Blank and background during determination of sulfur in steel by inductively coupled plasma atomic emission spectrometry
XU Jian-ping1,CHENG De-xiang2
1.The National Key Lab of Refractory Material and Metallurgy,Wuhan University of Science and Technology, Wuhan 430081,China; 2.Jianghan University,Wuhan 430049,China
Abstract：The blank correction was a challenge during determination of low content sulfur in steel. The detection limit of sulfur was low to 0.02 mg/L in determination by inductively coupled plasma atomic emission spectrometry(ICP-AES). According to this, the lower determination of sulfur was 0.000 5%. In order to realize the determination of sulfur in steel with content higher than 0.000 5%, the dissolution tests of steel in hydrochloric acid, nitric acid and perchloric acid were conducted. The blank during determination of sulfur in steel by ICP-AES was studied. It was found that the blank value of pure reagent was about 0.002% (mass fraction) higher than that of iron-based sample. The background and its deduction method of iron matrix were investigated. The results showed that the background intensity of iron matrix and the standard deviation of background intensity were higher than those of pure reagent and water. Partial measurement peak was annihilated by the high-intensity background of iron matrix, leading to the abnormal phenomenon above. The low limit of determination of analytical method increased due to the increase of standard deviation of iron matrix background. Therefore, the average background of multi-phases should be selected for correction.The sulfur in pure iron matrix sample was firstly removed by dissolution using hydrochloric acid. Then the sulfur-free iron matrix blank solution was prepared by adding nitric acid and perchloric acid. The accurate analysis results could be obtained by subtracting the sulfur-free iron matrix blank from sample. The proposed method was applied to the determination of sulfur in steel sample with mass fraction less than 0.01%. The relative standard deviation (RSD, n=5) was less than 10%. The found results were consistent with those obtained by infrared absorption analysis.
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