微波辅助法一步合成荧光碳点用于水中三价铁离子的检测

doi:10.7503/cjcu20180031

摘要/Abstract

摘要：

以柠檬酸为碳源, 丙三醇为反应溶剂和微波吸收介质, 通过微波辅助法一步合成了荧光碳点. 该方法快速、环保, 合成的碳点尺寸均一、分散性好. 利用透射电子显微镜、荧光光谱、紫外光谱、红外光谱和X射线光电子能谱对所合成碳点的结构和性质进行了表征. 基于三价铁离子能够选择性地猝灭碳点荧光的特性, 建立了基于碳点检测实际水样品中Fe³⁺的方法. 该方法线性范围为5~50 μmol/L, 检出限为2.16 μmol/L, 在加标样品中Fe³⁺的加标回收率为96.8%~106.0%.

关键词: 碳点, 微波辅助法, Fe³⁺检测, 荧光猝灭法

Abstract:

Carbon dots(CDs) were synthesized through one-pot microwave-assisted synthesis method using citric acid as carbon source, glycerol as solvent and passivation agent. The obtained CDs have uniform size and good dispersion. The proposed synthesis method is rapid, simple and eco-friendly. The CDs were applied to detecting Fe³⁺ in practical water samples based on fluorescence(FL) quenching mechanism with a linear range of 5—50 μmol/L, a detection limit of 2.16 μmol/L and the recoveries of 96.8%—106.0%, which showed good feasibility in detection of Fe³⁺ in practical water samples.

Key words: Carbon dots, Microwave-assisted method, Fe³⁺ detection, Fluorescence quenching method

TrendMD:

徐源, 陈艳华, 丁兰. 微波辅助法一步合成荧光碳点用于水中三价铁离子的检测. 高等学校化学学报, 2018, 39(7): 1420.

XU Yuan, CHEN Yanhua, DING Lan. One-pot Microwave-assisted Synthesis of Passivated Fluorescent Carbon Dots for Fe(Ⅲ) Detection^†. Chem. J. Chinese Universities, 2018, 39(7): 1420.

图/表 10

Scheme 1 Schematic illustration of the synthesis process

Fig.1 Quantum yields of the CDs with different dosages of citric acid(A) and different reaction time(B)

Fig.2 TEM image(A) and XRD pattern(B) of the CDs Insert of (A): corresponding size distribution.

Fig.3 FTIR(A) and XPS(B) spectra of the CDs and high resolution XPS spectra of C1s(C) and O1s(D) of the CDs

Fig.4 Fluorescence and UV-Vis absorption spectra of the CDs^ Insert: photographs of the CDs solution under UV light(left) and visible light(right).

Fig.5 FL intensity of the CDs at different pH values with and without the addition of 50 μmol/L Fe3+(A), FL intensity of the CDs under different concentration of NaCl(B), FL decay of the CDs in the absence and presence of 50 μmol/L Fe3+(C) and UV-Vis absorption spectra of the CDs before and after adding 50 μmol/L Fe3+(D)

Fig.6 Change of FL intensity of the CDs with 50 μmol/L Fe3+ against different incubation time(A) and effect of different metal ions(50 μmol/L) on the FL intensity of the CDs(B)

Fig.7 FL spectra of the CDs with different concentrations of Fe3+(A) and the linear relationship between

Table 1 Analytical results of Fe3+ in spiked practical water samples by the proposed method

Sample	Added/(μmol·L^-1)	Total found/(μmol·L^-1)	Recovery(n=3, %)	RSD(n=3, %)
Tap water 1	5	4.85	96.8	1.1
	10	9.75	97.4	0.4
	20	19.48	97.4	0.6
Tap water 1	5	5.18	103.8	0.5
	10	10.15	101.5	1.0
	20	20.03	100.2	0.7
Lake water	5	5.29	106.0	0.6
	10	10.58	105.9	0.6
	20	20.32	101.6	0.5

Table 2 Comparison of different CDs-based Fe3+ probe

Probe	Linear range/ (μmol·L^-1)	LOD/ (μmol·L^-1)	Ref.	Probe	Linear range/ (μmol·L^-1)	LOD/ (μmol·L^-1)	Ref.
CDs	0—7000	35	[27]	N-CDs	2—25	0.9	[31]
CDs	12.5—100	9.97	[28]	N-CDs	20—100	2.56	[32]
GQD	1—80	7.22	[29]	CDs	5—50	2.16	This work
N-CDs	0—4	1.17	[30]

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