Method for measuring content of phosphorus and iron in catalyst by using X-ray fluorescence method

A co-catalyst, X-ray technology, used in measurement devices, preparation of test samples, material analysis using wave/particle radiation, etc., to achieve accurate results, fast analysis speed, and high precision.

Active Publication Date: 2010-08-11
PETROCHINA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few bibliographical reports on the determination of element content in catalysts by X-ray fluorescence method, and there is no report concerning the method of simultaneously analyzing the content of phosphorus and iron.

Method used

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  • Method for measuring content of phosphorus and iron in catalyst by using X-ray fluorescence method
  • Method for measuring content of phosphorus and iron in catalyst by using X-ray fluorescence method
  • Method for measuring content of phosphorus and iron in catalyst by using X-ray fluorescence method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Preparation of standard samples

[0032] High-purity SiO 2 (purity 99.9%) and high purity Al 2 o 3 (Analytical pure) Mix evenly at a mass ratio of 3:7, then roast at 800°C for 1 hour to make a standard carrier; add a predetermined amount of phosphorus and iron standard solutions, and then add 2 o 3 : CeO 2 :Pr 5 o 11 :Nd 2 o 3 Mixed rare earths with a mass ratio of 20:70:2:2; add absolute ethanol, grind and mix to a uniform powder, transfer the powder into a porcelain crucible, and finally evaporate and dry, which is the standard sample A, in which phosphorus, iron See Table 1 for the content.

[0033] Table 1 Contents of phosphorus and iron in standard sample A

[0034]

[0035] The sample compression method is to add 1g of sample to the rimmed model, spread it evenly, and then add 1.5g of high-density polyethylene to it at 8000 kg / cm 2 compressed into tablets.

Embodiment 2

[0037] The preparation of standard sample B (SiO in the standard sample 2 :Al 2 o 3 The mass ratio is 3:7)

[0038] Accurately measure 10ml of the prepared phosphorus and iron solution, add it to 10.0023g of ZSM-5 molecular sieves roasted at 800°C for 1 hour, add 2g of mixed rare earth (La 2 o 3 : CeO 2 :Pr 5 o 11 :Nd 2 o 3 The mass ratio is 20:70:2:2), add 50ml of absolute ethanol (analytical grade), grind and mix until uniform. Then add 8g of pseudo-boehmite, 4g of alumina sol and 20g of kaolin, then add about 200ml of absolute ethanol (analytical grade), grind and mix until uniform, finally evaporate and dry, which is the standard sample B, wherein the contents of phosphorus and iron are shown in Table 2. Adopt the tabletting method identical with embodiment 1.

[0039] Table 2 Contents of phosphorus and iron in standard sample B

[0040]

Embodiment 3

[0042] By measuring the characteristic spectral line intensity I of phosphorus and iron elements in standard samples A and B respectively i , to get the standard curve equation X i = aI i 2 +bI i +c, where X i is the apparent content of phosphorus and iron, I i is the characteristic spectral line intensity of the element, and a, b, and c are the coefficients of the standard curve equation. Since the matrix effect is serious in X-ray fluorescence analysis, the standard curve equation must be corrected. The present invention corrects and adopts empirical equation Wi=(aI i 2 +bI i +c)(1+∑AijWj) to obtain the correction coefficient Aij, Aij is the correction coefficient for the influence of metal j in the standard sample on the determination of metal i, and Wj is the apparent content of metal element j in the standard sample.

[0043] The relationship curve between the apparent concentration and the spectral line intensity obtained by fitting the content of phosphorus and ...

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Abstract

The invention relates to a method for measuring content of phosphorus and iron in a catalyst by using an X-ray fluorescence method, which comprises the steps of: adding a prepared standard solution with a certain concentration of phosphorus and iron elements in a molecular sieve; loading on a silicon and aluminum carrier containing a mishmetal; and mixing, evaporating, drying and the like to prepare a standard sample. A phosphorus and iron working curve is established on an X-ray fluorescence analyzer, apparent contents of phosphorus and iron in the sample are measured by using the working curve through measuring the X-ray fluorescence strength of phosphorus and iron in a sample to be measured, and the apparent contents are subjected to matrix correction to obtain real contents of the phosphorus and the iron by using an empirical equation; thereby achieving the purpose of rapidly, accurately and simply measuring.

Description

technical field [0001] The invention relates to a method for measuring the content of elements in a cocatalyst by X-ray fluorescence analysis. Furthermore, it is a method for simultaneously determining the content of phosphorus and iron in the cocatalyst by using X-ray fluorescence method. Background technique [0002] In the analysis of catalyst phosphorus and iron elements, chemical analysis method and ICP method are commonly used at home and abroad. The colorimetric method described in the Q / SYLS0586-2002 standard can be used for the analysis of phosphorus content in catalytic cracking catalysts. The sample is extracted with hydrochloric acid, and in the nitric acid medium, under the joint action of phosphate ion, ammonium molybdate and ammonium vanadate, a soluble yellow complex of phosphomolybdovanadate is formed for colorimetric determination. The Q / SYLS0570-2002 standard stipulates the method for determining the content of iron oxide in clay-type cracking catalysts b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/223G01N1/28
Inventor 杨一青王亚红张忠东刘从华周卫军蔡进军马燕青潘志爽
Owner PETROCHINA CO LTD
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