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Qualitative and quantitative analysis method of elemental sulfur in light petroleum fractions and light petroleum products

A light oil, quantitative analysis technology, applied in the field of analytical chemistry, can solve the problems of many interference factors and low sensitivity, and achieve the effect of wide application, high precision and low detection limit

Active Publication Date: 2013-03-20
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the many interference factors and low sensitivity when FPD is used, the detection limit of elemental sulfur is only 0.2mg / L

Method used

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  • Qualitative and quantitative analysis method of elemental sulfur in light petroleum fractions and light petroleum products
  • Qualitative and quantitative analysis method of elemental sulfur in light petroleum fractions and light petroleum products
  • Qualitative and quantitative analysis method of elemental sulfur in light petroleum fractions and light petroleum products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Example 1 Qualitative Analysis of Elemental Sulfur Structure in Light Petroleum Distillates and Light Petroleum Products

[0054] Gas chromatography conditions:

[0055] Chromatographic column: non-polar quartz capillary column, 30m×0.25mm,

[0056] Carrier gas: high purity helium,

[0057] Head pressure: 110-150kPa,

[0058] Injection port temperature: 210-250°C,

[0059] Column temperature: the initial temperature is 35-50°C, the temperature is raised to 180°C at 20-30°C / min, the temperature is raised to 250°C at 7-10°C / min, and the temperature is raised to 270-300°C at 20-30°C / min.

[0060] Injection volume: 0.5-0.9μL.

[0061] Mass Spectrometry Conditions:

[0062] Interface temperature: 230-250°C,

[0063] Ionization method: electron ionization (EI),

[0064] Electron energy: 70eV,

[0065] Detector voltage: 1.9-2.2kV.

[0066] Straight-run gasoline, straight-run kerosene, straight-run light diesel oil, catalytically cracked gasoline, hydrogenated naphtha,...

Embodiment 2

[0068] Embodiment 2 determines the change of elemental sulfur structure under analytical conditions

[0069] Using analytically pure carbon disulfide as a solvent to prepare elemental sulfur S 8 Standard solution, S 8 The concentration is 16.86mg / L. Under the same conditions as in Example 1 and the injection port is 220°C, SIM analysis is performed. The solvent cutting time: 3.0min, the signal acquisition time: 3.0min, and the monitored ions are m / z 64, 96, 128, 160, 192, 224, 256, namely S 2 + , S 3 + , S 4 + , S 5 + , S 6 + , S 7 + , S 8 + . image 3 for the S 8 Standard solution analysis total ion chromatogram, from the mass spectrum analysis of No. 1, 2, 3 and 4 peaks in the figure, it can be known that No. 1, 2 and 4 peaks are 6 , S 7 , S 8 , No. 3 peak is the component in the carbon disulfide solvent.

[0070] For different concentrations of S 8 The standard solution was analyzed, and the peak area was used for quantification. The analysis results ar...

Embodiment 3

[0078] The establishment of embodiment 3 standard curve

[0079] 0.0100g high-purity elemental sulfur S 8 The powder was dissolved in 100mL of analytically pure toluene solution to prepare an elemental sulfur standard solution with a mass concentration of elemental sulfur of 100mg / L. This solution is diluted respectively to the elemental sulfur standard solution of 0.005, 0.05, 0.10, 0.40, 0.70, 1.00, 5.00, 10.00, 15.00, 20.00, 25.00mg / L, carries out SIM under the chromatographic and mass spectrometric conditions identical with embodiment 1 For quantitative analysis, the monitored ions are m / z 64, 96, 128, 160, 192, 224, and 256. When the elemental sulfur concentration is less than 1.00mg / L, the quantitative ion selection is m / z 64; when the elemental sulfur concentration is greater than 1.00mg / L, the quantitative ion selection is m / z 128. Each diluted standard solution was measured 3 times and the average value was taken. The linear regression of the least square method is...

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Abstract

The invention discloses a qualitative and quantitative analysis method of elemental sulfur in light petroleum fractions and light petroleum products, wherein the gas chromatography / mass spectrometry is adopted in the method. In the qualitative method, a scanning mode is adopted to analyze various samples, and the qualitative analysis is performed by utilizing the analysis of the obtained mass spectrum, combining the standard mass spectral library search and comparing with the retention time of an elemental sulfur guide sample. In the quantitative method, the ion monitoring mode is adopted and a standard curve is established to perform quantitative analysis, wherein a sample to be tested does not require pretreatment and can be directly sampled for analysis. The qualitative and quantitative analysis method has the advantages of wide linear range, low detection limit, high precision, wide coverage of samples, no interference in analysis, short analysis time and is simple in operation.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for qualitatively and quantitatively analyzing elemental sulfur in light petroleum fractions and light petroleum products by gas chromatography / mass spectrometry. Background technique [0002] The content of elemental sulfur in light petroleum distillates and petroleum products is very small, and it is not easy to quantitatively measure, but it is very corrosive to metal parts such as copper and silver alloys in production equipment and fuel systems. affect product quality. Traditionally, the corrosion activity of elemental sulfur in oil products is generally judged by copper and silver corrosion performance tests based on the color changes of copper and silver in oil. And determination of elemental sulfur content in petroleum products, establish a fast and accurate analysis method. [0003] There are many methods for analyzing elemental sulfur, such as spectrophoto...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/06
Inventor 赵惠菊刘明清王忠罗光汪昌华万义芳贾咏梅
Owner CHINA PETROLEUM & CHEM CORP
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