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A combined isopiestic and sub-boiling distillation method for the purification of hydrofluoric acid used for ICP-MS elemental analysis

机译:等渗和超沸混合蒸馏方法用于ICP-MS元素分析的氢氟酸的纯化

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摘要

Purification of hydrofluoric acid (HF) has been achieved by the combination of isopiestic and sub-boding distillation. For better yield and purity, the collection vessel's position is optimized. The distillation assembly is made from polyethylene which is available in any chemical laboratory. Impure acid (100 mL) is placed in a 1-L HDPE container and the collection vessel (PTFE beaker) containing 25 ml, pure water is kept inside the container on a perforated stand. The whole distillation set-up is heated in a water bath at 80 degrees C. After eight hours, 35 ml, of pure HF of similar to 40% strength is obtained from 100 ml, of impure 48% HF. The production of high purity HF can be increased by increasing the volume of the feed HF. The impurities in pure acid are preconcentrated in an in situ evaporating system and determined by ICP-MS after suitable dilution. The levels of impurity are in the sub-ng/g to ng/g range and the purity of the acid is close to a commercially available pure (Suprapur(R)) grade HF with respect to Cd, Co, Cr, Cu, Ga, In, Mg, Mn, Ni, Pb, Sr, and Zn.
机译:氢氟酸(HF)的纯化已通过等量蒸馏和次缩合蒸馏的组合实现。为了提高产量和纯度,优化了收集容器的位置。蒸馏组件由聚乙烯制成,可在任何化学实验室中使用。将不纯酸(100 mL)放入1 L HDPE容器中,并将装有25 ml纯水的收集容器(PTFE烧杯)放在带孔架子的容器内。将整个蒸馏装置在水浴中在80摄氏度下加热。八小时后,从100毫升不纯的48%HF中获得35毫升强度近似于40%的纯HF。可以通过增加进料HF的体积来增加高纯HF的产量。将纯酸中的杂质在原位蒸发系统中进行预浓缩,并在适当稀释后通过ICP-MS测定。杂质的含量在ng / g到ng / g范围内,酸的纯度相对于Cd,Co,Cr,Cu,Ga接近市售纯净(HF)级HF。 ,In,Mg,Mn,Ni,Pb,Sr和Zn。

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