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Method for microwave digestion of glass body

A microwave digestion and vitreous body technology, applied in the field of analysis and measurement, can solve the problems of incompletely digested vitreous body, etc., achieve the effect of reducing the requirements of digestion equipment, eliminating corrosion, and strong practicability

Inactive Publication Date: 2017-02-01
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional digestion methods do not completely digest the glass body formed by plasma melting fly ash

Method used

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  • Method for microwave digestion of glass body
  • Method for microwave digestion of glass body

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The method of microwave digestion of vitreous includes the following steps:

[0022] (1) Put the glass sample (fly ash slag) in the digestion tank, add 4 drops of ultrapure water to the glass sample, so that the glass sample is immersed in ultrapure water, add nitric acid to obtain a mixed solution, after the mixed solution is stable , Add perchloric acid, hydrofluoric acid and ultrapure water in turn, seal the digestion tank, put the digestion tank into the microwave digestion apparatus, microwave heating for 9 minutes;

[0023] (2) Take out the digestion tank; cool to room temperature, open the digestion tank lid, add ultrapure water to the 21ml mark, seal the digestion tank, place it in the microwave digestion apparatus again, and microwave for 8 minutes;

[0024] (3) Repeat step (2) 3 times;

[0025] (4) Take out the digestion tank; cool to room temperature, open the cover of the digestion tank, and transfer the digestion solution to a volumetric flask to make a constant vo...

Embodiment 2

[0028] The method of microwave digestion of vitreous includes the following steps:

[0029] (1) Put the glass sample (fly ash slag) in the digestion tank, add 3 drops of ultrapure water to the glass sample, so that the glass sample is immersed in ultrapure water, add nitric acid to obtain a mixed solution, after the mixed solution is stable , Add perchloric acid, hydrofluoric acid and ultrapure water in turn, seal the digestion tank, put the digestion tank into the microwave digestion apparatus, microwave heating for 8 minutes;

[0030] (2) Take out the digestion tank; cool to room temperature, open the digestion tank lid, add ultrapure water to the 20ml mark, seal the digestion tank, place it in the microwave digestion apparatus again, and microwave for 8 minutes;

[0031] (3) Repeat step (2) 3 times;

[0032] (4) Take out the digestion tank; cool to room temperature, open the cover of the digestion tank, and transfer the digestion solution to a volumetric flask to make a constant vo...

Embodiment 3

[0035] The method of microwave digestion of vitreous includes the following steps:

[0036] (1) Put the vitreous sample (household waste incineration residue) in the digestion tank, add 5 drops of ultrapure water to the vitreous sample, so that the vitreous sample is immersed in ultrapure water, add nitric acid to obtain a mixed solution, after the mixed solution is stable , Add perchloric acid, hydrofluoric acid and ultrapure water in turn, seal the digestion tank, put the digestion tank into the microwave digestion apparatus, microwave heating for 10 minutes;

[0037] (2) Take out the digestion tank; cool to room temperature, open the digestion tank lid, add ultrapure water to the 22ml mark, seal the digestion tank, place it in the microwave digestion apparatus again, and heat for 7 minutes in the microwave;

[0038] (3) Repeat step (2) twice;

[0039] (4) Take out the digestion tank; cool to room temperature, open the cover of the digestion tank, and transfer the digestion solution...

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Abstract

The invention discloses a method for microwave digestion of a glass body. The method comprises the following steps that 1, a glass body sample is put in a digestion tank, ultrapure water is added to make the glass body sample immersed in the ultrapure water, nitric acid, perchloric acid, hydrofluoric acid and ultrapure water are added in sequence, and the digestion tank is tightly closed and is put in a microwave digestion instrument for heating; 2, the digestion tank is taken out and cooled to room temperature, a digestion tank cover is opened, the ultrapure water is added, and the digestion tank is tightly closed and is put in the microwave digestion instrument for heating again; 3, the step 2 is repeated; 4, the digestion tank is taken out and cooled to room temperature, and the heavy metal content of a digestion solution is detected. The method determines metals of the glass body, achieves accurately determination of trace elements, reduces the requirement of a digestion device, adopts microwaves to digest the sample and performs direct determination through instruments without independent acid catching. The method has the advantages of including simple steps, making sample digestion complete and being good in practicability and low in reagent consumption, and meanwhile the sensitivity and accuracy of element analysis are improved.

Description

Technical field [0001] The invention relates to the technical field of analysis and determination, in particular to a microwave digestion method of a vitreous sample. Background technique [0002] There are many methods for sample digestion, such as melting method, ashing method, wet digestion, etc. At present, wet digestion is the most common method in the laboratory, that is, acid digestion. The acid digestion method can be operated with electric heating plates, microwave digestion apparatus, high pressure digestion apparatus, etc. [0003] Wet digestion is currently the most direct, effective and economical sample pretreatment method for elemental analysis, and is usually used for the detection of trace metal elements in samples. Nitric acid is a widely used pre-oxidant, which can destroy the organic matter in the sample. Hot perchloric acid is the strongest oxidant and dehydrating agent. Because of its high boiling point, it can continue to oxidize the sample after removing th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/44
CPCG01N1/44
Inventor 陈冠益方云豪马文超盛宏至徐永香
Owner TIANJIN UNIV
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