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迄今为止,纯钙中微量杂质元素的分析国外少见报导。国内已有的资料是用电感耦合高频等离子炬光谱测定金属钙中的7个杂质元素;用原子吸收光度法测定锂、钠、钾、镁、铁、锰、铜等10个杂质元素。前者可测定10毫克/毫升钙试液中的0.1—10微克/毫升的杂质元素,但仪器昂贵、成本高、不易推广。后者虽不经分离,手续简便,但只能用于纯度不太高的金属钙的分析。其灵敏度不高的原因,主要来自大量基体钙所造成的光散射的干扰。因此,分离基体是消除干扰、改善测定下限的主要途径。本文选择在弱酸性介质中,用草酸沉淀基体钙的简便分离方法,以空气/乙炔火焰同时测定微量锰、铜、铁、镍,其灵敏度(1%吸收)分别为0.05微克/毫升、0.1微克/毫升、0.1微克/毫升、0.1微克/毫升。回收率在93—102%之间。可满足99.99%以下金属钙的分析。一、仪器与试剂WFD-Y2原子吸收分光光度计。锰、铜、铁、镍空心阴极灯。
So far, trace impurities in pure calcium analysis of rare foreign reports. The available data in the country is the determination of seven impurity elements in metallic calcium by inductively coupled high frequency plasma torch spectrometry; and the determination of ten impurity elements such as lithium, sodium, potassium, magnesium, iron, manganese and copper by atomic absorption spectrophotometry. The former can be measured 10 mg / ml calcium test solution of 0.1-10 micrograms / ml of impurity elements, but the instrument is expensive, high cost, not easy to promote. Although the latter is not separated, the procedure is simple, but only for the analysis of metal calcium is not too high purity. The reason is not high sensitivity, mainly from a large number of matrix light scattering caused by interference. Therefore, the separation of the matrix is to eliminate interference and improve the lower limit of the main way. In this paper, a simple method for the precipitation of matrix calcium with oxalic acid was proposed in this paper. Simultaneous determination of trace amounts of manganese, copper, iron and nickel with air / acetylene flame was carried out in a weakly acidic medium with sensitivities (1% absorption) of 0.05 μg / ml and 0.1 μg / Ml, 0.1 μg / ml, 0.1 μg / ml. The recovery rate is between 93-102%. 99.99% to meet the following analysis of metal calcium. First, instruments and reagents WFD-Y2 atomic absorption spectrophotometer. Manganese, copper, iron, nickel hollow cathode lamp.