Arslan Zikri, Oymak Tulay, White Jeremy
Department of Chemistry, Physics and Atmospheric Sciences, Jackson State University, Jackson, MS 39217, USA.
Department of Chemistry, Physics and Atmospheric Sciences, Jackson State University, Jackson, MS 39217, USA; Faculty of Pharmacy, Department of Analytical Chemistry, Cumhuriyet University, Sivas, Turkey.
Anal Chim Acta. 2018 May 30;1008:18-28. doi: 10.1016/j.aca.2018.01.017. Epub 2018 Jan 20.
In this paper, we report an improved magnesium hydroxide, Mg(OH), coprecipitation method for the determination of 16 trace elements (Al, V, Cr, Mn, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Sb, Sn and Pb) and 18 rare earth elements (REEs), including Sc, Y, U and Th in seawater and estuarine water samples. The procedure involves coprecipitation of the trace elements and REEs on Mg(OH) upon addition of a small volume of triethylamine (TEA) followed by analysis of the dissolved pellet solutions by inductively coupled plasma mass spectrometry (ICP-MS). Three-step sequential coprecipitation was carried out on 10 mL aliquots of seawater to eliminate the matrix ions and to preconcentrate the analytes of interest into a 1 mL final volume. Spike recoveries varied from 85% (Th) to 105% (Y). Calcium (Ca), sodium (Na) and potassium (K) matrices were virtually eliminated from the analysis solutions. Collision reaction interface (CRI) technology utilizing H and He gases was employed to determine its effectiveness in removing the spectral interferences originating from the residual Mg matrix, TEA and plasma gases. H was more effective than He in reducing spectral interferences from TEA and plasma gases. Limits of detection (LODs) ranged from 0.01 ng L (Ho) to 72 ng L (Al). The method was validated by using certified seawater (CASS-4) and estuarine water (SLEW-3) reference materials. Precision for five (n = 5) replicate measurements were between 1.2% (Pr) and 18% (Lu). Fe, Pb, Sn, and Zn impurities in TEA were significant in comparison to the levels in CASS-4 and SLEW-3, while relatively high background signals impacted determinations of low levels of Sc and Th. The effects of these hurdles on precision and accuracy were alleviated by measuring these elements in spiked CASS-4 and SLEW-3.
在本文中,我们报告了一种改进的氢氧化镁(Mg(OH)₂)共沉淀法,用于测定海水和河口水样中的16种微量元素(铝、钒、铬、锰、铁、钴、镍、铜、锌、镓、砷、硒、锑、锡和铅)以及18种稀土元素(REEs),包括钪、钇、铀和钍。该方法包括在加入少量三乙胺(TEA)后,使微量元素和稀土元素在Mg(OH)₂上共沉淀,然后通过电感耦合等离子体质谱法(ICP-MS)分析溶解的沉淀溶液。对10 mL海水等分试样进行三步连续共沉淀,以消除基体离子,并将感兴趣的分析物预浓缩至1 mL最终体积。加标回收率在85%(钍)至105%(钇)之间。分析溶液中几乎消除了钙(Ca)、钠(Na)和钾(K)基体。采用利用氢气和氦气的碰撞反应界面(CRI)技术来确定其在消除源自残留镁基体、TEA和等离子体气体的光谱干扰方面的有效性。氢气在减少来自TEA和等离子体气体的光谱干扰方面比氦气更有效。检测限(LOD)范围为0.01 ng·L⁻¹(钬)至72 ng·L⁻¹(铝)。该方法通过使用认证海水(CASS-4)和河口海水(SLEW-3)标准物质进行了验证。五次(n = 5)重复测量的精密度在1.2%(镨)至18%(镥)之间。与CASS-4和SLEW-3中的含量相比,TEA中的铁、铅、锡和锌杂质含量较高,而相对较高的背景信号影响了低含量钪和钍的测定。通过在加标CASS-4和SLEW-3中测量这些元素,减轻了这些障碍对精密度和准确度的影响。