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Nickel determination in oily sludge leachates using isotope dilution inductively coupled plasma mass spectrometry following photochemical vapor generation: A feasibility study
Microchemical Journal ( IF 4.8 ) Pub Date : 2018-09-01 , DOI: 10.1016/j.microc.2018.05.029
Graziela Salvador , Bárbara Souza Soares , Daniel L.G. Borges

Abstract The feasibility of photochemical vapor generation for the production of volatile Ni species was evaluated and applied to the analysis of acetic acid leachates obtained from oily sludge samples. Sludge samples originating from a petrochemical plant were submitted to extraction using standardized procedures with solutions adjusted to pH 2.88 or 4.93, with acetic acid. The leachate solutions were subsequently treated with a mixture of acetic and formic acid and exposed to UV radiation from a Hg discharge lamp; the irradiated solution was pumped to a gas-liquid separator and the volatile species were transported by a stream of argon for detection using inductively coupled plasma mass spectrometry. Experimental variables, including the nature and concentration of low molecular weight acids, irradiation interval, carrier gas flow rate and the effect of concomitant species on the efficiency of photochemical production of volatile Ni species were systematically evaluated. Oxygenated anions, particularly nitrate, were found to suppress the analytical signal, whereas the effect of cationic species depended on the nature of the cation. Lead was found to induce substantial signal suppression even at ppb levels. Considering the significant influence of concomitant species on the overall efficacy of the photochemical process, isotope dilution calibration was adopted as a strategy to overcome non-spectral interferences. Under optimized conditions, relative standard deviations better than 8.5% were achieved, along with detection limits better than 40 μg L−1. The accuracy was statistically attested upon comparison of the results to those obtained from the analysis of leachates using sample introduction via pneumatic nebulization. The proposed photochemical vapor generation setup was proven efficient to carry out the determination of Ni in the leachates, although the technique is highly sensitive to the presence of concomitants.

中文翻译:

光化学蒸汽产生后使用同位素稀释电感耦合等离子体质谱法测定含油污泥浸出液中的镍:可行性研究

摘要 评价了光化学蒸汽产生用于生产挥发性镍物种的可行性,并将其应用于含油污泥样品醋酸浸出液的分析。来自石化厂的污泥样品使用标准化程序进行提取,溶液使用醋酸调节至 pH 值 2.88 或 4.93。浸出液随后用乙酸和甲酸的混合物处理,并暴露于来自汞放电灯的紫外线辐射;辐照后的溶液被泵送到气液分离器中,挥发性物质通过氩气流输送,用于电感耦合等离子体质谱检测。实验变量,包括低分子量酸的性质和浓度、辐照间隔、系统地评估了载气流速和伴随物质对挥发性 Ni 物质光化学生产效率的影响。发现含氧阴离子,尤其是硝酸根,会抑制分析信号,而阳离子种类的影响取决于阳离子的性质。发现即使在 ppb 水平,铅也会引起大量的信号抑制。考虑到伴随物质对光化学过程整体功效的显着影响,采用同位素稀释校准作为克服非光谱干扰的策略。在优化条件下,相对标准偏差优于 8.5%,检测限优于 40 μg L-1。将结果与通过气动雾化引入样品的渗滤液分析结果进行比较后,可以统计出准确性。尽管该技术对伴随物的存在高度敏感,但所提出的光化学蒸汽发生装置已被证明可以有效地进行浸出液中 Ni 的测定。
更新日期:2018-09-01
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