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机构地区:[1]广西壮族自治区环境监测中心站,南宁530028
出 处:《理化检验(化学分册)》2017年第7期787-791,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:环保公益性行业科研专项(201309050);广西自然科学基金重大项目(2015GXNSFEA139001)
摘 要:提出了用微波消解-电感耦合等离子体原子发射光谱法测定河流和湖泊沉积物中11种重金属元素(银、镉、钴、铬、铜、锰、镍、铅、锑、钒和锌)的方法。沉积物样品(0.100 0~0.500 0g)加入硝酸6mL,盐酸2mL,氢氟酸2mL,按程序升温微波消解,将消解液于130~140℃蒸发至近干,加水溶解残渣并定容至50mL。此溶液供电感耦合等离子体原子发射光谱法同时测定11种重金属元素含量,并选择了合适的分析谱线。光谱干扰运用背景扣除予以校准。测得各元素的检出限(3s)为0.20~2.00mg·kg^(-1)。以沉积物样品为基体,按标准加入法进行回收试验,测得回收率在81.6%~112%之间,相对标准偏差(n=6)均小于6.0%。按上述方法测定CRM(GBW 07360,GBW 07307a),测定值与认定值一致。The method was proposed for determination of 11 heavy metal elements (Ag, Cd, Co, Cr, Cu, Mn, Ni, Pb, Sb, V and Zn) in river and lake sediments by ICP-AES with microwave digestion. The sample of sediments (0. 100 0--0. 500 0 g) was treated with 6 mL of HNO3, 2 mL of HC1 and 2 mL of HF in a microwave digestor under programmed temperature elevatioru The digested solution was evaporated to near dryness at 130-- 140 ℃ and the residue was taken up with water and made up its volume to 50 mL. The sample solution was used for ICP-AES determination of 11 heavy metal elements. Analytical spectral lines were selected. Spectral interferences were overcome by background correction. Values of detection limits (3s) were in the range of 0. 20- 2. 00 mg · kg-1. The samples of sediments were used as matrix, and test for recovery was made by standard addition method, giving results in the range of 81.6%--112%, with RSDs (n=6) all less than 6. 0%. CRMs (GBW 07360, GBW 07307a) were analyzed by the proposed method, giving results in consistency with the certified values.
关 键 词:电感耦合等离子原子发射光谱法 微波消解 沉积物 重金属元素
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