Yu Chunhai, Cai Qiantao, Guo Zhong-Xian, Yang Zhaoguang, Khoo Soo Beng
Centre for Advanced Water Technology, Innovation Centre (NTU), Block 2, Unit 241, 18 Nanyang Drive, 637723 Singapore.
Anal Bioanal Chem. 2003 May;376(2):236-42. doi: 10.1007/s00216-003-1895-0. Epub 2003 Apr 11.
Under acidic conditions tellurium(IV) formed a complex with ammonium pyrrolidine dithiocarbamate (APDC). The tellurium(IV) complex was completely retained on a non-polar Isolute silica-based octadecyl (C(18)) sorbent-containing solid-phase extraction (SPE) cartridge, while the uncomplexed Te(VI) passed through the cartridge and remained as a free species in the solution. Only partial Te(IV) was retained on the SPE cartridge for samples without addition of APDC. On the basis of different retention behaviours of the complexed Te(IV) and uncomplexed Te(VI), a simple and highly sensitive method is proposed for the determination of total tellurium and Te(VI) by SPE separation and inductively coupled plasma mass spectrometry (ICP-MS) detection. The Te(IV) concentration was calculated as the difference between total tellurium and Te(VI) concentrations. The detection limit (3 sigma) is 3 ng L(-1) tellurium. Factors affecting the separation and detection of tellurium species were investigated. Coexisting ions did not show significant interferences with the Te(IV)-APDC complex retention and the subsequent ICP-MS detection of Te. The method has been successfully applied to the tellurium speciation analysis in waters with spiked recoveries for Te(IV) and Te(VI) of 86.0-108% and 87.1-97.4%, respectively.
在酸性条件下,碲(IV)与吡咯烷二硫代氨基甲酸铵(APDC)形成络合物。碲(IV)络合物完全保留在含有非极性Isolute硅胶基十八烷基(C(18))吸附剂的固相萃取(SPE)小柱上,而未络合的碲(VI)则通过小柱并以游离态留在溶液中。对于未添加APDC的样品,只有部分碲(IV)保留在SPE小柱上。基于络合的碲(IV)和未络合的碲(VI)不同的保留行为,提出了一种通过SPE分离和电感耦合等离子体质谱(ICP-MS)检测来测定总碲和碲(VI)的简单且高灵敏度的方法。碲(IV)浓度通过总碲浓度与碲(VI)浓度之差来计算。检测限(3σ)为3 ng L⁻¹ 的碲。研究了影响碲形态分离和检测的因素。共存离子对碲(IV)-APDC络合物的保留以及随后ICP-MS对碲的检测未显示出明显干扰。该方法已成功应用于水样中的碲形态分析,碲(IV)和碲(VI)的加标回收率分别为86.0 - 108%和87.1 - 97.4%。