1.南昌大学资源环境与化工学院，南昌 330031； 2.台州市台环环境检测科技有限公司，浙江台州 318020
Determination of bismuth in soil and sediment by atomic fluorescence spectrometry
ZHOU Zikai12, BAO Yifan2, YE Changlin2
1. School of Resources Environmental & Chemical Engineering, Nanchang University, Nanchang 330031, China; 2. Taizhou TaiHuan Environmental Detection Technology Co., Ltd., Taizhou 318020, China
摘要：为改进现有国家标准(HJ 680-2013)检测方法，采用水浴法消解样品，用原子荧光法测定土壤和沉积物中痕量铋。以国家一级土壤成分分析标准物质GSS-16，GSS-17，GSS-23与台州农业、建筑用土和管道淤泥沉积物样品为试验对象，探讨13种混合酸消解体系对复杂样品痕量铋测定结果的影响，筛选得到检测痕量铋含量的最佳实验条件。以盐酸-硝酸-硫酸(体积比为1∶3∶2)三酸体系为消解液，消解时间为0.5 h，总处理时间为2.0 h。铋的质量浓度在0.1～10.0 μg/L范围内线性关系良好，线性相关系数大于0.999，检出限为0.008 mg/kg，检测下限为0.024 mg/kg，测定结果的相对标准偏差为2.07%～3.84%(n=12)，样品加标回收率为101%～119%。该方法经国家一级土壤成分分析标准物质验证，准确可靠，已应用于农业、建筑用土和管道淤泥沉积物中痕量铋的测定，单次可批量处理72～84个样品，满足了高通量样品中痕量铋的测定需求。
Abstract：In order to improve the existing national standard test method (HJ 680-2013), the samples were digested by water bath method, and the trace bismuth in soil and sediment was determined by atomic fluorescence spectrometry. Taking the national standard materials for soil composition analysis(GSS-16, GSS-17, GSS-23) and Taizhou agricultural, construction soil and pipeline sludge sediment samples as the test objects, the influence of 13 mixed acid digestion systems on the determination results of trace bismuth in complex samples was discussed, and the best experimental conditions for the determination of trace bismuth were selected. The hydrochloric acid, nitric acid and sulfuric acid(volume ratio was 1∶3∶2) was used as the digestion solution in the three acids system. The digestion time was 0.5 h and the total treatment time was 2.0 h. The mass concentration of bismuth had a good linear relationship in the range of 0.1-10.0 μg/L, the linear correlation coefficient was more than 0.999, the detection limit was 0.008 mg/kg, the quantitative limit was 0.024 mg/kg. The relative standard deviations of the determination results were 2.07%-3.84%(n=12), and the recoveries of the samples were 101%-119%. This method has been verified by the national first-class standard material of soil composition analysis, which is accurate and reliable. It has been applied to the pretreatment of agricultural, construction soil and pipeline sludge sediment samples in the environment. 72-84 samples can be processed in batches at a time, which can meet the demand of high-throughput sample trace bismuth determination.
Keywords：trace bismuth; soil; sediment; digestion methods; environmental monitoring; atomic fluorescence spectrometry
ZHOU Z K，BAO Y F，YE C L. Determination of bismuth in soil and sediment by atomic fluorescence spectrometry[J]. Chemical analysis and meterage，2020，29(6)：61-66.