Quick extraction method for arsenic and selenium in different forms in flying ash

An extraction method and morphological technology, applied in the field of analytical chemistry, which can solve the problems of long cycle and achieve the effects of short time, good repeatability and reproducibility, and high extraction recovery rate.

Active Publication Date: 2019-01-15
NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the traditional Wenzel extraction method is oscillating extraction, and the cycle is long, so it is urgent to find a method for rapid and stable extraction of arsenic and selenium in fly ash. This method is still a hot and frontier topic in the field of analytical chemistry.

Method used

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  • Quick extraction method for arsenic and selenium in different forms in flying ash

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A fly ash sample from a power plant in Hebei was collected. After grinding, the fly ash sample was freeze-dried at low temperature for 24 hours, and then passed through a 200-mesh sieve by means of an automatic horizontal reciprocating vibrating sieving machine. The resulting sample was balanced under the conditions specified in GB / T 32722. The working parameters of the fixed ultrasonic instrument are: the working frequency is: 40kHz, the power is 250W, and the volume of the immersion liquid in the tank is 5.5L.

[0033] Extraction of non-specific adsorbed arsenic: Weigh 1g of the fly ash sample after the equilibrium treatment into a 50mL polyethylene centrifuge tube, add 25mL, 0.05M ammonium sulfate solution to fully mix the fly ash sample with the extract, and put the centrifuge tube into In a beaker containing 400 mL of ultrapure water, the beaker was placed in an ultrasonic instrument for ultrasonication. The ultrasonic was divided into 4 times. The cumulative ultrasoni...

Embodiment 2

[0040] A sample of fly ash from a power plant in Shanxi was collected, and the sample treatment was the same as in Example 1.

[0041] Extraction of non-specifically adsorbed arsenic and selenium: the extraction method and process are the same as in Example 1. The average concentration of non-specifically adsorbed arsenic and selenium (form 1) obtained by detection and analysis is 3.62±0.37 mg / kg and 2.98±0.22 mg / kg, respectively The average concentrations of non-specifically adsorbed arsenic and selenium extracted by traditional Wenzel shaking extraction were 3.91±0.62 mg / kg and 2.86±0.42 mg / kg, respectively. The average recovery rates of the ultrasonic-assisted extraction of non-specifically adsorbed arsenic and selenium with the method of the present invention are respectively 92.6% and 104.2% of the traditional shaking extraction.

[0042] Extraction of specific adsorbed arsenic and selenium: the extraction method and process are the same as in Example 1. The average concentrat...

Embodiment 3

[0048] The national standard material GBW08401 was collected as a fly ash sample, and the sample processing was the same as in Example 1.

[0049] Extraction of non-specifically adsorbed arsenic and selenium: The extraction method and process are the same as in Example 1. The average concentration of non-specifically adsorbed arsenic and selenium (form 1) obtained by detection and analysis is 4.12±0.62 mg / kg and 0.26±0.03 mg / kg, respectively The average concentrations of the non-specifically adsorbed arsenic and selenium extracted by the traditional Wenzel shaking extraction method were 4.55±0.52 mg / kg and 0.27±0.04 mg / kg, respectively. The average recovery rates of the ultrasonic-assisted extraction of non-specifically adsorbed arsenic and selenium in the method of the present invention are respectively 90.5% and 96.3% of the traditional shaking extraction.

[0050] Extraction of specific adsorption arsenic and selenium: the extraction method and process are the same as in Example...

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Abstract

The invention discloses a quick extraction method for arsenic and selenium in different forms in flying ash. The method comprises the following steps: pretreatment of a flying ash sample; extraction of arsenic and selenium in a non-specific adsorbed state (form 1); extraction of arsenic and selenium in a specific adsorbed state (form 2); extraction of arsenic and selenium in an amorphous and weakly crystallized iron aluminum hydrate oxide combined state (form 3); extraction of arsenic and selenium in a fully crystallized iron aluminum oxide combined state (form 4); and extraction of arsenic and selenium in a residual form (form 5), wherein different forms of arsenic selenium require different ultrasonic extraction time, and the ultrasonic extraction time for arsenic the form 1, the form 2and the form 3 are respectively 11 to 13 min, 23 to 25 min and 2 to 3 min; and the ultrasonic extraction time for selenium in the form 1, the form 2 and the form 3 are respectively 9 to 11 min, 19 to21 min and 27 to 29 min. Compared with a conventional oscillating extraction scheme, the method disclosed by the invention greatly shortens the extraction time, is stable in result and shows high repetitiveness and reproducibility.

Description

Technical field [0001] The invention relates to a rapid extraction method of different forms of arsenic and selenium in fly ash, and belongs to the technical field of analytical chemistry. Background technique [0002] In the global coal consumption, nearly 50% of coal consumption is used in the power industry, and large amounts of coal combustion have caused extremely serious trace element (TEs) emissions. Current studies have proved that fly ash has a significant enrichment effect on arsenic and selenium. It is inaccurate to evaluate the environmental effects solely by the concentration of arsenic and selenium in fly ash. There is a close relationship between arsenic and selenium in different occurrence states and bioavailability, toxicity, and mobility. At present, most of the speciation analysis research is based on the Tessier method, and the BCR method certified by the EU has been subsequently developed, but its extraction efficiency for arsenic and selenium is not satisfa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/34
CPCG01N1/34
Inventor 苑春刚何楷强史孟丹
Owner NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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