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.
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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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