CAJ | 학술논문

采用电晕放电激发源和手持式电荷耦合检测器组装了小型化原子发射光谱仪,将其用于检测痕量汞。以光化学蒸气发生技术作为进样手段,在甲酸辅助下用紫外光照射样品溶液产生汞蒸气,并由氩气带入电晕放电光源中,激发后产生汞原子发射光谱信号,用电荷耦合检测器在253.7 nm处检测。经优化得到的最佳实验条件为甲酸浓度4％,电晕放电电压90 V,载气流速200 mL/min；检测信号稳定,相对标准偏差为2.5％；标准曲线线性范围为0.5~1000μg/L,线性相关系数大于0.99,汞的检出限可以低至0.03μg/L。同时,对两种含汞的标准样品进行了分析, t检验表明,检测结果与样品标准值在95％的置信水平上无显著性差异；另外,对成都市府南河水和四川大学校园荷花池水的汞含量进行了测定,加标回收率在93.8％~103％范围之内。该小型化原子发射光谱测汞仪具有组装简单、低能耗、高灵敏度、便携式适用于现场分析等优点。
채용전훈방전격발원화수지식전하우합검측기조장료소형화원자발사광보의,장기용우검측흔량홍。이광화학증기발생기술작위진양수단,재갑산보조하용자외광조사양품용액산생홍증기,병유아기대입전훈방전광원중,격발후산생홍원자발사광보신호,용전하우합검측기재253.7 nm처검측。경우화득도적최가실험조건위갑산농도4％,전훈방전전압90 V,재기류속200 mL/min；검측신호은정,상대표준편차위2.5％；표준곡선선성범위위0.5~1000μg/L,선성상관계수대우0.99,홍적검출한가이저지0.03μg/L。동시,대량충함홍적표준양품진행료분석, t검험표명,검측결과여양품표준치재95％적치신수평상무현저성차이；령외,대성도시부남하수화사천대학교완하화지수적홍함량진행료측정,가표회수솔재93.8％~103％범위지내。해소형화원자발사광보측홍의구유조장간단、저능모、고령민도、편휴식괄용우현장분석등우점。
A miniaturized atomic emission spectrometer composed of a corona discharge source and a handheld charge-coupled device detector was constructed for the sensitive determination of trace mercury, with photochemical vapor generation for sample introduction. By using formic acid, mercury vapor was generated under the irradiation of UV light, and then the vapor was introduced into the corona discharge area with the carrier gas flow of argon. The optical signals were captured and analyzed by the charge-coupled device detector at 253. 7 nm. Under the optimized conditions including 4% formic acid, discharge voltage of 90 V, and carrier gas flow rate of 200 mL/min, the stable detection signals were obtained ( RSD=2. 5%). The calibration curves were plotted with the concentration of mercury ranging from 0. 5 to 1000 ng/mL, with a correlation coefficient >0. 99 and the limit of detection of 0. 03 ng/mL. Two certified reference materials were analyzed, and a t-test demonstrated that the determined results by the proposed method had no significant difference with the certified values at the confidence level of 95%. Water samples collected from both Funan River in Chengdu and the Lotus Pond on campus of Sichuan University were analyzed as well, with the recoveries of standard addition between 93 . 8% and 103%. The miniaturized instrumentation demonstrated several advantages including easy construction, low power consumption, high sensitivity, and portability for field analysis.