[Study on the solid sorbent tube for capturing mercury in the workplace air and determination by cold vapor atomic absorption spectrometry].

A new KMnO4-MnO2 solid multisorbent tube for capturing mercury in workplace air was developed. Experimental conditions for solid multisorbent tube, efficiency of sampling, desorption efficiency and stability were studied. Mercury and its compounds in air were captured by solid KMnO4-MnO2 sorbent filled tube and desorbed with 0. 90 mol L-1 sulfuric acid solution. Mercury and its compounds were quantitatively analyzed according to the method of GBZ/T 160. 14-2004 cold vapor atomic absorption spectrometry. The linear range of the proposed method was 0. 000 2-0. 015 0 mg L-1 with r=0. 999 1, the average efficiency of sampling was 99. 9%-100. 0% in the concentration range of 0. 001-2. 820 mg m-3 , and the breakthrough capacity was more than 505.4 microg for 300 mg KMnO4-MnO2 solid multisorbent, the average recovery rate was 96. 4% approximately103. 8%, the intra-day and inter-day precision was 3. 0% approximately 3. 3% and 3. 5% approximately 5. 2% respectively, the limit of detection was 0. 0013 mg m-3 (7. 5 L of air ) and 0. 000 6 mg m-3 (96 L of air), after sampling, and the solid multisorbent tube could be kept at least 30 d at room temperature without significant loss. The present method was simple and suitable for capturing mercury and its compounds in the workplace air and ambient air. The solid multisorbent tube was useful for personal sampling and time weighted average sampling.

Magnetic single-walled carbon nanotubes-dispersive solid-phase extraction method combined with liquid chromatography-tandem mass spectrometry for the determination of paraquat in urine.

In this study, magnetic single-walled carbon nanotubes (MSWCNTs) were prepared by impregnating magnetic Fe3O4 nanoparticles onto the surfaces of carboxylic single-walled carbon nanotubes based on electrostatic interactions. The prepared MSWCNTs were used as the adsorbent for the dispersive solid-phase extraction (DSPE) of paraquat from human urine. After adsorption, the paraquat was quantitatively desorbed with 5%TFA in acetonitrile and determined by HPLC-MS. Extraction parameters such as the type of CNT adsorbent, extraction time, sample volume, wash solvent, and the type and volume of desorption solvent were optimized to obtain high DSPE recoveries and extraction efficiencies. Under the optimized conditions, the calibration curve was linear in the range 3.75-375.0 µg/L with a correlation coefficient of 0.999 45. The LOD (S/N=3) and LOQ (S/N=10) were 0.94 and 2.82 µg/L, respectively. The recoveries ranged from 92.89 to 108.9% for spiked real urine samples with RSDs below 3.21%. Finally, the new method was successfully used to determine paraquat in urine samples of suspected paraquat poisoning patients. The MSWCNTs exhibited suitable properties and a high adsorption capacity for the extraction of paraquat.