硫酸硝酸消解iCAP-AES测定锑矿石中锑

Determination of Antimony in Antimony Ore by Sulfuric Acid and Nitric Acid Digestion and iCAP-AES

样品经硫酸和硝酸分解,在10%的硫酸和盐酸的混合介质中,用iCAP-AES测定锑矿石中锑的含量,试样置于聚四氟乙烯(PEFE)坩埚中,加入一定量的硫酸和硝酸分解样品,按照操作流程进行样品消解,消解完成后,加入10%的盐酸和硫酸的混合溶液,定容于50 mL比色管中,用电感耦合等离子体原子发射光谱法(iCAP-AES)测定锑的含量。用此方法测定了3个GBW标准物质,测定结果与标准物质证书值之间的相对误差为0.47%~1.66%,其(n=3)相对标准偏差为≤4.01%。该方法与经典方法相比,检测范围宽、简便快速,结果准确可靠,适应于锑矿石中锑含量的测定。

The sample is decomposed by sulfuric acid and nitric acid, and the antimony content in antimony ore is determined by iCAP-AES in a mixture of sulfuric acid and hydrochloric acid of 10%. The sample is placed in a polytetrafluoroethylene crucible and a certain amount of sulfuric acid and nitric acid is added to decompose the sample, the sample was digested according to the operation prcedure. After digestion, 10% HCl and H;SO;solution was added into the 50 mL colorimetric tube. The antimony content was determined by inductively coupled plasma atomic emission spectroscopy(iCAP-AES). The relative standard deviation(N = 3)of 3 GBW certified reference materials is ≤4. 01% and the relative error is 0. 47%-1. 66%. Compared with the classical method, this method has the advantages of wide detection range, simple and rapid, accurate and reliable results, and is suitable for the determination of antimony in antimony ores.