电感耦合等离子体原子发射光谱法同时测定磷矿中12种组分

样品采用偏硼酸锂熔剂,加入溴化锂脱模剂、硝酸锂氧化剂在1 050℃高频熔样机上熔融4min,硝酸酸化提取定容后,采用基体匹配法配制校准曲线消除基体效应的影响,选取高盐雾化器进样直接用电感耦合等离子体原子发射光谱法(ICP-AES)测定磷矿中五氧化二磷、氧化镁、氧化铁、氧化铝、二氧化硅、氧化钙、氧化钾、氧化钠、二氧化钛、氧化锰、氧化锶、总硫。试验进行了熔剂与样品的稀释比、脱模剂选择、氧化剂选择、熔样温度、熔样时间、溶液酸度和溶液稳定性等条件试验,确定了最佳试验条件。方法检出限为0.000 2~0.025 8μg/g。按照实验方法测定磷矿样品中五氧化二磷、氧化镁、氧化铁、氧化铝、二氧化硅、氧化钙、氧化钾、氧化钠、二氧化钛、氧化锰、氧化锶、总硫,结果的相对标准偏差(RSD,n=11)为0.48%~1.3%。按照实验方法测定GBW 07210、GBW 07211、GBW 07212共3个磷矿石标准样品中五氧化二磷、氧化镁、氧化铁、氧化铝、二氧化硅、氧化钙、氧化钾、氧化钠、二氧化钛、氧化锰、氧化锶、总硫,测定值与认定值(或者国家标准方法 GB/T 1880—1995的测定值)基本一致。

Simultaneous determination of twelve components in phosphate ore by inductively coupled plasma atomic emission spectrometry

The sample was fused in high frequency fusion machine at 1 050 ℃ for 4 min using lithium metaborate as flux, lithium bromide as releasing agent and lithium nitrate as oxidizing agent. After acidification and extraction with nitric acid, the solution was diluted to the mark. The influence of matrix effect was eliminated by preparing calibration curves using matrix matching method. The high salt nebulizer injection was adopted for the direct determination of phosphorus pentoxide, magnesium oxide, iron oxide, aluminum oxide, silicon dioxide, calcium oxide, potassium oxide, sodium oxide, titanium dioxide, manganese oxide, strontium oxide and total sulfur in phosphate ores by inductively coupled plasma atomic emission spectrometry (ICP-AES). The conditional tests were conducted, including the dilution ratio between flux and sample, selection of releasing agent, selection of oxidizing agent, sample fusion temperature, sample fusion time, pH and stability of solution. The optimal experiment conditions were obtained. The detection limits of method were between 0.000 2 μg/g and 0.025 8 μg/g. The content of phosphorus pentoxide, magnesium oxide, iron oxide, aluminum oxide, silicon dioxide, calcium oxide, potassium oxide, sodium oxide, titanium dioxide, manganese oxide, strontium oxide and total sulfur in phosphate ore sample was determined according to the experimental method. The relative standard deviations (RSD, n=11) were between 0.48% and 1.3%. The content of phosphorus pentoxide, magnesium oxide, iron oxide, aluminum oxide, silicon dioxide, calcium oxide, potassium oxide, sodium oxide, titanium dioxide, manganese oxide, strontium oxide and total sulfur in three certified reference materials (GBW 07210, GBW 07211 and GBW 07212) was determined according to the experimental method. The found results were consistent with the certified values (or those obtained by national standard method GB/T 1880—1995).