Application Of X-ray Fluorescence Spectrometry In Industrial Inorganic Determination Without Standard

Modern X-ray fluorescence spectrometry(XFS)has a high application value in the analysis of industrial inorganics composition,and it is one of the fastest develop-ing and most commonly used analytical methods in chemical element analysis methods.XFS has a short analysis periods,low cost,and is easy to be used.The advantages of XFS good reproducibility,high accuracy,and no harm to the environment have led to widespread application in many fields.However,due to the lack of some standard materials or the difficulty in setting artificial synthetic standards,it is difficult and limited to apply standard methods to the analysis of metal components in industrial inorganic materials.In this study,based on XFS without standard analysis method,the content of the catalysis,barium sulfate in barite and the glass glaze of ceramic in industrial inorganics were studied,the effects of sample preparation methods,flux selection,sample flux ratio,the choice and amount of release agent,and the temperature of fusion sample,adhesive selection,pressure,etc.,on the sample preparation effect and analysis process were studied.The contrastive experiments were carried out using gravimetric method,volumetric method,atomic absorption spectrophotometry,ultraviolet spectrophotometry,inductively coupled plasma-optical emission spectrome try and inductively coupled plasma mass spectrometry.The experimental results show that the sample preparation method and various sample preparation factors have a very important influence on the sample preparation effect and the analysis process.During preparation of catalysts and barite samples in industrial inorganics,using fusion sample preparation method,the mixture of Li₂B₄O₇and Li BO₂ with a mass ratio of 67:33 were used as a flux,and NH₄I and Li Br with different doses were used as the release agent.The melting temperature was not lower than 1150°C and the melting was continued for 400s to finally make the surface smooth,translucent,non-cracking slides.;during the sample preparation of ceramic glaze samples,using the tablet preparation method,choose microcrystalline cellulose as the binder,the ratio of sample to binder is 10:1,and the sample weight is 4.0000 g and 0.4000 g,respectively.The mixing and grinding time is greater than 20minutes in the agate mortar.In minutes,the tablet press continues to pressurize for 20 s under a pressure of 30t to finally obtain a compact,flat,smooth sample that meets the X fluorescence measurement conditions.Finally,qualitative and quantitative analysis of the main components of the catalyst,such as aluminum,silicon,zirconium,hafnium,tantalum,calcium,magnesium,and manganese,was performed simultaneously using XFS without standard analysis,the precision of each ingredient is 0.11%-1.87%;the barium sulfate content of barium metal insoluble in water and acid was analyzed,the Ba SO₄ content was calculated by weight method,the precision of Ba SO₄ was 0.58%;the content of silicon,sodium,potassium and other elements in ceramic glass glaze was analyzed,and the precision of each component was 0.662%-6.739%.The results obtained by applying the method are in good agreement with the results of the comparative experiment method.