Determination method for volatile element arsenic in coal combustion product

A product and element technology, applied in the field of analytical chemistry, can solve the problems of low detection value, large detection limit of the instrument, complicated equipment debugging, etc., and achieve the effect of reducing volatilization loss and low detection limit

Inactive Publication Date: 2013-08-28
TIANJIN UNIV
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Problems solved by technology

Among them, the burning and reduction process of the target substance will lead to the volatilization loss of elements; at the same time, the quantitative analysis instrument cold atomic absorption spectrometry and cold atomic absorption spectrophotometry are used, the detection limit of the instrument is large, and the detection of trace elements may not reach To achieve sufficient accuracy, equipment debugging is more cumbersome, requiring the experimenter to have rich analysis experience and skills
For volatile elements, during the sample preparation process, the elements are easy to volatilize, the detection value is low, and the measurement effect cannot meet the standard

Method used

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  • Determination method for volatile element arsenic in coal combustion product

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Embodiment Construction

[0014] The technical solutions of the present invention will be further described below in conjunction with specific embodiments.

[0015] Use the coal fly ash component analysis standard material (GBW08401), and use third-grade analytical pure nitric acid (BV-III grade, 65% by mass) for microwave digestion for pretreatment, that is, the coal fly ash component analysis standard material and the third-grade nitric acid Grade analytically pure nitric acid is mixed in a digestion tank, and then put into a microwave digestion instrument for microwave digestion (CEM digestion instrument in the United States, which can realize automatic pressure control), and the microwave power is 1600W.

[0016] Each sampling volume is 0.1g, respectively select 9mLHNO 3 , 9mLHNO 3 +2mLHF, 9mLHNO 3 +2mLH 2 o 2 Microwave digestion was carried out separately, and 160°C, 190°C, and 210°C were selected as the experimental temperature, and the temperature was raised from room temperature (25°C). The...

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Abstract

The invention discloses a determination method for the volatile element arsenic in a coal combustion product. The method comprises the following steps: mixing a sample with a digestion solution and carrying out microwave digestion; adding deionized water to allow a constant volume of 100 mL to be obtained; and carrying out quantitative determination by using an inductively coupled plasma mass spectrometer. The determination method provided by the invention is a novel method which can overcome the disadvantages that arsenic easily suffers from volatilization loss in the process of pretreatment, time for sample treatment is long, a detection limit of a quantitative analysis instrument is not accurate enough and the like and has the advantages of high selectivity, easy and convenient operation, speed and high precision of determination results.

Description

technical field [0001] The invention relates to the field of analytical chemistry, and more specifically, belongs to a method for quantitative analysis of volatile trace elements. Background technique [0002] As is a toxic and carcinogenic element in various chemical forms. Arsenic poisoning can affect the human gastrointestinal system, circulatory system, liver, kidney, nerves and other organs and skin. Therefore, the rapid quantitative detection of As is of great significance. The national standard (As: GB / T3058-2008) has cumbersome pretreatment steps for the quantitative detection of As. It is necessary to mix and burn the target substance and the reagent, and the target element needs to go through a series of redox reactions to convert it into the substance to be tested. . Among them, the burning and reduction process of the target substance will lead to the volatilization loss of elements; at the same time, the quantitative analysis instrument cold atomic absorption s...

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Application Information

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IPC IPC(8): G01N27/64G01N1/44
Inventor 陈冠益王钦颜蓓蓓张莹马文超
Owner TIANJIN UNIV
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