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机构地区:[1]漳州市产品质量检验所,福建漳州363000 [2]漳州师范学院化学与环境科学系,福建漳州363000
出 处:《分析测试学报》2011年第4期413-417,共5页Journal of Instrumental Analysis
基 金:福建省质量技术监督局科技基金资助项目(BIA010092-F07);福建省教育基金重点资助项目(JA08152)
摘 要:该文合成了2,3-二氢-9,10-二羟基-1,4-蒽醌(R),并借助核磁共振谱、红外光谱、质谱及紫外光谱等方法确定其结构。基于R在醋酸纤维素膜固体基质上能产生强而稳定的固体基质室温燐光(SS-RTP),α,α'-联吡啶可活化Hg2+催化H2O2氧化R转化成无燐光化合物,导致固体基质室温燐光急剧猝灭,建立了催化H2O2氧化R固体基质室温燐光猝灭法测定痕量汞的新方法。在最佳条件下,Hg2+含量在1.60~160 fg/斑(0.004 0~0.40μg/L,0.4μL点样量)范围内与燐光发射光强度(ΔIp)符合比尔定律,其回归方程为ΔIp=11.56+0.549 2m(fg/斑),相关系数r=0.999 1,检出限为0.26 fg/斑(对应Hg2+质量浓度为6.5×10-10 g/L)。方法的加标回收率为97%~103%,相对标准偏差为2.3%~4.1%。对0.004 0、0.40μg/L的Hg2+分别测定11次,其RSD分别为2.6%、4.1%。该方法重复性好、灵敏、准确,用于实际样品中汞含量的测定,结果满意。2, 3-Dihydro-9, 10-dihydroxy -1, 4-anthraquinone (R)was synthesized and characterized by 1H NMR, IR, MS and UV -Vis spectrometry. Based on the facts that R can emit intense and stable solid substrate - room temperature phosphorescence( SS - RTP) on solid substrate, and α,α'-dipyridine can activate Hg2+ to catalyze the reaction of H2 02 oxidizing R to form non-phosphorecence compound, a new solid substrat - room temperature phosphorescence quenching method was established for the determination of trace mercury. Under the optimum condition, the relationship between the Alp of the emitting intensity and 1.60 -160 fg/spot Hg2+( corresponding concentration: 0. 004 0 -0. 40 μg/L, sample volume: 0.4 μL/spot) conformed to Beer' law. The regression equa- tion was Alp = 11.56 + 0. 549 2 m (fg/spot) ( r=0. 999 1 ). The limit detection was 0. 26 fg/spot (corresponding Hg2+ concentration: 6.5 ×10^-10g/L). The spiked recoveries were in the range of 97% -103% with RSDs of 2.3% -4. 1%. The RSDs(n=ll) of 0.004 0 μg/L and0.40 μg/L Hg2+ were 2.6% and 4. 1% , respectively. The method showed good repeatability, sensitivity and high precision. It was applied in the determination of trace mercury ( II ) in real samples with satisfactory results.
分 类 号:O561.3[理学—原子与分子物理] O614.243[理学—物理]
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