氢化物发生-原子荧光光谱法测定镀锌钢板镀层中痕量锑

通过对仪器测量参数、镀层基体锌、酸度、褪镀液中六次甲基四胺浓度、以及氢氟酸用量等试验条件的研究，建立了镀锌钢板镀层中痕量锑的氢化物发生-原子荧光光谱分析方法。研究表明，锌的基体效应可以通过基体匹配法消除，酸度控制在40%(V/V)，褪镀液中的六次甲基四胺和试样处理中的少量氢氟酸（不超过2 mL）对锑的测定没有影响。锑浓度在0.001～0.1 μg/mL范围内与荧光强度呈良好的线性关系；方法测定下限为0.2 μg/L。方法应用于两个镀锌钢板样品镀层中锑的分析，相对标准偏差（RSD）为1.0%和1.2%，样品加标回收率为96%~101%，测定结果与ICP-MS法一致。

Determination of trace antimony in galvanized plate coatingby hydride generation-atomic fluorescence spectrometry

After investigating the instrument parameters，matrix effect of zinc，concentration of hexamethylene tetramine in stripping solution，degree of acidity and dosage of HF，a new method for determination of trace antimony in coating of galvanized plate by hydride generation-atomic fluorescence spectrometry has been established. The results indicated that matrix effect of zinc was avoided by matrix matching，40% HCl (V/V) was fit for measurement，dosage of HF less than 2 mL needed for digestion of samples and hexamethylene tetramine in stripping solution almost do not influence the determination of antimony. The fluorescence intensity was linear with the concentration of antimony in the range of 0.001-0.1 μg/mL，with detection limit of 0.2 μg/L. The proposed method has been applied for two galvanized plate samples. The relative standard deviation (RSD) was 1.0% and 1.2%. The recovery rate of antimony was 96%-101%. The results of this method were in a good agreement with those obtained by ICP-MS.