摘要
由于中低含量固定碳的石墨矿石组分比较复杂,各种干扰元素并存,多年来虽然测量方法很多,但步骤都相对繁琐,结果不稳定。本文着重对含碳酸盐和有机碳的中低量固定碳的结构、性质进行深入研究,并对样品的前期处理、酸度选择、温度控制、滴定时间以及干扰去除等项目,进行了条件试验。试验结果表明,对样品采取硝酸处理、低温灼烧,并添加了KMnO4、A1C1,及浓H2SO4的除干扰设备,可以有效去除滴定过程中的多种干扰因素,提高了结果的稳定性和检测效率。该方法用固定碳标准物质进行验证,结果与标准值相符,而且精密度较好,相对标准偏差〈3.08%,回收率在98.2%~102.6%之间,较适宜基层实验室中低含量的固定碳的批量分析测试。
Due to the low content of fixed carbon in graphite ore, the composition is complicated, various kinds of interference elements coexist, over the years while measuring method are many, but all steps, the result is unstable. In view of the fixed carbon containing carbonate and organic carbon, were reviewed in this paper, the structure, properties, the further research, preliminary processing of samples, choice of acidity, temperature control, titration time and, in addition to the interference such as project condition experiment was carried out. The experimental results show that the samples treated by nitric acid and low temperature burning, improve and add the KMnO4, AICI3, and thick - H2SO4 etc. In addition to jamming equipment, can effectively remove various interference factors in the process of titration, greatly improved the stability of the results and efficiency. Validated the method adopt fixed carbon standard material, the result accords with the standard values, and has good precision, RSD 〈 3.08%, recovery rate between 98.2% and 102.6%. More suitable for the laboratory of low content of fixed carbon mass analysis test.
出处
《中国非金属矿工业导刊》
2014年第3期27-29,43,共4页
China Non-Metallic Minerals industry
关键词
非水滴定法
固定碳
除干扰设备
non-aqueous titration
fixed carbon
interference equipment