加氧系统进样-电感耦合等离子体原子发射光谱法测定抗燃油中的8种磨损金属的含量

Determination of 8 Worn Metals in Fire-Retardant Oil by ICP-AES with Oxygen Adding System

取适量于60℃均匀化的样品（称准至±0．1mg），必要时按一定比例加入基础油稀释后再加入含有钴内标的航空煤油稀释至要求体积。此作为样品溶液用电感耦合等离子体原子发射光谱法测定其中铁、镍、铜、钒、锌、锰、铬及铝等8种磨损金属的含量。仪器带有加氧系统，以流量40mL·min^-1供氧以除去矩管积碳。选择上述8种元素的分析谱线依次为259．94，217．467，324．754，311．837，213．856，257．610，283．563，308．22nm。8种磨损，金属的线性范围均为100．0mg·L^-1以内，方法的检出限（3s）在0．0021-0．056μg·g^-1之间。在3个浓度水平上对方法的回收率进行试验，测得回收率在99．59／6-1089／6之间，测定值的相对标准偏差（n=10）在0．16％-2．0％之间。

The oil sample was homogenized at 60℃, and an appropriate amount （weighed to the nearest ＋0. 1 mg） of the sample was taken. The sample, if necessary, was diluted with the base oil at a definite ratio, and the total volume of the oil sample was controlled at a required value by adding aviation kerosene which contains cobalt as internal standard. 8 worn metals, i. e. , Fe, Ni, Cu, V, Zn, Mn, Cr and Al, in the oil sample were determined by ICP-AES appended with an oxygen-adding system which supplies oxygen at a flow rate of 40 mL·min^-1 to have the clogging of the torch-tube by carbon eliminated effectively. The analytical spectral lines chosen for the 8 worn metals were 259. 94, 217. 467, 324. 754, 311. 837, 213. 856, 257. 610, 283. 563, 308. 22 nrn respectively. Linearity ranges of the 8 worn metals was found in the same range within 100. 0 mg·L^-1 with detection limits （3s） in the range of 0. 002 1-0. 056μg·g^-1. Test for recovery was made at 3 concentration levels, giving values of recovery in the range of 99. 5%-108%, with values of RSD＇s （n=10） ranged from 0.16% to 2.0%.