Abstract：With the aid of pulse distribution analysis (PDA) technology, the content of acid soluble aluminum in low alloy steel was determined by spark discharge atomic emission spectrometry. The effects of three sample preparation methods (Al2O3 grinding wheel, SiC grinding wheel and turn milling), argon excitation flow rate, pressure and purity on analysis results were explored. It was found that the sample preparation by turn milling was the best choice. Meanwhile, the following experimental conditions were finally selected: the argon excitation flow rate was controlled at 10L/min, the input pressure was 0.20-0.30MPa, and the argon purity was higher than 99.99%. Fe 287.2nm and Al 394.4nm was used as internal standard line and analysis line, respectively. The flush time of argon was 3s, the pre-burning time was 1700 pulse, and the integral time was 3600 pulse. The calibration curve was regressed by linear fitting and quadratic fitting. The results indicated that the quadratic fitting was better with correlation coefficient of 0.99989. The overlapping interference of V, Ti and Nb was corrected. Four kinds of low alloy steel certified reference materials were used for precision (n=10) and accuracy tests. The absolute error between the certified value and the determination value,the critical difference of CD0.95, the standard deviation and standard deviation corresponding to repeatability limit could meet the requirements in GB/T 4336—2016. The proposed method was applicable for the determination of acid soluble aluminum content with mass fraction of 0.008%-0.25% in low alloy steel.
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