难溶高碳合金钢消解方法的探讨

采用盐酸和硝酸并利用微波消解法完全消解难溶高碳合金钢,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定其中的主要合金元素含量。试验对消解方法、消解试剂的选择及用量、水用量对高硅样品消解的影响、微波消解程序等进行了探讨。最终确立了最佳消解条件为:称取0.2g样品,依次加入10.0mL水、5.0mL盐酸、5.0mL硝酸,在目标温度达到180℃条件下进行微波消解处理。而对于硅质量分数在1.0%以上的高硅难溶高碳合金钢样品,应适当增加水用量。按照实验方法处理多个难溶高碳合金钢样品,并采用ICP-AES测定其中的主要合金元素Si、Mn、Ni、Cr、Mo、V,结果的相对标准偏差(RSD,n=8)为0.23%~4.7%;按照实验方法处理4个难溶高碳合金钢标准样品,并使用ICP-AES测定Si、Mn、Ni、Cr、Mo、V,测定结果与认定值相吻合。

Discussion on digestion method of refractory high carbon alloy steel

The refractory high carbon alloy steel was completely digested in hydrochloric acid and nitric acid by microwave digestion. The content of major alloy elements was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The digestion method, the selection and dosage of digestive reagent, the effect of water dosage on digestion of high-silicon sample, and the microwave digestion procedures were discussed. The optimal digestion conditions were finally obtained as below: 0.2 g of sample was weighed, and then 10.0 mL of water, 5.0 mL of hydrochloric acid and 5.0 mL of nitric acid were added successively. The sample was treated by microwave digestion at 180 ℃. For the refractory high carbon alloy steel samples containing high-silicon (the mass fraction of silicon was higher than 1.0%), more water should be added. Several refactory high carbon alloy steel samples were treated according to the experimental method, and the content of main alloy elements (Si, Mn, Ni, Cr, Mo and V) was determined by ICP-AES. The relative standard deviations (RSD, n=8) were between 0.23% and 4.7%. Four standard samples of refractory high carbon alloy steel were treated according to the experimental method. The content of Si, Mn, Ni, Cr, Mo and V was determined by ICP-AES. The found results were consistent with the certified values.