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Powder X-ray diffraction method for determining magnesium aluminate spinel phase content in catalyst

A magnesia-aluminum spinel, X-ray technology, applied in the direction of material analysis using radiation diffraction, to achieve the effect of improving accuracy

Active Publication Date: 2017-10-31
PETROCHINA CO LTD
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Problems solved by technology

At present, there are no patents, standards or research reports on the detailed determination of magnesium-aluminum spinel phase content in biofuel hydrogenation catalysts by powder X-ray diffraction method

Method used

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  • Powder X-ray diffraction method for determining magnesium aluminate spinel phase content in catalyst
  • Powder X-ray diffraction method for determining magnesium aluminate spinel phase content in catalyst
  • Powder X-ray diffraction method for determining magnesium aluminate spinel phase content in catalyst

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Embodiment Construction

[0044] The embodiments of the present invention are described in detail below: the present embodiment is implemented under the premise of the technical solution of the present invention, and detailed implementation methods and processes are provided, but the protection scope of the present invention is not limited to the following embodiments, the following The experimental method that does not indicate specific condition in the embodiment, generally according to routine condition.

[0045] combine figure 1 , and further specifically describe the powder X-ray diffraction process for determining the content of the magnesium-aluminum spinel phase in the biofuel hydrogenation catalyst through the examples, including:

[0046] 1. Sample preparation

[0047] Take about 1.0 g of the sample to be tested, grind it finely, and sieve it (10 μm ~ 15 μm). Take about 0.5 g of 10 μm ~ 15 μm sieve for later use.

[0048] Preparation of mixed standard samples: Take 0.5 g of the standard sa...

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Abstract

The invention provides a powder X-ray diffraction method for determining the magnesium aluminate spinel phase content in a catalyst. The method comprises the steps of grinding and sieving a to-be-detected biofuel hydrogenation catalyst sample to prepare a mixed sample of the to-be-detected biofuel hydrogenation catalyst sample and a corundum phase sample; simultaneously preparing a mixed standard sample of a magnesium aluminate spinel phase standard sample and a corundum phase standard sample; starting a powder X-ray diffractometer, verifying that the comprehensive stability of the diffractometer is smaller than or equal to 0.1% by using silicon powder after the diffractometer is stable to meet the determination requirements; and collecting copper target Kalpha X-ray diffraction data of the mixed standard sample and the mixed sample within a 2theta angle range of 34-40 degrees under the same working conditions of the X-ray diffractometer separately, processing programs of system software by using powder X-ray diffraction data to obtain peak intensity of a magnesium aluminate spinel phase (311) crystal surface and a corundum phase (104) crystal surface in each sample and determining the mean value, and calculating the magnesium aluminate spinel phase content in the to-be-detected biofuel hydrogenation catalyst sample by using a K-value method.

Description

technical field [0001] The patent of the present invention relates to a powder X-ray diffraction method for determining the content of magnesium-aluminum spinel phase in catalysts, in particular to a powder X-ray diffraction method for determining the content of magnesium-aluminum spinel phase in biofuel hydrogenation catalysts. Background technique [0002] The content of magnesium aluminum spinel phase is an important quality control index of biofuel hydrogenation catalyst. The traditional determination method is to carry out elemental analysis on the catalyst raw material magnesia-aluminum spinel, and convert the content of magnesia-aluminum spinel in the raw material from the elemental analysis results, but due to the impurity and The presence of unreacted magnesium oxide and other components in the reaction product affects the analysis results of magnesium aluminum spinel content, which cannot meet the analysis requirements of magnesium aluminum spinel content in biofue...

Claims

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Application Information

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IPC IPC(8): G01N23/20
CPCG01N23/20
Inventor 李瑞峰王磊王东军杨玉和代跃利
Owner PETROCHINA CO LTD
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