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High pressure digestion ICP-MS method for determining rare earth element content in crude oil

A technology of ICP-MS and ICP-OES, which is applied in the direction of measuring devices, preparation of test samples, material analysis through electromagnetic means, etc., can solve problems such as lack of accuracy and affect the determination results of ICP-MS method, and achieve improvement The effect of the digestion effect

Active Publication Date: 2011-11-23
邬蓓蕾
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, high-pressure digestion measures the completeness of digestion by the clarity of the digestion solution and the color of the solution. The results lack accuracy and may easily affect the determination results of ICP-MS.

Method used

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  • High pressure digestion ICP-MS method for determining rare earth element content in crude oil
  • High pressure digestion ICP-MS method for determining rare earth element content in crude oil
  • High pressure digestion ICP-MS method for determining rare earth element content in crude oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0091] Weigh 0.4012g of Dopa crude oil sample and place it in a 100mL high-pressure digestion tank, add 2mL of hydrogen peroxide with a concentration of 30%, then add 12mL of nitric acid with a concentration of 709%, tighten the lid of the tank, put it in a blast drying oven, and heat up to 195°C Keep the temperature for another 5 hours, then turn off the power and let it cool down naturally. After digestion, open the lid of the tank, place the sample solution in a fume hood and let it stand until the sample solution is clear, then transfer it to a 25mL plastic volumetric flask, and dilute to 25mL with ultrapure water to obtain a sample digestion solution. The digestion solution obtained above was measured with an inductively coupled plasma spectrometer, that is, an ICP-OES instrument, to measure the spectral intensity of carbon contained in the digestion solution at 193.027nm, and the measured carbon intensity value was 32108.

[0092] Use the ICP-MS method to quickly determi...

Embodiment 3

[0105] Weigh 0.4086g of the Escalante crude oil sample and place it in a 100mL high-pressure digestion tank, add 2mL of hydrogen peroxide with a concentration of 30%, then add 12mL of nitric acid with a concentration of 70%, tighten the lid of the tank, put it in a blast drying oven, and heat up to Keep the temperature at 195°C for another 5 hours, then turn off the power and let it cool down naturally. After digestion, open the lid of the tank, place the sample solution in a fume hood and let it stand until the sample solution is clear, then transfer it to a 25mL plastic volumetric flask, and dilute to 25mL with ultrapure water to obtain a digestion solution. The digestion solution obtained above was measured with an inductively coupled plasma spectrometer, that is, an ICP-OES instrument, to measure the spectral intensity of carbon contained in the digestion solution at 193.027nm, and the measured carbon intensity value was 33158.

[0106] Use the ICP-MS method to quickly det...

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Abstract

A high pressure digestion ICP-MS (inductively coupled plasma mass spectrometry) method for determining rare earth element contents in crude oil belongs to a chemical detection method for detecting 16 rare earth elements in crude oil, such as Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu, etc. In a sample high pressure digestion process, an ICP-OES (inductively coupled plasma optical emission spectrometry) method is first used to determine a wave spectrum intensity at 193.027nm of a carbonaceous element in a digestion solution, in order to determine a digestion degree; so that problems of apparatus loss and pollution caused by incomplete digestion and large result deviation caused by high matrix interference in a high pressure digestion method are solved. In an ICP-MS apparatus determination of the sample digestion solution, an on-line adding of internal standard solution and a collision reaction cell technology are employed to eliminate interferences and optimize apparatus working conditions. The method has a detection limit reaching 0.01[mu]g / kg-0.7[mu]g / kg and a recovery rate between 80.4%-105.2%, has advantages of low detection limit, rapidness and accuracy, etc., and can satisfy detection requirements of rare earth elements in crude oil.

Description

technical field [0001] The invention relates to a chemical detection method for the content of rare earth elements in crude oil, in particular to a method for measuring the content of rare earth elements in crude oil by high-pressure digestion ICP-MS. Background technique [0002] Rare earth refers to the general term of scandium, yttrium and lanthanide elements in the periodic table of elements. Rare earth elements are heavy metal elements. In the process of crude oil processing, rare earth elements in crude oil will not only reduce the activity of the catalyst, permanently poison the catalyst, shorten the service life of the catalyst, but also reduce the selectivity of the target product in crude oil. Process and product quality have a great influence, so the content of rare earth elements in crude oil is an important index to evaluate the quality of crude oil, and accurate determination of its content is of great significance. [0003] At present, the analysis methods of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/62G01N21/73G01N1/38G01N27/626
Inventor 邬蓓蕾叶佳楣王豪林振兴袁丽凤奚中威任飞王谦
Owner 邬蓓蕾
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