Morganti Andrea, Becagli Silvia, Castellano Emiliano, Severi Mirko, Traversi Rita, Udisti Roberto
Department of Chemistry, University of Florence, Scientific Pole, via della Lastruccia 3, 50019 Sesto F.no (FI), Italy.
Anal Chim Acta. 2007 Nov 12;603(2):190-8. doi: 10.1016/j.aca.2007.09.050. Epub 2007 Sep 29.
A method was developed for the quantitative determination of cations and anions in Antarctic ice cores at microgL(-1) and sub-microgL(-1) levels by ion chromatography (IC), after ultra-clean decontamination procedures. Strict manipulation and decontamination procedures were used in sub-sampling, in order to minimise sample contamination. Na+, NH4+, K+, Mg2+ and Ca2+ were determined by 12-min isocratic elution (H2SO4 eluent). Contemporaneously, in a parallel device, F-, MSA (methanesulfonic acid), Cl-, NO3- and SO4(2-) were analysed in a single 12-min run with multiple-step elution using Na2CO3/NaHCO3 as eluent. Melted ice samples were pumped from their still-closed containers (polystyrene accuvettes with polyethylene caps), shared between the two ion chromatographic systems, online filtered (0.45 microm Teflon membrane) and pre-concentrated (anions and cations pre-concentration columns) using a flow analysis system, thus avoiding uptake of contaminants from the laboratory atmosphere. Sensitivity, linear range, reproducibility and detection limit were evaluated for each chemical species. Anion or cation detection limits ranged from 0.01 to 0.15 microgL(-1) by using a relatively small sample volume (1.5 mL). Such values are significantly lower than those reported in literature for almost all the components. These methods were successfully applied to the analysis of cations and anions at trace levels in the Dome C ice core. The composition of the atmospheric aerosol for the last 850 kyr was reconstructed by high-resolution continuous chemical stratigraphies. Concentration trends in the last nine glacial-interglacial climatic cycles were shown and briefly discussed.
通过超净去污程序,开发了一种利用离子色谱法(IC)在微克每升(μg L⁻¹)和亚微克每升(sub-μg L⁻¹)水平定量测定南极冰芯中阳离子和阴离子的方法。在子采样过程中采用了严格的操作和去污程序,以尽量减少样品污染。通过12分钟等度洗脱(硫酸洗脱液)测定Na⁺、NH₄⁺、K⁺、Mg²⁺和Ca²⁺。同时,在一个平行装置中,使用碳酸钠/碳酸氢钠作为洗脱液,通过多步洗脱在单次12分钟运行中分析F⁻、甲磺酸(MSA)、Cl⁻、NO₃⁻和SO₄²⁻。将融化的冰样从其仍密封的容器(带有聚乙烯帽的聚苯乙烯微量比色管)中泵出,在两个离子色谱系统之间共享,在线过滤(0.45微米聚四氟乙烯膜)并使用流动分析系统进行预浓缩(阴离子和阳离子预浓缩柱),从而避免从实验室大气中吸收污染物。对每种化学物质的灵敏度、线性范围、重现性和检测限进行了评估。通过使用相对较小的样品体积(1.5 mL),阴离子或阳离子检测限范围为0.01至0.15 μg L⁻¹。这些值明显低于几乎所有组分在文献中报道的值。这些方法已成功应用于 Dome C 冰芯中痕量水平的阳离子和阴离子分析。通过高分辨率连续化学地层学重建了过去85万年的大气气溶胶组成。展示并简要讨论了过去九个冰期 - 间冰期气候周期中的浓度趋势。