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Determination of lead in vinegar by ICP-MS and GFAAS: evaluation of different sample preparation procedures

机译:ICP-MS和GFAAS测定醋中的铅:评估不同样品制备程序

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Lead concentrations of 59 different types of vinegars(15-307(mug 1~(-1)in balsamic vinegars and 36-50 mug 1~(-1)in wine vinegars)were determined using both inductively coupled plasma mass spectrometry(ICP-MS)and graphite furnace atomic absorption spectrometry(GFAAS).Although the precision of direct analyses,following simple aqueous dilutions,with either instrumental method was poor;that precision,following nitric acid and/or hydrogen peroxide digestions,markedly improved with either instrument and the values obtained with the two instruments were in good agreement.The efficacy of different digestions,including(1)nitric acid using a heating block,with or without addition of hydrogen peroxide and(2)mixtures of nitric acid and hydrogen peroxide using ultraviolet(UV)photolysis,were then assessed.The latter procedure was found to be much faster and more efficient,but it was limited by the relatively high levels of contaminant lead in hydrogen peroxide.Consequently,it is recommended that lead concentrations in vinegar be measured following a nitric acid digestion and UV photolysis to oxidize all organic matter before ICP-MS or GFAAS analysis;and it is further recommend that the thermal settings for the latter analyses be adjusted to account for the apparent presence of relatively volatile organolead compounds in vinegar digests.
机译:两种电感耦合等离子体质谱法(ICP- (MS)和石墨炉原子吸收光谱法(GFAAS)。尽管直接分析的精度较高,但在简单的水稀释后,使用任何一种仪器方法都较差;在硝酸和/或过氧化氢消解之后,使用任何一种仪器和方法显着提高了精密度这两种仪器获得的值非常吻合。不同消解的功效,包括(1)使用加热块的硝酸,是否添加过氧化氢和(2)使用紫外线的硝酸和过氧化氢的混合物(然后评估了紫外线)的光解作用。发现后者的过程更快,更有效,但由于过氧化氢中铅的含量相对较高而受到限制。因此,建议将在进行ICP-MS或GFAAS分析之前,应先进行硝酸消化和UV光解以氧化所有有机物,然后测量醋中的d浓度;进一步建议调整后一种分析的热设置以考虑到相对醋消化液中的挥发性有机铅化合物。

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