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
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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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