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Analysis method of polycyclic aromatic hydrocarbon content and application thereof

A polycyclic aromatic hydrocarbon and analysis method technology, applied in the application field of content, can solve the problems that the detection sensitivity cannot meet the needs of environmental protection rubber oil analysis, the separation and enrichment is difficult, etc., and achieves high repeatability, good repeatability, and operation. easy effect

Active Publication Date: 2016-05-04
BC P INC CHINA NAT PETROLEUM CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the detection of polycyclic aromatic hydrocarbons has long been a routine method in the analysis of environmental samples, the detection sensitivity of existing standard methods cannot meet the analysis needs of environmentally friendly rubber oil
Since the target PAHs exist in very complex petroleum matrices, it is difficult for existing analytical techniques to selectively identify these PAHs with extremely low content, and then realize the quantitative analysis of PAHs. The separation and enrichment of polycyclic aromatic hydrocarbons is a technical problem

Method used

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  • Analysis method of polycyclic aromatic hydrocarbon content and application thereof
  • Analysis method of polycyclic aromatic hydrocarbon content and application thereof
  • Analysis method of polycyclic aromatic hydrocarbon content and application thereof

Examples

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Embodiment 1

[0063] This embodiment provides a method for quantitatively analyzing polycyclic aromatic hydrocarbons in an environmentally friendly rubber filler oil with low aromatic content (China Petroleum Liaohe Petrochemical Company, naphthenic type environmentally friendly rubber filler oil), the specific steps are as follows:

[0064] First, 15 ml and 10 ml of n-hexane were respectively used to wet the solid phase extraction column (silica gel column) filled with silica gel filler and the solid phase extraction column (alumina column) filled with alumina filler.

[0065] Weigh 1 gram of sample oil into a small beaker, add 0.5 micrograms of D 12 - Perylene, D 12 - As an internal standard, dissolve the sample with 3-5 ml of n-hexane (HEX, the volume is part of the n-hexane for flushing the saturated fraction), and transfer to the top of the silica gel column. Rinse with 30 ml of n-hexane to obtain a saturated fraction.

[0066] The silica gel column and the alumina column are connect...

Embodiment 2

[0078] This embodiment provides a method for quantitative analysis of polycyclic aromatic hydrocarbons in high aromatic content environment-friendly rubber filler oil (China Petroleum Liaohe Petrochemical Company, aromatic hydrocarbon type environment-friendly rubber filler oil, denoted as 1# oil sample), the specific steps are as follows:

[0079] First, 15 mL and 10 mL of n-hexane were used to wet the silica gel column and the alumina column, respectively.

[0080] Weigh 200 mg of sample oil into a small beaker, add 0.5 μg of D 12 - Perylene, D 12 -Ji as an internal standard, dissolve the sample with 3-5 milliliters of n-hexane (this volume is a part of the n-hexane for flushing the saturated fraction), and transfer to the top of the silica gel column, rinse with 30 milliliters of n-hexane to obtain the saturated fraction.

[0081] The silica gel column and the alumina column are connected in series, with the silica gel column at the top and the alumina column at the bottom...

Embodiment 3

[0090]This embodiment provides a method for quantitative analysis of polycyclic aromatic hydrocarbons in the production of environmentally friendly rubber extension oil raw material oil (China Petroleum Liaohe Petrochemical Branch, denoted as 2# oil sample), and its specific steps are as follows:

[0091] First, 15 mL and 10 mL of n-hexane were used to wet the silica gel column and the alumina column, respectively.

[0092] Weigh 20 mg of sample oil into a small beaker, add 2 micrograms of D 12 - Perylene, D 12 - Make the internal standard, dissolve the sample with 3-5 ml of n-hexane (the volume is part of the n-hexane for washing the saturated fraction), and transfer to the top of the silica gel column, rinse with 30 ml of n-hexane to obtain the saturated fraction.

[0093] The silica gel column and the alumina column are connected in series, with the silica gel column at the top and the alumina column at the bottom. Prepare 30 ml of a mixed solution of dichloromethane and ...

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Abstract

The invention provides an analytical method of polycyclic aromatic hydrocarbon content and application thereof. The method includes the steps of: dissolving a to-be-tested sample and an internal standard substance in n-hexane, using n-hexane to perform elution on a silica gel column to obtain saturate fraction; connecting the silica gel column to the upper end of an alumina column in series, flushing the silica gel column and the alumina column with a mixed solution of n-hexane and dichloromethane to obtain aromatic fraction 1; separating the silica gel column from the alumina column, using a mixed solution of dichloromethane and n-hexane to flush the alumina column to obtain aromatic fraction 2; then using a mixed solution of dichloromethane and anhydrous ethanol to flush the alumina column to obtain aromatic fraction 3; concentrating the aromatic fraction 3, then employing toluene to bring the substance to a constant volume, and performing GC / MS analysis, thus obtaining the polycyclic aromatic hydrocarbon content of the to-be-tested sample. The method provided by the invention can perform quantitative analysis on the polycyclic aromatic hydrocarbon contained in environment friendly rubber filling oil and raw oil thereof.

Description

technical field [0001] The present invention relates to a method for analyzing the content of polycyclic aromatic hydrocarbons and its application, in particular to a method for analyzing the content of polycyclic aromatic hydrocarbons using solid phase extraction technology and GC / MS analysis technology and its application in the analysis of environmentally friendly rubber filler oil and its raw materials The invention relates to an application in the content of polycyclic aromatic hydrocarbons contained in oil; it belongs to the field of analysis technology. Background technique [0002] Rubber filler oil is one of the main raw materials in the rubber production process. Its addition can improve the plasticity of rubber, reduce the viscosity and mixing temperature of rubber, and reduce the production cost of rubber. Environmentally friendly rubber extender oil has very high limit standards for the content of polycyclic aromatic hydrocarbons (PAHs). Among them, the EU stan...

Claims

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Application Information

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IPC IPC(8): G01N30/72G01N30/06
CPCG01N30/06G01N30/72
Inventor 史权马苏甜曾海雷霞
Owner BC P INC CHINA NAT PETROLEUM CORP
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