重量法测定二乙基次膦酸铝中磷含量的研究

Determination of Phosphorus in Aluminum Diethylphosphinate by Gravimetric Method

为了建立二乙基次膦酸铝(Al Pi)中磷含量的分析方法,采用磷钼酸喹啉沉淀法(重量分析法),分别探讨氧化剂过硫酸铵的添加量、喹钼柠酮试剂添加量、过滤时采用砂芯漏斗规格等检测条件对磷测定值的影响。结果表明,试样为0. 1～0. 2 g,过硫酸铵添加量为2. 5 g,喹钼柠酮体积为30 m L,选择G4规格的砂芯漏斗过滤时,其结果与理论值更接近,通过精密度试验,精确度高,准确度好,加标回收率为98. 84%～99. 34%,较仪器分析更接近理论值,适用于Al Pi产品磷含量的检测。

To establish an analytical method for phosphorus content in aluminum diethylphosphinate ( AlPi), the quinoline phosphomolybdate precipitation method ( gravimetric analysis) was adopted to investigate and discuss the influence on the measured value of phosphorus by the addition amount of oxidant ammonium persulfate,quimociac reagent, and the specifications of sand core funnel during the filtration.The results suggested: when the sample weighed between 0. 1~ 0. 2 g, the additional amount of ammonium persulfate added was 2. 5 g, and the volume of quimociac was 30 mL, and the result was closer to the theoretical value when the sand core funnel of G4 size was selected for filtration.The precision test suggested that this method had high precision and good accuracy,with the recoveries of the standard addition between 98. 84%~ 99. 34%,which was closer to the theoretical value than the instrumental analysis,making it suitable for the detection of phosphorus content in AlPi products.