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Method for measuring boilling point distribution of coal and rock oil deriving heavy oil products with liquid phase chromatography

A liquid chromatography and high performance liquid chromatography technology, applied in the field of determination of the boiling point distribution of heavy oil products, can solve the problems of limited maximum distillation temperature, inability to distill heavy substances, long distillation time of equipment, etc., and achieve sample processing The effect of small amount, low toxicity and low pollution

Inactive Publication Date: 2011-09-21
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has some unavoidable disadvantages, such as large amount of solvent used, high toxicity, long distillation time of equipment, limited maximum distillation temperature, only the relationship between boiling point and volume is given, and a considerable part of heavy substances cannot be distilled out, etc.

Method used

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  • Method for measuring boilling point distribution of coal and rock oil deriving heavy oil products with liquid phase chromatography
  • Method for measuring boilling point distribution of coal and rock oil deriving heavy oil products with liquid phase chromatography
  • Method for measuring boilling point distribution of coal and rock oil deriving heavy oil products with liquid phase chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] ①Sample name: a kind of coal tar.

[0039] ②Analysis process:

[0040] Sample preparation: prepare a 0.1 g / 100 ml tetrahydrofuran analysis sample.

[0041] Chromatographic analysis: the model of the chromatographic column used is SHIMPACK GPC-801, the length of the chromatographic column is 30 cm, the inner diameter is 0.8 cm, the flow of tetrahydrofuran is the mobile phase, the flow rate is 1.2 ml / min, the temperature of the chromatographic column: 25 ° C, under this condition , the sample was injected into the column with 2 microliters, and the chromatographic peak of the sample was recorded until the end.

[0042] Processing of chromatograms: After the chromatographic analysis is completed, obtain the time and chromatographic peak response value, and replace the time (Z coordinate) with the boiling point °C value through Y=940.91268-97.10393×Z, that is, the boiling point °C-peak response diagram of the sample is obtained. The chromatogram is divided into different ...

Embodiment 2

[0046] ①Sample name: a petroleum vacuum residue

[0047] ② analysis process: same as embodiment 1.

[0048] ③Analysis results: The boiling point distribution results of the samples are listed in Table 3, and the chromatogram is shown in Figure 2.

[0049] A kind of petroleum vacuum residue boiling point distribution (W%) measurement result of table 3

[0050] Boiling point °C

Embodiment 3

[0052] ①Sample name and type: a kind of coal tar pitch

[0053] ②Analysis process: Divide the chromatogram into different specific areas, that is, the areas with boiling points 600, and then pass the chromatographic peak area corresponding to the boiling point range. The percentage of the total chromatographic peak area of ​​the range can be used to obtain the content of different boiling point ranges. All the other are the same as in Example 1.

[0054] ③Analysis results: The results of the boiling point distribution of the samples are listed in Table 4, and the chromatogram is shown in Figure 3. It can be seen from Table 4 that the quantitative deviation is very small.

[0055] The boiling point distribution (W%) measurement result of a kind of coal tar pitch of table 4

[0056] Boiling point °C

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Abstract

The invention relates to a method for using liquid chromatography to test the boiling point distribution of coal and oil derivative heavy oil product, which uses shimazu LC-3A high-effect liquid chromatograph, assisted with a UVD-2 ultraviolet detector, while wavelength is 254nm and the type of chromatographic column is SHIMPACK GPC-801, the column length is 30cm and the inner diameter is 0.8cm, the flow phase is tetrahydrofuran. The invention has the advantages of low sample processing amount, low toxicity, quick operation and high repeatability.

Description

technical field [0001] The invention belongs to an analysis and testing method, in particular to a method for measuring the boiling point distribution of heavy oil products derived from coal and petroleum by liquid chromatography. technical background [0002] There are many complex and mixture products, such as shale oil, petroleum residue, asphalt, heavy coal tar, anthracene oil, direct coal liquefaction products, etc. In the 21st century, the in-depth development of such complexes has received great attention, and the relationship between mastering their boiling point distribution characteristics (also called boiling range determination) and fully developing them is very close. There are distillation methods for measuring boiling range, and there are standard methods in my country (data ①. Standard test method for original distillation, National Standard of the People’s Republic of China, GB / T 17280-1998, State Supervision Bureau, 1998-03-20; ②. Test method for distillati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G06F17/00
Inventor 张昌鸣黄张根
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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