Method for measuring trivalent antimony and pentavalent antimony by magnetic solid-phase extraction-ICP-MS (Inductively Coupled Plasma Mass Spectrometry) method

A-ICP-MS, pentavalent antimony technology, applied in the field of magnetic solid phase extraction-ICP-MS measurement of trivalent antimony and pentavalent antimony, which can solve the problems of unsatisfactory use requirements, expensive equipment, and a lot of time

Inactive Publication Date: 2021-04-23
江苏荣坔环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, inductively coupled plasma emission spectrometry and flame atomic absorption spectrometry have low sensitivity and are difficult to apply to the detection of antimony in environmental water.
In addition, such methods are difficult to distinguish the speciation of antimony without sample pretreatment
Different kinds of antimony can be determined by liquid ch

Method used

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  • Method for measuring trivalent antimony and pentavalent antimony by magnetic solid-phase extraction-ICP-MS (Inductively Coupled Plasma Mass Spectrometry) method
  • Method for measuring trivalent antimony and pentavalent antimony by magnetic solid-phase extraction-ICP-MS (Inductively Coupled Plasma Mass Spectrometry) method
  • Method for measuring trivalent antimony and pentavalent antimony by magnetic solid-phase extraction-ICP-MS (Inductively Coupled Plasma Mass Spectrometry) method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A method for measuring trivalent antimony and pentavalent antimony by magnetic solid phase extraction-ICP-MS method, comprising the following steps:

[0037] (1) Preparation of raw materials: obtain aqueous solution and raw materials, and then synthesize magnetic graphene oxide particles by co-precipitation method;

[0038] Raw materials include analytical grade purity trivalent antimony standard solution, analytical grade purity pentavalent antimony standard solution, FeSO4 7H2O, FeCl3 6H2O, HNO3, HCl, NaOH and graphene oxide powder;

[0039] The steps for synthesizing magnetic graphene oxide particles by co-precipitation method include:

[0040] ①. Add 0.25g of graphene oxide into 450ml of ultrapure water, and then perform ultrasonic dispersion for 30min;

[0041] ②. Stir the graphene oxide solution, and slowly add 0.92gFeCl3·6H2O and 0.52gFeSO4·7H2O to the graphene oxide solution;

[0042] ③. Use NaOH solution to adjust the pH of the graphene oxide solution to 10, ...

Embodiment 2

[0056] In step (2), step I can also use diluted NaOH to adjust the pH of the 50ml aqueous solution to 2-10, and the other steps remain unchanged to detect the adsorption efficiency. The test results are as follows: figure 2 As shown, the adsorption efficiency of trivalent antimony remains almost constant, indicating that the change of solution pH value has little effect on the adsorption of trivalent antimony; on the contrary, the adsorption efficiency of pentavalent antimony decreases gradually with the solution pH value from 2-10, when the solution pH When adjusted to 9, the synthetic rGO / Fe3O4 hardly absorbs pentavalent antimony. The different adsorption rates of trivalent antimony and pentavalent antimony at different pH values ​​of the solution are due to the different types of antimony, and adjusting pH to 9 is the best parameter.

Embodiment 3

[0058] In step (2), step I can also add different amounts of magnetic graphene oxide, and the other steps remain unchanged. To study the extraction efficiency of trivalent antimony, the test results are as follows image 3 As shown, when the solid-liquid ratio is greater than 0.2, the extraction efficiency of trivalent antimony can reach more than 97%. When the solid-liquid ratio is 0.1, the extraction efficiency of trivalent antimony is low because there are fewer effective adsorption points. Therefore, a solid-to-liquid ratio of 0.2 is the optimal parameter

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Abstract

The invention discloses a method for measuring trivalent antimony and pentavalent antimony by a magnetic solid-phase extraction-ICP-MS (Inductively Coupled Plasma Mass Spectrometry) method, which comprises the following steps: raw material preparation: obtaining an aqueous solution and raw materials, and synthesizing magnetic graphene oxide particles by a coprecipitation method; and adsorbing trivalent antimony: adjusting the pH value of the aqueous solution, and selectively adsorbing trivalent antimony by the magnetic graphene oxide. According to the method for measuring trivalent antimony and pentavalent antimony through the magnetic solid-phase extraction ICPMS method, magnetic particles and graphene oxide are compounded, magnetic graphene oxide is synthesized through a coprecipitation method, the solid-liquid separation capacity of the magnetic graphene oxide is improved, and the selective adsorption capacity of the magnetic graphene oxide to trivalent antimony is improved on the basis of the specific PH value; the concentrations of trivalent antimony and total antimony in the environmental water sample are detected by inductively coupled plasma mass spectrometry, the pentavalent concentration of the environmental water sample is calculated by using a subtraction method; and the method is quick, convenient, simple and feasible, and is suitable for quantitative determination of trivalent antimony and pentavalent antimony in the environmental water body.

Description

technical field [0001] The invention relates to the field of antimony recovery, in particular to a magnetic solid phase extraction-ICP-MS method for measuring trivalent antimony and pentavalent antimony. Background technique [0002] With the development of science, the risk of releasing the toxic metal antimony into the environment has attracted increasing global attention. Although the background concentrations of Sb in natural water bodies and soils are low, it is worth noting that human anthropogenic activities play an important role in increasing Sb concentrations in the environment. High levels of antimony have been reported to be found in both biological and geological environmental media. Concentrations of antimony can reach hundreds of μg / L in polluted rivers from mining, smelting, burning of fossil fuels and use of antimony products. The organic form of antimony is less toxic than the inorganic form. The inorganic form of antimony predominates in natural waters....

Claims

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Application Information

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IPC IPC(8): G01N27/62G01N1/28
CPCG01N27/62G01N1/28
Inventor 杨建杨远任力恒罗琳周耀渝
Owner 江苏荣坔环保科技有限公司
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