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机构地区:[1]淮海工学院化学工程学院,江苏连云港222005 [2]连云港师范高等专科学校,江苏连云港222006
出 处:《现代食品科技》2013年第12期3026-3030,共5页Modern Food Science and Technology
基 金:江苏高校优势学科建设工程资助项目;国家自然科学基金项目(21101069)
摘 要:采用微波消解对鱼进行前处理,根据Hg2+在乙酸-乙酸钠缓冲液中对1,10-菲啰啉和灿烂黄所产生的共振光散射具有显著增强作用,建立了共振光散射法测定痕量汞的新方法。考察实验影响因素,确定最佳测定条件为10 mL比色管中加入pH 5.7乙酸-乙酸钠缓冲液1.5 mL、1.0×10-4 mol/L 1,10-菲啰啉溶液1.0 mL和4.0×10-5 mol/L灿烂黄溶液0.8 mL,反应温度25 ℃,反应时间5 min。最大共振光散射峰位于451.6 nm,共振散射光强度增加值与Hg2+质量浓度在0~50 μg/L范围内线性关系良好,方法的检出限为0.54 μg/L。大量的共存离子不干扰测定,Cu2+和Fe3+的干扰可加入氟化钠-硫脲混合掩蔽剂消除。将该法用于测定鱼中汞含量,结果与冷原子吸收光谱法一致,相对标准偏差为1.38~2.19% (n=5),平均回收率为99.33~102.00%。该方法灵敏准确、简便快速、精密度高、选择性好,高效环保,适用于鱼中汞的测定。The fish samples were pretreated by using microwave digestion Based on the obvious enhancing effect of Hg2+ in acetic acid- sodium acetate buffer solution on resonance light scattering (RLS) produced by 1,10-phenanthroline monohydrate and brilliant yellow, RLS method for determination of trace amount of mercury in fish was established. The results showed that the optimal determination conditions were: 1.5 mL acetic acid-sodium acetate buffer solution at pH 5.7, 1.0 mL 1.0×10-4 mol/L 1,10-phenanthroline monohydrate solution and 0.8 mL 4.0×10-5 mol/L brilliant yellow, reaction temperature 25 ℃ and reaction time 5 min. Good linear relationship was obtained between the enhanced RLS intensity and Hg2+ concentration in the range of 0~50 μg/L with the maximum RLS peak at 451.6 nm. The detection limit was 0.54 μg/L. Interfering ions as Cu2+ and Fe3+ could be masked by a mixture of sodium fluoride and thiourea. The result of measured mercury content in fish was in accordance with that measured by cold vapor atomic absorption spectrometry. The relative standard deviation was 1.38~2.19% (n = 5), and the average recovery was 99.33~102.00%. This method was sensitive, accurate, simple, rapid and environmentally friendly, which was suitable for determination of mercury in fish.
关 键 词:共振光散射 微波消解 汞 1 10-菲啰啉 灿烂黄 鱼
分 类 号:X832[环境科学与工程—环境工程]
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