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Development of an N-methyl pyrrolidone based method of analysis for lead in paint

机译:基于N-甲基吡咯烷酮的油漆中铅分析方法的开发

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A method suitable for the field determination of lead-containing paint by atomic absorption was developed. N-Methyl pyrrolidone (NMP) was used as a pretreatment to soften the paint samples. No heating, mechanical grinding, or other chemical treatments were necessary prior to final sample dilution. Addition of 2% nitric acid was sufficient to dissolve the lead species in as little as 30 minutes. The total sample preparation time was 60 minutes. Using FAAS, ICP-MS, and portable ETAAS, the proposed method was found to give results equivalent to the NIOSH 7082 acid digestion method for a lead paint SRM and several laboratory samples. The proposed method used only two reagents (NMP and dilute nitric acid) to prepare the sample for analysis which makes it specifically suited for determinations performed outside of a traditional laboratory. The presence of NMP in solution required the use of an internal standard to avoid positive bias in ICP-MS analysis. FAAS showed a small negative bias from NMP in solution. Accurate ETAAS determinations required the use of a phosphate matrix modifier. Raman spectroscopy of acidic NMP solutions revealed that the NMP was not chemically degraded under the conditions used for lead determination. However, at higher acid concentrations, loss of the N-methyl was observed.
机译:提出了一种适用于原子吸收法现场测定含铅涂料的方法。 N-甲基吡咯烷酮(NMP)用作软化涂料样品的预处理。最终样品稀释前无需加热,机械研磨或其他化学处理。添加2%的硝酸足以在短短30分钟内溶解铅物质。样品制备的总时间为60分钟。使用FAAS,ICP-MS和便携式ETAAS,发现该方法可提供与NIOSH 7082酸消解法等效的铅涂料SRM和一些实验室样品的结果。所提出的方法仅使用两种试剂(NMP和稀硝酸)来准备要分析的样品,这使其特别适合在传统实验室之外进行的测定。溶液中NMP的存在要求使用内标以避免ICP-MS分析中的正偏差。 FAAS对溶液中的NMP表现出较小的负偏差。准确的ETAAS测定需要使用磷酸盐基质改性剂。酸性NMP溶液的拉曼光谱显示,在用于铅测定的条件下,NMP不会化学降解。然而,在较高的酸浓度下,观察到N-甲基的损失。

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