Method for forecasting leading chromatographic peak shape under multi-order programmed temperature condition

A temperature-programmed, chromatographic peak technology, applied in the field of gas chromatography, can solve the problems of chromatographic peak shape prediction that have not been reported yet

Inactive Publication Date: 2012-06-20
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, domestic and foreign work on chromatographic peak shape prediction under constant temperature conditions has ...

Method used

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  • Method for forecasting leading chromatographic peak shape under multi-order programmed temperature condition
  • Method for forecasting leading chromatographic peak shape under multi-order programmed temperature condition
  • Method for forecasting leading chromatographic peak shape under multi-order programmed temperature condition

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Experimental program
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Effect test

Embodiment 1

[0082] Instruments: HP6890 gas chromatograph, hydrogen flame ionization detector, 6890 gas chromatograph workstation;

[0083] Chromatographic column: non-polar HP-5 (5% phenylmethylpolysiloxane) column;

[0084] Conditions: The temperature of the detector is 250°C, and the temperature of the injection port is 250°C;

[0085] Carrier gas: use high-purity nitrogen gas (purity not less than 99.999%), constant flow operation mode, that is, the carrier gas is at the outlet of the column,

[0086] The mass flow rate is kept constant at 1mL / min;

[0087] Injection method: split injection, the split ratio is 50:1, each injection volume is 0.2 μL, and the concentration is 1 μg / mL;

[0088] (1) Select heptanoic acid as the compound to be tested, and measure its retention time at six constant temperatures of 30°C, 50°C, 100°C, 150°C, 200°C and 250°C on the HP-5 column, which are 25.01min, 14.32min, 7.30min, 3.07min, 2.34min and 2.08min;

[0089] (2) Take the virtual dead time ...

Embodiment 2

[0106] Experimental apparatus, chromatographic column, condition, carrier gas and sample injection mode are the same as embodiment 1;

[0107] (1) Heptanoic acid was selected as the compound to be tested, and its retention times at six constant temperatures of 30°C, 50°C, 100°C, 150°C, 200°C and 250°C were measured on the HP-5 column, which were 25.01min, 14.32min, 7.30min, 3.07min, 2.34min and 2.08min;

[0108] (2) Take the virtual dead time τ=1.85min, and calculate the retention factors of heptanoic acid at six constant temperatures according to formula 1, which are respectively: 2.53, 1.91, 1.08, -0.42, -1.33 and -2.12. At lower temperatures, the distribution of heptanoic acid between the two phases is relatively slow, and is affected by mass transfer resistance diffusion items, etc. Therefore, when using Equation 2 to fit the curves of the relationship between retention factor and temperature at six constant temperatures , the above parameters need to be corrected, and fi...

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Abstract

The invention discloses a method for forecasting a leading chromatographic peak shape under the multi-order programmed temperature condition. The method mainly comprises the followings: evaluating a chromatographic retention factor value under different temperatures according to a virtual dead time; searching out a peak shape parameter PSP under the constant temperature condition through a computer program according to nonlinear plate theory; establishing the functional relations between the retention factor as well as the peak shape parameter and the temperature through the regression analysis based on the retention factor and the peak shape parameter of a to-be-detected compound under different constant temperatures; and setting the temperature program, obtaining the forecasted leading chromatographic peak shape through calculation of the computer and comparing with a testing peak shape obtained under the same programmed temperature condition. The invention provides a vital basis for qualification of the type of chromatographic peak shape such as the leading chromatographic peak, optimizes the chromatographic fractionation condition, and provides a new way for accurate quantification of overlapping chromatographic peak common in a laboratory at the same time; and furthermore, the method is widely applicable, and has high forecasting accuracy.

Description

technical field [0001] The invention relates to a method for predicting the peak shape of a tongue protruding chromatogram under the condition of multi-stage temperature programming, and belongs to the technical field of gas chromatography. Background technique [0002] In the field of chromatographic analysis, the prediction of chromatographic peak shape is a very important research content. For complex compounds with a wide range of boiling points and compositions, it is necessary to use temperature programming conditions to achieve separation between components. If based on the retention time and peak shape parameter data of a small number of samples, with the help of computer programs, the prediction of the chromatographic peak shape under the condition of programmed temperature rise can be realized, not only the accurate prediction of the retention time can be realized, the chromatographic separation conditions can be optimized, and the chromatographic qualitative can b...

Claims

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Application Information

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IPC IPC(8): G01N30/86
Inventor 范国樑李登科龚彩荣
Owner TIANJIN UNIV
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