天津工业大学学报
天津工業大學學報
천진공업대학학보
JOURNAL OF TIANJIN POLYTECHNIC UNIVERSITY
2014年
3期
34-39
,共6页
于璐洋%王会才%赵修青%李一明%李海涛
于璐洋%王會纔%趙脩青%李一明%李海濤
우로양%왕회재%조수청%리일명%리해도
巯基功能化%石墨烯%玻碳电极%差分脉冲溶出伏安法%重金属离子%痕量镉
巰基功能化%石墨烯%玻碳電極%差分脈遲溶齣伏安法%重金屬離子%痕量鎘
구기공능화%석묵희%파탄전겁%차분맥충용출복안법%중금속리자%흔량력
thiol functionalized%graphene%glassy carbon electrode%differential pulse stripping voltammetry%heavy metal%trace cadmium
建立了巯基功能化石墨烯修饰玻碳电极检测水中痕量重金属镉的方法.将Hummers法制备的氧化石墨烯经过溴乙酸羧基化、水合肼还原、氯化亚砜酰氯化后与巯基乙醇反应制备巯基功能化石墨烯,采用X-射线光电子能谱、拉曼光谱对巯基功能化石墨烯进行表征分析;将巯基功能化石墨烯修饰玻碳电极制备重金属传感器,采用循环伏安法和电化学阻抗法研究了修饰电极的电化学行为,并结合差分脉冲溶出伏安法,建立了痕量重金属镉的检测方法.结果表明:在最优化条件下,溶出峰电流与镉离子浓度在1×10-9~150×10-9范围内呈现良好的线性关系,线性相关系数为0.993,检出限为0.015×10-9(S/N =3),并具有良好的重现性(RSD =1.67%,n =11)。
建立瞭巰基功能化石墨烯脩飾玻碳電極檢測水中痕量重金屬鎘的方法.將Hummers法製備的氧化石墨烯經過溴乙痠羧基化、水閤肼還原、氯化亞砜酰氯化後與巰基乙醇反應製備巰基功能化石墨烯,採用X-射線光電子能譜、拉曼光譜對巰基功能化石墨烯進行錶徵分析;將巰基功能化石墨烯脩飾玻碳電極製備重金屬傳感器,採用循環伏安法和電化學阻抗法研究瞭脩飾電極的電化學行為,併結閤差分脈遲溶齣伏安法,建立瞭痕量重金屬鎘的檢測方法.結果錶明:在最優化條件下,溶齣峰電流與鎘離子濃度在1×10-9~150×10-9範圍內呈現良好的線性關繫,線性相關繫數為0.993,檢齣限為0.015×10-9(S/N =3),併具有良好的重現性(RSD =1.67%,n =11)。
건립료구기공능화석묵희수식파탄전겁검측수중흔량중금속력적방법.장Hummers법제비적양화석묵희경과추을산최기화、수합정환원、록화아풍선록화후여구기을순반응제비구기공능화석묵희,채용X-사선광전자능보、랍만광보대구기공능화석묵희진행표정분석;장구기공능화석묵희수식파탄전겁제비중금속전감기,채용순배복안법화전화학조항법연구료수식전겁적전화학행위,병결합차분맥충용출복안법,건립료흔량중금속력적검측방법.결과표명:재최우화조건하,용출봉전류여력리자농도재1×10-9~150×10-9범위내정현량호적선성관계,선성상관계수위0.993,검출한위0.015×10-9(S/N =3),병구유량호적중현성(RSD =1.67%,n =11)。
The detection method of trace amounts of cadmium was established based on thiol functionalized graphene modi-fied glassy carbon electrode. The graphene oxide prepared by Hummers method was modified through bromoacetic acid carboxylation, hydrazine reduction, acylation reaction, and then reacted with 2-mercaptoethanol to produce thiol functionalized graphene. X-ray photoelectron spectroscopy and Raman spectroscopy were used to character-ize the produced functionalized graphene. Heavy metal sensor was prepared by thiol functionalized graphene modified glassy carbon electrode. Cyclic voltammetry and electrochemical impedance spectroscopy were employed to study the electrochemical behavior of the modified electrode. Combined modified glassy carbon electrode with differential pulse stripping voltammetry, a method for detecting trace amounts of cadmium was established. The results showed that at optimal conditions, the linear calibration curves ranged from 1×10-9-150×10-9 for Cd2+with the linear correlation coefficient of 0.993, the detection limit was estimated to be around 0.015×10-9(S/N=3), and it also showed a good reproducibility (RSD=1.67%, n=11).