Uv-induced Chemical Vapor Generation - Effective And Robust Interface Coupling Hplc With Afs And Icp-ms For Determination Of Selenium And Mercury Speciation

Elements in the environment and morphological analysis in biological analysis is especially important, because the element toxicology effect, beneficial effects, in biological metabolic mechanism and transform rule in the environment of migration in to a large extent depend on the elements in chemical form, also in the samples in a certain extent and related form physical solubility and volatile relevant. Environmental and biological samples morphological analysis has become environmental analysis chemistry and environment toxicology research focus.This paper mainly studies high-performance liquid chromatography coupled with atomic spectrometry/mass spectrometry, by ultraviolet induction vapor generation device for interface, in view of the different sample matrix, has established an online analysis method for mercury and selenium speciation, the main work and the conclusions are as follows:A novel UV vapor generation interface was developed to provide an effective and robust sample introduction unit for high-performance liquid chromatography system coupled to atomic fluorescence spectrometry (HPLC-CVG-AFS) for determination mercury speciation. Experiments on the height of atoms, flow rate of carrier gas, flow rate of shielding gas, reducing agent concentration, flow rate of reducing agent, the selection of high performance liquid chromatography mobile phase, flow rate of HPLC mobile phase, high performance liquid chromatography retention time, acidity of sample, sample substrate influence to carry on the condition experiment highly, and find the optimal value. Under the optimized experiment conditions, the methyl mercury and the inorganic mercury's fluorescence signal and the density become the linear relationship in 0¹00 ng·mL^-1, the linear correlation coefficient respectively are 0.9928, 0.9999. Detection limit of methyl mercury and inorganic mercury are 1.02 and 1.16 ng·mL^-1, respectively. The accuracy is 3.0% and 1.6%, respectively. And determined the methyl mercury content in the fish sample with the establishment method, the recovery of the methyl mercury is 81⁸9 percent. The method was validated with the certified reference material(DORM-2)with satisfactory results. The equipment is simple, the sensitivity is high, can be used for rapid detection of mercury species in the biological sample.A novel UV vapor generation interface was developed to provide an effective and robust sample introduction unit for high-performance liquid chromatography system coupled to inductively coupled plasma mass spectrometry (HPLC-CVG-ICP–MS) for determination mercury speciation. The capability of the system was evaluated by inorganic mercury (iHg) and methylmercury (MeHg). Under the optimized experiment conditions, the detection limits (as Hg), based on three times the standard deviation of a standard solution, 0.0106 ng·mL^-1 for inorganic mercury and 0.0093 ng mL^-1 for MeHg were obtained, with an injection volume of 100μL. And analyzed quantitatively by area normalization, the reproducibility (n=10) is 0.72% and 0.66% for 6 ng·mL^-1 inorganic mercury and 6 ng·mL^-1 MeHg, respectively. After 4 hour continuous sample introduction, no carbon was deposited on the tip of the interface cones. The method was validated with the certified reference material (DORM-2) with satisfactory results. This interface was applied to determination of mercury speciation in a fresh lake water sample. The recovery was 80¹20 percent for spark lake water. Results show that the UV photo-CVG HPLC-ICP-MS connection System is the best choice for ultratrace mercury detection for its superior detectability, high effective, quick speed of analysis, simple, low cost, environmentally friendly, continuous monitoring on-line in the complex system and freedom from interference.Occurs by the ultraviolet ray induction chemistry vapor generation as interface and increases the ultraviolet photooxidation digestion system to further digest organic selenium into inorganic selenium, combined with high performance liquid chromatography and atomic fluorescence establish HPLC CVG-AFS coupled system-form of selenium is analyzed, and using external hydrogen generator for argon hydrogen flame provide hydrogen, ensure the purity hydrogen supply and stability, reduced the flame noise effectively, effectively reduced the flame noise and improve the instrument detect limit enhances testing precision. The antithetical couplet each subsystem's different parameter carries on the optimization with the system, and the system's performance is evaluated with Se (Ⅳ) the +Se-Cys+Se-Met selenium mix standard solution. Under optimization experimental conditions, Se (Ⅳ), Se-Cys and Se-Met detect limit are 6.60, 11.40 and 45.60 ng·mL-1, respectively. The accuracy (n=11) is 0.60%, 2.1% and 1.0%, respectively. Determination of selenium species in yeast piece with this system, the recovery was 95%¹06%. The results show that ultraviolet light induced chemical vapor generation HPLC-AFS coupled system can be used in the determination of trace selenium species online, the method has the equipment small advantage, the operating cost inexpensively, easy to be realized, etc.Establishes HPLC-CVG-ICP-MS selenium species online analysis method, combined Dynamic Reaction Cell (DRC) to eliminate the spectrum disturbance which causes by 39Ar39Ar+ to 78Se+. The antithetical couplet each subsystem's different parameter carries on the optimization with the system, and the system's performance is evaluated with Se (Ⅳ) the +Se-Cys+Se-Met selenium mix standard solution. Under optimization experimental conditions, Se (Ⅳ), Se-Cys and Se-Met detect limit are 0.07, 0.12 and 0.50 ng·mL^-1, respectively. The accuracy (n=11) is 0.90%, 1.3% and 1.8%, respectively. Determination of selenium species in yeast piece with this system, the recovery was 95%⁹8%. The results show that ultraviolet light induced chemical vapor generation HPLC-ICP-MS coupled system suitable for rapid, batch determination of trace selenium species.