乳浊液进样-火焰原子吸收光谱法测定润滑脂中锌和铅

FAAS determination of zinc and lead in lubricating grease with emulsion sampling

将乳浊液进样技术应用于火焰原子吸收光谱法 ,成功地测定了润滑脂中锌和铅。样品用苯、甲基异丁基酮、冰乙酸混合溶剂及硝酸溶解 ,以吐温 -2 0、邻苯二甲酸二丁酯混合乳化剂乳化成乳浊液 ,取适量样品乳浊液 ,加入适量琼脂溶液配制成试液 ,喷入火焰 ,以氘灯进行背景吸收扣除 ,用工作曲线法测定。通过在工作曲线标准系列溶液中加入适量氯化石蜡乳浊液 ,及以同样量的氯化石蜡乳浊液 ,配制成空白溶液作为参比 ,解决了试液与工作曲线标准溶液粘度不同的问题。提出了配制与试液粘度相同的空白溶液的原理及方法。方法简便、快速、准确。

The emulsion sampling technique had been applied to flame atomic absorption spectrometry to determine successfully zinc and lead in lubricating grease. Dissolve samples in mixed solvent of benzene, methyl isobutyl ketone and glacial acetic acid and in concentrated nitric acid, then emulsify sample solution into emulsion with mixed emulsifier of Tween-20 and dibutyl phthalate. Test solutions prepared by adding proper amount of agar solution in appropriate amount of the emulsion were injected into air acetylene flame and working curve method was used to determine with background absorption correction of deuterium lamp. Solve a problem of different viscosity between test solution and standard solutions of working curve by adding proper amount of paraffin chloride emulsion in standard solutions of working curve and with the blank solution prepared by same amount of paraffin chloride as reference. A principle and method of preparing blank solution having the same viscosity with test solution had been advanced. A analytical method for rapid determination of zinc and lead in lubricating grease had been developed. This method is convenient, rapid and accurate.