Method for quantitative analysis of manganese in gasoline by using gas chromatography/mass spectrometry

A gas chromatography and quantitative analysis technology, applied in the field of quantitative analysis of manganese in gasoline, can solve the problems of troublesome handling, hazards to operators, and insufficient sensitivity, and achieve the effect of simple method and less sample consumption

Inactive Publication Date: 2015-11-25
CHINA PETROLEUM & CHEM CORP
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  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

The sensitivity of this analysis method is not high enough, and the environmental pollution of the sample pretreatment is large, which is harmful to the operator
It has been reported in the literature (Lei Cunxi, No. 6, 2009 of the Spectrum Laboratory) that microwave digestion is used to treat gasoline samples. Since microwave digestion is carried out in a closed container, the amount of reagents used is small and the pollution is small, and microwaves are an internal heating method for samples. method, the digestion speed is fast, and the manganese content of the processed sample is determined by graphite furnace atomic absorption spectrometry. The sensitivity of the analysis method is high, but the sample pretreatment is troublesome.

Method used

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  • Method for quantitative analysis of manganese in gasoline by using gas chromatography/mass spectrometry
  • Method for quantitative analysis of manganese in gasoline by using gas chromatography/mass spectrometry
  • Method for quantitative analysis of manganese in gasoline by using gas chromatography/mass spectrometry

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] Qualitative analysis of components in the MMT auxiliary agent in the production site of embodiment 1

[0072] Gas chromatography conditions:

[0073] Chromatographic column: non-polar quartz capillary column, 30m×0.25mm,

[0074] Carrier gas: high purity helium,

[0075] Head pressure: 90kPa,

[0076] Injection port temperature: 250°C,

[0077] Column temperature: the initial temperature is 100°C, the programmed temperature rise rate is 5°C / min, and the final temperature is 200°C.

[0078] Split ratio: 20:1.

[0079] Mass Spectrometry Conditions:

[0080] Interface temperature: 230°C,

[0081] Ionization method: electron ionization (EI),

[0082] Electron energy: 70eV,

[0083] Detector voltage: 1.5kV.

[0084] Under the above analysis conditions, scan (SCAN) analysis was carried out on the MMT additives used in the production site of Sinopec Jiujiang Branch. The total ion chromatogram (TIC) obtained from the analysis is shown in figure 1 , according to the a...

Embodiment 2

[0085] Embodiment 2 carries out quantification with dehydrated alcohol as MMT solvent

[0086] Gas chromatography conditions:

[0087] Chromatographic column: non-polar quartz capillary column, 30m×0.25mm,

[0088] Carrier gas: high purity helium,

[0089] Head pressure: 90kPa,

[0090] Injection port temperature: 230°C,

[0091] Column temperature: Initial temperature is 60°C, keep for 1min, raise temperature to 250°C at 25°C / min, keep for 6.4min,

[0092] Injection volume: 0.8μL,

[0093] Split ratio: 12:1

[0094] Mass Spectrometry Conditions:

[0095] Interface temperature: 230°C,

[0096] Ionization method: electron ionization (EI),

[0097] Electron energy: 70eV,

[0098] Detector voltage: 1.8kV.

[0099] Establishment of quantitative working curve for manganese in gasoline:

[0100] Under the analytical conditions determined above, the manganese contained in gasoline was quantified by the external standard method. Using the purchased high-purity MMT standard...

Embodiment 3

[0112] Embodiment 3 carries out quantification with catalytic cracking gasoline as MMT solvent

[0113] Gas chromatography conditions:

[0114] Chromatographic column: non-polar quartz capillary column, 30m×0.25mm,

[0115] Carrier gas: high purity helium,

[0116] Head pressure: 90kPa,

[0117] Injection port temperature: 230°C,

[0118] Column temperature: Initial temperature is 60°C, keep for 1min, raise temperature to 250°C at 25°C / min, keep for 6.4min,

[0119] Injection volume: 0.8μL,

[0120] Split ratio: 50:1

[0121] Mass Spectrometry Conditions:

[0122] Interface temperature: 230°C,

[0123] Ionization method: electron ionization (EI),

[0124] Electron energy: 70eV,

[0125] Detector voltage: 1.5kV.

[0126] Establishment of quantitative working curve for manganese in gasoline:

[0127] For oil refining production, the manganese content in gasoline is generally 1mg / L to 16mg / L. For the convenience of analysis, a quantitative working curve is established ...

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Abstract

The invention relates to a method for quantitative analysis of manganese in gasoline by using gas chromatography / mass spectrometry. The method comprises: analyzing a methylcyclopentadienyl manganese tricarbonyl MMT auxiliary agent at an oil refining production site by using a scanning SCAN way; carrying out component qualitation by combining mass spectrometry standard library search according to the analysis of the obtained mass spectrum; carrying out quantitation by using an external standard method; using the MMT as a standard substance; and selecting an ion monitoring SIM mode, and drawing the manganese quantitation work curve by using linear regression of the least square method. The method of the present invention has characteristics of low detection limit, high accuracy, wide linear range, no interference during analysis, convenience, rapidness, direct sample injection, and no requirement of pre-treatment.

Description

technical field [0001] The invention relates to a method for quantitatively analyzing manganese in gasoline by gas chromatography / mass spectrometry. Background technique [0002] With the rapid development of the automobile industry and the requirements for environmental protection and energy saving, the demand for unleaded gasoline and the requirements for gasoline quality are getting higher and higher. Methylcyclopentadiene manganese tricarbonyl (MMT) is currently widely used as a gasoline antiknock agent in China because it can significantly increase gasoline octane number, increase fuel combustion efficiency, reduce automobile exhaust emissions, and save gasoline. The state stipulates that antiknock agents should be added to make the manganese content in gasoline not higher than 16mg / L. At present, the domestic determination of manganese content in gasoline generally adopts the atomic absorption spectrometry SH / T0711-2002, and the minimum detection concentration of this ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 赵惠菊刘明清王忠罗光万义芳邹庐荣刘炜贾咏梅刘芳蔡伟吴维娟
Owner CHINA PETROLEUM & CHEM CORP
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