本文選題：溶出伏安法 + 絲網(wǎng)印刷金電極��； 參考：《山西農(nóng)業(yè)大學(xué)》2016年碩士論文

【摘要】：重金屬不僅污染土壤、水體及大氣環(huán)境,還污染畜產(chǎn)品、水生生物及農(nóng)作物等,因此,在環(huán)境、食品、藥物、農(nóng)藥殘留等方面,檢測(cè)分析重金屬一直是分析工作者關(guān)注和研究的課題之一,基于傳統(tǒng)檢測(cè)重金屬的方法往往存在儀器設(shè)備大型昂貴、實(shí)驗(yàn)步驟操作復(fù)雜、需要有經(jīng)驗(yàn)的操作者操作等問題,本研究嘗試采用電化學(xué)分析方法中的差分脈沖陽極溶出伏安法,利用修飾液修飾過的絲網(wǎng)印刷金電極來檢測(cè)土壤重金屬銅的含量,具體工作如下：(1)為了改善電極表面的電化學(xué)特性,本研究將原絲網(wǎng)印刷金電極放入稀硫酸溶液中進(jìn)行循環(huán)伏安掃描活化處理,然后觀察分析其在鐵氰化鉀溶液中的循環(huán)伏安曲線圖,得出：較未活化的絲網(wǎng)印刷金電極,活化后的電極其氧化峰和還原峰電位差值變小,峰電流變大,表明活化后的絲網(wǎng)印刷金電極其電化學(xué)性能增強(qiáng)。(2)為了提高測(cè)定土壤重金屬的靈敏度,適應(yīng)定量、快速的測(cè)定要求,本研究觀察分析了絲網(wǎng)印刷金電極,鉍修飾的絲網(wǎng)印刷金電極,Nafion (0.1%)修飾的絲網(wǎng)印刷金電極,鉍/Nafion修飾的絲網(wǎng)印刷金電極在鐵氰化鉀溶液中的循環(huán)伏安掃描曲線,得出：較未修飾的絲網(wǎng)印刷金電極,修飾液修飾過的電極其電化學(xué)性能均有增強(qiáng),并且鉍/Nafion修飾的絲網(wǎng)印刷金電極電化學(xué)性能明顯增強(qiáng),其氧化峰與還原峰的電壓差值最小,峰電流值也最大。(3)為了獲得實(shí)驗(yàn)的最優(yōu)參數(shù),本研究采用差分脈沖陽極溶出伏安法,鉍/Nafion修飾的絲網(wǎng)印刷金電極測(cè)量一定濃度的標(biāo)準(zhǔn)銅溶液�；谇叭搜芯康幕A(chǔ),據(jù)測(cè)得的重金屬銅含量大小,通過控制變量法設(shè)置實(shí)驗(yàn)的各個(gè)參數(shù),得出實(shí)驗(yàn)的最佳沉積時(shí)間360s、沉積電勢(shì)-0.7 V、靜止時(shí)間10s、溶出電位0.6V、清洗電位0.8 V、清洗時(shí)間30 s、電解質(zhì)HAc-NaAc溶液PH=2、鉍溶液濃度6000 ug/L、Naf ion溶液體積4ul,并繪制了銅濃度-電流的標(biāo)準(zhǔn)曲線圖,其線性回歸方程為Y=6.54833+0.00505x,線性相關(guān)系數(shù)大于0.9926。(4)為了實(shí)現(xiàn)對(duì)實(shí)際土壤樣本重金屬銅的測(cè)量,本研究首先將實(shí)際土樣經(jīng)過濕法消解,過濾配置成相應(yīng)的土壤溶液,然后利用最優(yōu)參數(shù)結(jié)合標(biāo)準(zhǔn)曲線圖,應(yīng)用差分脈沖陽極溶出伏安法測(cè)量實(shí)際土壤樣本中的重金屬銅的含量,最后將測(cè)得的土壤重金屬銅含量與采用國(guó)際標(biāo)準(zhǔn)法原子分光光度計(jì)測(cè)量的相同土壤中的重金屬銅含量進(jìn)行比較分析,發(fā)現(xiàn)兩者檢測(cè)結(jié)果基本一致,說明該電化學(xué)檢測(cè)方法具有較好的準(zhǔn)確性,抗干擾能力強(qiáng),分析速度快,成本低、對(duì)環(huán)境無污染,適合于土壤重金屬的檢測(cè)。
[Abstract]:Heavy metals not only pollute the soil, water and atmospheric environment, but also pollute animal products, aquatic organisms and crops. Therefore, it is one of the subjects of concern and research to detect and analyze heavy metals in the environment, food, medicine and pesticide residues. The experimental procedure is complicated and requires experienced operators. This study attempts to use the differential pulse anodic stripping method in electrochemical analysis to detect the content of heavy metal copper in soil by modified silk screen printing gold electrode. The specific work is as follows: (1) to improve the electrochemical characteristics of the electrode surface. In this study, the original silk screen printed gold electrode was activated by cyclic voltammetry in dilute sulfuric acid solution, and then the cyclic voltammetry curve of the potassium ferricyanide solution was observed and analyzed. The results showed that the difference between the oxidation peak and the reduction peak potential of the activated electrode was smaller than that of the unactivated screen printing gold electrode, and the peak current became larger. In order to improve the sensitivity of heavy metals in soil, and to meet the requirements of quantitative and rapid determination, this study has observed and analyzed the silk screen printing gold electrode, bismuth modified screen printing gold electrode, Nafion (0.1%) modified screen printing gold electrode and bismuth /Nafion modified screen printing in order to improve the sensitivity of soil heavy metals. (2) The cyclic voltammetric scanning curve of the gold electrode in the potassium ferricyanide solution shows that the electrochemical performance of the modified electrode is enhanced, and the electrochemical performance of the gold electrode modified by the bismuth /Nafion modified screen is obviously enhanced, and the voltage difference between the oxidation peak and the reduction peak is the least, and the peak current is the peak current. (3) (3) in order to obtain the optimal parameters of the experiment, this study uses the differential pulse anodic stripping method and the bismuth /Nafion modified screen printing gold electrode to measure a certain concentration of standard copper solution. Based on the basis of previous research, according to the measured heavy metal copper content, the parameters of the experiment are set by the control variable method. The optimum deposition time is 360s, the deposition potential -0.7 V, the stationary time 10s, the dissolution potential 0.6V, the cleaning potential 0.8 V, the cleaning time 30 s, the electrolyte HAc-NaAc solution PH=2, the bismuth solution concentration 6000 ug/L, the Naf ion solution volume, and the standard curve of the copper concentration current are plotted, and the linear regression equation is the linear phase relation. In order to realize the measurement of heavy metal copper in the actual soil sample, the number of soil samples was measured by 0.9926. (4). First, the actual soil sample was dissolved by wet method, and the filter was formed into a corresponding soil solution. Then, the content of heavy metal copper in the actual soil samples was measured by the optimal parameter combined with the standard curve map. Finally, the content of heavy metal copper in soil was compared with the content of heavy metal copper in the same soil measured by the international standard atomic spectrophotometer. It was found that the results of the two tests are basically the same. It shows that the electrochemical detection method has good accuracy, strong anti interference ability, fast analysis speed and low cost. No pollution, suitable for the detection of heavy metals in the soil.
【學(xué)位授予單位】：山西農(nóng)業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2016
【分類號(hào)】：S151.93

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