Abstract: Accurate determination of gallium(Ga),vanadium(V) and phosphorus(P) contents in coal and gangue is of great significance for the resource utilization of associated elements,coal quality evaluation and environmental pollution assessment.Current national standard methods(GB/T 8208-2007,GB/T 19226-2003 and GB/T 216-2003) require high temperature ashing of samples at different temperatures,followed by separate determination of Ga,V and P via spectrophotometry.Such procedures are relatively cumbersome,and high temperature treatment easily causes volatile loss of partial elements,making simultaneous pretreatment and multi-element determination unavailable.In this study,based on the strong oxidation of HNO₃,H₂SO₄,and H₂O₂,the organic matters in samples were oxidized and removed in the form of CO₂,which effectively eliminated the adsorption and encapsulation of Ga,V and P by carbon-containing substances and avoided the carbon removal process by high temperature ignition.Furthermore,HF was introduced to form a mixed acid system together with HNO₃ and H₂SO₄,which greatly improved the decomposition efficiency of silicon-bearing minerals.On this basis,a method for the simultaneous determination of Ga,V and P in coal and gangue sample by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established.The correlation coefficients(r) of calibration curves for all elements were 1.000 0.The limits of detection(LOD) of Ga,V and P ranged from 0.29 μg/g to 2.43 μg/g,and the limits of quantification(LOQ) were between 1.2 μg/g and 9.7 μg/g.The contents of Ga,V and P in coal and gangue were determined according to the experimental method,and the relative standard deviations(RSD,n=7) of the determination results were between 1.7% and 9.4%.The method comparison results indicated that there was no significant difference between the proposed method and national standard methods via t-test, demonstrating the accuracy and reliability of the established method.