Institute of Quality Standard and Testing Technology for Agro-products, Chinese Academy of Agricultural Sciences, And Key Laboratory of Agro-food Safety and Quality, Ministry of Agriculture and Rural Affairs, Beijing, 100081, China; College of Instrumentation & Electrical Engineering, Jilin University, Changchun, 130023, China.
Beijing Ability Technology Company, Limited, Beijing, 100081, China.
Talanta. 2020 Oct 1;218:121161. doi: 10.1016/j.talanta.2020.121161. Epub 2020 May 22.
In this work, a portable and reliable optical emission spectrometric (OES) instrument based on solid acid hydride generation (HG) and subsequent in situ dielectric barrier discharge (DBD) preconcentration was first developed for simultaneous and field analysis of ultratrace As and Sb in environmental water. In situ DBD fulfilled both gas phase enrichment (GPE) and excitation; effective enrichment made it possible to use a low-cost charge coupled device (CCD) as detector. To simplify field protocol, solid tablet made from sulfamic acid was first used to replace hydrochloric acid for co-generation of As and Sb hydrides. Moisture interference was eliminated by carrier gas sweeping without any desiccant. After calculating peak volume for emission data handling, detection limits (LODs) were 0.5 μg L for As and 0.2 μg L for Sb, respectively, with <3% relative standard deviations (RSDs) at 10 μg L; linear dynamic ranges (R>0.995) were 2-200 μg L for As and 1-200 μg L for Sb, respectively. The results agreed with certified values of CRMs and recoveries were 87-97% vs. inductively coupled plasma mass spectrometry. The running costs can be controlled within one dollar per use. This HG-in situ DBD trap-OES scheme, with demonstrated advantages in sensitivity, low-cost, power (<60 W), size (0.6 m × 0.5 m × 0.3 m), weight (15 kg), gas consumption (300 measurements per 4 L tank), and multi-element capability, was implemented in a miniature spectrometer for field analysis.
本工作首次开发了一种基于固体酸氢化物发生（HG）和随后的原位介质阻挡放电（DBD）预浓缩的便携式可靠的光学发射光谱（OES）仪器，用于环境水中痕量 As 和 Sb 的同时现场分析。原位 DBD 同时实现了气相富集（GPE）和激发；有效的浓缩使得可以使用低成本的电荷耦合器件（CCD）作为检测器。为了简化现场协议，首先使用由氨基磺酸制成的固体片剂代替盐酸来共同生成 As 和 Sb 氢化物。通过载气吹扫消除了水分干扰，无需干燥剂。在对发射数据进行峰面积计算后，As 的检测限（LOD）为 0.5μg/L，Sb 的检测限为 0.2μg/L，在 10μg/L 时相对标准偏差（RSD）<3%；线性动态范围（R>0.995）分别为 2-200μg/L 和 1-200μg/L。结果与 CRMs 的认证值吻合，与电感耦合等离子体质谱法相比，回收率为 87-97%。运行成本可以控制在每次使用一美元以内。该 HG-原位 DBD 阱-OES 方案在灵敏度、低成本、功率（<60W）、尺寸（0.6m×0.5m×0.3m）、重量（15kg）、气体消耗（4L 罐可进行 300 次测量）和多元素能力方面具有优势，已在现场分析的微型光谱仪中实施。
