Department of Environmental Science, Kongju National University, Kongju 314-701, Republic of Korea.
Anal Chim Acta. 2012 Sep 5;741:32-7. doi: 10.1016/j.aca.2012.06.046. Epub 2012 Jul 5.
A robotic method has been established for the determination of bromate in sea water and drinking deep-sea water. Bromate in water was converted into volatile derivative, which was measured with headspace solid-phase micro extraction and gas chromatography-mass spectrometry (HS-SPME GC-MS). Derivatization reagent and the HS-SPME parameters (selection of fibre, extraction/derivatization temperature, heating time and; the morality of HCl) were optimized and selected. Under the established conditions, the detection and the quantification limits were 0.016 μg L(-1) and 0.051 μg L(-1), respectively, and the intra- and inter-day relative standard deviation was less than 7% at concentrations of 1.0 and 10.0 μg L(-1). The calibration curve showed good linearity with r(2)=0.9998. The common ions Cl(-), NO(3)(-), SO(4)(2-), HPO(4)(2-), H(2)PO(4)(-), K(+), Na(+), NH(4)(+), Ca(2+), Mg(2+), Ba(2+), Mn(4+), Mn(2+), Fe(3+) and Fe(2+) did not interfere even when present in 1000-fold excess over the active species. The method was successfully applied to the determination of bromate in sea water and drinking deep-sea water.
已建立一种用于测定海水和深海饮用水中溴酸盐的机器人方法。水中的溴酸盐被转化为挥发性衍生物，然后用顶空固相微萃取和气相色谱-质谱联用（HS-SPME GC-MS）进行测量。优化并选择了衍生试剂和 HS-SPME 参数（纤维选择、萃取/衍生化温度、加热时间和 HCl 的浓度）。在建立的条件下，检测限和定量限分别为 0.016μg/L 和 0.051μg/L，在 1.0 和 10.0μg/L 浓度下，日内和日间相对标准偏差均小于 7%。校准曲线呈良好的线性关系，r(2)=0.9998。即使存在 1000 倍过量的活性物质，常见离子 Cl(-)、NO(3)(-)、SO(4)(2-)、HPO(4)(2-)、H(2)PO(4)(-)、K(+)、Na(+)、NH(4)(+)、Ca(2+)、Mg(2+)、Ba(2+)、Mn(4+)、Mn(2+)、Fe(3+)和 Fe(2+)也不会干扰。该方法成功应用于海水和深海饮用水中溴酸盐的测定。
