微晶萘负载PMBP微柱分离预富集与电热蒸发-电感耦合等离子体原子发射光谱联用测定痕量稀土元素

报道了微晶萘负载1-苯基-3-甲基-4-苯甲酰基-5-吡唑酮(PMBP)微型柱分离预富集与电热蒸发-电感耦合等离子体原子发射光谱(ETV-ICP-AES)联用测定痕量稀土元素(Sc,Y,La和Yb)的新方法.试验了影响分离/预富集待测物的各种因素(包括溶液酸度、流速、试样体积、微柱尺寸);研究了吸附有待测物的微晶萘的溶解方法及共存元素对分离/测定的影响.在优化的实验条件下,方法的相对检出限为14pg/mL(Sc),32pg/mL(Y),190pg/mL(La)和26pg/mL(Yb),相对标准偏差(RSD)分别为3.1%,3.5%,4.8%和3.4%(n=9,c=10ng/mL).本法已成功地应用于生物样品中痕量稀土元素(Sc,Y,La和Yb)的测定,结果满意.

Determination of Trace Amounts of Rare Earth Elements by ETV-ICP-AES Combined with Microcolumn Separation/Preconcentration

A sensitive and rapid method for electrothermal vaporization inductively coupled plasma atomic emission spectrometry determination of rare earth elements(Sc, Y, La and Yb) after separation/preconcentration by a micro column packed with immobilized 1-phenyl-3-methyl-4 bonzoyl-5-pyrazone on micro-crystalline naphthalene has been developed. Various influencing factors, such as the acidity of the aqueous solution, flow rate, volume of the sample, dimension of the micro column were investigated in detail. It was found that acetone could be used to dissolve the adsorbed material packed in micro-column. The detection limits for ETV-ICP-AES determinations of Sc, Y, La and Yb with PMBP as a chemical modifier are 14, 32, 190 and 26 pg/mL. The relative standard deviations were 3.1%, 3.5%, 4.8% and 3.4% for Sc, Y, La and Yb, respectively ( n =9, c =10 ng/mL). The Sc, Y, La and Yb contents in a standard reference material of GBW07602(GSV-2) and a real tea sample determined by the proposed method are satisfactory.