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
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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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