CN108535227B - CdTe QD@ZIF-8纳米复合材料在检测铬离子中的应用 - Google Patents
CdTe QD@ZIF-8纳米复合材料在检测铬离子中的应用 Download PDFInfo
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Abstract
本发明属于环境中样品检测技术领域，公开一种CdTe QD@ZIF‑8纳米复合材料在检测铬离子中的应用。将CdTe QDs@ZIF‑8纳米复合材料分散于HEPEs缓冲溶液中，加入不同浓度的Cr6+和Cr3+离子的标准样品，化学稳定后，利用荧光光谱仪检测荧光强度，绘制F/F0随铬离子浓度变化的标准曲线；将CdTe QDs@ZIF‑8纳米复合材料分散于HEPEs缓冲溶液中，加入不同含有铬离子的待测样品，化学稳定后，利用荧光光谱仪检测荧光强度，通过标准曲线确定待测样品中Cr6+的含量，同时根据荧光强度区分Cr6+和Cr3+。本发明直接相比于其他检测铬离子的方法，操作简单，成本低，离子抗干扰能力强，能够区分Cr3+和Cr6+，在铬离子检测中具有较大优势。
Description
技术领域
本发明属于环境中样品检测技术领域，具体涉及一种CdTe QDs@ZIF-8纳米复合材料在检测环境样品中铬离子的应用。
背景技术
铬是一种重要的金属元素，常见于岩石、火山灰和动植物体中，在制造不锈钢、电镀、皮革鞣制、印染等方面有广泛应用。铬在自然界中主要以六价铬(Cr6+)和三价铬(Cr3+)两种形式存在。铬的毒性与铬的价态密切相关，其中Cr3+是人体必需的微量元素，而Cr6+则对人体有害，由于其具有强氧化性和细胞渗透性，极易被人体吸收并在细胞内蓄积，产生剧毒和致癌性。Cr3+毒性较低，在某些情况下需要区分其是否被氧化成Cr6+，因此检测环境中的铬离子是非常重要的。针对环境中高毒性的铬污染，目前检测铬离子的方法主要有电感耦合等离子体质谱法(ICP-MS)、电感耦合等离子体发射光谱法(ICP-OES)、电感耦合等离子体原子发射光谱法(ICP-AES)、石墨炉原子吸收光谱法(GFAAS)、光电化学法(PEC)等，但其中大部分方法成本较高、操作复杂且无法区分铬离子价态。因此，亟需开发一种能够快速简单、成本低廉且持之有效的方法来检测环境中的铬离子含量并区分Cr6+和Cr3+。
金属有机框架(MOFs)作为一种新型的具有高比表面积、尺寸可调和较好的化学稳定性的多孔材料，已被用于化学催化、气体储存与分离、离子交换和传感器等多个领域。最近，人们通过将不同类型的纳米颗粒(NPs)以良好分散的方式并入MOFs的晶体内来构建新型的功能化NPs@MOFs复合材料，从而赋予MOFs材料新的功能。量子点(QDs)是一种尺寸范围为2-10nm的半导体纳米晶体，它具有宽吸收、窄发射、发射波长尺寸相关性等特点，已经被广泛应用于目标物的检测研究中。Buso等人合成了QD@MOF-5复合材料并将其作为MOF-5笼内分子的尺寸选择性扩散的敏感实时探针(Buso D,Jasieniak J,Lay MDH,et al.Small,2012,8,80-88)。Zhao等人合成了一种ZnO@MOF纳米复合材料并将其作为检测磷酸盐的荧光检测平台(Zhao D,Wan X,Song H,et al.Sens.Actuators,B.2014,197,50-57)。以上报道表明，该类荧光功能化复合材料在化学传感方面的可行性，因此通过合成此类制备简单、成本低廉、检测灵敏度较高的荧光功能化复合材料，极有可能解决在检测铬离子方面所遇到的环境样品组分复杂、含量较低、大型仪器检测昂贵、操作复杂，小型仪器无法快速灵敏检测的难题。
发明内容
本发明所要解决的技术问题在于为CdTe QDs@ZIF-8纳米复合材料提供一种新的应用。
解决上述技术问题所采取的技术方案是：CdTe QDs@ZIF-8纳米复合材料在检测铬离子中的应用，具体检测方案如下：
将CdTe QDs@ZIF-8纳米复合材料分散于pH＝7.0的HEPEs缓冲溶液(10mM)中，其中，CdTe QDs@ZIF-8纳米复合材料的浓度为50-250mg/L；再加入不同浓度的Cr3+和Cr6+离子的标准样品，化学稳定15min后，利用荧光光谱仪检测荧光强度，绘制F0/F随Cr6+离子浓度变化的标准曲线。
将CdTe QDs@ZIF-8纳米复合材料分散于pH＝7.0的HEPEs缓冲溶液(10mM)中，其中，CdTe QDs@ZIF-8纳米复合材料的浓度为50-250mg/L；再加入待测样品，化学稳定15min后，利用荧光光谱仪检测荧光强度，判断溶液中有无Cr3+和Cr6+，并根据绘制F0/F随Cr6+离子浓度变化的标准曲线读出待测样品中的Cr6+含量，因此，根据荧光强度即可区分Cr3+和Cr6+的存在。
本发明的检测原理是：由于CdTe QDs@ZIF-8保留了MOFs材料比表面积大和多孔的性质，因此其对于Cr3+和Cr6+具有差异性吸附能力，可以将金属离子吸附到CdTe QDs@ZIF-8复合材料的表面。由于荧光内滤作用的存在，Cr6+使得CdTe QDs@ZIF-8纳米复合材料内部的量子点荧光发生淬灭，从而CdTe QDs@ZIF-8纳米复合材料的荧光强度下降；而Cr3+与CdTeQDs@ZIF-8内部的量子点之间无荧光内滤作用存在，无法有效引起荧光猝灭。相关结果表明荧光强度与Cr6+浓度负相关，通过检测荧光猝灭的效率，即可检测样品中的Cr6+浓度，并判断有无Cr3+的存在。
本发明的有益效果为：直接以CdTe QDs@ZIF-8纳米复合材料作为检测试剂，利用Cr6+离子能够使纳米复合材料的荧光猝灭，并且与其浓度有明显的指数关系，而Cr3+离子则不能明显猝灭该复合材料的荧光的差异，从而利用荧光分光光度法即可区分Cr3+和Cr6+，并对Cr6+进行定量检测。其中CdTe QDs@ZIF-8纳米复合材料具有表面积大，荧光稳定性好，尺寸可调节且材料质地均匀等优点，相比于其他检测铬离子的方法，本发明检测方法具有操作简单，成本低，离子抗干扰能力强，能够区分Cr3+和Cr6+，因此在未来铬离子检测中具有较大的优势。
附图说明
图1是利用CdTe QDs@ZIF-8纳米复合材料的制备及检测铬离子的示意图。
图2是所合成CdTe QDs@ZIF-8(A)与ZIF-8(B)的透射电子显微镜(TEM)图像。
图3是所合成CdTe QDs@ZIF-8与ZIF-8的X射线衍射(XRD)图像。
图4是所合成CdTe QDs@ZIF-8对不同浓度的Cr6+的荧光响应曲线(A)以及荧光淬灭率与Cr6+浓度的拟合曲线(B)；图4A中箭头方向代办浓度依次增大。
图5是所合成CdTe QDs@ZIF-8对不同浓度的Cr3+的响应；图5中箭头方向代办浓度依次增大。
具体实施方式
下面结合附图和实施例对本发明进一步详细说明，但本发明的保护范围不仅限于这些实施例。
将CdTe QDs@ZIF-8纳米复合材料应用在检测溶液中的铬离子，CdTe QDs@ZIF-8纳米复合材料的制备方法为：
取干燥的CdTe QDs(根据Wu S,Dou J,Zhang J,et al.J.Mater.Chem.,2012,22,14573-14578所公开的方法制备)于50mL反应瓶中，加入六水合硝酸锌，加入超纯水溶解，避光搅拌30min；取2-甲基咪唑超声分散于去离子水中，将2-甲基咪唑溶液与反应瓶中的溶液在搅拌的条件下混合。此时合成液中各成分的摩尔比为Zn2+：2-甲基咪唑：水＝1：70：1238。经过24h的恒温磁力避光搅拌之后，使用离心机(10000r/min)对溶液进行固液分离，得到的样品用超纯水洗涤多次，直至上层清液无荧光而下层固体有荧光。将洗涤后的固体在40℃下真空干燥过夜，即可得所要的CdTe QDs@ZIF-8纳米复合材料。
上述制备方法中CdTe QDs固体的制备方法如下：取CdTe QDs溶液并加入1.2倍体积的乙醇，以8000r/min的转速离心5min，过滤，在40℃过夜真空干燥后，即可得CdTe QDs固体。
以下是CdTe QDs@ZIF-8纳米复合材料在检测铬离子中应用的具体实施例：
实施例1
在20mL(1.33mM)的CdTe QDs溶液中加入24mL的乙醇溶液，在8000r/min下离心5min，取下层固体至反应瓶中，加入200μL的超纯水复溶，加入0.01046g六水合硝酸锌，避光恒温磁力搅拌30min。然后用585μL的超纯水将0.20224g的2-甲基咪唑超声分散溶解，并加入反应瓶中。经过24h的恒温磁力避光搅拌之后，使用离心机(10000r/min)对溶液进行固液分离，得到的样品用超纯水洗涤多次，直至上清液无荧光而下层固体有荧光。将洗涤后的固体在40℃下真空干燥过夜，即可得所要的CdTe QDs@ZIF-8纳米复合材料。利用透射电子显微镜和X射线衍射仪对所合成的CdTe QDs@ZIF-8纳米复合材料进行表征，所得到的透射电子显微镜图(TEM)和X射线衍射图(XRD)分别如图2和图3所示。实验结果表明所得CdTe QDs@ZIF-8纳米复合材料尺寸约为100nm，与ZIF-8的尺寸相当，CdTe QDs均匀分布在ZIF-8的表面和内部，且未破坏ZIF-8完整的晶体结构。以上结果表明其CdTe QDs成功地嵌入到ZIF-8多孔材料中，CdTe QDs@ZIF-8纳米复合材料制备成功。
由于相关报道称，在酸性条件下，ZIF-8结构不稳定，且根据相关实验表明，在pH<6.0时，量子点溶液的荧光会发生较明显的猝灭，而在碱性条件下，重金属离子易形成固体氢氧化物，影响实验结果。故选用pH＝7.0的中性HEPEs缓冲液作为反应体系，进行下一步研究。利用pH＝7.0的中性HEPEs缓冲液配置标准的CdTe QDs@ZIF-8溶液和铬离子溶液，在浓度为150mg/L的CdTe QDs@ZIF-8溶液分别加入一系列浓度Cr6+溶液(0-40μM)和Cr3+溶液(0-40μM)，并利用荧光光谱检测仪检测其荧光强度，具体实验结果如图4A和图5所示。
结果表明，Cr6+离子能有效引起材料荧光的猝灭，且材料荧光强度与Cr6+离子的浓度成负相关，拟合方程为：
(图4B)，因此可根据拟合方程计算得到未知样品中Cr6+离子的含量；而Cr3+离子并未有效引起荧光猝灭，且荧光强度与Cr3+离子的浓度无明显的相关关系，将此作为分辨Cr6+和Cr3+离子的依据。
为了确定本发明的效果，发明人进行了大量的实验室样品研究，具体试验情况如下：
1)干扰性实验
固定CdTe QDs@ZIF-8纳米复合材料浓度为150mg/L，缓冲液pH值为7等条件，保持测试溶液中Cr6+离子浓度为20μM，然后加入对不同类型(Al3+、Fe2+、Fe3+、Cr3+、MnO4 -)和不同浓度的干扰物(Cr6+:干扰物＝1:5、1:1、5:1)进行荧光强度检测，将荧光淬灭效率和与Cr6+单独存在时的标准偏差列于表1中。
表1.干扰性实验结果表
由表可知，干扰物所带来的标准偏差-2.18％─+1.68％之间，表明干扰物对CdTeQDs@ZIF-8纳米复合材料的检测无任何影响。
2)实际样品分析
为了研究所合成的CdTe QDs@ZIF-8纳米复合材料在实际样品中检测铬离子的可行性，选取实际环境样品(自来水)进行加标分析，分析结果如下表2所示：
表2.自来水加标实验结果表
| Cr<sup>6+</sup>加标浓度(μM) | Cr<sup>6+</sup>检测浓度(μM) | RSD | 回收率 |
| 7 | 6.11±0.19 | 3.18％ | 87％ |
| 18 | 15.77±0.23 | 1.51％ | 88％ |
| 32 | 27.26±0.46 | 1.70％ | 85％ |
将已知浓度的Cr6+加标到自来水样品中，回收率为85％-88％，说明CdTe QDs@ZIF-8纳米复合材料具有在实际样品中检测Cr6+的潜力。
以上所述实施例仅表达了本发明的实施方式，但并不能因此而理解为对本发明专利的范围的限制，应当指出，对于本领域的技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些均属于本发明的保护范围。
Claims (3)
1.CdTe QDs@ZIF-8纳米复合材料在检测铬离子中的应用，其特征在于：将CdTe QDs@ZIF-8纳米复合材料分散于HEPEs缓冲溶液中，加入不同浓度的Cr6+和Cr3+离子的标准样品，化学稳定后，利用荧光光谱仪检测荧光强度，绘制F/F0随铬离子浓度变化的标准曲线；将CdTe QDs@ZIF-8纳米复合材料分散于HEPEs缓冲溶液中，加入不同含有铬离子的待测样品，化学稳定后，利用荧光光谱仪检测荧光强度，通过标准曲线确定待测样品中Cr6+的含量，同时根据荧光强度区分Cr6+和Cr3+。
2.根据权利要求1所述的CdTe QDs@ZIF-8纳米复合材料在检测铬离子中的应用，其特征在于：所述HEPEs缓冲液中的CdTe QDs@ZIF-8复合纳米材料的浓度为50-250mg/L。
3.根据权利要求1或2所述的CdTe QDs@ZIF-8纳米复合材料在检测铬离子中的应用，其特征在于：所述的HEPEs缓冲溶液的pH＝7.0。
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