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锑白粉(主体Sb_2O_3)中微量杂质元素的光谱分析,一般采用化学光谱法,先以化学法分离杂质元素再进行光谱测定。因此手续繁琐,且易受污染。我们试验了直接测定锑白粉中的Si、Ti、Pb、Mg、Mn、W、Cr、Fe、Bi、Al、Mo、Ca、Cu十三种杂质元素的方法。用碳粉为载体,四硼酸钠为缓冲剂,在10安培电流下能有效控制易挥发元素Sb_2O_3的喷溅,稳定了弧温,提高了分析灵敏度。此法简便,准确度高,相对标准偏差在10%以下。试验部分一条件选择选定影响分析灵敏度较大的困素如电极头规格、激发电流、试样与碳粉的配比等予以试验。试验结果表明,φ4×4mm杯形电极分析灵敏度较高;随着电流的增大,大部分元素的灵敏度也提高。本法最后选用终电流为10安培,试样与碳粉的配比为1:1。
Antimony white powder (main body Sb_2O_3) trace impurities in the spectral analysis, the general use of chemical spectroscopy, chemical separation of impurities before the first spectral determination. Therefore, the procedure is tedious and easily contaminated. We tested the direct determination of antimony white powder Si, Ti, Pb, Mg, Mn, W, Cr, Fe, Bi, Al, Mo, Ca, Cu thirteen kinds of impurity elements. Using carbon powder as carrier and sodium tetraborate as buffer, the splatter of volatile element Sb_2O_3 can be effectively controlled under the current of 10 A, the arc temperature is stabilized, and the analysis sensitivity is improved. This method is simple, high accuracy, the relative standard deviation of 10% or less. The experimental part of a conditional selection of factors affecting the analysis of the sensitivity of the larger factors such as the tip specifications, excitation current, the ratio of sample and toner to be tested. The experimental results show that the sensitivity of the cup-shaped electrode of φ4 × 4mm is high, and the sensitivity of most of the elements increases with the increase of the current. The final choice of this law the final current of 10 amps, sample and toner ratio of 1: 1.