电感耦合等离子体原子发射光谱法测定增碳剂中钛和钙

研究了增碳剂样品的溶解、分析谱线的选择、共存元素的干扰和介质的酸度对测定的影响,建立了用电感耦合等离子体原子发射光谱法(ICP-AES)测定增碳剂中钛和钙含量的分析方法。样品在马弗炉中灰化后,采用盐酸、氢氟酸、硝酸和高氯酸溶解得到的灰分。以钛和钙标准溶液配制的标准系列溶液建立校准曲线,选择324.199 nm和317.933 nm 波长的谱线作为钛和钙的分析线,在0.6 mol/L盐酸介质中用ICP-AES进行测定。钛和钙的检出限分别为0.04 μg/mL和0.07 μg/mL,线性范围分别为0～20 μg/mL和0～60 μg/mL。方法用于煤、煤矸石、沥青、石油焦等增碳剂中钛和钙的测定,测定值与标样的认定值一致,回收率在96%～105%之间。

Determination of titanium and calcium in recarburizer by inductively coupled plasma atomic emission spectrometry

The effect of sample dissolution, selection of analysis line, interference of coexisting elements and the acidity of medium on the analysis of recarburizer was studied. The determination method of titanium and calcium in recarburizer by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The sample was firstly ashed in muffle furnace followed by dissolution with hydrochloric acid, hydrofluoric acid, nitric acid and perchloric acid. The standard series solutions of titanium and calcium were prepared to plot the calibration curve. The spectral line at 324.199 nm and 317.933 nm were selected as analytical lines for titanium and calcium, respectively. The ICP-AES determination was conducted in 0.6 mol/L hydrochloric acid medium. The detection limit for titanium and calcium was 0.04 μg/mL and 0.07 μg/mL, respectively. The linear range for titanium and calcium was 0-20 μg/mL and 0-60 μg/mL, respectively. The proposed method was applied to the determination of titanium and calcium in recarburizer samples such as coal, gangue, asphalt and petroleum coke. The found results were consistent with the certified values of standard sample. The recoveries were between 96% and 105%.