两个大洋多金属结核标准物质中27种元素的等离子体质谱法测定

Determination of 27 elements in two polymetallic nodule reference samples from the Pacific Ocean by ICP-MS

从样品制备、仪器操作参数最佳化、内标补偿等几方面着手 ,利用两个标准物质 (GSPN - 2 ,GSPN - 3 )发展了大洋多金属结核中 2 7种元素的等离子体质谱 (ICP-MS)测定方法 .这 2 7种元素包括Ba ,Ce ,Co ,Cu ,Dy ,Er,Eu ,Gd ,Ho ,La ,Li,Lu ,Mo ,Nd ,Pr,Sb ,Sc ,Sm ,Tb ,Th ,Tm ,U ,V ,W ,Y ,Yb和Zn .各元素测定值与保证值相当吻合 .对GSPN - 2和GSPN - 3 ,Ba ,Sb ,Sc,Y ,Zn等 5种元素可用外标校准法准确测定 ,其平均回收率 (n =3 )在 91 4%～ 1 0 6 9%之间 ;可用内标 (10 3Rh)校准法准确测定其他 2 2种元素 ,其平均回收率 (n =3 )在 89 4%～ 1 1 0 2 %之间 ;各元素 3次测定的相对标准偏差 (RSD)为 0 0 %～ 1 1 0 % .

A rapid and accurate method for 27 elements determination in polymetallic nodules by ICP MS was developed on 2 standard reference materials of polymetallic nodules (GSPN 2 and GSPN 3). The 27 elements include Ba, Ce, Co, Cu, Dy, Er, Eu, Gd, Ho, La, Li, Lu, Mo, Nd, Pr, Sb, Sc, Sm, Tb, Th, Tm, U, V, W, Y, Yb and Zn. Mass interferences and matrix effects were properly reduced or compensated by careful sample preparation, instrumental operating parameters optimization and internal standard ( 103 Rh) correlation. For the 27 elements in GSPN 2 or GSPN 3, the analytical results obtained were in good agreement with the corresponding certified values with RSD% in the range of 0.0%～11.0% ( n =3). The method can be conveniently applied to the analysis of real polymetallic samples.