Analysis Of Impurity Elements In High Purity Special Engineering Plastics By ICP-OES/MS

Aromatic specialty engineering plastics?PSF,PEEK,PI,PPS etc?have excellent mechanical properties and thermal stability,high impedance and good biocompatibility.They were widely used in aerospace,pharmaceutical,semiconductor and other high-tech fields.The presence of impurity elements in special engineering plastics had an important effect on the properties of the material and limited its'application in some fields.Therefore,the accurate and rapid determination of impurities is an important part.In this work,a new method was established based on the sulfonation reaction,the ICP-OES/MS was used as an analytical method to determine the residual of high purity specialty engineering plastics accurately and quickly.The research works are as follows:A new method for the rapid determination of As,Cd,Na and Fe in PSF/PEEK samples by ICP-OES was established.The sample was sulfurate by concentrated sulfuric acid and dissolved in dilute acid reagent which replace the sample digestion.To achieve the purpose of rapid sample preparation,key factors affecting the sample preparation effect were systematically investigated.The internal online standard method was used for overcome high viscosity sulfuric acid caused by physical interference during ICP analysis.The results showed that the recovery rate of each element above 90%,and the total treatment time was less than 20 min.The RSD was between 2.1%and 5.1%.The detection limit?3??was between 0.001 mg/kg and0.253 mg/kg.The method was successfully applied for the real PSF/PEEK sample analysis.The use of autochthonous fuming sulfuric acid reaction solved the problem that the polyimide sample was not complete sulfurated by concentrated sulfuric acid and the background value of fuming sulfuric acid is too high.The effects of P₂O₅ for PI samples were discussed.The results show that the method could analyze more than 20elements including As,Cd and so on.The recovery of each element was in the range of 100%±10%,and the Hg was analyzed by standard addition method.The RSD of the parallel samples was between 0.4%and 8.2%.The detection limit?3??was between 0.120 mg/kg and 13.9 mg/kg.The processing time of this method is less than30 min,and it has the advantages of high efficiency,environment friendliness and multi-element determination.This method was successfully applied for the two real PI samples.A new method for the rapid determination of 20 elements such as Cu,Fe and Co in PPS samples was established by ICP-OES which based on the treatment of H₂SO₄ at high temperature.Key factors affecting the sample preparation effect were systematically investigated,and developed two different treatment methods according to the different properties of the elements:high temperature exposure method and high pressure sealing method,the recovery rate of each element is more than 90%,and the RSD was between 1.2%and 7.8%,and the detection limit?3??was between0.108 mg/kg and 5.94 mg/kg.The total treatment period of high temperature exposure method is less than 20 min,and the high pressure sealing method is suitable for the detection of low boiling point elements such as Hg.The method was successfully applied to two practical PPS samples.