微波消解-电感耦合等离子体原子发射光谱法(ICP-AES)测定高速工具钢中锰、磷、镍、铜、铬、钒

高速工具钢为高碳高合金工具钢,常温下样品酸溶分解较为困难,因此建立了微波消解电感耦合等离子体原子发射光谱法(ICP-AES)测定高速工具钢中锰、磷、镍、铜、铬、钒的方法,利用微波消解提高溶样的温度和压力,在王水、氢氟酸和硫酸介质中使样品充分消解,再用饱和硼酸溶液络合过量的氢氟酸,基体匹配消除铁基体的影响,ICP-AES法同时测定锰、磷、镍、铜、铬、钒的含量。测定高速工具钢标准样品,测定值与标样值相吻合,方法的相对标准偏差在0.55%~4.1%。加标回收率在95.6%~114.8%,满足测定要求。

Determination of Manganese,Phosphorus, Nickel,Copper, Chromium and Vanadium in High-Speed Tool Steel by ICP-AES Together with Microwave Digestion Technique

High speed tool steel is a kind of high alloy tool steel with high carbon and is dissolved at room temperature. In this paper, a microwave digestion ICP-AES method was determine Manganese, Phosphorus, Nickel, Copper, Chromium and Vanadium in high speed using microwave digestion technique, digestion temperature and pressure were increased. difficult to be established to tool steel. By Samples were fully digested in hydrofluoric acid, sulfuric acid and aqua regia medium. To eliminate the excess of hydrogen fluoride acid, saturated boric acid solution was added to the solution to form complex with the hydrogen fluoride acid. Through matrix matching, influence of the iron matrix was eliminated and thus ensured the application of ICP-AES method to simultaneously determine the contents of manganese, phosphorus, copper, nickel, ,chromium, vanadium. High speed tool steel standards were tested and the measured value was consistent with the certified values. The precisions of this method were in the range of 0.55% -4.1% and the recoveries were between 95.6O,/oo and 114.8%. This method can meet the requirements for analysis of high speed tool steel.