Development And Application Of Standard Samples Of Pd Alumina Catalyst For X-ray Fluorescence

In the field of modern chemical industry,the application of catalysts has occupied a pivotal position.In recent years,domestic precious metal catalysts are gradually replacing imported catalysts.Palladium-alumina catalysts are increasingly used in petrochemical industry,pharmaceutical industry,environmental protection and other fields due to their strong catalytic capabilities.In the field of analytical chemistry,the application of standard samples as a guarantee for reliable analytical measurement results makes it an indispensable quality control tool for testing laboratories.In the testing equipment calibration,laboratory accreditation,metrology certification,training of testing personnel and the establishment of a new detection method validation and other aspects,it plays an indispensable role.In view of the need of performance characterization and quality inspection of palladium alumina catalyst products in domestic related industries,this project develops accurate and rapid new detection methods and technologies to meet the needs of it.A series of standard samples have been developed for use in new methods,new technology development and calibration verification.This standard sample has passed the acceptance appraisal organized by the national standard sample technical committee in July 2018 and has been submitted to the national department of standardization administration for approval and promulgation.In the development process of this national standard sample,it not only covers the preparation,test of uniformity and stability of the physical standard sample,but also involves the research and application of the standard sample constant evaluation work method,which is a tremendous and complicated project.During this development work,it has been obtained 150 sets of palladium-alumina catalyst physical standard samples which have the size of 40g*5 bottles,and each contains five points of standard grade handicap of palladium-alumina catalyst standard sample.At the same time the standard chemical evaluation method for Al,Fe,Na,Si and Cl five elements is established.The series of standard samples have been preliminarily applied to the X-ray fluorescence spectrum and energy spectrometer.It lays a solid foundation for the development of accurate,nondestructive and rapid analytical methods for palladium alumina catalyst products in the next step.1.Established and improved the standard analytical method for fluoride precipitation EDTA complex titration,and realized the simple and accurate analysis of high content of aluminum in palladium alumina catalyst.The sample is dissolved in platinum crucible with the borax and sodium carbonate mixed solvent,hexamethylenetetramine(C₆H₁₂N₄)as buffer,and xylenol orange as indicator.Ammonium fluoride is precipitated in the condition of PH 5.8 and titrated with zinc standard fluid.This method has been applied to the confirming of constant value work of standard samples of palladium alumina catalyst,and satisfactory results have been obtained.2.Refined and improved the applicability of the original Pd,Fe,Na and Si detection methods according to the requirements and characteristics of palladium alumina catalyst standard sample,improving detection accuracy and precision.It has been applied to the constant value work of standard samples and succeeded in great result.3.Carried out the composition design,synthesis preparation,uniformity and stability test and joint determination of evaluation of the standard sample through the study of the performance indicators and testing requirements of the palladium-alumina catalyst.It has prepared 150 sets of palladium-alumina catalyst physical standard samples which have the size of 40g*5 bottles,and each contains five points of standard grade handicap of palladium-alumina catalyst standard sample,which has passed the acceptance identified by the National Technical Committee and will be approved and issued as a national standard sample.4.Applied the series of standard samples to the X-ray fluorescence spectrum and X-ray energy spectrometer and the standard working curves of Al,Pd,Si,Fe,Na are drawn.It shows that the curves of Al,Pd,Fe and Na are good in line shape.It lays a solid foundation for the establishment of X-ray fluorescence detection of palladium-alumina catalyst in the next step.5.Preliminarily established the method for detecting the chloride ion of palladium-alumina catalyst,and the determination results of chlorine ions in palladium alumina catalyst standard samples are regarded as reference values,providing users with more information.