Qualitative and quantitative analysis method for element sulfur in liquefied petroleum gas

A technology for quantitative analysis of liquefied petroleum gas, applied in the field of analytical chemistry, can solve the problems of low analysis accuracy and sensitivity, elemental sulfur cannot be directly measured, etc., and achieve the effects of good accuracy, fast quantification and high precision

Active Publication Date: 2012-11-21
CHINA PETROLEUM & CHEM CORP
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0004] In the article "Determination of Elemental Sulfur in Liquefied Gas by Gas Chromatography" (Petroleum Refining and Chemical Industry, 2004, 35 (12): 57), Fu Xiaoqin et al. used toluene solvent to extract elemental sulfur in liquefied gas. By adding triphenylphosphine reagent, Elemental sulfur is converted into triphenylphosphine sulfide and then determined by gas chromatography with a flame photometric detector (FPD). This method cannot be directly determined. Elemental sulfur must be converted into other measurable forms. Therefore, the analysis low precision and sensitivity
[0005] Zhao Huiju in "Determination of Elemental Sulfur in Gasoline by Gas Chromatography / Mass Spectrometry" (Chromatography, 2003, 21 (3): 210) and "Analysis of Elemental Sulfur Content in Gasoline" (Journal of Petroleum (Petroleum Processing), 2004, 20( 3): 67) and "Analysis of Elemental Sulfur Content in Light Oil" (Journal of Analysis and Testing, 2005, 24 (6 Supplement): 380) using gas chromatography / mass spectrometry (GC / MS) technology to analyze Determination of elemental sulfur content in some gasoline, this method is only applicable to the determination of elemental sulfur content in straight-run gasoline, catalytically cracked gasoline and catalytically reformed gasoline produced by oil refining

Method used

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  • Qualitative and quantitative analysis method for element sulfur in liquefied petroleum gas
  • Qualitative and quantitative analysis method for element sulfur in liquefied petroleum gas
  • Qualitative and quantitative analysis method for element sulfur in liquefied petroleum gas

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Example 1 Structural Analysis of Elemental Sulfur in Liquefied Petroleum Gas

[0047] Gas chromatography conditions:

[0048] Chromatographic column: non-polar quartz capillary column, 30m×0.25mm,

[0049] Carrier gas: high purity helium,

[0050] Head pressure: 90kPa,

[0051] Injection port temperature: 195°C,

[0052] Column temperature: the initial temperature is 70°C, keep for 2min, raise the temperature to 210°C at 40°C / min, then raise the temperature to 230°C at 6°C / min, keep for 6min.

[0053] Injection volume: 0.8 μL.

[0054] Mass Spectrometry Conditions:

[0055] Interface temperature: 210°C,

[0056] Ionization method: electron ionization (EI),

[0057] Electron energy: 70eV,

[0058] Detector voltage: 1.5kV.

[0059] With toluene as solvent, S 0 Standard sample (S 8 ) to prepare a standard solution, under the above analysis conditions, for S 0 The standard solution was scanned (SCAN) for analysis, the solvent cutting time was 4.5 min, and the sig...

Embodiment 2

[0061] The establishment of embodiment 2 standard curve

[0062] Gas chromatography conditions:

[0063] Chromatographic column: non-polar quartz capillary column, 30m×0.25mm,

[0064] Carrier gas: high purity helium,

[0065] Head pressure: 100kPa,

[0066] Injection port temperature: 200°C,

[0067] Column temperature: the initial temperature is 60°C, keep for 2min, raise the temperature to 200°C at 35°C / min, then raise the temperature to 225°C at 5°C / min, keep for 3min.

[0068] Injection volume: 0.9 μL.

[0069] Mass Spectrometry Conditions:

[0070] Interface temperature: 220°C,

[0071] Ionization method: electron ionization (EI),

[0072] Electron energy: 70eV,

[0073] Detector voltage: 1.7kV.

[0074] 0.0100g S 0 Standard sample (S 8 ) was dissolved in 100mL toluene solution to prepare S 0 S with a mass concentration of 100mg / L 0 standard solution. The solution was diluted to 0.10, 0.50, 1.00, 10.00, 20.00 mg / L of S 0 Standard solution, add internal st...

Embodiment 3

[0078] The investigation of embodiment 3 precision

[0079] in S 0 In the standard solution with a concentration of 0.25 mg / L, the internal standard n-undecane was added to be 1.00 mg / L. Under the analytical conditions for establishing a standard curve, the solution was measured 6 times, and the standard deviation of the determination was 0.01 mg / L , the relative standard deviation is 4.0%; in S 0 In the standard solution with a concentration of 2.20 mg / L, the internal standard n-undecane was added to be 1.00 mg / L, and the solution was measured 6 times, with a standard deviation of 0.08 mg / L and a relative standard deviation of 3.6%.

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Abstract

The present invention discloses a qualitative and quantitative analysis method for element sulfur in liquefied petroleum gas (LPG) by using gas chromatography-mass spectrometry combination, and relates to the field of analytical chemistry. According to the qualitative method, a scanning way is adopted to analyze a large amount of LPG samples; according to analysis of the resulting mass spectrometry spectrogram, a mass spectrometry standard library search is combined, comparison with an element sulfur standard sample retention time is performed, and element sulfur structure analysis is performed. According to the quantitative method, an internal standard is adopted, n-hendecane is adopted as an internal standard substance, and a quadratic fit standard curve is established by selecting an ion monitoring way to carry out quantitative analysis. A LPG sample requiring detection is treated by a toluene solvent, and then is directly subjected to structure and content analysis of element sulfur. The method of the present invention has characteristics of low detection limit, high accuracy, no interference during analysis, and short analysis time, and provides strong technical supports for guidance of normal LPG production and prevention of processing apparatuses and transport equipment from sulfur corrosion.

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 liquefied petroleum gas by gas chromatography / mass spectrometry. Background technique [0002] Elemental sulfur (S 0 ) content in liquefied petroleum gas 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 transportation systems, and the presence of elemental sulfur will also affect liquefied petroleum gas. product quality. Traditionally, the corrosion activity of elemental sulfur in liquefied petroleum gas is judged based on the color change of copper and silver in liquefied petroleum gas through copper corrosion and silver corrosion performance tests. Therefore, it is necessary to Determination of elemental sulfur content in air, establish a fast and accurate analysis method. [0003] For ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/72
Inventor 赵惠菊徐燕平刘明清王忠郑京禾罗光万义芳汪昌华刘炜贾咏梅蔡伟
Owner CHINA PETROLEUM & CHEM CORP
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