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GC high-temperature high-pressure sample directly-sampling method and equipment

A gas chromatography, high temperature and high pressure technology, applied in the field of gas chromatography sampling, can solve the problems of loss of dissolved gas, complicated operation, large error, etc., and achieve the effect of quantitative accuracy and simple operation

Inactive Publication Date: 2004-10-13
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

This method is complex to operate, with many influencing factors and great error
Especially for the determination of high-temperature and high-pressure samples, during the process of cooling and depressurizing the samples, heavy components in the sample will stick to the wall, resulting in the problem of more injections of light components and less injection of heavy components.
If the gas-liquid mixed sample after depressurization and cooling is separated from the gas and liquid and then injected separately, the dissolved gas in it will be lost when the liquid sample is injected.
Therefore, the traditional atmospheric pressure analysis method cannot truly reflect the composition of reactants and products under the reaction conditions (reaction temperature and reaction pressure), or the composition of underground oil and natural gas oil and gas mixture samples.

Method used

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  • GC high-temperature high-pressure sample directly-sampling method and equipment
  • GC high-temperature high-pressure sample directly-sampling method and equipment
  • GC high-temperature high-pressure sample directly-sampling method and equipment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1: Determination of composition of liquid phase product of hexene-1 by valve injection under normal pressure

[0024] The auxiliary gas flow is controlled at 4mL / min by a steady flow valve, VALCO ten-way liquid phase valve, the sample quantitative tube is a 25μm×120mm quartz capillary, 0.1μL, the eluting tube is a 100μm×120mm quartz capillary, 0.5μL, and the eluent is For n-pentane, the capillary sampling tube is a 50 μm × 25 cm quartz capillary tube, split injection, the split ratio is 40:1, the analytical column is 30 m × 0.53 mm inner diameter × 1.5 μm large diameter SE-54 quartz capillary column, and the detector is FID , The valve switching time is instantaneous switching. The chromatogram is shown in Figure 2.

Embodiment 2

[0025] Embodiment 2: Determination of the composition of the liquid phase product of hexene-1 injected into a micro-syringe under normal pressure

[0026] A micro-syringe was used to inject samples, the injection volume was 0.1 μL, and the split injection was performed with a split ratio of 40:1. The analytical column was a 30m×0.53mm×1.5μm large-diameter SE-54 quartz capillary column, and the detector was an FID. The chromatogram is shown in Figure 3.

Embodiment 3

[0027] Example 3: Determination of liquid phase composition of hexene-1 reaction under 50kg pressure by online valve collection and injection

[0028] The auxiliary gas flow rate is controlled at 4mL / min by a steady flow valve, VALCO ten-way liquid phase valve, the sample quantitative tube adopts a 25μm×120mm quartz capillary tube, 0.1μL, the damping tube adopts a 10m×25μm quartz capillary tube, and the elution solvent quantitative tube adopts a 100μm× 120mm quartz capillary, 0.5μL, n-pentane is used as eluent, 50μm×25cm quartz capillary is used as capillary sampling tube, split injection, split ratio 40:1, analytical column is 30m×0.53mm×1.5μm large diameter SE -54 quartz capillary column, the detector is FID, and the valve switching time is instantaneous. The chromatogram is shown in Figure 4.

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Abstract

The invention provides a gas-phase chromatographic sampling method and device which can online analyze high-temperature high-pressure gas-liquid mixing sampling source. The sample enters ten-way valve quantitative tube from the high-pressure sampling source (high-pressure kettle or container) through high-pressure resisting tube, and after filling up the tube, is directly placed in the air through damping tube or high-pressure, doubled-pressure, pressure-stabilizing valve, to keep the pressures of the quantitative tube and the sampling source consistent; at the same time it pours eluting solvent in the eluting solvent quantitative tube; turns the ten-way valve to the sampling position, so that the auxiliary carrier gas feeds the eluting solvent together with the sample into gas chromatographic sampler, then quantitatively analyzes by area normalization with response factor, and obtains the composition of high-pressure sample by primarily sampling. The device includes auxiliary carrier gas flow stabilizing system, high-temperature resisting ten-way valve, damping tube or high-pressure, pressure-doubling, pressure stabilizing valve, eluting solvent system and sample transmission capillary.

Description

technical field [0001] The invention relates to a gas chromatography sampling technology, in particular to a capillary gas chromatography sampling technology, in particular to a direct sampling method for online collection of high temperature and high pressure samples and completion of normalized quantitative analysis in one injection. [0002] The present invention also relates to a device used for realizing the above sample injection method. Background technique [0003] Gas chromatography has been widely used in the separation and analysis of various gases and liquid samples under normal pressure, medium pressure or negative pressure. However, the direct analysis of some high-pressure samples, especially the direct injection technology of high-pressure volatile liquid samples and high-pressure gas-liquid mixture samples, has not been reported so far. Industrial gas-liquid reactions are often carried out under high pressure. It is extremely important to control the reacti...

Claims

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Application Information

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IPC IPC(8): G01N30/20G01N30/24
Inventor 关亚风赵景红
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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