Method for performing microwave-assisted extraction on different forms of arsenic selenium from coal ash sequentially

A microwave-assisted, fly ash technology, applied in the field of analytical chemistry, can solve problems such as long cycle, and achieve the effects of short time, good repeatability and reproducibility, and high extraction recovery rate

Active Publication Date: 2019-01-08
NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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  • Abstract
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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

Method used

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  • Method for performing microwave-assisted extraction on different forms of arsenic selenium from coal ash sequentially

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The fly ash samples from a power plant in Hebei were collected. After the fly ash samples were ground and freeze-dried at low temperature for 24 hours, they were passed through a 200-mesh sieve with the help of an automatic horizontal reciprocating oscillating sieving machine. The obtained samples were balanced under the conditions specified in GB / T 32722 , Calibrate the pressure and temperature of the microwave digestion instrument before the experiment.

[0037] Extraction of non-specifically adsorbed arsenic: Weigh 0.5g of the fly ash sample after equilibrium treatment into a microwave digestion tank, add 12.5mL, 0.05M ammonium sulfate solution, oscillate to mix the fly ash sample and the extract fully, and tighten Digest the inner tank of the tank, and tighten the outer tank at 45° under the condition of the initial resistance, and set the program of the microwave digestion instrument in three steps. When the power of the microwave digestion instrument is 3000W and t...

Embodiment 2

[0044] A fly ash sample from a power plant in Shanxi was collected, and the sample treatment was the same as in Example 1.

[0045] Extraction of non-specifically adsorbed arsenic and selenium: the extraction method and process are the same as in Example 1, and the average concentrations of arsenic and selenium in the non-specific adsorbed state (form 1) obtained by detection and analysis are 3.76±0.43 mg / kg and 2.57±0.33 mg / kg respectively , the average concentrations of non-specifically adsorbed arsenic and selenium extracted by traditional Wenzel method were 3.91±0.62 mg / kg and 2.86±0.42 mg / kg, respectively. The average recoveries of the microwave-assisted extraction of non-specifically adsorbed arsenic and selenium by the method of the present invention are respectively 96.2% and 89.9% of those of traditional vibration extraction.

[0046] Extraction of specifically adsorbed arsenic and selenium: the extraction method and process are the same as in Example 1, and the avera...

Embodiment 3

[0052] The national standard substance GBW08401 was collected as a fly ash sample, and the sample treatment was the same as in Example 1.

[0053] Extraction of non-specifically adsorbed arsenic and selenium: the extraction method and process are the same as in Example 1, and the average concentrations of arsenic and selenium in the non-specific adsorbed state (form 1) obtained by detection and analysis are 4.04±0.64 mg / kg and 0.31±0.06 mg / kg respectively , the measured average concentrations of non-specifically adsorbed arsenic and selenium extracted by traditional Wenzel shaking were 4.55±0.52 mg / kg and 0.27±0.04 mg / kg, respectively. The average recoveries of the microwave-assisted extraction of the non-specifically adsorbed arsenic and selenium by the method of the present invention are respectively 88.8% and 114.8% of those of the traditional vibration extraction.

[0054] Extraction of specifically adsorbed arsenic and selenium: the extraction method and process are the s...

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Abstract

The invention relates to a method for performing microwave-assisted extraction on different forms of arsenic selenium from coal ash sequentially. According to the method, arsenic selenium with different adsorption states is extracted by using a microwave digestion instrument and adding different extracting agents under different microwave conditions. The method comprises the following steps: performing earlier-stage treatment on a coal ash sample; extracting arsenic selenium with a nonspecific adsorption state (form 1); extracting arsenic selenium with a specific adsorption state (form 2); andextracting arsenic selenium with an amorphous form and weak crystalline iron aluminum hydrated oxide combined state (form 3), wherein different forms of arsenic selenium need different microwave extraction power, temperature and time. Compared with the traditional vibrating extraction scheme, the method has the following advantages: the extraction time is greatly shortened, the result is stable,and high repeatability and reproducibility are presented.

Description

technical field [0001] The invention relates to a microwave-assisted sequential extraction method for different forms of arsenic and selenium in fly ash, which belongs to the technical field of analytical chemistry. Background technique [0002] In the global coal consumption, nearly 50% of the coal consumption is used in the power industry, and a large amount of coal combustion has caused extremely serious trace element (TEs) emission problems. Current studies have shown that fly ash has a significant enrichment effect on arsenic and selenium. It is inaccurate to evaluate the environmental effect 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 speciation analysis studies are based on the Tessier method, and the EU-certified BCR method was subsequently developed, but its extraction efficiency for arsenic and s...

Claims

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Application Information

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IPC IPC(8): G01N1/44G01N21/64
CPCG01N1/44G01N21/6404
Inventor 苑春刚何楷强史孟丹
Owner NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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