Key Laboratory for Advanced Materials and Research Center of Analysis Test, East China University of Science and Technology, Meilong Rd 130, Shanghai 200237, PR China.
Anal Chim Acta. 2010 Jun 18;670(1-2):39-43. doi: 10.1016/j.aca.2010.04.064. Epub 2010 May 6.
A micro near infrared spectroscopy (MicroNIRS) technique based on monolithic column enrichment has been developed to detect low concentration metallic ions in water. Glycidyl methacrylate-ethylene dimethacrylate-iminodiacetic acid (GMA-EDMA-IDA) monolithic material was synthesized to construct an enrichment device, which can enrich metallic ions more efficiently than chelating resin materials such as D401. Cu(2+) solutions passed through the enrichment device and concentrated on the surface of the material, and then diffuse reflection NIR (DRNIR) spectra were measured by touching the NIR probe on the surface. The spectra were pretreated with multiplicative scatter correction (MSC) and the MSC-pretreated spectra showed high linear correlation to the Cu(2+) concentrations in spectral regions of 900-1350 nm, 1420-1480 nm and 1970-2050 nm for all concentration ranges. PLS models built with leave-one-out cross-validation also yielded good features. The mean relative error (MRE) of prediction was 10.0% in the 0.0001-0.0010 microg mL(-1) range. The concentration has low to ppb-level, but the MRE was not more than 10%, which was acceptable for trace analysis. The results revealed that the MicroNIRS technique enhanced the sensitivity of NIRS dramatically and widened the NIRS technique to micro and trace analysis field.
一种基于整体柱富集的微近红外光谱(MicroNIRS)技术已经被开发出来,用于检测水中低浓度的金属离子。合成了甲基丙烯酸缩水甘油酯-二乙烯基苯-亚氨基二乙酸(GMA-EDMA-IDA)整体材料,以构建一个富集装置,该装置可以比螯合树脂材料(如 D401)更有效地富集金属离子。Cu(2+)溶液通过富集装置并浓缩在材料表面,然后通过触摸表面上的近红外探头测量漫反射近红外(DRNIR)光谱。用乘法散射校正(MSC)预处理光谱,在光谱区域 900-1350nm、1420-1480nm 和 1970-2050nm 中,MSC 预处理光谱与所有浓度范围内的 Cu(2+)浓度具有高度线性相关。用留一法交叉验证建立的 PLS 模型也具有良好的性能。在 0.0001-0.0010μgmL(-1)范围内,预测的平均相对误差(MRE)为 10.0%。浓度低至 ppb 级,但 MRE 不超过 10%,这对于痕量分析是可以接受的。结果表明,MicroNIRS 技术极大地提高了近红外光谱的灵敏度,并将近红外光谱技术扩展到微痕量分析领域。