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高纯石墨于马弗炉中900℃下至完全灰化,碱熔融分解灰分,盐酸溶解熔块,电感耦合等离子体质谱测定高纯石墨灰分中L i、Be、Ti、V、Cr、Mn、N i、Co、Cu、Ga、Sr、Y、Zr、In、Sb、Ba、La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、B i等31种杂质元素。考察了熔解灰分的助熔剂中各成分的比例,优化了仪器工作条件,选择同位素克服质谱干扰,比较了4种内标元素的校正效果。杂质元素的检出限在0.000 8~0.1 ng/mL,加标回收率达到93%~105%,相对标准偏差(RSD,n=10)为0.57%~6.5%,该法适用于高纯石墨中痕量杂质元素的测定。
High purity graphite was measured in a muffle furnace at 900 ℃ for complete ashing, alkali melting and decomposing ash, hydrochloric acid dissolving clinker and inductively coupled plasma mass spectrometry for determination of L i, Be, Ti, V, Cr, Mn, Ni, Co, Cu, Ga, Sr, Y, Zr, In, Sb, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, B i and other 31 kinds of impurity elements. The proportions of the components in the flux of the ash were investigated. The working conditions of the instrument were optimized. The isotopes were selected to overcome the interference of the mass spectra. The calibration effects of the four kinds of internal standard elements were compared. The detection limits of impurity elements ranged from 0.000 8 to 0.1 ng / mL, the recoveries were 93% -105% and the relative standard deviations (RSDs, n = 10) were 0.57% ~ 6.5% Determination of Trace Impurities.