含钒废触媒除油制样及五氧化二钒测定方法的研究

Study on removing oil from spent vanadium catalyst sample and determination of vanadium pentoxide

废触媒含有大量油渍，粘稠、不易进行分析样品的制备和测定。选用酒精燃烧除油法除去样品中油渍使其成为松散样品，选择样品前处理的最佳温度为500～600℃，对两种测定五氧化二钒方法即直接测定法和两步测定法进行了比较。结果表明，直接测定法测定废触媒中五氧化二钒含量，不需要进行烧失量校正，简化了分析步骤，相对标准偏差为0．18％～0．60％，回收率在98．4％～103．4％之间。分别进行不同实验室之间及ICP—AES法测定结果比较，结果吻合较好，该方法具有较好的适用性和可操作性。

Spent catalyst samples are difficult to be prepared and dissolved for analysis because they usually contain a great deal of sticky oils. A novel method for burning with alcohol to remove oil from samples was provided in this study. The samples became incompact after oil removal. Under the optimal pretreatment temperature of 500--600 ℃, two determination methods of vanadium pentoxide, i. e. direct determination and two-steps determination were compared thoroughly. The results showed that direct determination of vanadium pentoxide in spent catalyst did not need to correct the loss on ignition, simplifying the analysis. The relative standard deviations（RSD） and recovery were 0.18%--0. 60% and 98.4%--103.4%,respectively. The determination results from three laboratories and ICPAES were respectively compared, showing good agreement. This method had excellent applicability and operability.