CN107991372B - 一种用于铅离子检测的方法 - Google Patents
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Abstract
本发明涉及电化学分析技术领域，具体涉及一种用于铅离子检测的方法。该方法以AgNWs/PDMS可塑电极为工作电极，Ag/AgCl电极为参比电极，铂丝为辅助电极组成三电极系统，将该三电极系统置于Pb2+离子待测液和支持电解质中。设置初始电位为‑0.1V，终止电位为‑1V，电位增量为0.01V，记录Pb2+的交流阻抗‑电位关系曲线，并利用Pb2+在峰电位点的阻抗值用标准曲线法进行Pb2+离子的定量分析。本发明利用PDMS良好的柔韧性并结合银纳米线良好的导电性制得一种对铅离子具有高灵敏度的电极，且该电化学分析方法操作简单、检测时间短、准确度和灵敏度高，可广泛应用于实际样品测定。
Description
技术领域
本发明涉及电化学分析技术领域，具体涉及一种可用于铅离子测定的新方法。
背景技术
铅通过食物链不可逆的富集在人体内，一旦超标将引起人体产生多种疾病，如贫血、记忆力减退、心情烦躁，特别是导致儿童神经发育迟缓。传统的铅离子检测方法，如分光光度法、原子吸收光谱法和原子发射光谱法，虽灵敏度高，特异性好，但存在操作流程复杂、成本高、需专业人员操作、设备庞大等问题。电化学方法设备小型、操作简单、成本低、检测速度快，是目前研究金属离子检测的热点之一。
发明内容
为弥补现有技术的不足，本发明提供一种利用交流阻抗法建立检测铅离子的新的分析方法。
为实现上述目的，本发明采用的技术方案为：
以AgNWs/PDMS可塑电极为工作电极，Ag/AgCl电极为参比电极，铂丝为辅助电极组成三电极系统，将该三电极系统置于Pb2+离子待测液和支持电解质中。然后，设置初始电位为-0.1V，终止电位为-1V，电位增量为0.01V，记录浓度范围分别为0.1～7mg/L，0.006～0.03mg/L，0.0001～0.0009mg/L的Pb2+的交流阻抗-电位关系(IMPE)曲线，并利用Pb2+在峰电位点的阻抗值用标准曲线法进行Pb2+离子的定量分析。
具体的操作步骤包括：
(1)制备AgNWs/PDMS可塑电极：在硅片表面旋涂光刻胶，制得到硅片模板；向硅片模板浇注质量比为10:1的PDMS混合溶液，抽净气泡、加热、固化、清洗，得到带有固定形状凹槽的PDMS基片；配制质量百分数为2％PVA与5％Gly的混合水溶液，将制备好的PDMS基片浸泡于PVA和Gly混合溶液中20min，再放入60℃的真空烘箱中干燥；重复浸泡、干燥步骤，将PDMS基片热固定，得到表面亲水的PDMS基片；将无水乙醇与水按9:1的体积比混合作为溶剂，配制浓度为5mg/mL的银纳米线溶液，均匀地铺展在PDMS基片表面的凹槽内，室温下放置干燥一天以上，即制备出AgNWs/PDMS可塑电极；
(2)Pb2+离子峰电位的确定：利用循环伏安法，在-1～0V的电位范围内进行扫描，记录Pb2+的峰电位为-0.55V；
(3)Pb2+离子定量分析：以AgNWs/PDMS可塑电极为工作电极，Ag/AgCl电极为参比电极，对电极为铂丝电极，组成三电极系统；将该三电极系统置于Pb2+离子待测液和支持电解质中，记录浓度范围分别为0.1～7mg/L，0.006～0.03mg/L，0.0001～0.0009mg/L的Pb2+的IMPE曲线，并利用Pb2+在峰电位点的阻抗值用标准曲线法进行Pb2+离子的定量分析。
进一步的，所述支持电解质含有0.3mol/LKNO3溶液。
本发明采用交流阻抗法，利用低频阻抗建立标准曲线，建立极化电流和待测液浓度间的函数关系曲线，可消除电解质支持液对目标分析物扩散过程产生的误差，进而可以免去电解质支持液的优化试验。本发明利用PDMS良好的柔韧性并结合银纳米线良好的导电性制得一种对铅离子具有高灵敏度的电极，且该电化学分析方法操作简单、检测时间短、准确度和灵敏度高，可广泛应用于实际样品测定。
附图说明
图1为铅离子的循环伏安曲线；
图2为不同浓度Pb2+的阻抗分析曲线及其标准曲线。其中，(a)是浓度范围0.1～7mg/L，(b)是浓度范围0.006～0.03mg/L，(c)是浓度范围0.0001～0.0009mg/Lmg/L。
具体实施方式
下面通过具体实施例详述本发明，但不限制本发明的保护范围。如无特殊说明，本发明所采用的实验方法均为常规方法，所用实验器材、材料、试剂等均可从化学公司购买。
下述实施例AgNWs/PDMS可塑电极的制备方法为：
采用光刻技术制作PDMS基片。在洁净的硅片表面旋涂光刻胶，遮蔽含有电极图形的掩膜版，最后进行曝光及显影，得到硅片模板。将硅片模板置于一次性培养皿中，浇注质量比为10:1的PDMS混合溶液；再放入真空干燥器中负压抽净PDMS混合溶液中的气泡，用时2h；取出后放入80℃的恒温烘箱中加热固化1h，并切分成12个电极基片；将做好的电极基片用胶带(购自美国3M公司)处理清除表面附着的灰尘，然后放入紫外臭氧清洗机中清洗2min，得到带有固定形状凹槽的PDMS基片。
PDMS基片表面亲水层修饰。具体步骤如下：(1)配制质量百分数为2％PVA与5％Gly的混合水溶液；(2)将制备好的PDMS基片浸泡于PVA和Gly混合溶液中20min，再放入60℃的真空烘箱中干燥2h；(3)重复步骤(2)一次；(4)将PDMS基片放入100℃的真空烘箱中热固定20min；(5)重复步骤(2)、(4)一次，得到表面亲水层修饰的PDMS基片。
电极制备。将无水乙醇与水按9:1的体积比混合作为溶剂，配制浓度为5mg/mL的银纳米线溶液，将银纳米线溶液均匀地铺展在PDMS基片表面的凹槽内，于室温下放置干燥一天以上，即制备出AgNWs/PDMS可塑电极。
实施例1浓度范围为0.1～7mg/L铅离子检测
将三电极体系置于含有0.3mol/L KNO3溶液作为支持电解质的Pb2+待测液中。首先，利用循环伏安法，在-1～0V的电位范围内进行扫描，记录Pb2+的峰电位为-0.55V，如附图1所示。然后，设置初始电位为-0.1V，终止电位为-1V，电位增量为0.01V，记录Pb2+的IMPE曲线，并利用Pb2+在峰电位点的阻抗值，采用origin软件制作标准曲线。线性回归方程为：log(Z/ohm)＝0.0066c(mg/L)+1.1343，相关系数R2为0.9981，线性范围的最下限为0.0001mg/L。
实施例2浓度范围为0.006～0.03mg/L铅离子检测
将三电极体系置于含有0.3mol/LKNO3溶液作为支持电解质的Pb2+待测液中。首先，利用循环伏安法，在-1～0V的电位范围内进行扫描，记录Pb2+的峰电位为-0.55V，如附图1所示。然后，设置初始电位为-0.1V，终止电位为-1V，电位增量为0.01V，记录Pb2+的IMPE曲线，并利用Pb2+在峰电位点的阻抗值，采用origin软件制作标准曲线。
线性回归方程为：log(Z/ohm)＝1.3296c(mg/L)+1.1480，相关系数R2为0.9961。
实施例3浓度范围为0.0001～0.0009mg/L铅离子检测
将三电极体系置于含有0.3mol/LKNO3溶液作为支持电解质的Pb2+待测液中。首先，利用循环伏安法，在-1～0V的电位范围内进行扫描，记录Pb2+的峰电位为-0.55V，如附图1所示。然后，设置初始电位为-0.1V，终止电位为-1V，电位增量为0.01V，记录Pb2+的IMPE曲线，并利用Pb2+在峰电位点的阻抗值，采用origin软件制作标准曲线。
线性回归方程为：log(Z/ohm)＝50.3095c(mg/L)+1.2117，相关系数R2为0.9982。
应用例自来水总铅离子的测定
检测对象：大连市地区自来水
检测方法：以AgNWs/PDMS可塑电极为工作电极，Ag/AgCl电极为参比电极，铂丝为辅助电极置于铅离子待测液中利用交流阻抗法检测自来水中Pb2+。将三电极体系置于含有0.3mol/LKNO3溶液作为支持电解质的Pb2+待测液中，在初始电位为-0.1V，终止电位为-1V，电位增量为0.01V的实验条件下，记录Pb2+的IMPE曲线。实验结果如表1所示。平行测定10次，得到的平均阻抗值为1.23，代入线性回归方程：
log(Z/ohm)＝50.3095c(mg/L)+1.2117，相关系数R2为0.9982。
计算出水样中Pb2+的平均浓度为4.4×10-4mg/L。《生活饮用水卫生标准》(GB5749-2006)中规定，Pb2+的含量应≤0.01mg/L。该样品的分析结果属于合格的质量范围。10次平行测定的相对标准偏差RSD值为2.65％。加标回收率为102.74％。
表1自来水中Pb2+的测定结果
以上所述，仅为本发明创造较佳的具体实施方式，但本发明创造的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明创造披露的技术范围内，根据本发明创造的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明创造的保护范围之内。
Claims (4)
1.一种用于铅离子检测的方法，其特征在于，以AgNWs/PDMS可塑电极为工作电极，Ag/AgCl电极为参比电极，铂丝为辅助电极组成三电极系统，将该三电极系统置于Pb2+离子待测液和支持电解质中；然后，设置初始电位为-0.1V，终止电位为-1V，电位增量为0.01V，记录浓度范围分别为0.1～7mg/L，0.006～0.03mg/L，0.0001～0.0009mg/L的Pb2+的交流阻抗-电位关系曲线，并利用Pb2+在峰电位点的阻抗值用标准曲线法进行Pb2+离子的定量分析；浓度范围为0.1～7mg/L线性回归方程为：log(Z/ohm)＝0.0066c(mg/L)+1.1343；浓度范围为0.006～0.03mg/L线性回归方程为：log(Z/ohm)＝1.3296c(mg/L)+1.1480；浓度范围为0.0001～0.0009mg/L线性回归方程为：log(Z/ohm)＝50.3095c(mg/L)+1.2117。
2.根据权利要求1所述的方法，其特征在于，所述AgNWs/PDMS可塑电极的制备方法为：在硅片表面旋涂光刻胶，制得到硅片模板；向硅片模板浇注质量比为10:1的PDMS混合溶液，抽净气泡、加热、固化、清洗，得到带有固定形状凹槽的PDMS基片；配制质量百分数为2％PVA与5％Gly的混合水溶液，将制备好的PDMS基片浸泡于PVA和Gly混合溶液中20min，再放入60℃的真空烘箱中干燥；重复浸泡、干燥步骤，将PDMS基片热固定，得到表面亲水的PDMS基片；将无水乙醇与水按9:1的体积比混合作为溶剂，配制浓度为5mg/mL的银纳米线溶液，均匀地铺展在PDMS基片表面的凹槽内，室温下放置干燥一天以上，即制备出AgNWs/PDMS可塑电极。
3.根据权利要求1所述的方法，其特征在于，Pb2+离子峰电位的确定方法为：利用循环伏安法，在-1～0V的电位范围内进行扫描，记录Pb2+的峰电位为-0.55V。
4.根据权利要求1所述的方法，其特征在于，所述支持电解质含有0.3mol/L KNO3溶液。
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