关键词:
antimony
antimony impregnated graphite
cerium sulfate titration
nitric acid
perchloric acid
potassium sulfate
Raman spectroscopy
sulfuric acid
摘要:
The accurate determination of antimony content in antimony impregnated graphite is of great significance for optimizing production process and improving material performance. The antimony impregnated graphite contains graphite with stable structure,which is difficult to be decomposed completely. In experiments, the sample was decomposed with 20 mL of sulfuric acid-1. 0 g of potassium sulfate-1. 5 mL of perchloric acid-1. 5 mL of nitric acid. If the graphitization degree of sample was too high which could not be decomposed completely at one time, the sample could be fully decomposed by adding 1. 5 mL of perchloric acid,l. 5 mL of nitric acid for several times. The method for the analysis of antimony in antimony impregnated graphite by eerie sulfate titration was established. 2 # antimony impregnated graphite sample (the graphitization degree was 98%) was selected as the object of investigation. The sample before decomposition, the residue after the first decomposition, and the solution after adding perchloric acid and nitric acid for four times were characterized by Raman spectroscopy. The results showed that the D peak which represented the lattice defect of carbon atom in residue disappeared after the first decomposition, while the G peak and 2D peak(which represented in-plane telescopic vibration of spz hybrid and interlayer stacking,respectively) still existed but the strength was weakened. It indicated that the defective graphite was decomposed firstly,and the residue was non-defective graphite with perfect structure. After adding perchloric acid and nitric acid for four times,the G peak and 2D peak of solution disappeared,indicating that the non-defective graphite could be decomposed completely after adding perchloric acid and nitric acid for several times. The experimental method was applied to the determination of antimony in antimony impregnated graphite samples. The relative standard deviations(RSD, n = 7) of determination results were 0. 32% and 0. 78%, an