CN111948165B - 一种基于光学探针检测施工材料次氯酸根离子的方法 - Google Patents
一种基于光学探针检测施工材料次氯酸根离子的方法 Download PDFInfo
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Abstract
本发明公开了一种基于光学探针检测施工材料次氯酸根离子的方法，先做标准曲线，取相应探针溶液溶于水中加入不同浓度的ClO‑，即滴定实验得到标准曲线。取待测液加入探针溶液，测其吸收光谱和发射光谱。对应标准曲线，得知所含ClO‑浓度。采用光学探针对建筑施工原材料进行施工前检测，具有准确及时、操作简单、耗材低等优点；在施工现场能够及时掌握原材料的性能，科学规范施工，施工安全并提高施工速度；并且在确保满足试验要求质量标准前提下，以取得更好的经济效益和社会效益。
Description
技术领域
本发明涉及一种基于光学探针的检测施工材料检测方法，尤其是基于光学探针检测施工材料中次氯酸根离子的方法，属于化学检测技术领域。
背景技术
随着经济建设的快速发展，工程试验水平已不断提高，但许多原材料力学和化学性能指标的检测方法仍不够稳定和成熟，尤其是许多化学性能指标的检测确定还是依靠各种传统的分析检测方法来实现，不但需要昂贵的仪器设备、充足的检测时间，而且还需要有经验的人力资源。空间、时间及仪器成本的压力，原材料化学性能指标检测的不准确及时，都会导致检测费用的增加、影响施工进度、缩短目标建筑的使用寿命、降低企业经济效益。因此，在桥梁、地下工程、建筑工程等施工生产中，简易快速检测、控制原材料化学性能指标至关重要。
目前建筑施工原材料的化学指标检测以对混凝土用料有危害的离子ClO-为主。用于材料检测的常见方法有：传统化学滴定方法、原子吸收光谱法、原子发射光谱法、分光光度法等，其中用于施工材料的检测手段以传统滴定方法见多，但是各个方法都有其技术不足之处。
发明内容
本发明的目的采用光学探针对建筑施工原材料进行施工前检测，具有准确及时、操作简单、耗材低等优点；在施工现场能够及时掌握原材料的性能，科学规范施工，施工安全并提高施工速度；并且在确保满足试验要求质量标准前提下，才能取得更好的经济效益和社会效益。
本发明采用的技术方案为一种基于光学探针的检测施工材料检测方法，称取C16.9mg溶于2mL DMF配成浓度为5.0×10-3mol/L的探针溶液备用。先做标准曲线，取6μL探针溶液溶于3mL水中，探针溶液中探针分子的浓度为1.0×10-5mol/L，加入不同浓度的ClO-，即滴定实验得到标准曲线。检测时，取待测液3mL，加入6μL探针溶液，测其吸收光谱和发射光谱，含有不同浓度的ClO-，在814nm处的吸收光谱明显降低；发射光谱834nm处的荧光强度明显降低。对应标准曲线，得知所含ClO-浓度。
附图说明
图1为探针分子C1在未加入ClO-(●)和加入ClO-(■)随pH值的变化曲线。
具体实施方式
以下结合附图和实施例对本发明进行详细说明。
探针分子C1的合成如下：
采用紫外-可见光谱对探针分子C1与各种常见离子识别的吸收光谱行为进行研究。在浓度为2.0×10-5mol/L的溶液体系中，探针分子C1的吸收光谱在814nm处显示其特征吸收峰，当加入5倍的其他离子(Ac-,BF4 -,Br-,ClO-,Cl-,ClO4 -,CO3 2-,F-,HCO3 -,H2PO4 -,HPO4 2-,P2O7 2-,OH-,PO4 -,HSO4 -,NO2 -,NO3 -,S2-,SO4 2-,TBHP)时，探针分子C1在814nm处的吸收光谱没有显著的变化，这表明探针分子C1和这些离子之间没有强相互作用，因而对探针在814nm处的紫外吸收不产生较强的影响；相反，在加入5倍ClO-之后，探针分子C1在814nm处的吸收光谱明显降低，这表明探针分子C1和ClO-之间发生了较强的作用。
为了进一步确定探针分子C1对ClO-的选择性，在上述溶剂体系中，考察了探针分子C1与不同离子的荧光光谱识别行为。探针分子C1自身有很强的荧光发射峰，发射峰的位置在834nm。当加入了5倍的其他离子后(5.0×10-5mol/L)，虽然某些离子也会引起荧光光谱强度的微弱下降，但只有ClO-的猝灭效应最显著。上述现象表明，在水溶液体系中，探针分子C1能够作为ClO-选择性识别探针。
在水溶液中，探针分子C1对ClO-有很好的选择性，对ClO-的检测限可以达到10- 7mol/L。并且在广泛pH的范围内仍然可以检测ClO-，这对于探针分子C1在实际快速检测氯离子的应用中具有重要的意义。
从图1中可以看出，pH值在5.5～10.0的范围内，荧光强度对pH值的变化都不敏感。这表明探针分子C1在广泛的酸碱变化范围内可以与ClO-相互作用，这对于探针分子C1在实际检测ClO-的应用中具有重要的意义。
Claims (1)
1.一种基于光学探针检测施工材料次氯酸根离子的方法，其特征在于：该方法包括ClO-浓度检测，ClO-浓度检测过程如下，称取探针分子C1 6.9 mg溶于2 mL DMF配成浓度为5.0×10-3 mol/L的探针溶液备用；先做标准曲线，取6 μL探针溶液溶于3 mL水中，探针溶液中探针分子的浓度为1.0×10-5 mol/L，加入不同浓度的ClO-，测其紫外可见光吸收光谱和荧光发射光谱；含有不同浓度的ClO-在814 nm处的吸收光谱明显降低；发射光谱834 nm处的荧光强度明显降低，得到标准曲线；检测时，取待测液3mL，加入6 μL探针溶液，测其紫外可见光吸收光谱和荧光发射光谱，对应标准曲线，得到待测液所含ClO-浓度；
探针分子C1的合成如下：
。
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| CN106841148A (zh) * | 2017-03-15 | 2017-06-13 | 湖北文理学院 | 快速检测次氯酸根的荧光探针和方法及其在自来水样检测中的应用 |
| CN110174397A (zh) * | 2019-06-15 | 2019-08-27 | 贵州医科大学 | 一种比色探针的应用 |
| CN110372632A (zh) * | 2019-07-26 | 2019-10-25 | 广东轻工职业技术学院 | 一种快速识别次氯酸根离子的荧光探针分子及其制备方法和应用 |
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| CN106841148A (zh) * | 2017-03-15 | 2017-06-13 | 湖北文理学院 | 快速检测次氯酸根的荧光探针和方法及其在自来水样检测中的应用 |
| CN110174397A (zh) * | 2019-06-15 | 2019-08-27 | 贵州医科大学 | 一种比色探针的应用 |
| CN110372632A (zh) * | 2019-07-26 | 2019-10-25 | 广东轻工职业技术学院 | 一种快速识别次氯酸根离子的荧光探针分子及其制备方法和应用 |
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