罗丹明荧光自组装膜制备及其对苯酚测定

doi:10.16085/j.issn.1000-6613.2018-2194

摘要/Abstract

摘要：

以石英片作为基底，利用吸附作用力将壳聚糖组装到硅烷化的石英表面，罗丹明B通过与壳聚糖的酯化反应间接组装到石英表面，构建壳聚糖-罗丹明B自组装膜。对该膜进行扫描电镜（SEM）表征、荧光显微镜表征，考察膜的组装条件、膜的性质、膜与苯酚的相互作用机理及抗干扰实验。结果表明苯酚与该膜在一定的范围内呈良好的线性关系，线性范围为0.00～20.00×10^-10g/L，检出限（DL）为0.13×10^-10g/L，该膜具有良好的稳定性和可再生性。并且将壳聚糖-罗丹明B自组装膜应用于芳名湖水和绶溪河水中的苯酚污染物含量的测定，发现二者水中的苯酚含量均达到了国家Ⅰ类水标准，样品加标回收率在91%～97%，该自组装膜适合于痕量样品的分析检测。

关键词: 罗丹明B, 膜, 制备, 荧光, 吸附, 苯酚

Abstract:

By using Quartz as the substrate, chitosan was assembled on the silanization layer of the quartz surface by the adsorption force. Then RhB was indirectly assembled onto the surface of quartz substrate through its esterification of chitosan, and hence the chitosan-RhB self-assembled monolayer was constructed. The chitosan-RhB self-assembled membrane was characterized by SEM and fluorescence microscope, so that the assembly conditions of the self-assembled film, the properties of the self-assembled membrane, the interaction with the phenol and the anti-interference test were investigated. Linear relationship between the phenol concentration and the RhB self-assembled membrane was found in the range of 0—20×10^-10g/L, and the detection limit (DL) was 0.13×10^-10g/L, and the membrane showed good stability and reproducibility. Furthermore, the chitosan-RhB self-assembled membrane was applied to detect phenol in the water of lake and stream. It was found that the phenol content in both water samples reached the national water standard of Class Ⅰ, and the sample recovery rate was between 91% and 97%, which suggests that the self-assembled membrane is suitable for the analysis and detection of trace samples.

Key words: Rhodamine B, membrane, preparation, fluorescence, adsorption, phenol

中图分类号:

O657.31

胡文英,陈彰旭,王天东. 罗丹明荧光自组装膜制备及其对苯酚测定[J]. 化工进展, 2019, 38(08): 3889-3895.

Wenying HU,Zhangxu CHEN,Tiandong WANG. Preparation of Rhodamine fluorescence self-assembly membrane and its determination of phenol[J]. Chemical Industry and Engineering Progress, 2019, 38(08): 3889-3895.

图/表 13

图1 壳聚糖-罗丹明B自组装膜组装过程示意图

图2 罗丹明B溶液和壳聚糖-罗丹明B自组装膜荧光谱图

图3 壳聚糖-罗丹明B自组装膜荧光显微谱图

图4 壳聚糖-罗丹明B自组装膜和壳聚糖自组装膜的SEM图

图5 壳聚糖-罗丹明B自组装膜的稳定荧光谱图

表1 不同时间下壳聚糖-罗丹明B自组装膜的荧光强度

时间/min	荧光强度
0	294.76
2	295.56
4	295.67
6	295.77
8	295.27
10	296.56
12	295.77
14	296.75
16	296.27
18	297.12

图6 不同浓度苯酚溶液中壳聚糖-罗丹明B自组装膜荧光谱图

图7 不同苯酚浓度对荧光强度的线性方程

表2 共存离子对苯酚测定的干扰影响

干扰离子	干扰离子/苯酚(质量比)	空白时的荧光强度	加入相应干扰离子后的荧光强度	相对误差/%
K⁺	500	299.72	313.64	4.64
Na⁺	500	299.72	313.66	4.65
Mg²⁺	500	299.72	312.36	4.22
Cl^-	500	299.72	313.76	4.68
$S O 4 2 -$	500	299.72	314.74	5.00
NO^3-	500	299.72	311.64	4.00
$C O 3 2 -$	500	299.72	313.26	4.52
I^-	1	299.72	317.48	5.93
葡萄糖	50	299.72	311.82	4.10
间苯二酚	1	296.47	284.44	4.10
邻苯二酚	1	296.47	309.79	4.50

表2 共存离子对苯酚测定的干扰影响

干扰离子	干扰离子/苯酚(质量比)	空白时的荧光强度	加入相应干扰离子后的荧光强度	相对误差/%
K⁺	500	299.72	313.64	4.64
Na⁺	500	299.72	313.66	4.65
Mg²⁺	500	299.72	312.36	4.22
Cl^-	500	299.72	313.76	4.68
$S O 4 2 -$	500	299.72	314.74	5.00
NO^3-	500	299.72	311.64	4.00
$C O 3 2 -$	500	299.72	313.26	4.52
I^-	1	299.72	317.48	5.93
葡萄糖	50	299.72	311.82	4.10
间苯二酚	1	296.47	284.44	4.10
邻苯二酚	1	296.47	309.79	4.50

表3 壳聚糖-罗丹明B自组装膜测定不同水样中的苯酚

样品	水样中苯酚的含量/×10^-10g·L^-1			平均值/×10^-10 g·L^-1	相对标准偏差/%
样品	1次	2次	3次	平均值/×10^-10 g·L^-1	相对标准偏差/%
湖水	12.85	11.92	11.13	11.97	7.19
河水	4.13	4.02	4.29	4.15	3.27

表4 加标回收试验

样品	苯酚标液加入量/×10^-10g·L^-1	苯酚标液检出量/×10^-10g·L^-1	回收率/%
湖水	2.00	1.94	97
河水	1.00	0.91	91

图8 再生前后壳聚糖-罗丹明B自组装膜的荧光谱图

图9 再生后罗丹明B自组装膜测定苯酚的荧光谱图

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