Research & Development, T.E. Laboratories Ltd. (TelLab), Tullow, Carlow, Ireland; Insight Centre for Data Analytics, National Centre for Sensor Research, School of Chemical Sciences, Dublin City University, Dublin 9, Ireland.
Research & Development, T.E. Laboratories Ltd. (TelLab), Tullow, Carlow, Ireland.
J Chromatogr A. 2019 Oct 11;1603:8-14. doi: 10.1016/j.chroma.2019.05.036. Epub 2019 May 21.
A low cost, UV absorbance detector incorporating a 235 nm light emitting diode (LED) for portable ion chromatography has been designed and fabricated to achieve rapid, selective detection of nitrite and nitrate in natural waters. The optical cell was fabricated through micromilling and solvent vapour bonding of two layers of poly (methyl methacrylate) (PMMA). The cell was fitted within a 3D printed housing and the LED and photodiode were aligned using 3D printed holders. Isocratic separation and selective detection of nitrite and nitrate was achieved in under 2.5 min using the 235 nm LED based detector and custom electronics. The design of the new detector assembly allowed for effective and sustained operation of the deep UV LED source at a low current (<10 mA), maintaining consistent and low LED temperatures during operation, eliminating the need for a heat sink. The detector cell was produced at a fraction of the cost of commercial optical cells and demonstrated very low stray light (0.01%). For retention time and peak area repeatability, RSD values ranged from 0.75 to 1.10 % and 3.06-4.19 %, respectively. Broad dynamic linear ranges were obtained for nitrite and nitrate, with limits of detection at ppb levels. The analytical performance of the IC set up with optical cell was compared to that of an ISO-accredited IC through the analysis of five various water samples. Relative errors not exceeding 6.86% were obtained for all samples. The detector was also coupled to a low pressure, low cost syringe pump to assess the potential for use within a portable analytical system. RSD values for retention time and peak area using this simple configuration were <1.15% and <3.57% respectively, highlighting repeatability values comparable to those in which a commercial HPLC pump was used.
已设计并制作了一种低成本、采用 235nm 发光二极管(LED)的紫外吸收检测器,用于便携式离子色谱法,以实现对天然水中亚硝酸盐和硝酸盐的快速、选择性检测。该光学池通过微铣削和两层聚甲基丙烯酸甲酯(PMMA)的溶剂蒸气键合制成。该池安装在 3D 打印外壳内,使用 3D 打印支架对准 LED 和光电二极管。使用基于 235nm LED 的检测器和定制电子设备,在不到 2.5 分钟的时间内实现了亚硝酸盐和硝酸盐的等度分离和选择性检测。新检测器组件的设计允许深紫外 LED 源以低电流(<10mA)有效且持续运行,在运行过程中保持 LED 温度一致且较低,无需散热器。检测器池的制造成本仅为商业光学池的一小部分,并表现出非常低的杂散光(0.01%)。对于保留时间和峰面积重复性,RSD 值范围分别为 0.75-1.10%和 3.06-4.19%。亚硝酸盐和硝酸盐均获得了较宽的动态线性范围,检测限达到 ppb 水平。通过对五种不同水样的分析,将带有光学池的 IC 与经过 ISO 认证的 IC 的分析性能进行了比较。对于所有样品,相对误差均不超过 6.86%。该检测器还与低压、低成本注射器泵耦合,以评估其在便携式分析系统中的潜在用途。使用这种简单配置时,保留时间和峰面积的 RSD 值分别<1.15%和<3.57%,突出了与使用商业 HPLC 泵时相当的重复性值。