Chromatograph on-line analysis method for source rock by closed ball milling, heating analysis and cold trap trapping

A technology of heating analysis and analysis method, which is applied in the field of online extraction and analysis of various hydrocarbon contents, can solve the problem of excessive component loss, and achieve the effect of reducing loss, avoiding loss and avoiding oxidation.

Active Publication Date: 2010-12-01
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The usual analysis method for dispersed organic matter in source rocks is the chloroform-bitumen extraction method. Due to the limitation of this analysis method, the loss o

Method used

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  • Chromatograph on-line analysis method for source rock by closed ball milling, heating analysis and cold trap trapping
  • Chromatograph on-line analysis method for source rock by closed ball milling, heating analysis and cold trap trapping
  • Chromatograph on-line analysis method for source rock by closed ball milling, heating analysis and cold trap trapping

Examples

Experimental program
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Effect test

Embodiment 1

[0021] refer to figure 1 . Source rock airtight ball milling, heating analysis, cold trap trap chromatography online analysis device, mainly composed of sealed ball milling tank 3, ball milling tank heating insulation body 4, transmission pipeline 5, pipeline heating insulation body 6, chromatograph 7 and temperature control device 8 composition. The sealed ball milling tank 3 mainly includes a tank body and an upper cover. The tank body is cylindrical, with an inner diameter of 110 mm, a height of 106 mm, and a diameter of 80 mm. The upper cover has an air outlet, an air inlet and a pressure gauge port. Install a pressure gauge on the pressure gauge port. The sealed ball mill jar 3 upper cover is fixed on the jar mouth and is sealed by a gasket.

[0022] The air inlet of the sealed ball milling tank 3 is airtightly connected with a helium gas pipeline 2, the helium gas pipeline 2 is connected with a mass flow meter 1, and outside (around) the sealed ball milling tank 3, t...

Embodiment 2

[0034] Taking a light crude oil from Well Pinghu 4 as an example, the light fraction compounds were analyzed by means of source rock closed ball milling, heating analysis, and cold trap trap chromatography on-line analysis methods. The purpose of this experiment is to test the reliability and repeatability of this device . Operation method is the same as embodiment 1, difference:

[0035] The light crude oil sample from Pinghu No. 4 Well was directly injected into the vacuumized sealed ball mill tank 3, and the rest of the operations were the same as in Example 1. The results of five consecutive repeated tests are shown in Table 2.

[0036] Table 2 Repeatability experiment results of five consecutive analyzes of light crude oil in Well Pinghu 4

[0037]

[0038] It can be seen from Table 2 that the same light oil was analyzed five times C 6 ~C 13 The peak area of ​​each n-alkane relative to C 6 ~C 13 The standard deviations of the percentage content of the total area ...

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Abstract

The invention discloses a chromatograph on-line analysis method for source rock by closed ball milling, heating analysis and cold trap trapping, which is used for analyzing light fraction compound and percentage composition thereof in the dispersed organic matter of the source rock, and is characterized by comprising the following steps: carrying out vacuum sealing and ball milling on a source rock sample, carrying out ball milling, crushing, then heating to 300DEG C, and carrying out thermal desorption; blowing the pyrolysed hydrocarbon to a liquid helium cold trap by utilizing helium; placing the cold trap into a chromatograph furnace; and trapping, then carrying out chromatograph or Chromatographic-MS on-line analysis to obtain the qualitative data of chromatograph fine separation and/or Chromatographic-MS analysis of the light fraction in the source rock. The separation degree of the sample can approximate to the separation effect of the light dydrocarbon chromatograph separation of crude oil; the invention has good repeatability, reduces the volatilization loss of the light fraction in the crushing process because of the large volume of the sample before being put in a ball milling tank; and the qualitative analysis result can be used for researching the maturity and the environment of sedimentation of the source rock and carrying out oil source comparison.

Description

technical field [0001] The invention relates to the technical field of petroleum organic geochemical source rock research, in particular to an online extraction and analysis method for various hydrocarbon contents in the source rock research. Background technique [0002] At present, various hydrocarbon contents such as free hydrocarbons, pyrolysis hydrocarbons, hydrocarbon production potential, etc. usually mentioned in petroleum geology refer to residual hydrocarbons in source rocks, light distillates (C 5 -C 13 ) is a very important component, for light oil and condensate oil, C 5 -C 13 Fractions account for more than 90% of the total oil quality, and are undoubtedly representative. The geochemical information contained in them cannot be ignored. There have been many research results at home and abroad. Corresponding to the research project of light fractions of crude oil, K.F.M. Thompson used more than 2,000 fresh cuttings and borehole core samples in 1979, purged wit...

Claims

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Application Information

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IPC IPC(8): G01N30/06
CPCG01N1/286G01N1/4022G01N2001/4033
Inventor 徐冠军王培荣肖廷荣任冬苓刘建宪张斌
Owner PETROCHINA CO LTD
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