宏伟许国旺
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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