用增压焖罐溶样及催化极谱测定重油中的镍含量

本文用硝酸为溶剂的增压低温焖罐溶样法代替常规的炭化-灰化法处理渣油样。试验证明,置焖罐于160℃干燥箱中恒温4小时,可得到黄色透明液体,该液体能用于镍的极谱法测定。其优点是,可避免污染,样品用量少,不用高温加热设备。本文优选了丁二酮肟极谱法测定镍的底液,在所试的0～0.05ppm镍浓度范围内呈线性,灵敏度提高4倍多,有限次数测定焖罐溶解重油样中镍含量的相对误差小于7％(相对于AAS和ICP光谱测得值而言),标准偏差<0.97％,变异系数<3.1％,符合要求,方法可行。

THE DETERMINATION METHOD OF NICKEL CONTENT IN HEAVY OIL

The article deals with the replacement of normal carbonization and ashing method for treating heavy oil sample with the dissolving sample method of using nitric acid as solvent in a braising pot with, increasing pressure and low temperature. The experiment shows that the sample contained in the braising pot which is placed in dry oven with constant temperature of 160 centigrade changes into yellow transparent liquid in 4 hours. The obtained liquid can be used to determine nickel and vanadium with polarographic method. This method can prevent the environment from pollution and use less sample. The cond'tions of the bottom liquid for determination of nickel by the polarographic method of dime thylglyoxitne have been optimized. It has been confirmed that there is a linear relation in the range of 0-0.05 ppm of nickel concentration. The measuring sensitivity has increased by 4 times or more. Under the condition of limited determination of nickel content by dissolving heavy oil sample in braising pot the relative error is less than 7% (based on spectral determination values of AAS and ICP), standard deviations less than 0.97, variance coefficients less than 3.1%.