Telford K, Maher W, Krikowa F, Foster S
Ecochemistry Laboratory, Institute of Applied Ecology, University of Canberra, Belconnen, 2601, Australia.
J Environ Monit. 2008 Jan;10(1):136-40. doi: 10.1039/b715465h. Epub 2007 Dec 7.
This paper describes the measurement of total antimony and antimony species in "real world" mine contaminated sediments using ICPMS and HPLC-ICPMS. Low and high temperature microwave extraction procedures (90 degrees C and 150 degrees C, respectively) using a range of nitric-hydrochloric acid combinations were examined as to their efficacy to extract antimony from six mine contaminated soils and a certified reference material. The use of the higher temperature with nitric-hydrochloric acid (1:2 (v/v)) was suitable to release antimony from sediments and the certified reference material, NIST 2710 Montana soil. Antimony concentrations obtained using this acid mixture were similar to those obtained using a more aggressive extraction with nitric, hydrochloric, perchloric and hydrofluoric acid mixture. A 25 mM citric acid solution at 90 degrees C for 15 min extracted 47-78% of antimony from soils. A Hamilton PRP X-100 anion exchange column with 20 mM EDTA mobile phase, pH 4.5, flow rate 1.5 mL min(-1) and column temperature of 50 degrees C was used to separate antimony species. Column recoveries ranged from 78-104%. The predominant form of antimony was Sb(5+). Little conversion of Sb(5+) occurred (<5%) during extraction, however, significant conversion of Sb(3+) occurred (approximately 36%). The extraction of antimony species with citric acid should be useful in the determination of inorganic antimony available to plants, as plants commonly excrete carboxylic acids, including citric acid, into their rhizospheres to mobilise trace elements for nutritional purposes.
本文描述了使用电感耦合等离子体质谱仪（ICPMS）和高效液相色谱-电感耦合等离子体质谱仪（HPLC-ICPMS）对“实际”矿山污染沉积物中的总锑和锑形态进行的测量。研究了分别使用一系列硝酸-盐酸组合的低温和高温微波萃取程序（分别为90℃和150℃）从六种矿山污染土壤和一种有证标准物质中提取锑的效果。使用较高温度的硝酸-盐酸（1:2（v/v））适合从沉积物和有证标准物质NIST 2710蒙大拿土壤中释放锑。使用这种酸混合物获得的锑浓度与使用硝酸、盐酸、高氯酸和氢氟酸混合物进行更剧烈萃取获得的浓度相似。90℃下用25 mM柠檬酸溶液萃取15分钟可从土壤中萃取出47-78%的锑。使用Hamilton PRP X-100阴离子交换柱，流动相为20 mM乙二胺四乙酸（EDTA），pH 4.5，流速1.5 mL min⁻¹，柱温50℃来分离锑形态。柱回收率在78-104%之间。锑的主要形态是Sb(5+)。萃取过程中Sb(5+)的转化很少（<5%），然而，Sb(3+)发生了显著转化（约36%）。用柠檬酸萃取锑形态对于测定植物可利用的无机锑应该是有用的，因为植物通常会将包括柠檬酸在内的羧酸分泌到根际以调动微量元素用于营养目的。
