CN111948164A - 一种基于光学探针检测施工材料硫酸根的方法 - Google Patents
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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硫酸根的方法，先做标准曲线，取相应探针溶液溶于水中加入不同浓度HSO4 ‑，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HSO4 ‑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硫酸根的方法，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(HSO4 -)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，HSO4 -浓度检测过程如下，称取L13.81 mg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乙醇-水(1:1)溶液，溶液中探针分子的浓度为1.0×10- 5mol/L，加入不同浓度的HSO4 -，即滴定实验得到标准曲线。实际检测时，取待测液3mL，加入6μL的L1探针溶液，测吸收光谱和发射光谱，含有不同浓度HSO4 -待测液，在556nm处的吸收光谱明显降低，逐渐454nm会有新的吸收峰产生；发射光谱546nm处有显著的荧光增强和峰值蓝移。对应曲线，得知所含HSO4 -浓度，溶液颜色会发生变化得知所含HSO4 -浓度。
所述HSO4 -浓度检测过程中的L1能够用L2替换。
附图说明
图1为L1和L2在乙醇-水(体积比为1:1)的溶剂体系中，加入10当量的被测阴离子后溶液颜色变化。(a)和(c)是在自然光下的照片，(b)和(d)是在波长为365nm的紫外灯照射下的照片。照片中从左到右依次为L1或L2,F-,Cl-,Br-,I-,HSO4 -,Ac-,H2PO4 -,NO2 -,NO3 -和SO4 2-。
图2为在乙醇-水＝1:1的溶剂体系中，10倍其它被测阴离子存在时L1(10μM)在546nm,L2(10μM)在572nm处加入HSO4 -后的荧光强度变化率(激发波长分别为454nm,476nm；狭缝宽度为10.0nm,10.0nm)。其中1至10分别代表Ac-,Br-,Cl-,F-,H2PO4 -,HSO4 -,I-,NO2 -,NO3 -,SO4 2-。
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L系列的合成如下：
可溶性硫酸盐的侵蚀作用会大大缩短施工建筑的使用寿命。可溶性硫酸盐的侵蚀作用主要体现在如下两方面：一方面，混凝土与可溶性硫酸盐作用生成体积膨胀的二水石膏，也可以和水化铝酸钙作用生成膨胀系数更大的含结晶水的硫铝酸钙，从而导致混凝土结构开裂；另一方面，和氯离子一样，硫酸根离子可以锈蚀钢筋，严重时引起预应力钢筋脆性断裂，并且导致锈蚀体体积大幅度膨胀引起混凝土严重开裂而造成重大安全隐患。因此，控制混凝土材料中的硫酸盐含量，防止可溶性硫酸盐对混凝土的侵蚀非常重要。然而目前采用的国家标准(GB/T176-2008)中水泥、掺合料等三氧化硫的检测需要静止放置12h以上，操作费时、所需试剂多样，同样对现场材料检测造成困扰。
水经二次蒸馏后使用；N-甲基-2,3,3-三甲基吲哚鎓碘化物，N-乙基-2,3,3-三甲基苯并吲哚鎓碘化物，N-乙基-2-甲基喹啉鎓碘化物，3,4-二羟基苯甲醛，6-羟基-2-萘甲醛，4-羟基苯甲醛，4-二甲氨基苯甲醛，无水乙醇等药品为试验室已有试剂，在探针分子识别性能表征实验中所用到的阴离子均为分析纯盐；除特殊提及之外，均为商品化试剂，未经处理直接使用。
染料分子的聚集性质与浓度密切相关。因此利用吸收光谱和发射光谱研究了浓度对探针分子L1,L2光学性质的影响。具体实验步骤如下：取不同体积5.0×10-3mol/L的探针分子溶解在3mL乙醇与水混合的溶剂体系(体积比为1:1)中，配成不同浓度的溶液(5.0×10-6M～8.0×10-5M)。摇晃均匀后，静置，在室温下测其紫外-可见吸收和荧光发射光谱。
随着探针分子浓度增大，L1,L2单体的特征吸收峰(556nm,576nm)呈线性增加，但在短波长方向并没有新的吸收峰出现，说明增加探针分子的浓度并不能形成H-聚集体。L1,L2在波长大于500nm的位置均存在两个发射峰，这说明探针分子存在两种结构即“苯环构形”(A)和“醌式构形”(B)的平衡状态。此外在探针浓度大于10μM时，发射光谱长波长处表现出明显的红移“内滤效应”。通过把以上结果与上面加入HSO4 -后的紫外吸收光谱对比，可以得出结论，即HSO4 -在探针分子形成H-聚集体的过程中起着至关重要的作用。同时，探针可用于实际施工检测。
此外，从图1可以看出，在加入HSO4 -后两个探针分子的溶液颜色都发生了明显的变化：L1,L2分别由枚红色、紫色变为黄色。此外在365nm的紫外灯照射下，加入HSO4 -的溶液与加入其它离子的溶液相比颜色也明显不同，以上结果说明L1和L2都具有作为可视选择性检测HSO4 -的荧光分子探针的潜力。
为了进一步研究L1,L2作为可选择性检测HSO4 -的荧光探针的实际应用可能性，做了离子干扰实验。操作步骤为：在3mL浓度为1.0×10-5mol/L的探针分子溶液中先加入1.0×10-2mol/L的其它阴离子30μL(10倍)，再加入相同浓度的HSO4 -30μL(10倍)，摇匀后测定荧光发射光谱(如图2，激发波长分别为454nm、476nm)。从图中可以看出，各种阴离子如Ac-,Br-,Cl-,F-,H2PO4 -,I-,NO2 -,NO3 -和SO4 2-的存在对L1+HSO4 -,L2+HSO4 -的荧光发射强度影响不大，还是可以看到明显的荧光增强。
合成了新型光学探针分子L系列，并其对常见离子的光谱识别行为。其中在乙醇水溶液中，探针分子L2对HSO4 -有极好的选择性，对HSO4 -的检测限可以达到10-7M。并且在广泛pH的范围内仍然可以检测HSO4 -，这为今后实际施工材料的现场环境快速检测硫酸根离子提供了很好的技术检测手段。
Claims (3)
1.一种基于光学探针检测施工材料硫酸根的方法，其特征在于：HSO4 -浓度检测过程如下，称取L1 3.81mg溶于2mLDMF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乙醇-水(1:1)溶液，溶液中探针分子的浓度为1.0×10-5mol/L，加入不同浓度的HSO4 -，即滴定实验得到标准曲线；实际检测时，取待测液3mL，加入6μL的L1探针溶液，测吸收光谱和发射光谱，含有不同浓度HSO4 -待测液，在556nm处的吸收光谱明显降低，逐渐454nm会有新的吸收峰产生；发射光谱546nm处有显著的荧光增强和峰值蓝移；对应曲线，得知所含HSO4 -浓度，溶液颜色会发生变化得知所含HSO4 -浓度。
2.根据权利要求1所述的一种基于光学探针检测施工材料硫酸根的方法，其特征在于：所述HSO4 -浓度检测过程中的L1能够用L2替换。
3.根据权利要求1所述的一种基于光学探针检测施工材料硫酸根的方法，其特征在于：探针分子L1和L2的合成如下：
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Citations (3)
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|---|---|---|---|---|
| US20140010763A1 (en) * | 2011-03-15 | 2014-01-09 | Ramot At Tel-Aviv University Ltd. | Activatable fluorogenic compounds and uses thereof as near infrared probes |
| CN104418874A (zh) * | 2013-08-28 | 2015-03-18 | 苏州罗兰生物科技有限公司 | 一种水溶液中检测氟离子荧光分子探针及其合成与应用 |
| CN105424661A (zh) * | 2015-11-13 | 2016-03-23 | 贵州大学 | 一种比率荧光、比率吸收或目视检测微量f-的探针方法 |
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| US20140010763A1 (en) * | 2011-03-15 | 2014-01-09 | Ramot At Tel-Aviv University Ltd. | Activatable fluorogenic compounds and uses thereof as near infrared probes |
| CN104418874A (zh) * | 2013-08-28 | 2015-03-18 | 苏州罗兰生物科技有限公司 | 一种水溶液中检测氟离子荧光分子探针及其合成与应用 |
| CN105424661A (zh) * | 2015-11-13 | 2016-03-23 | 贵州大学 | 一种比率荧光、比率吸收或目视检测微量f-的探针方法 |
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