An analytical method for low concentration uranium and plutonium was developed. In this method uranium and plutonium sampled from nuclear fuel reprocessing solutions were simultaneously determined by highly oriented pyrolytic graphite (HOPG) pre-diffraction EDXRF. The matrix influence was corrected by plotting I(U)/Ic(Ag)-p(U) and I(Pu)/rc(Ag)-p(Pu) instead of I(U)-m(U) and I(Pu)-m(Pu) as their calibration curves where I(Ag) was the intensity of a scattered line from a silver target. The square of correlation coefficient (r2) is better than 0. 999 0 for both uranium and plutonium in the concentration range 2. 00-1 000. 00 mg/L. The experimental measurement results show that the precision (sr) is better than 5% for both uranium and plutonium, and the relative error is less than 3. 0% and 4. 0% for uranium and plutonium, respectively.%利用石墨晶体预衍射X射线荧光法同时测定后处理工艺料液中的低浓铀和钚,建立了测定工艺料液中低浓铀和钚的分析方法.采用Ag靶散射线校正基体效应,以I(U)/Ic(Ag)-ρ(U)和Ⅰ(Pu)/Ic(Ag)-ρ(Pu)作校正曲线,铀和钚的质量浓度均在2.00～1000.00 mg/L时线性相关系数(r2)均大于0.999 0.测定结果表明U和Pu的精密度(Sr)均优于5％,U的相对误差小于3.0％,Pu的相对误差小于4.0％.
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