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Indirect determination of iodide by tungsten coil atomic emission spectrometry

机译:钨线圈原子发射光谱法间接测定碘

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The spectroscopic determination of iodide is a difficult challenge, especially in small sample volumes.Thestrongest transition lines for this element lie in the vacuum ultraviolet region of the spectrum, so mostconventional instruments produce very weak signals. This work describes a tungsten coil atomic emissionprocedure for the indirect determination of iodide.A 25 μl aliquot of a solution containing a known amountof indium is deposited on the tungsten coil and dried with a simple heating program.Once the coil is dry,25 μl of an iodide solution is added to the coil.The solution is dried and vaporized at high current.The atomicemission signal for In at 451.1 nm is monitored. In the presence of iodide,InI is formed and the In emission signal is attenuated.This attenuation is proportional to iodide concentration with a method detection limit of0.6 mg l1 iodide using an In concentration of 10 mg l1,and 3 mg l1 iodide using an In concentration of50 mg l1.Linear calibration curves span a range of two orders of magnitude.Analysis of a deionized water sample spiked with 50 mg l1 iodide gives a recovery of 100% and a precision of 5.5% relative standarddeviation.Analysis of a tap water sample spiked with 50 mg l1 iodide gives a recovery of 140% and a precision of 7.1% relative standard deviation.The poor accuracy for the tap water analysis may arise from thereaction of In with other halides in the sample.This is the first report of determination of a halogen using thetungsten coil atomizer.
机译:碘化物的光谱测定是一项艰巨的挑战,尤其是在小样本量中。该元素最强的跃迁线位于光谱的真空紫外区域,因此大多数常规仪器产生的信号非常微弱。这项工作描述了用于间接测定碘的钨线圈原子发射程序。将25μl等分试样的包含已知量铟的溶液沉积在钨线圈上,并通过简单的加热程序进行干燥。一旦线圈干燥,就将25μl将碘化物溶液添加到线圈中,将溶液干燥并在大电流下蒸发。监测451.1 nm处In的原子发射信号。在存在碘化物的情况下,会形成InI并减弱In发射信号。此衰减与碘化物浓度成正比,使用10 mg l1的In浓度时的方法检出限为0.6 mg l1碘化物,使用10 mg l1的碘化物时为3 mg l1碘化物浓度为50 mg l1时,线性校准曲线跨越两个数量级的范围。对掺有50 mg l1碘化物的去离子水样品进行分析,回收率达到100%,相对标准偏差的精度为5.5%。加标50 mg碘化物的水样品的回收率为140%,相对标准偏差的准确度为7.1%。自来水分析的准确性差可能是由于In与样品中其他卤化物的反应所致。钨线圈雾化器测定卤素的方法

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