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Determination method for 18 polycyclic aromatic hydrocarbons (PAHs) in tire filling oil

A technology of polycyclic aromatic hydrocarbons and determination methods, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of unsatisfactory purification effect of filling oil, interference, harmful environment and human health, etc., to achieve accurate determination and removal of interference , good purification effect

Inactive Publication Date: 2018-06-15
CHINA FIRST AUTOMOBILE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Aromatic oils tend to contain carcinogenic polycyclic aromatic hydrocarbons (PAHs), which are very harmful to the environment and human health.
The EU REACH regulations stipulate the content of polycyclic aromatic hydrocarbons in tire filler oil, which is tested by "AfPS GS 2014:01 PAK Testing and Assessment of Polycyclic Aromatic Hydrocarbons (PAH) in the course of awarding the GS-Mark", but this method is not The purification effect of extender oil is not ideal, and the interference is serious. In view of this, it is urgent to find a highly sensitive and practical detection method for the content of polycyclic aromatic hydrocarbons in tire extender oil.

Method used

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  • Determination method for 18 polycyclic aromatic hydrocarbons (PAHs) in tire filling oil
  • Determination method for 18 polycyclic aromatic hydrocarbons (PAHs) in tire filling oil
  • Determination method for 18 polycyclic aromatic hydrocarbons (PAHs) in tire filling oil

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0055] (a) Sample preparation: Weigh 0.4g of tire filler oil into a 5.0mL test tube, add 3.0mL of n-hexane, then add 250μL of internal standard solution (stock solution 2), shake well, and make the filler oil Dissolved into a homogeneous solution A.

[0056] (b) Solid-phase extraction (polycyclic aromatic hydrocarbons special-purpose solid-phase extraction column with polymer filler): first inject 5.0mL of dichloromethane into the solid-phase extraction column, and then inject 5.0mL of n-hexane, and use it immediately after activation ; Inject the prepared sample solution A into the small column, and after it is completely drained, rinse the test tube and the inner wall of the small column twice with 5.0 mL of n-hexane; then, inject 6.0 mL of n-hexane, and let it drain by gravity Discard the eluent; finally, inject 10.0 mL of dichloromethane to collect the eluent B; use a rotary evaporator or blow nitrogen to concentrate the eluent B to 1.0 mL, and transfer it to a 5.0 mL volu...

Embodiment 1

[0064] The above-mentioned experimental conditions were used to extract and detect the tire filler oil sample 1, and the extracted ion chromatograms of the target substance in the mixed standard solution, sample blank solution and spiked sample solution were as follows: figure 2 shown by figure 2 It can be seen that all 18 kinds of PAHs have been effectively separated. In order to detect the applicability of the present invention, 18 kinds of PAHs were extracted under the spiked concentrations of 15.0ng / mL, 40.0ng / mL and 100.0ng / mL respectively to the tire filling oil sample 1, and the results obtained by the spiked recovery test Listed in Table 3. As can be seen from Table 3, the extraction recovery of the target compound in the extraction sample of the present invention ranges from 82.65% to 115.90%, and the relative standard deviation is 0.67% to 3.67%, which proves that the present invention is feasible and effective.

[0065] Table 3 The spike recovery and precision o...

Embodiment 2

[0073] The above-mentioned experimental conditions were used to extract and detect the tire filler oil sample 2, and the extracted ion chromatogram of the target in the sample solution is as follows: image 3 shown by image 3 It can be seen that the interfering components in the extender oil are purified, and all 18 kinds of PAHs have been effectively detected. In order to detect the applicability of the present invention, 18 kinds of PAHs were extracted under the spiked concentrations of 15.0ng / mL, 40.0ng / mL and 100.0ng / mL respectively for the tire filling oil sample 2, and the results obtained by the spiked recovery test Listed in Table 5. It can be seen from Table 5 that the extraction recovery of the target compound in the extraction sample of the present invention ranges from 80.58% to 112.27%, and the relative standard deviation is 0.78% to 3.24%, which proves that the present invention is feasible and effective.

[0074] Table 5 The recovery rate and precision of the...

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Abstract

The invention relates to a determination method for 18 polycyclic aromatic hydrocarbons (PAHs) in tire filling oil. The method is characterized by including the following specific detection steps: preparation of a mixed standard solution and an internal standard substance mixed stand solution, sample preparation, solid phase extraction, GC-MS test: taking of an extracted liquid C for gas chromatography-mass spectrometry qualitative and quantitative analysis, drawing of a standard work curve, and result calculation. The method provided by the invention uses solid phase extraction for sample purification, employs internal standard method for quantitative analysis, and uses a selected ion monitoring mode of GC-MS for detection and analysis, the method needs short time for extraction, can achieve a highest extraction recovery rate, also avoids the matrix interference, and has the advantages of simplicity and practicability, high purification efficiency and short extraction time.

Description

technical field [0001] The present invention relates to a method for determining 18 kinds of polycyclic aromatic hydrocarbons (PAHs) in tire filler oil, in particular to a method for simultaneously detecting 18 kinds of polycyclic aromatic hydrocarbons (PAHs) in tire filler oil by solid phase extraction-gas phase mass spectrometry, which is a detection method. Background technique [0002] Polycyclic aromatic hydrocarbons (polycystic aromatic hydrocarbons; PAH) are hydrocarbons containing two or more benzene rings in their molecules. According to the connection mode of benzene rings, PAHs can be divided into three types: polyphenylaliphatic hydrocarbons, biphenyls and fused PAHs. There are more than 200 known polycyclic aromatic hydrocarbons and their derivatives. Polycyclic aromatic hydrocarbons have strong carcinogenicity, mutagenicity and reproductive system toxicity. They can cause human diseases through inhalation or direct skin contact, and can easily lead to disease...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88G01N2030/045G01N2030/062G01N2030/8854
Inventor 孙硕王慧娟应坤姜伟男
Owner CHINA FIRST AUTOMOBILE
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