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    砷快速检测剂的研制及其在现场水质分析中的应用

    Preparation of Rapid Detection Reagents for Arsenic and Its Application to On-Site Water Quality Analysis

    • 摘要: 按10∶2∶1的质量比称取硼氢化钠、乙酸钠和硫酸铜,混合均匀,取0.20 g用胶囊包装,制得砷检测剂Ⅰ;按1∶0.25∶2.5∶7.5∶10的质量比称取硝酸银、聚乙烯醇(PVA-1788)、硝酸、乙醇和水,混合均匀,制得砷吸收液Ⅱ;按1∶10的质量比称取磷酸和磷酸二氢钾,混合均匀,于105℃烘干1~2 h,取0.30 g压片,用胶囊包装,制得砷检测剂Ⅲ。移取25 mL待测水样于多功能样品处理仪的反应管中,加入砷检测剂Ⅰ,摇动溶解;滴加0.15 mL砷吸收液Ⅱ于5 mL普通白酒(40~60度)中,倒入吸收管内;向反应管中加入砷检测剂Ⅲ,迅速用连接管将反应管与吸收管连接起来,反应5 min后,以0.2 L·min-1的流量通入空气5 min,将吸收液转移至比色池,立即用矢量色度法在波长400 nm处进行测定。砷的质量浓度在0.020~0.200 mg·L-1内与矢量色度呈二次函数关系,检出限(3s/k)为0.005 mg·L-1,检测剂可以稳定3个月。采用此方法测定实际水样,结果与ICP-AES测定结果相符,加标回收率在99.8%~112%之间。

       

      Abstract: In mass ratio of 10:2:1, sodium borohydride, sodium acetate and copper sulfate were weighed and mixed homogeneously, and a portion of 0.20 g of the mixture was encapsulated in a small capsule to prepare arsenic detection reagent Ⅰ. In mass ratio of 1:0.25:2.5:7.5:10, silver nitrate, polyvinyl alcohol (PVA-1788), nitric acid, ethanol and water were weighed and mixed homogeneously to prepare arsenic absorption solution Ⅱ. Phosphoric acid and potassium dihydrogen phosphate were weighed in mass ratio of 1:10 and mixed well, and the mixture was dried at 105℃ for 1-2 h. The dried podwer (0.30 g) was taken and pressed into tablets, which were packed into a capsule to prepare arsenic detection reagent Ⅲ. The water sample (25 mL) and arsenic detection reagent Ⅰ were added into the reaction tube of the multi-function sample processor, and the mixture was shaken well for dissolution. Then 0.15 mL of arsenic absorption solution Ⅱ was added into 5 mL of common white spirits (40-60 degree), and the mixture was added into the absorption tube. Arsenic detection reagent Ⅲ was added into the reaction tube, which was quickly connected to the absorption tube with a connecting tube. After reaction for 5 min, air was passed though at a flow rate of 0.2 L·min-1 for 5 min, and the absorption liquid was transferred into a colorimetric cell and its vector chromaticity was measured immediately at the wavelength of 400 nm by vector colorimetry. Quadratic function relationship was found between values of vector chromaticity and mass concentration of arsenic in the range of 0.020-0.200 mg·L-1, with detection limit (3s/k) of 0.005 mg·L-1. The detection reagents could be kept stable for 3 months. The determination results of arsenic in actual water samples obtained by this method were consistent with those obtained by ICP-AES. Values of recovery obtained by standard addition method were in the range of 99.8%-112%.

       

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