微波消解-电感耦合等离子体原子发射光谱法测定中低合金钢中铌钨锆钴钒锡

中低合金钢中的铌、钨、锆、钴、钒可以改善钢的性能，提高钢的强度、耐腐蚀性、焊接性能等，而锡则是钢中的有害元素，因此对钢中这些元素的测定十分必要。本文利用微波消解法消解中低合金钢样品，由于溶样的温度和压力提高,样品在硫酸和氢氟酸介质中能够快速和完全地溶解。试样溶解后加入草酸络合铌，硼酸络合过量的氢氟酸，并在配制校准曲线系列溶液时加入与被测试液相同量铁、溶解酸，使校准曲线系列溶液和被测试液中的基体、酸度基本一致以消除基体带来的干扰，然后用电感耦合等离子体原子发射光谱法 （ICP-AES）测定了试液中铌、钨、锆、钴、钒、锡含量。用本法测定了中低合金钢标样中铌钨锆钴钒锡，测定值与认定值吻合，测定结果的相对标准偏差在0.03%～1.2%。

Microwave digestion and inductively coupled plasma atomic emission spectrometric method for the determination of niobium,tungsten,zirconium,cobalt,vanadium and tin in low-medium alloy steel

Niobium,tungsten,zirconium,cobalt and vanadium in low-medium alloy steel could improve the performance of the steel,for example,enhancing the strength,corrosion resistance and weldability.However,tin was a kind of harmful element in the steel.Therefore,it was necessary to determine these elements in steel.The microwave digestion was used for the dissolution of sample in this study.Because of the increase of temperature and pressure of dissolved sample,the sample was dissolved in sulfuric acid and hydrofluoric acid medium quick and completely.Then,oxalic acid and boric acid were added to complex niobium and excessive hydrofluoric acid,respectively.The same amount of iron and acid as in testing solution were added into calibration curve series solutions to make the matrix and acidity in calibration curve series solutions and testing solution consistent.So the interference of matrix effect could be eliminated.Then,the simultaneous determination of niobium,tungsten,zirconium,cobalt,vanadium and tin in testing solution by inductively coupled plasma atomic emission spectrometry(ICP-AES) was carried out.The proposed method was applied to the determination of niobium,tungsten,zirconium,cobalt and vanadium in low-medium alloy steel standard sample,and the determination values were in good agreement with the certified values.The relative standard deviations(RSD) were 0.03%-1.2%.