电感耦合等离子体光谱法测定煤中铍镓磷

Determination of Be,Ga and P in Coal by Inductively Coupled Plasma Optical Emission Spectrometry(ICP-OES)

提出电感耦合等离子体光谱法测定煤炭中铍、镓、磷元素的分析方法,即结合煤样处理、煤样加标灰化、消解方法选择等样品处理试验,从样品加标回收率、氢氧化钙悬浊液对测试的影响、酸溶方式的影响等方面分析煤样的加标回收试验,探讨了使用氢氟酸-硝酸-高氯酸中低温消解样品时煤中微量元素铍、镓是否生成氯化物损失,并给出了电感耦合等离子体光谱法的检出限及样品测试的精密度。在射频功率提高至1350W的情况下,仪器检出限铍元素为0.0006mg/L、镓元素为0.024mg/L、磷元素为0.29mg/L,相对标准偏差在0.24%~1.95%。煤样氢氧化钙处理后,铍元素的平均加标回收率为94%~98%。实验证明:电感耦合等离子体光谱法具有较高的精密度及较低的检测限,方法准确、可靠,适用于煤样品中铍、镓、磷元素的同时测定。

An analytical method for the determination of beryllium, gallium and phosphorus in coal by ICP-OES was presented, combining with coal sample treatment, coal sample standard material adding ashing and digestion method, from aspects such as sample standard material adding recovery rate, effect of calcium hydroxide suspension on determination and effect of acid-soluble methods, the coal sample standard material adding recovery experiment was analyzed, this paper discussed whether the trace elements beryllium and gallium in coal would generate chloride loss when hydrofluoric acid-nitric acid-perchloric acid was used for sample digestion at medium and low temperature, and detection limit of ICP-OES and the accuracy of sample test were given. When the RF power was increased to 1 350 W, the detection limit of the instrument was 0.000 6 mg/L for beryllium, was 0.024 mg/L for gallium, and was 0.29 mg/L for phosphorus;the relative standard deviation was between 0.24%~1.95%. The average standard material adding recovery rate of beryllium after calcium hydroxide treatment was 94%~98%. The experimental results showed that this method has higher precision and lower detection limit, and it is accurate and reliable. It is suitable for simultaneous determination of beryllium, gallium and phosphorus in coal samples.