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Method for detecting trivalent chromic ions by using gamma-polyglutamic acid stabilized triiron tetraoxide nano grains

A technology of ferric oxide and polyglutamic acid, which is applied in the analysis of nuclear magnetic resonance, etc., can solve the problems of low-cost real-time detection, system influence, and bulky volume, and achieve good aqueous solution stability, short response time, and sensitivity high effect

Inactive Publication Date: 2015-01-21
DONGHUA UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0003] The traditional detection of trivalent chromium ions is mainly by means of large-scale instruments, most of which use atomic absorption spectrometry, voltammetry, surface plasmon field-enhanced resonance light scattering, and colorimetric detection methods that have attracted much attention recently, although these methods Trivalent chromium ions can be detected, but due to bulky or low precision, it is difficult to achieve high-precision low-cost real-time detection
For example, the common diphenylcarbazide spectrophotometry has the advantages of simple equipment, low detection limit, and precision, and is widely used. However, in the use of this method, heating is required to boil and digest, which is easy to cause bumping, and the remaining volume of the boiled water sample Difficult to grasp, thus affecting the accuracy and precision of detection
Although ferrous ammonium sulfate titration can be used to determine trivalent chromium ions, the vanadium contained in the sample can have a great impact on the system, which limits the use of this method
Inductively coupled plasma emission spectrometry is a kind of spectral analysis method that uses an inductively coupled plasma torch as an excitation light source. It has been widely used in routine analysis and has the advantages of high precision and fast analysis speed. However, the test sample needs to be digested. Moreover, large instruments are required, which is not conducive to real-time detection

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  • Method for detecting trivalent chromic ions by using gamma-polyglutamic acid stabilized triiron tetraoxide nano grains
  • Method for detecting trivalent chromic ions by using gamma-polyglutamic acid stabilized triiron tetraoxide nano grains
  • Method for detecting trivalent chromic ions by using gamma-polyglutamic acid stabilized triiron tetraoxide nano grains

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Experimental program
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Effect test

Embodiment 1

[0051] Add γ-polyglutamic acid solution into the ferric chloride solution, stir and add sodium sulfite solution, stir for 30 minutes, add ammonia water in a 60°C water bath, and react for 1.5 hours. The upper layer solution was taken by centrifugation, and dialyzed to obtain a solution of iron ferric oxide nanoparticles stabilized by γ-polyglutamic acid. Wherein the mass ratio of ferric chloride to polyglutamic acid is 7:1, and the molar ratio of ferric chloride to sodium sulfite is 7:1.

[0052] Observation by transmission electron microscope to the ferric oxide nanoparticles stabilized by gamma-polyglutamic acid prepared by the present invention shows that the ferric oxide nanoparticles formed are uniform, the average particle size is 5.3nm, and they are distributed in narrower range (see attached figure 1). The hydrodynamic particle size was measured by dynamic light scattering, and the result showed that the particle size was about 217.5nm. X-ray diffraction test proves...

Embodiment 2

[0054] Take 50 μL (concentration of 20 μM) of the γ-polyglutamic acid-stabilized iron ferric oxide nanoparticle solution prepared in Example 1, and add different volumes (0, 20, 40, 60, 80, 100 μL) of Cr 3+ Solution (concentration is 10nM), and set the volume to 1mL, place at room temperature for 10min, test the T of ferroferric oxide nanoparticles 2 The relaxation time changes, resulting in Cr 3+ Content and T 2 Quantitative relationship of relaxation times.

[0055] By adding different concentrations of Cr to the ferric oxide nanoparticles stabilized by gamma-polyglutamic acid prepared in the present invention 3+ The magnetic resonance detection results showed that the r 2 Value varies with Cr 3+ Concentration increases gradually (see appendix Figure 6 ), and its linear correlation coefficient R 2 = 0.9998. From Figure 6 It can be seen that Cr 3+ The addition of T to Fe3O4 nanoparticles 2 The relaxation time curve has a greater influence, while with the Cr 3+ co...

Embodiment 3

[0057] Get the gamma-polyglutamic acid stable iron ferric oxide nanoparticle solution 50 μ L (concentration is 20 μ M) that embodiment 1 prepares to be diluted to 1mL, test its T 2 relaxation time. In the same way, take a series of γ-polyglutamic acid-stabilized ferric oxide nanoparticle solutions, mix with 100 μL aqueous solution of chromium nitrate and potassium chloride, lead nitrate, cobalt chloride, nickel nitrate, calcium nitrate, magnesium chloride, Lithium sulfate and copper sulfate were mixed, diluted to 1mL solution, left at room temperature for 10min, and the T of ferric oxide nanoparticles was tested. 2 Relaxation time changes to verify the effect of Fe3O4 nanoparticles on Cr 3+ detection specificity. Wherein the concentration of potassium chloride, lead nitrate, cobalt chloride, nickel nitrate, calcium nitrate, magnesium chloride, lithium sulfate, copper sulfate is 10nM (final concentration is 1nM).

[0058] The magnetic resonance detection of ferric oxide solu...

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Abstract

The invention provides a method for detecting trivalent chromic ions by using gamma-polyglutamic acid stabilized triiron tetraoxide nano grains. The method comprises the following steps: adding a gamma-polyglutamic acid solution into an iron trichloride solution; stirring and adding a sodium sulfite solution; stirring and reacting; adding ammonia water under a water bath condition; reacting, centrifuging and dialyzing to obtain a gamma-polyglutamic acid stabilized triiron tetraoxide nano grain solution; adding a Cr<3+> solution into the gamma-polyglutamic acid stabilized triiron tetraoxide nano grain solution; mixing and then diluting; standing; and testing the change of relaxation time T2 of the triiron tetraoxide nano grains to obtain a quantitative relation between the concentration of Cr<3+> and the relaxation time T2. According to the method provided by the invention, the triiron tetraoxide nano grains are prepared by adopting the macromolecular structure property of gamma-polyglutamic acid; the preparation method is simple, the reaction conditions are moderate and the operation is easy; and the gamma-polyglutamic acid stabilized triiron tetraoxide nano grains prepared by the invention have good selectivity and extremely-high sensitivity on the detection of the trivalent chromic ions.

Description

technical field [0001] The invention belongs to the detection field of heavy metal ions, and in particular relates to a method for detecting trivalent chromium ions by using gamma-polyglutamic acid stabilized iron ferric oxide nanoparticles. Background technique [0002] Chromium is a common chemical element in life and is widely distributed on the earth. The common compounds of chromium are mainly +3 and +6 valences, which play an extremely important role in regulating plant growth, ensuring human health, and promoting industrial development. In terms of plant growth, trace amounts of chromium can effectively increase enzyme activity in plants, enhance plant photosynthesis, increase plant resistance to diseases and increase crop yields. In terms of human health, trace amounts of trivalent chromium play an important role in maintaining the physiological health of the human body. Firstly, chromium can regulate glucose metabolism, which is an important part of glucose tolera...

Claims

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Application Information

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IPC IPC(8): G01N24/08
Inventor 史向阳于智博朱建志
Owner DONGHUA UNIV
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