A method of rapidly detecting metal ions and small-molecule compounds through nuclear magnetic resonance

A technology of small molecular compounds and metal ions, which is applied in the analysis of nuclear magnetic resonance, etc., can solve the problems of complex pretreatment, high cost, unsuitable for real-time and rapid detection, etc.

Active Publication Date: 2016-10-19
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these high-sensitivity and multi-component analysis methods are complicated in pre-treatment and high in cost, often require specialized instruments and operators, and are not suitable for real-time and rapid detection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0141] A representative method for preparing the detection stock solution is as follows:

[0142] a-1) providing a first solution, a second solution and a third solution, wherein,

[0143] The second solution comprises a second solvent and a metal salt dissolved in the second solvent;

[0144] The third solution comprises a third solvent and a reducing agent dissolved in the third solvent;

[0145] When the metal ion and / or small molecular compound to be detected is a magnetic substance, the first solution includes a first solvent and a surfactant dissolved in the first solvent;

[0146] When the metal ion and / or the small molecular compound to be detected is a non-magnetic substance, the first solution is prepared as follows: a magnetic material is added to a first solvent in which a surfactant is dissolved to obtain a surface-modified magnetic material uniformly dispersed first solution;

[0147] The first solvent, the second solvent and the third solvent may be the same ...

Embodiment 1

[0259] Example 1 Based on CTAB and ammonia functionalized AgNPs on Fe 3+ detection

[0260] Preparation of detection stock solution 1

[0261] Add 4mL 5mM CTAB aqueous solution to 94mL water, mix and stir for 5min, then slowly add 1mL 20mM AgNO 3 Aqueous solution, continue to stir and mix; add 1mL 0.1M NaBH dropwise 4 Aqueous solution, continue stirring for 2 min after adding, to obtain functionalized AgNPs. The prepared AgNPs are oxidized by oxygen in the solution, which will form Ag on the surface of the nanoparticles. + , in the process of adding excess ammonia water, ammonia water will form Ag(NH 3 ) 2 OH complex.

[0262] Detection of Fe 3+

[0263] Take 850 μL of AgNPs and add 50 μL of different concentrations of NH 3 ·H 2 O, adjust the pH value of the solution to 5-12 after mixing, and obtain multiple groups of detection stock solutions. Then 100 μL containing different concentrations of Fe 3+ The solution to be tested was added to the obtained detection sto...

Embodiment 2

[0270] Example 2 Au@Fe based on 8-hydroxyquinoline (8-HQ) and oxalate functionalization 3 o 4 to Hg 2+ detection

[0271] Preparation of detection stock solution 2

[0272] Weigh the Fe functionalized with o-phenylenediamine 3 o 4 Nanoparticles 30mg, dispersed in 20mL water, add 1mM NaAuCl 4 8mL aqueous solution, stirred for 30min, then added 10mL of 20mM sodium oxalate solution, stirred for 30min, and the obtained nanoparticles were washed with water; the second step: dispersed the washed nanoparticles in 10mL of 0.2g / mL sodium citrate trihydrate aqueous solution, Stir for 30min, wash with water; the third step: disperse the obtained nanoparticles in 40mL water, add 1mM NaAuCl 4 10mL aqueous solution, stirred for 30min, then added 2mL of 10mM ascorbic acid aqueous solution, stirred for 30min, to obtain Au@Fe 3 o 4 . With Au@Fe 3 o 4 Au@Fe 3 o 4 The sol was diluted, and then 8-hydroxyquinoline (8-HQ) was added dropwise to the diluted Au@Fe at a volume ratio of 1:9...

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Abstract

The invention relates to a method of quantitatively detecting metal ions and/or small-molecule compounds through nuclear magnetic resonance. The method includes steps of 1) providing a liquid to be detected and a detection primary liquid, and 2) adding the liquid to be detected into the detection primary liquid, measuring the nuclear magnetic resonance transverse relaxation time of the liquid mixture, and acquiring the content of the metal ions and/or small-molecule compounds in the liquid to be detected according to the measured nuclear magnetic resonance transverse relaxation time. The method has advantages of simple operation, rapidness, a low cost, good selectivity, high sensitivity and capability of on-site real-time operation. The method is suitable for lake and river water quality survey, sewage discharging port water quality detection, and detection of melt mineral compounds, household water and various water samples or ethanol samples after treatment, and can be widely applied for the fields of food science, biomedicine, environmental science, analysis science, and the like.

Description

technical field [0001] The invention relates to the field of detection of metal ions and small molecular compounds, in particular to a detection method for rapidly detecting metal ions and / or small molecular compounds using nuclear magnetic resonance technology. Background technique [0002] With the development of science and technology and the rapid progress of society, human production activities are increasingly dependent on material support from nature. Heavy machinery industry, mining industry, chemical industry, etc. continue to export pollutants to nature, including heavy metal ions. Pollution caused by metalloid ions and small molecular compounds has become a social phenomenon that cannot be ignored and has far-reaching effects. [0003] Unlike other environmental pollutants, heavy metals are not biodegradable, they can only be converted from one form to another. It is precisely because heavy metals are not degraded, they will persist, accumulate and migrate after ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N24/08
Inventor 吴爱国陈宁怡张玉杰
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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