Preparation method of nanocluster composite substrate AuNPs (SG) X used for detecting Pb<2+> by aggregation-induced emission

A technology of aggregation-induced luminescence and nano-clusters, which is applied in the field of analysis and detection, can solve the problems of high selectivity/sensitivity and affecting detection sensitivity, etc., and achieve the effects of strong selectivity, improved accuracy, and simple synthesis method

Inactive Publication Date: 2017-08-22
NEIJIANG NORMAL UNIV
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Problems solved by technology

In recent years, most of the reports on the detection of heavy metal ions using fluorescent nanoclusters are based on the mechanism of fluorescence quenching. Because there are many compounds that inhibit fluorescence, fluorescence quenching is more common and has a greater impact on selectivity / sensitivity.
Another report detects heavy metal cations based on the Aggregation-Induced Emission (AIE) mechanism. At present, the detection of heavy metal ions using the AIE principle of metal nanoclusters mainly uses the aggregation of nanocluster substrates to meet the metal ions to be tested and enhance the fluorescence. phenomenon, but most of the prepared metal nanocluster substrates already have weak background fluorescence, relying on fluorescence enhancement to detect heavy metal ions, this method will undoubtedly affect the detection sensitivity

Method used

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  • Preparation method of nanocluster composite substrate AuNPs (SG) X used for detecting Pb&lt;2+&gt; by aggregation-induced emission
  • Preparation method of nanocluster composite substrate AuNPs (SG) X used for detecting Pb&lt;2+&gt; by aggregation-induced emission
  • Preparation method of nanocluster composite substrate AuNPs (SG) X used for detecting Pb&lt;2+&gt; by aggregation-induced emission

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] In this example, the nano-cluster composite substrate AuNPs@(SG) X The specific preparation process is as follows:

[0035] 1) Mix 1.0mL of HAuCl with a concentration of 10mmol / L 4 Mix the aqueous solution with 1.0mL of GSH solution with a concentration of 25mmol / L, add 5mL of ultrapure water, and slowly stir for 15min at a temperature of 30°C at a speed of 200rpm to form a flocculent precipitate;

[0036] 2) Adjust the pH of the above mixed solution to 5.5 to completely dissolve the precipitate, and the solution becomes clear and transparent;

[0037] 3) After aging for 2 hours, adjust the pH of the mixed solution to 7.5 to obtain the nanocluster composite substrate AuNPs@(SG) of the present invention X .

[0038] The nanocluster composite substrate AuNPs@(SG) prepared in this example X It presents a colorless, clear and transparent aqueous solution. The composite substrate AuNPs@(SG) prepared in this example X The electron microscope picture is as figure 1 show...

Embodiment 2

[0045] In this example, the nano-cluster composite substrate AuNPs@(SG) X The specific preparation process is as follows:

[0046] 1) Mix 1.0mL of HAuCl with a concentration of 10mmol / L 4 Mix the aqueous solution with 1.0mL of GSH solution with a concentration of 20mmol / L, add 5mL of ultrapure water, and slowly stir for 10min at a temperature of 25°C at a speed of 250rpm to form a flocculent precipitate;

[0047] 2) Adjust the pH of the above-mentioned mixed solution to 6.0 to completely dissolve the precipitate, and the solution becomes clear and transparent;

[0048] 3) After aging for 1.8h, adjust the pH of the mixed solution to 7.8 to obtain the nanocluster composite substrate AuNPs@(SG) of the present invention X .

[0049] The nanocluster composite substrate AuNPs@(SG) prepared in this example X Contains Au 7 (SG) 4 ,Au 8 (SG) 5 ,Au 9 (SG) 8 and Au 11 (SG) 7 , for its specific component content, the ratio between Au:SG, and the Pb 2+ Aggregation occurs under...

Embodiment 3

[0051] In this example, the nano-cluster composite substrate AuNPs@(SG) X The specific preparation process is as follows:

[0052] 1) Mix 1.0mL of HAuCl with a concentration of 10mmol / L 4 Mix the aqueous solution with 1.0mL of GSH solution with a concentration of 30mmol / L, add 5mL of ultrapure water, and slowly stir for 20min at a temperature of 35°C at a speed of 150rpm to form a flocculent precipitate;

[0053] 2) Adjust the pH of the above-mentioned mixed solution to 5.0 to completely dissolve the precipitate, and the solution becomes clear and transparent;

[0054] 3) After aging for 2.5 hours, adjust the pH of the mixed solution to 8.0 to obtain the nanocluster composite substrate AuNPs@(SG) of the present inventionX .

[0055] The nanocluster composite substrate AuNPs@(SG) prepared in this example X Contains Au 7 (SG) 4 ,Au 8 (SG) 5 ,Au 9 (SG) 8 and Au 11 (SG) 7 , for its specific component content, the ratio between Au:SG, and the Pb 2+ Aggregates occur unde...

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Abstract

The invention provides a preparation method of nanocluster composite substrate AuNPs@ (SG) X used for detecting Pb<2+> by aggregation-induced emission, and belongs to the technical field of analysis and detection. The method includes the steps of (1) mixing HAuCl4 aqueous solution with GSH solution, adding ultrapure water to the mixed solution, and stirring the mixed solution at a certain temperature to form floc precipitation; (2) adjusting the pH value of the mixed solution to 5-6, making the precipitation completely dissolved and the mixed solution clear and transparent; (3) after aging the mixed solution for 1.5-3 h, adjusting the pH value of the mixed solution to 7.2-8.5 to obtain the nanocluster composite substrate AuNPs@ (SG) X. The preparation method adopts the direct reaction of HAuCl4 and GSH to prepare the AuNPs@ (SG) X in one step, and the synthesis method is simple and controllable. The nano Au-ion of the nanocluster composite substrate AuNPs@ (SG) prepared by the method is well dispersed to almost not overlap and aggregate, and the synthetized composite substrate mixed solution presents colorless, clear, transparent and stable under the visible light; moreover, the composite substrate prepared by the method has the advantages of strong selectivity and no self-fluorescence, and is favorable for further inducing metal ions to produce aggregation emission, and studying high sensitivity sensing.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, in particular to an aggregation-induced luminescence detection Pb 2+ Nanocluster Composite Substrate AuNPs@(SG) X method of preparation. Background technique [0002] The pollution of heavy metal ions in daily life is becoming more and more serious, which poses a serious threat to human health. Among them, lead exists in large quantities in environmental water samples, and the harm of lead to human health is well known. In 2006, a serious "lead poisoning incident" occurred in Huixian County, Gansu Province. In 2009, "lead poisoning incidents" occurred successively in Wugang, Hunan Province and Fengxiang, Shaanxi Province. ". Among them, the "lead poisoning" incident in Fengxiang County, Shaanxi Province caused nearly 900 children with hair loss, stunted growth, and mental impairment. In 2010, a lead pollution incident in Nigeria killed more than 250 people. "Lead poisoning" in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/58C09K11/70G01N21/64
CPCC09K11/58C09K11/70G01N21/643
Inventor 霍峰李道华曹琨朱俊
Owner NEIJIANG NORMAL UNIV
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