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非完全消化-火焰原子吸收光谱法测定润滑油中钙锌
FAAS Determination of Calcium and Zinc in Lubricating Oil with Incomplete Digestion of Sample
【摘要】 在低温加热的条件下,油样用浓硝酸消化,所得试液中加入适量Triton X-100及Tween 80使乳化从而得到均匀的透明或半透明的呈橙黄色或黄绿色的试样溶液,供火焰原子吸收光谱法(FAAS)测定钙及锌。对非完全消化所用的酸和乳化剂的选择和FAAS测定中的化学干扰、背景干扰以及空白溶液及试样溶液粘度的一致性等分析条件进行了试验和优化。钙及锌两元素的线性范围依次为0~12 mg.L-1和0~1.6 mg.L-1,检出限(3σ/s)依次为0.14 mg.L-1及0.018 mg.L-1。此方法应用于润滑油实样分析,所得两元素分析结果的RSD(n=6)值均小于5%,回收率均在100.0%~102.1%之间。
【Abstract】 The lubricating oil sample was digested with conc.HNO3 under moderate heating,and the sample solution obtained after incomplete digestion was emulsified with Triton X-100 and Tween 80 to make it a homogeneous and transparent or semitransparent,yellowish orange or yellowish green colored solution.The solution was diluted to 25 mL in a volumetric flask and used for FAAS determination of calcium and zinc.Analytical conditions,including the acid and emulsifying agent used in the in complete digestion of sample as well as the chemical interferences,background interference and consistency of viscosities between blank solution and sample solution were studied and optimized.Linear relationships between the absorbance and concentration of calcium and zinc were obtained in the ranges of 0-12 mg·L-1 and 0-1.6 mg·L-1 respectively.Detection limits(3σ/s) of the method were found as 0.14 mg·L-1(for Ca),and 0.018 mg·L-1(for Zn).In its application to the analysis of substantial oil samples,values of RSD′s(n=6) obtained were less than 5%,and values of recovery test were in the range of 97.0%-104.8% for both elements.
【Key words】 FAAS; Incomplete sample digestion; Lubricating oil; Calcium; Zinc;
- 【文献出处】 理化检验(化学分册) ,Physical Testing and Chemical Analysis(Part B:Chemical Analysis) , 编辑部邮箱 ,2007年05期
- 【分类号】TE622.1
- 【被引频次】6
- 【下载频次】103