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    Omim6Mo7O24碳糊离子选择性电极测定环境水体中的PF6-

    Determanation of PF6- in Environmental Water by Omim6Mo7O24 Carbon Paste Ion Selective Electrode

    • 摘要: 采用自制的Omim6Mo7O24碳糊离子选择性电极(ISE)测定水中PF6-的含量。试验采用1-辛基-3-甲基咪唑四氟硼酸盐和钼酸铵制备Omim6Mo7O24固态离子液体,并用傅里叶变换红外光谱仪(FT-IR)和X射线衍射仪(XRD)进行表征,结果表明:Omim6Mo7O24固态离子液体已被成功制备;热重(TG)分析结果表明:该离子液体在28~280℃内的热稳定性较好。将制备的Omim6Mo7O24固态离子液体粉末与石墨粉按照质量比为1:9的比例混合,再将该混合粉末与二甲基硅油按照质量比6:1的比例混合制备碳糊ISE。在30℃下,以碳糊ISE为指示电极,Ag/AgCl电极为参比电极,在体积比为1:1的工作缓冲溶液(由硼酸、柠檬酸和磷酸钠混合制备,pH 9)和Na2EDTA溶液的混合溶液中测定水中PF6-的含量。结果显示:在PF6-的浓度为1.0×10-8~1.0×10-1mol·L-1时,其浓度的负对数与对应的碳糊ISE电位响应值呈线性关系,检出限为5.4×10-9mol·L-1。PF6-的加标回收率大于95.0%,测定值的相对标准偏差(n=5)不大于2.5%。采用该方法和离子色谱法同时分析了3组PF6-盲样,取得了较为一致的结果。用该方法分析环境水体时,由于PF6-的易水解性,未检出PF6-的残留,采用该方法考察了PF6-在常规酸度范围(pH 6~8)水体中的水解过程,发现PF6-的半衰期为0.426~0.444 h,且常规水体的酸度变化不会影响PF6-的水解。

       

      Abstract: A self-madeOmim6Mo7O24 carbon paste ion selective electrode (ISE) was used to determine the content of PF6- in water. The solid ionic liquidOmim6Mo7O24 was prepared by 1-octyl-3-methylimidazolium tetrafluoroborate and ammonium molybdate, and characterization results from FT-IR and XRD showed that solid ionic liquidOmim6Mo7O24 was successfully prepared. The TG analysis showed that the ionic liquid had good thermal stability in the range of 28-280℃. After mixing the solid ionic liquidOmim6Mo7O24 powder with graphite powder with the mass ratio of 1:9, the above mixed powder was mixed with dimethyl silicone oil with the mass ratio of 6:1 to prepare carbon paste ISE. The content of PF6- in water was determined at 30℃ with carbon paste ISE as indicator electrode and Ag/AgCl electrode as reference electrode in the mixed solution composed of working buffer solution (containing boric acid, citric acid and sodium phosphate, pH 9) and Na2EDTA solution with volume ratio of 1:1. The results showed that the linearity relationship between the negative logarithm of PF6- concentration and carbon paste ISE potential response was kept in the range of 1.0×10-8-1.0×10-1mol·L-1, with detection limit of 5.4×10-9mol·L-1. The recovery of PF6- obtained was more than 95.0%, and the RSD (n=5) of the determined values was less than 2.5%. Three groups of PF6- spiked blind samples were analyzed by the proposed method and ion chromatography from reference, obtaining a consistent result. When using this method to analyze the environmental water, due to the easy hydrolysis of PF6-, no residue of PF6- was detected. Therefore, this method was used to investigate the hydrolysis process of PF6- in water with a normal acidity range (pH 6-8), finding that the half-life of PF6- was in the range of 0.426-0.444 h, and the acidity changes of conventional water did not affect the hydrolysis of PF6-.

       

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