Lead speciation in rainwater samples by modified fused silica capillaries coupled to a direct injection nebulizer (DIN) for sample introduction in ICP-MS

Lead speciation using modified silica capillaries for the introduction of l iquid samples to a direct injection nebulizer of an inductively Coupled pla sma quadrupole mass spectrometer is described and demonstrated. The fused s ilica capillaries were coated by covalently bonding a cation exchange activ e organic molecule to the activated capillary surface. The best results wer e obtained by introducing it bifunctional reagent in a prior step. In this case, a silane reagent was chosen which acted as a methacrylic acid group f or further binding. The influence of the chemical modification of the surfa ce of the sample capillary or the DIN oil the selective retention or inorga nic lead (Ph2+) and triethyllead (Et3Pb+) and hence separation and quantifi cation has been investigated. The strong cation exchanger covering has been tested for its stability over a wide rill range (2-9). The interaction of Et3Pb+ with the strong cation exchanger was negligible while the inorganic lead can be selectively retained at pH > 7. Upon flushing with 10(-2) mol L (1) hydrochloric acid, the capillary can be easily regenerated. In order t o remove retained inorganic lead several eluents were investigated. Paramet ers affecting the inorganic and organic lead separation such as sample pH, carrier solution, eluent strength. sample size and flow rate characteristic s were studied in addition to optimal DIN-ICP-MS conditions. The detection limits for triethyllead and for inorganic lead were 90 and 200 ng L-1 respe ctively, i.e., absolute detection limits or 0.3 and 0.6 pg respectively. In order to demonstrate the capability of the technique for the analysis of a n environmental matrix, a sample of artificial rainwater was analysed.