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Determination method for trace impurity elements such as sodium, magnesium, calcium, iron and lead in high-purity boric acid

A technology of high-purity boric acid and determination method, which is applied in the preparation of test samples, measurement of color/spectral properties, thermal excitation analysis, etc. The effect of eliminating matrix differences and high sensitivity

Inactive Publication Date: 2013-02-13
INST OF MULTIPURPOSE UTILIZATION OF MINERAL RESOURCES CHINESE ACAD OF GEOLOGICAL SCI
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Problems solved by technology

[0005] And there are corresponding recommended test methods, but the pretreatment steps of each method are different, it is impossible to realize the simultaneous determination of multiple elements, the processing steps are cumbersome, and a large amount of organic reagent methanol is required in the process

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  • Determination method for trace impurity elements such as sodium, magnesium, calcium, iron and lead in high-purity boric acid

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Embodiment Construction

[0040] Such as figure 1 Shown, the assay method of trace impurity element sodium, magnesium, calcium, iron, lead in the high-purity boric acid provided by the invention, its steps are as follows:

[0041] Accurately weigh 5.000 g of the high-purity boric acid sample to be tested, pour it into a polytetrafluoroethylene (PTFE) crucible, add 10 mL of hydrofluoric acid (HF) and 5 mL of hydrochloric acid (HCl), and steam on a temperature-controlled electric heating plate at 200 °C. Dry;

[0042] Add 5 mL HF and evaporate to dryness again to remove the boric acid matrix as much as possible;

[0043] Add 5 mL of 1:1 (v / v) newly prepared aqua regia and 10 mL of ultrapure water into a polytetrafluoroethylene (PTFE) crucible, heat to boiling on an electric heating plate, take it off after 5 min, and let it cool naturally Dilute to a 25 mL stoppered colorimetric tube with ultrapure water, shake well to be tested;

[0044] The working conditions of the selected instruments are as foll...

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Abstract

The invention discloses a determination method for trace impurity elements such as sodium, magnesium, calcium, iron and lead in high-purity boric acid. The determination method comprises the following specific steps of: heating hydrofluoric acid and hydrochloric acid to remove boron; extracting soluble salts by using aqua regia; setting constant volume by using ultrapure water; determining by an atomic absorption spectrometer and an inductively coupled plasma emission spectrometer; and performing quantitative enriching and assay determination on the trace impurity elements in a high-purity boric acid sample. According to the determination method, the boron is removed by the hydrofluoric acid; the using amount of reagents is small; the sample blank rate is low; sample computer analysis is facilitated by removing boric acid matrixes; and a single element and multiple elements can be simultaneously determined by means of atomic spectrums comprising the atomic absorption spectrometer and the inductively coupled plasma emission spectrometer. The determination method is suitable for the assay determination of the trace impurity elements in the high-purity boric acid sample and has the advantages of low detection limit, high sensitivity, wide linear range and the like. The average processing time of a single high-purity boric acid sample is not more than 2 hours.

Description

technical field [0001] The invention relates to the analysis and determination technology of trace impurity elements sodium, magnesium, calcium, iron and lead in high-purity boric acid. The boric acid matrix is ​​removed by dissolving, heating and evaporating in hydrofluoric acid, soluble salts are extracted with aqua regia, and ultrapure water is used to extract soluble salts. After constant volume, the content of the element to be measured was determined by atomic spectroscopy. Background technique [0002] Boric acid is widely used in glass, enamel, ceramics, metallurgy, chemical industry and other industries. Adding boric acid in the manufacturing process of glass (optical glass, acid-resistant glass, heat-resistant glass, and glass fiber for insulating materials) can improve the heat resistance and transparency of glass products, increase mechanical strength, and shorten melting time. In the enamel and ceramic industries, boric acid is used to improve the gloss and fas...

Claims

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Application Information

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IPC IPC(8): G01N21/31G01N21/73G01N1/28G01N1/44
Inventor 李可及易建春刘卫雷勇
Owner INST OF MULTIPURPOSE UTILIZATION OF MINERAL RESOURCES CHINESE ACAD OF GEOLOGICAL SCI
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