测定润滑油添加剂中钙钡的乳浊液进样-火焰原子发射光谱法

Determination of Calcium and Barium in Lube Additivesby Emulsion Sampling-Flame Atomic Emission Spectrometry

将乳浊液进样技术应用于火焰原子发射光谱法 ,建立了测定润滑油添加剂中钙和钡的灵敏、快速分析方法。对乳化剂的选择、化学干扰的消除、空白溶液的选择及检出限进行了考察。将样品的苯溶液用乳化剂OP乳化成乳浊液 ,取适量样品乳浊液加入适量琼脂溶液及释放剂配制成试液 ,喷入火焰 ,用标准加入法测定。该法的测定结果与灰化 -火焰原子发射光谱法一致 ,相对误差小于±2.9 %,t检验表明两种方法之间无显著性差异。方法的相对标准偏差小于2.7%,检出限:钙0.12mg/L、钡0.99mg/L。

A rapid and sensitive analytical method for the determination of calcium and barium in lube additives has been developed by emulsion sampling- flame atomic emission spectrometry. The test solution is prepared by solving the sample in benzene, emulsifying the solution with emulsifier OP and then adding proper amounts of agar solution and releasing agent La(Ⅲ)to the emulsion. Choice of emulsifier and blank solution, elimination of chemical interference were studied. Standard addition method is used for the determination. The determination results are consistent with those obtained by ashing method. The relative errors between them are less than ±2.9%. The t _ test showed that no significant difference was found between the results obtained by the two methods. RSD of the method is less than ±2.7%. The detection limit are 0.12 mg/L for calcium and 0.99 mg/L for barium.