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A method for microwave digestion pretreatment of silica
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A microwave digestion and pretreatment technology, used in the preparation of test samples, can solve the problems of long time, poor stability, fast time, etc., and achieve the effects of short processing time, high stability and simple steps
Active Publication Date: 2015-09-02
HUBEI XINGFA CHEM GRP CO LTD
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Problems solved by technology
[0003] At present, the country mainly adopts the high-temperature alkali fusion method in GB / T6901-2008 "Chemical Analysis Methods of Silicon Refractory Materials", and some enterprises adopt the acid dissolution method. The former treatment method takes a long time and lasts for 1-2 days, and it is harmful to the environment. Larger; the latter time is fast, but the stability is poor
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Embodiment 1
[0017] A method for microwave digestion pretreatment silica, comprising the following steps:
[0018] 1) Accurately weigh 0.1g of silica sample and place it in a digestion tank, add 0.5g of concentrated nitric acid and 12g of hydrofluoric acid, mix well, seal the digestion tank, put it into a microwave digestion instrument, and use pressure control mode for digestion. 10min;
[0019] 2) After the digestion is completed and the solution is cooled, the solution is clarified. Put the digestion tank on the electric heating plate and heat it until the white smoke is exhausted. Sample pretreatment.
Embodiment 2
[0021] A method for microwave digestion pretreatment silica, comprising the following steps:
[0022] 1) Accurately weigh 0.2g of silica sample and place it in a digestion tank, add 3.5g of concentrated nitric acid and 14g of hydrofluoric acid, mix well, seal the digestion tank, put it into a microwave digestion instrument, and use pressure control mode for digestion. 10min;
[0023] 2) After the digestion is completed and the solution is cooled, the solution is clarified. Put the digestion tank on the electric heating plate and heat it until the white smoke is exhausted. Sample pretreatment.
Embodiment 3
[0025] A method for microwave digestion pretreatment silica, comprising the following steps:
[0026] 1) Accurately weigh 0.3g of silica sample and place it in a digestion tank, add 3g of concentrated nitric acid and 15g of hydrofluoric acid, mix well, seal the digestion tank, put it into a microwave digestion instrument, and use pressure control mode for digestion, keep at 1MPa for 10min ;
[0027] 2) After the digestion is completed and the solution is cooled, the solution is clarified. Put the digestion tank on the electric heating plate and heat it until the white smoke is exhausted. Sample pretreatment.
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Abstract
The invention provides a pretreatment method for silica through microwave digestion. The method comprises the following steps: 1) adding a silica sample into a digestion tank, adding concentrated nitric acid and hydrofluoric acid, uniformly mixing the above mentioned substances in the digestion tank, enclosing the digestion tank, putting the digestion tank into a microwave digestion instrument, carrying out digestion in a pressure control mode and maintaining the digestion tank at a temperature of 1 MPa for 10 min; and 2) placing the digestion tank on an electric hot plate when digestion is completed and a solution is cooled, heating the digestion tank until white smoke is completely evaporated, carrying out cooling and fixing a volume to a constant value so as to obtain a solution in which the sample is thoroughly dissolved, thereby finishing pretreatment of the silica sample. According to the invention, microwave digestion is utilized for pretreatment of silica, so processing time in a national standard method is substantially shortened, and production benefits are effectively increased.
Description
technical field [0001] The invention relates to the pretreatment of silica samples, in particular to a method for microwave digestion pretreatment of silica. Background technique [0002] Silica is a new type of energy. It is mainly used to produce silicon compounds and silicates in the chemical industry. Therefore, the pretreatment and detection of silica has become an important step to ensure the quality of silica. [0003] At present, the country mainly adopts the high-temperature alkali fusion method in GB / T6901-2008 "Chemical Analysis Methods of Silicon Refractory Materials", and some enterprises adopt the acid dissolution method. The former treatment method takes a long time and lasts for 1-2 days, and it is harmful to the environment. Larger; the latter time is fast, but the stability is poor. Contents of the invention [0004] The technical problem to be solved by the present invention is to provide a method for microwave digestion pretreatment of silica, which ha...
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