Measurement of element sulfur content in distillate by oscilloscopic polarography

A technology of oscillographic polarography and elemental sulfur, which is applied in measurement devices, chemical method analysis, analysis materials, etc., can solve the problem of high cost of gas chromatography and achieve the effect of preventing sulfur corrosion

Active Publication Date: 2006-08-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method is limited to the analysis of catalytically cracked gasoline, and the cost of gas chromatography used is relatively high

Method used

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  • Measurement of element sulfur content in distillate by oscilloscopic polarography
  • Measurement of element sulfur content in distillate by oscilloscopic polarography

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0031] Establish the standard curve of polarographic peak current and elemental sulfur content described in the present invention.

[0032] Take an appropriate amount of elemental sulfur storage solution, and use toluene to prepare standard solutions with elemental sulfur content of 0.1, 0.5, 1.0, 2.0, 4.0, 8.0, 10.0, 20.0, 30.0, and 40.0 μg / ml.

[0033] Take 1ml of the prepared standard solution, dilute it to 10ml with the supporting electrolyte, then transfer the diluted solution into a 10ml electrolytic cup, use the saturated calomel electrode as the reference electrode, the platinum electrode as the auxiliary electrode, and the mercury drop as the indicator electrode. Start scanning at the starting potential -0.10V, record as figure 1 The first derivative curve of the voltage-current generated by the triphenylphosphine sulfide in the standard solution is shown, and the peak current value is measured, that is, the current value of the highest peak.

[0034] The oscillograp...

example 2

[0036] Investigate the precision and accuracy of the method of the present invention for determining the elemental sulfur content of samples.

[0037]Take an appropriate amount of elemental sulfur storage solution, and prepare sample solutions with elemental sulfur content of 1.0, 5.0, 10.0, and 25.0 μg / ml with toluene respectively. Get the sample solution prepared by 1ml and dilute it to 10ml with supporting electrolyte, then transfer the diluted solution into a 10ml electrolytic cup, carry out oscillopolarographic determination of sample solutions with different elemental sulfur contents by the method of example 1, each sample is measured Six times, the peak current value generated by its triphenylphosphine sulfide was used to obtain the elemental sulfur content of the sample through the standard curve, and the results are shown in Table 1.

[0038] As can be seen from Table 1, the repeatability of the sample measurement results in 1 to 25 μg / ml for the elemental sulfur cont...

example 3

[0040] This example examines the influence of other sulfur compounds on the assay results of the present invention.

[0041] Take an appropriate amount of elemental sulfur storage solution, and prepare sample solutions with elemental sulfur content of 10.0 and 12.0 μg / ml with toluene respectively. Take 1ml of the sample solution, add dimethyl disulfide, mercaptan and thioether respectively, and make the concentration of the added sulfur compound 2000μg / ml, then dilute to 10ml with supporting electrolyte, and then transfer the diluted solution into 10ml of electrolytic In the cup, carry out oscillopolarographic measurement to the sample solution that adds different sulfur compounds by the method for example 1, every kind of sample solution measures 5 times, the peak current value that is produced by its triphenylphosphine sulfide obtains the sample by standard curve. Elemental sulfur content, the results are shown in Table 2.

[0042] As can be seen from Table 2, the presence ...

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Abstract

The present invention relates to a method for determining element sulfur content in distillate by adopting oscilloscopic polarography. Said method includes the following steps: adding triphenyl phosphorus in the sample to make it be reacted with element surfur to form triphenyl phosphonosulfide, preparing standard solution with different element sulfur contents, making the polarographic wave crest electric current value produced by triphenyl phosphonosulfide in standard solution be related to its element sulfur content to create standard curve, then utilizing polarographic wave crest electric current value produced by tested sample and making it pass through the standard curve so as to obtain the element sulfur content in the sample.

Description

technical field [0001] The invention relates to a method for measuring elemental sulfur content in distillate oil, specifically, a method for measuring elemental sulfur content in distillate oil by oscillographic polarography. Background technique [0002] Elemental sulfur in petroleum and its products not only affects the quality of oil, but also corrodes oil refining equipment, mechanical equipment and storage and transportation facilities. Therefore, it is of great significance to develop a method for rapid analysis of elemental sulfur in petroleum fractions and petroleum products. [0003] There are many methods for analyzing elemental sulfur, such as spectrophotometry, colorimetry, gravimetric method, etc. However, these methods are usually difficult to apply to the analysis of complex substances such as hydrocarbons. In many cases the analysis of elemental sulfur was hampered by the interference of other sulfur species in the sample. The polarographic method uses th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/48G01N31/00
Inventor 田松柏赵霞赵杉林
Owner CHINA PETROLEUM & CHEM CORP
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