Method for detecting content of metal elements in polyether amine solid catalyst

Abstract

The invention discloses a method for detecting the content of metal elements in a polyether amine solid catalyst, which comprises the following steps: (1) simultaneously preparing a test sample solution and a blank solution: preparing the test sample solution: weighing a test sample, adding sulfuric acid and phosphoric acid to carry out first microwave digestion, adding hydrofluoric acid to carry out second microwave digestion, and carrying out second microwave digestion; diluting with ultrapure water, shaking uniformly, adding an acid solution, diluting, and shaking uniformly to obtain a test solution; (2) preparing a mixed standard curve solution; (3) preparing an internal standard mixed standard solution; and (4) respectively determining the blank solution, the mixed standard curve solution, the test solution and the internal standard mixed standard solution by using inductively coupled plasma mass spectrometry, adding the internal standard mixed standard solution in an online standard adding manner, and quantifying by using the obtained standard curve corrected by the internal standard. The method is simple, accurate, good in reproducibility and high in precision and accuracy; and simultaneous detection of multiple elements can be realized.

Description

Technical field [0001] The present invention relates to a method for detecting the content of metal elements, in particular to a polyetheramine solid catalyst in the detection of metal element content. Background [0002] Polyetheramine, also known as terminal amine polyether, is a class of polyoxyene compounds whose molecular backbone is polyether backbone and whose end is terminated by amino. The catalyst used in the synthesis is a supported catalyst, which has a certain tendency to dehydrogenate, which is conducive to the higher selectivity of the reaction of carbonyl groups with amines. The metal content supported in the catalyst will greatly affect the catalytic efficiency. Characterization is required after catalyst preparation. The proportioning of the active components of the loading has an extremely important impact on the amination efficiency of the polyetheramine preparation process. Therefore, the accurate determination of metal content in polyetheramine solid catalys...

AI Technical Summary

Problems solved by technology

Detection is difficult due to the presence of these poorly soluble carriers

At present, the detection of metal content in solids at home and abroad has the disadvantages of long sample pretreatment time, cumbersome operation, easy introduction of interference and loss, low sensitivity of detection methods, poor accuracy and stability, etc.

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