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A kind of rapid detection method of metallic mercury

A metal mercury and solution technology, applied in chemical instruments and methods, measuring devices, material analysis through observation of the influence of chemical indicators, etc., can solve the problems of long response time and low detection sensitivity, and achieve large Stokes displacement, Low cytotoxicity and the effect of visual detection

Active Publication Date: 2020-12-01
SHANDONG AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of the above-mentioned prior art, the purpose of the present invention is to provide a rapid detection method of metallic mercury, which realizes efficient, sensitive and visual detection of metallic mercury; Problems such as low detection sensitivity

Method used

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  • A kind of rapid detection method of metallic mercury
  • A kind of rapid detection method of metallic mercury
  • A kind of rapid detection method of metallic mercury

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] Example 1: Synthesis of CDs / AuNCs@ZIF-8

[0070] (1) Synthesis of CDs:

[0071]Mix 2.10 g of citric acid, 67 μL of ethylenediamine and 20 mL of double deionized water at room temperature, transfer to a 50 mL polytetrafluoroethylene-lined autoclave, heat at 200 °C for 5 h, and cool to room temperature to obtain a dark solution. Centrifuge at 10000rpm for 15min to remove impurities. The impurity-removed solution was subjected to anti-distillation dialysis through a dialysis membrane with a molecular weight cut-off of 2000, and the dialysis time was 72 hours to obtain a CDs solution.

[0072] (2) Synthesis of AuNCs:

[0073] 5 mL of HAuCl with a solution temperature of 37 °C and a concentration of 10 mmol / L 4 Aqueous solution, add 5mL of BSA solution with a concentration of 50mg / mL and a temperature of 37°C under vigorous stirring. After stirring for 2 minutes, add 0.5mL of ascorbic acid solution with a concentration of 1.0mol / L. After 5 minutes, add a solution with a c...

Embodiment 2

[0076] Embodiment 2: the establishment of the specific fluorescence detection linear equation of metallic mercury

[0077] (1) Prepare 2ml of CDs / AuNCs@ZIF-8 (prepared in Example 1) solution with a concentration of 20mg / mL, add 30μL of double deionized water, shake well, and record the values ​​at 440nm and 640nm after 1 minute under 360nm excitation. Fluorescence intensity data, calculated fluorescence intensity ratio (I 640 / I 440 ).

[0078] (2) Add 30 μL of solutions with mercury concentrations of 3, 6, 9, 12, 15, 18, 21, 24, 27, and 30 nmol / L to the 2 ml CDs / AuNCs@ZIF-8 solution obtained in step (1), and shake well After incubation for 1 minute, use 360nm to excite the fluorescence spectrum, record the fluorescence intensity data at 440nm and 640nm, and calculate the fluorescence intensity ratio (I 640 / I 440 ).

[0079] (3) draw the fluorescence intensity ratio (I) according to the data obtained in step (2) 640 / I 440 ) and the linear relationship graph of mercury...

Embodiment 3

[0080] Embodiment 3: the detection of mercury content in the sample to be tested

[0081] (1) Prepare 2 mL of a solution of CDs / AuNCs@ZIF-8 (prepared in Example 1) with a concentration of 20 mg / mL and a pH of 7.

[0082] (2) Add 30 μL of the sample solution to be tested to the CDs / AuNCs@ZIF-8 solution obtained in step (1), shake it at room temperature and incubate for 1 minute, then use 360nm to excite the fluorescence spectrum, record the fluorescence intensity data at 440nm and 640nm, and Calculate the fluorescence intensity ratio (I 640 / I 440 ).

[0083] (3) the fluorescent intensity ratio that step (2) obtains (I 640 / I 440 ) into (embodiment 2 obtains) linear equation I 640 / I 440 =-0.0327x+0.9711, (R 2 =0.9947), calculate the content of metallic mercury in the sample to be tested.

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Abstract

The invention discloses a quick detection method of metal mercury, which comprises the following steps: coating biomimetic mineralization of AuNCs and CDs to form a nano composite material CDs / AuNCs (ZIF) ZIF-8 with a ZIF-8 shell layer on the surfaces of the CDs and the AuNCs. The preparation method is based on a room temperature environment CDs / AuNCs (at) ZIF-8 under the excitation of 360nm; twoexcellent emission peaks appear at the positions of 440 nm and 640 nm, fluorescence at the position of 640 nm is quenched in the presence of metal mercury, fluorescence at the position of 440 nm is not affected, and detection of heavy metal mercury is achieved through the fluorescence intensity ratio (I640 / I440). And the detection system has high sensitivity, and the detection can be completed inonly one minute. Along with the increase of the concentration of the metal mercury, under a portable UV lamp, the color change from red to blue is obvious, and the color can be clearly seen by naked eyes. The detection system is high in stability, simple and convenient to operate, high in targeting property, high in sensitivity, low in cost and capable of realizing visual detection.

Description

technical field [0001] The invention relates to the technical field of heavy metal analysis and detection, in particular to a rapid detection method for metallic mercury. Background technique [0002] Mercury is harmful to the environment and human health, it is not biodegradable, it can continuously accumulate in the environment and living systems, even at ultra-trace levels mercury can cause serious damage to the brain, kidneys, central nervous system and immune system . Therefore, metallic mercury is widely considered to be the most harmful pollutant in aquatic ecosystems. To ensure the safety of aquatic ecosystems, it is necessary to monitor the metallic mercury content of aquatic ecosystems in real time. In addition, due to the pollution of metallic mercury to the ecosystem, plants and animals in the living system may accumulate metallic mercury, thereby affecting food safety. To ensure food safety, it is necessary to monitor whether the raw materials contain metallic ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/64G01N21/78C09K11/65C09K11/02
CPCC09K11/02C09K11/65G01N21/643G01N21/78G01N2021/775
Inventor 李向阳李宗益郭曼莉迟静甜
Owner SHANDONG AGRICULTURAL UNIVERSITY
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