电感耦合等离子体原子发射光谱法测定高纯六氟化钨中13种金属元素  

ICP-AES Determination of 13 Metal Elements in High-Purity Tungsten Hexafluoride

作　　者：郑秋艳[1] 王少波[1] 李绍波[1] 李本东[1] 李翔宇[1] 

机构地区：[1]中国船舶重工集团公司第七一八研究所,邯郸056027

出　　处：《理化检验（化学分册）》2010年第8期952-954,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：提出用电感耦合等离子体原子发射光谱法（ICP-AES）测定高纯六氟化钨中铬、锰、铁、钴、镍、铜、锌、镁、钙、钠、钾、铅及钼等13种金属元素的含量。六氟化钨易与空气中水分反应,为此设计了一套空气隔离的密闭取样系统,其中取样管与取样器采用可溶性聚四氟乙烯材料制成。在减压条件下使液态六氟化钨从储样钢罐中引入透明的取样器中,并观察引入的样品液面的高度估计所取样品的质量。关闭进口阀门,打开出口阀门,使取样器中六氟化钨挥发并进入吸收瓶中,最后向取样器中通入高纯氦使六氟化钨完全挥发并接受于吸收瓶中。根据吸收瓶在吸收六氟化钨前后的质量差可得样品的准确质量,待测的各金属元素则留存于取样器中,先后加入稀氨水、硝酸及氢氟酸使其溶解后,定容至100 mL,供ICP-AES测定。各元素的检出限（3s）均小于0.005 mg.L^-1。方法的回收率为90.5%-104.2%,测定值的相对标准偏差（n=11）为3.2%-7.8%。ICP-AES was applied to the determination of Cr,Mn,Fe,Co,Ni,Cu,Zn,Mg,Ca,Na,K,Pb and Mo in high purity tungsten hexafluoride（WF6）.To prevent the reaction of WF6 with moisture in air,a closed pipeline system for taking the sample was designed.Sample of the liquid WF6 was sucked into the transparent PTFE sample receptor from the sample container until the liquid surface reached to a definite height,from which the sample mass was estimated.The inlet value was closed and the outlet of the sample receptor was opened to let the WF6 vapor to leave the receptor and enter into the absorption bottle and finally high purity helium was passed through the sample receptor to drive WF6 completely into the absorption bottle.The exact sample mass was calculated from the difference of masses of the absorption bottle before and after the absorption of WF6.The metal elements remained in the sample receptor,after the driving of WF6,were dissolved in dil.aqueous ammonia,dil.HNO3 and dil.HF,and the solution was diluted to 100 mL,which was used for ICP-AES determination.Values of detection limit（3s） for the 13 elements mentioned above were all less than 0.005 mg·L-1.Tests for recovery and precision were made,giving values of recovery in the range of 90.5% to 104.2%,and RSD′s（n=11） in the range of 3.2% to 7.8%.

关 键 词：电感耦合等离子体原子发射光谱法 六氟化钨 金属元素 

分 类 号：O657.31[理学—分析化学]