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A kind of method for measuring nickel element content in hydrogenation catalyst

A technology of hydrogenation catalyst and nickel element, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of inaccurate measurement, uncertain content, and difficult to control errors, so as to shorten measurement time, improve accuracy, and eliminate absorption. effect of action

Active Publication Date: 2019-06-07
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] CN1601261A has proposed a kind of Ni element content in the determination catalytic cracking catalyst with X-ray fluorescence method, but there are some deficiencies in X-ray fluorescence method: (1) fluorescence intensity is easily affected by instrument operation fluctuation; (2) some elements (such as ytterbium element) is very close to the characteristic spectral line of Ni element, which will interfere with the accurate determination of nickel element; (3) Kα spectral line is used to measure Ni element, and its excitation limit is 8.3eV. When there are certain elements in the sample, When their characteristic spectral line energy reaches or exceeds 8.3eV, these elements will re-excite Ni element to generate Kα characteristic spectral line, and the closer the energy is to 8.3eV, the stronger the ability to re-excite Ni element is, due to the presence of this interfering element in the sample The content is uncertain, and its interference on the Ni element cannot be determined, resulting in inaccurate measurement
For complex systems with many types of elements, it is impossible to determine the exact solution
For the actual catalyst system, there are many kinds of elements and their contents vary greatly. The Compton scattering lines produced by the sample will fluctuate due to the change of the sample composition, or be absorbed by some elements in the sample. These phenomena will bring interference, the error is difficult to control, and the method provided in this paper will not be able to accurately determine the nickel content in the catalyst

Method used

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  • A kind of method for measuring nickel element content in hydrogenation catalyst
  • A kind of method for measuring nickel element content in hydrogenation catalyst
  • A kind of method for measuring nickel element content in hydrogenation catalyst

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Embodiment 1

[0044] The X-ray fluorescence instrument model used in the embodiment of the present invention is PRIMUS II top-illuminated X-ray fluorescence spectrometer, manufactured by Rigaku Corporation. The operating parameters of the X-ray fluorescence instrument are set as follows:

[0045] X-ray tube target element: Rh

[0046] X-ray tube working voltage and current: 50KV-40mA

[0047] 2θ angle: 18.36°

[0048] Spectroscopic crystal: LiF1

[0049] Collimator: S2

[0050] Detector: SC

[0051] Attenuator: 1 / 1

[0052] PHA pulse height measurement range: 100-300

[0053] Measurement time: 20s

[0054] The gas of the gas flow proportional counter is a mixture of 10% methane and 90% argon.

[0055] Measurement spectrum line: Compton scattering line of rhodium element Kα.

[0056] Preparation of nickel standard solution: Weigh 19.4615g of nickel nitrate (analytical pure), dissolve it in water in a small beaker, transfer to a 100mL volumetric flask to constant volume, the solution...

Embodiment 2

[0081] The X-ray fluorescence instrument model used in the embodiment of the present invention is PRIMUS II top-illuminated X-ray fluorescence spectrometer, manufactured by Rigaku Corporation. The operating parameters of the X-ray fluorescence instrument are set as follows:

[0082] X-ray tube target element: Rh

[0083] X-ray tube working voltage and current: 50KV-80mA

[0084] 2θ angle: 18.36°

[0085] Spectroscopic crystal: LiF1

[0086] Collimator: S2

[0087] Detector: SC

[0088] Attenuator: 1 / 1

[0089] PHA pulse height measurement range: 100-300

[0090] Measurement time: 20s

[0091] The gas of the gas flow proportional counter is a mixture of 10% methane and 90% argon.

[0092] Measurement spectrum line: Compton scattering line of rhodium element Kα.

[0093] Preparation of nickel standard solution: Weigh 19.4615g of nickel nitrate (analytical pure), dissolve it in water in a small beaker, transfer to a 100mL volumetric flask to constant volume, the solution...

Embodiment 3

[0116] The X-ray fluorescence instrument model used in the embodiment of the present invention is PRIMUS II top-illuminated X-ray fluorescence spectrometer, manufactured by Rigaku Corporation. The operating parameters of the X-ray fluorescence instrument are set as follows:

[0117] X-ray tube target element: Rh

[0118] X-ray tube working voltage and current: 60KV-40mA

[0119] 2θ angle: 18.36°

[0120] Spectroscopic crystal: LiF1

[0121] Collimator: S2

[0122] Detector: SC

[0123] Attenuator: 1 / 1

[0124] PHA pulse height measurement range: 100-300

[0125] Measurement time: 20s

[0126] The gas of the gas flow proportional counter is a mixture of 10% methane and 90% argon.

[0127] Measurement spectrum line: Compton scattering line of rhodium element Kα.

[0128] Preparation of nickel standard solution: Weigh 19.4615g of nickel nitrate (analytical pure), dissolve it in water in a small beaker, transfer to a 100mL volumetric flask to constant volume, the solution...

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Abstract

The invention relates to a method for determining the content of nickel element in a hydrogenation catalyst. The method includes: grinding the hydrogenation catalyst into fine powder and tabletting the fine powder into a tablet sample, testing the target line Compton scattering signal intensity of the sample by an X-ray fluorescence spectrometer under definite conditions, and using a regression formula to calculate the content of nickel element in the to-be-tested sample. The method has the characteristics of simple equipment operation, negligible other element interference, wide measurement range, good repeatability, and accurate result. The formula is shown as: y=(a-x) / b (wherein, y refers to the nickel element content of the to-be-tested sample, x represents the Compton scattering intensity of the to-be-tested sample, and a and b are the constants of corresponding equipment's different working parameters).

Description

technical field [0001] The invention belongs to a method for measuring the content of elements in a catalyst, more specifically, relates to a method for measuring the content of nickel in a hydrogenation catalyst. Background technique [0002] In order to meet the increasingly stringent gasoline and diesel quality standards, hydrogenation process has become an important means in petroleum refining. The content of nickel in the hydrogenation catalyst directly determines the catalytic performance of the hydrogenation catalyst. If the content is too low, the reaction will not be complete and the product will not meet the standard. If the content is too high, it will affect the manufacturing cost of the catalyst. Therefore, it is necessary to accurately measure the nickel content in the hydrogenation catalyst Very important. Because hydrogenation catalysts often contain fluorine, silicon, ytterbium, sulfur, molybdenum, tungsten and other elements, conventional analysis methods ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N23/223
Inventor 余颖龙翟旭丽曹青张志华王延飞安谧张雅琳付凯妹马晨菲王春燕庄梦琪梁迎春喻昊霍明辰修远
Owner PETROCHINA CO LTD