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Separation and enrichment of silica gel modified with thiomalic acid - flame atomic absorption spectrometry for the determination of trace lead and cadmium in water samples

A flame atomic absorption and thiomalic acid technology, applied in the field of rapid determination of trace lead and cadmium, can solve the problems of low selectivity and no related research on absorption spectroscopy methods, so as to improve sensitivity and selectivity, and be easy to automate Effect

Inactive Publication Date: 2015-12-09
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Directly using silica gel as an adsorbent for separation and enrichment has low selectivity. Therefore, it is necessary to chemically modify the surface of silica gel to prepare a selective adsorbent, and then separate and enrich lead and cadmium in the sample solution. to test
[0004] At present, there is no relevant research on the separation and enrichment of silica gel modified with thiomalic acid-determination of trace amounts of lead and cadmium in water samples by flame atomic absorption spectrometry

Method used

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  • Separation and enrichment of silica gel modified with thiomalic acid - flame atomic absorption spectrometry for the determination of trace lead and cadmium in water samples
  • Separation and enrichment of silica gel modified with thiomalic acid - flame atomic absorption spectrometry for the determination of trace lead and cadmium in water samples

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Experimental program
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Embodiment Construction

[0024] (1) Preparation of thiomalic acid modified silica gel adsorbent:

[0025] Weigh 30 g of 30-70 mesh microsphere silica gel, put it in a 250 mL three-necked flask, install a condenser tube, add 150.0 mL of hydrochloric acid with a concentration of 6.0 mol / L, heat the solution to reflux and mechanically stir for 5 hours, and filter out after cooling. Silica gel, wash the silica gel with distilled water until the washing solution is neutral (use 2% silver nitrate to check whether the washing solution has chloride ions), and vacuum dry to obtain activated silica gel.

[0026] Weigh 30.0g of the above activated silica gel, put it in a 250ml three-necked flask, add 100.0mL of analytically pure toluene and 13.0mL of chemically pure γ-aminopropyltriethoxysilane (KH550) after distillation and purification, stir mechanically and heat under reflux. After 6 hours, the solid product was filtered after cooling, and the solid product was washed 3 times with analytically pure toluene an...

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Abstract

The invention discloses a flame atomic absorption spectrum method for separating, enriching and determining trace lead and cadmium in a water sample by using thiomalamic acid modified silica gel. The flame atomic absorption spectrum method comprises the following steps: taking macro-porous silica gel as a carrier and taking thiomalamic acid as a functional molecule to prepare the thiomalamic acid modified silica gel; taking the thiomalamic acid modified silica gel as an adsorbent to dynamically separate and enrich the lead and the cadmium, and establishing the flame atomic absorption spectrum method. In a concentration range of 0.5-10.0 micrograms / milliliter, a Pb (II) absorbance in an eluting solution and the concentration form a good linear relation: A=0.0122*C-0.0011 (C: micrograms / milliliter); in a concentration range of 0.1-5.0 micrograms / milliliter, a Cb (II) absorbance in the eluting solution and the concentration form a good linear relation: A=0.1898*C+0.001 (C: micrograms / milliliter); the detection limits of the Pb (II) and the Cd(II) are 12.41ng / mL and 0.79ng / mL. According to the flame atomic absorption spectrum method, the sensitivity and the selectivity of the detection are improved and the detection of low-concentration Pb (II) and Cd(II) is easy to be automatic.

Description

technical field [0001] The invention relates to a method for rapidly determining trace amounts of lead and cadmium by using chemical modification to prepare an adsorbent, enrichment and separation, and atomic absorption spectroscopy. Background technique [0002] With the advancement of global industrialization, heavy metal lead and cadmium pollution has posed a great threat to human beings. Therefore, it is urgent to develop sensitive, fast and convenient separation and enrichment technology of lead and cadmium to meet the needs of environmental testing and other aspects. . [0003] At present, the methods for separating and enriching lead and cadmium in water include chemical precipitation, chemical reduction, ion exchange, biological treatment and adsorption. Among them, the adsorption method is widely used because of its simplicity, high efficiency, and the regenerable and recyclable adsorbent. Among various solid adsorption materials, silica gel has good adsorption pe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/33G01N1/34G01N1/40
Inventor 吴雄志李丽李菲萍
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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