分析测试学报
分析測試學報
분석측시학보
JOURNAL OF INSTRUMENTAL ANALYSIS
2009年
12期
1405-1409
,共5页
何晓英%张艳%李容%蒋晓丽%范向明
何曉英%張豔%李容%蔣曉麗%範嚮明
하효영%장염%리용%장효려%범향명
钠基蒙脱土%十六烷基三甲基溴化铵%化学修饰电极%电化学行为%方波溶出伏安
鈉基矇脫土%十六烷基三甲基溴化銨%化學脩飾電極%電化學行為%方波溶齣伏安
납기몽탈토%십륙완기삼갑기추화안%화학수식전겁%전화학행위%방파용출복안
montmorillonite%hexadecyltrimethylammonium bromide%chemically modified electrode%electrochemical behavior%square-wave stripping voltammetry
用十六烷基三甲基溴化铵(CTAB)对钠基蒙脱土进行改性,并用红外光谱、X衍射对CTAB-NaMMT进行表征,制备了改性钠基蒙脱土修饰电极(CTAB-NaMMT-CMC/GCE),研究了水杨酸在该修饰电极上的循环伏安行为.结果表明,在pH 0.8的H_2SO_4-Na_2SO_4电解质溶液中,SA在1.19 V出现一明显的氧化峰,在40 ~400 mV/s范围内,其氧化峰电流与扫描速率的平方根(v~(1/2))呈良好线性关系,表明电极过程为受扩散控制不可逆过程.测得SA在该修饰电极上的反应电子数、质子数、传递系数及扩散系数分别为2、2、0.389、1.275×10~(-6) cm~2/s.方波溶出伏安法的氧化峰电流(I_(pa))与SA浓度在8.0×10~(-7) ~1.25×10~(-4) mol/L范围内呈良好的线性关系(r=-0.999 6),检出限为2.27×10~(-7) mol/L,加标回收率为96% ~101%.
用十六烷基三甲基溴化銨(CTAB)對鈉基矇脫土進行改性,併用紅外光譜、X衍射對CTAB-NaMMT進行錶徵,製備瞭改性鈉基矇脫土脩飾電極(CTAB-NaMMT-CMC/GCE),研究瞭水楊痠在該脩飾電極上的循環伏安行為.結果錶明,在pH 0.8的H_2SO_4-Na_2SO_4電解質溶液中,SA在1.19 V齣現一明顯的氧化峰,在40 ~400 mV/s範圍內,其氧化峰電流與掃描速率的平方根(v~(1/2))呈良好線性關繫,錶明電極過程為受擴散控製不可逆過程.測得SA在該脩飾電極上的反應電子數、質子數、傳遞繫數及擴散繫數分彆為2、2、0.389、1.275×10~(-6) cm~2/s.方波溶齣伏安法的氧化峰電流(I_(pa))與SA濃度在8.0×10~(-7) ~1.25×10~(-4) mol/L範圍內呈良好的線性關繫(r=-0.999 6),檢齣限為2.27×10~(-7) mol/L,加標迴收率為96% ~101%.
용십륙완기삼갑기추화안(CTAB)대납기몽탈토진행개성,병용홍외광보、X연사대CTAB-NaMMT진행표정,제비료개성납기몽탈토수식전겁(CTAB-NaMMT-CMC/GCE),연구료수양산재해수식전겁상적순배복안행위.결과표명,재pH 0.8적H_2SO_4-Na_2SO_4전해질용액중,SA재1.19 V출현일명현적양화봉,재40 ~400 mV/s범위내,기양화봉전류여소묘속솔적평방근(v~(1/2))정량호선성관계,표명전겁과정위수확산공제불가역과정.측득SA재해수식전겁상적반응전자수、질자수、전체계수급확산계수분별위2、2、0.389、1.275×10~(-6) cm~2/s.방파용출복안법적양화봉전류(I_(pa))여SA농도재8.0×10~(-7) ~1.25×10~(-4) mol/L범위내정량호적선성관계(r=-0.999 6),검출한위2.27×10~(-7) mol/L,가표회수솔위96% ~101%.
The montmorillonite was reformed by hexadecyltrimethylammonium bromide(CTAB).The modified clay(CTAB-MMT) was characterized by infrared(IR) spectrometry and X diffraction(XRD) spectrometry.A novel CTAB-MMT clay-modified glassy carbon electrode(CTAB-NaMMT- CMC/GCE)was prepared and the effective area of CTAB-NaMMT-CMC/GCE was calculated to be 0.105 4 cm~2.The electrochemical behavior of salicylic acid(SA) on modified electrode was studied by cyclic voltammetry(CV).The results indicated that in pH 0.8 H_2SO_4-Na_2SO_4 buffer,an obvious oxidation peak of SA appeared at 1.19 V on the modified electrode.The oxidation peak current was linear over the square root of the scanning rate in the range of 40-400 mV/s,indicating the electrode process of SA was irreversible and controlled by diffusion.Reaction electronic numbers(n),proton numbers(m),transfer coefficient(β) and diffusion coefficient of SA were obtained to be 2,2,0.389 and 1.275×10~(-6) cm~2/s,respectively.Experimental parameters were optimized and the correlation between peak current(I_(pa)) and concentration was studied by square-wave stripping voltammetry(SWSV).Under the optimal conditions,the calibration curve showed a good linearity between the oxidation peak current(I_(pa)) and SA concentration in the range of 8.0×10~(-7)-1.25×10~(-4) mol/L(r=-0.999 6) with a detection limit of 2.27×10~(-7) mol/L.The spiked recoveries were in the range of 96%-101%.