Avila Orozco Francisco D, Kovachev Nikolay, Aguirre Pastor Miguel Ángel, Domini Claudia E, Fernández Band Beatriz S, Canals Hernández Antonio
Lab. FIA, Sección Química Analítica, INQUISUR (UNS-CONICET), Universidad Nacional del Sur, Avenida Alem 1253, B8000CPB, Bahía Blanca, Argentina.
Dpto. Química Analítica, Nutrición y Bromatología e Instituto Universitario de Materiales, Facultad de Ciencias, Universidad de Alicante, Apdo. 99, Alicante, Spain.
Anal Chim Acta. 2014 May 27;827:15-21. doi: 10.1016/j.aca.2014.04.016. Epub 2014 Apr 13.
A simple and fast method for determining the content of Na, K, Ca, Mg, P, and 20 heavy metals in biodiesel samples with inductively coupled plasma optical emission spectrometry (ICP OES) using a two-nozzle Flow Blurring(®) multinebulizer prototype and on-line internal standard calibration, are proposed. The biodiesel samples were produced from different feedstock such as sunflower, corn, soybean and grape seed oils, via a base catalyst transesterification. The analysis was carried out without any sample pretreatment. The standards and samples were introduced through one of the multinebulizer nozzles, while the aqueous solution containing yttrium as an internal standard was introduced through the second nozzle. Thus, the spectral interferences were compensated and the formation of carbon deposits on the ICP torch was prevented. The determination coefficients (R(2)) were greater than 0.99 for the studied analytes, in the range 0.21-14.75 mg kg(-1). Short-term and long-term precisions were estimated as relative standard deviation. These were acceptable, their values being lower than 10%. The LOQ for major components such as Ca, K, Mg, Na, and P, were within a range between 4.9 ng g(-1) for Mg (279.553 nm) and 531.1 ng g(-1) for Na (588.995 nm), and for the other 20 minor components they were within a range between 1.1 ng g(-1) for Ba (455.403 nm) and 2913.9 ng g(-1) for Pb (220.353 nm). Recovery values ranged between 95% and 106%.
提出了一种简单快速的方法,使用双喷嘴流动模糊(Flow Blurring®)多雾化器原型和在线内标校准,通过电感耦合等离子体发射光谱法(ICP OES)测定生物柴油样品中的钠、钾、钙、镁、磷和20种重金属含量。生物柴油样品由向日葵、玉米、大豆和葡萄籽油等不同原料通过碱催化酯交换反应制得。分析过程无需任何样品预处理。标准溶液和样品通过其中一个多雾化器喷嘴引入,而含有钇作为内标的水溶液通过第二个喷嘴引入。这样,光谱干扰得到补偿,同时防止了ICP炬管上积碳的形成。对于研究的分析物,在0.21 - 14.75 mg kg(-1)范围内,测定系数(R(2))大于0.99。短期和长期精密度以相对标准偏差估计。这些值是可接受的,均低于10%。钙、钾、镁、钠和磷等主要成分的定量限在镁(279.553 nm)的4.9 ng g(-1)至钠(588.995 nm)的531.1 ng g(-1)之间,其他20种微量元素的定量限在钡(455.403 nm)的1.1 ng g(-1)至铅(220.353 nm)的2913.9 ng g(-1)之间。回收率在95%至106%之间。