CN-121994580-A - Method for detecting content of zirconium element in high-purity quartz sand

Abstract

The invention discloses a method for detecting the content of zirconium element in high-purity quartz sand, which comprises the steps of heating and digesting the high-purity quartz sand by using an acid digestion solution in a closed environment, evaporating a solvent after digestion is finished to obtain a residue, transferring the residue into a heat-resistant container by using nitric acid, evaporating the solvent to dryness, adding strong base, heating to perform alkali dissolution reaction, wherein the alkali dissolution reaction comprises the steps of heating to 200-300 ℃ for a period of time, heating to 550-950 ℃ for a period of time, cooling after the alkali dissolution reaction is finished, dissolving alkali dissolution reaction products by using nitric acid, and fixing the volume by using pure water to obtain a sample solution, preparing a standard impurity solution and a blank sample solution, and performing test analysis on the sample solution, the standard impurity solution and the blank sample solution by using ICP-OES or ICP-MS to obtain the content of zirconium element in the high-purity quartz sand.

Inventors

• YU XUEGONG
• ZHOU HUILI
• HU ZECHEN
• YANG DEREN

Assignees

• 浙江大学杭州国际科创中心

Dates

Publication Date

20260508

Application Date

20260204

Claims (10)

1. 1. The method for detecting the content of the zirconium element in the high-purity quartz sand is characterized by comprising the following steps of: Heating and digesting high-purity quartz sand by using an acid digestion solution in a closed environment, and evaporating a solvent after digestion is completed to obtain a residue; transferring the residue into a heat-resistant container by using nitric acid, evaporating the solvent, adding strong alkali, and heating to perform alkali dissolution reaction, wherein the alkali dissolution reaction comprises heating to 200-300 ℃ for a period of time, and heating to 550-950 ℃ for a period of time; cooling after the alkali dissolution reaction is finished, dissolving an alkali dissolution reaction product by nitric acid, and fixing the volume by pure water to obtain a sample solution; Preparing a standard impurity solution and a blank sample solution; and (3) carrying out test analysis on the sample solution, the standard impurity solution and the blank sample solution through ICP-OES or ICP-MS to obtain the content of zirconium element in the high-purity quartz sand.
2. 2. The method for detecting the content of zirconium element in the high-purity quartz sand according to claim 1, wherein the mass content of silicon dioxide in the high-purity quartz sand is more than 99.998%.
3. 3. The method for detecting the content of zirconium element in the high-purity quartz sand according to claim 1, wherein the acid digestion solution comprises nitric acid and hydrofluoric acid; the volume ratio of nitric acid to hydrofluoric acid in the acid digestion solution is 1:1-3; the mass fraction of HNO 3 in the nitric acid is 65% -70%; The mass fraction of HF in the hydrofluoric acid is 40% -50%.
4. 4. The method for detecting the content of zirconium element in the high-purity quartz sand according to claim 1, wherein the dosage of the high-purity quartz sand is 0.3-1 g; the acid digestion solution comprises hydrofluoric acid; The ratio of the volume of hydrofluoric acid in the acid digestion solution to the mass of the high-purity quartz sand is 8-20 mL/1 g.
5. 5. The method for detecting the content of zirconium element in the high-purity quartz sand according to claim 1, wherein the temperature of the heating digestion is 120-200 ℃; And the heating digestion time is 2-5 hours.
6. 6. The method for detecting the content of zirconium element in the high-purity quartz sand according to claim 1, wherein the residue is transferred into a heat-resistant container by using nitric acid with a mass concentration of HNO 3 of 1% -10%.
7. 7. The method for detecting the content of zirconium element in the high-purity quartz sand according to claim 1, wherein the mass ratio of the added mass of the strong base to the high-purity quartz sand is (5-8): 1.
8. 8. The method for detecting the content of zirconium element in the high-purity quartz sand according to claim 1, wherein strong base is added in a dry environment; The strong alkali comprises one or more than two of sodium hydroxide, potassium hydroxide and sodium peroxide.
9. 9. The method for detecting the content of zirconium element in high-purity quartz sand according to claim 1, wherein in the alkali dissolution reaction: the temperature rising rate is not more than 1 ℃ per second; Preserving heat for 10-60 min at 200-300 ℃; and preserving heat for 10-120 min at 550-950 ℃.
10. 10. The method for detecting the content of zirconium element in the high-purity quartz sand according to claim 1, wherein nitric acid with the mass concentration of HNO 3 of 1% -10% is used for dissolving alkali-soluble reaction products.

Description

Method for detecting content of zirconium element in high-purity quartz sand Technical Field The invention relates to the technical field of high-purity quartz sand detection, in particular to a method for detecting the content of zirconium element in high-purity quartz sand. Background The high-purity quartz sand is a silicon dioxide material processed by natural crystal and quartz minerals or chemically synthesized, is a key base material, and is widely applied to high and new technical industries such as semiconductors, optical fibers, photovoltaics, electric light sources, bioengineering and the like. The purity of high purity silica sand has an absolute impact on its use, and therefore, it is often desirable in the industry to accurately analyze the purity of silica sand. The vast majority of the zirconium element in quartz sand exists in the form of zircon (ZrSiO 4), and small amounts exist in the form of baddeleyite (ZrO 2) and others. Because of the extremely high melting point (zircon: 2750 ℃ C., baddeleyite 2950 ℃ C.) of the zirconium-containing minerals, when quartz sand is used as a raw material for producing quartz products such as quartz glass, quartz optical fibers, etc., the zirconium-containing minerals often exist in the form of stones, which can have a fatal influence on the quality of the quartz products. At present, the most commonly used method for measuring the content of impurity elements in high-purity quartz sand is inductively coupled plasma emission spectrometry (ICP-OES) or inductively coupled plasma mass spectrometry (ICP-MS), and the method has the advantages of capability of measuring various trace elements simultaneously, low detection limit, high analysis speed and the like. The method firstly needs to digest quartz sand for sample preparation and then test. The main component of quartz sand is silicon dioxide, and part of impurity elements exist in the surface of quartz sand particles and in a crack structure in a mineral form, and part of impurity elements replace silicon oxygen atoms to exist in crystal lattices, so that the silicon oxygen tetrahedron structure in quartz sand crystals needs to be broken to dissolve the impurity elements when the quartz sand to be tested is prepared into samples for ICP-OES and ICP-MS tests. The most commonly used method for digesting quartz sand at present is an acid dissolution method, which is to digest quartz sand to be tested by using hydrofluoric acid, nitric acid and other strong acids, convert all silicon dioxide into silicon tetrafluoride for removal, dissolve residues by using nitric acid and then test by using ICP-OES or ICP-MS. For example, patent specification with publication No. CN120404897A discloses a method for measuring impurity element content in high-purity quartz by ICPMS, which comprises the following steps of S1, drying a sample, S2, weighing the sample, S3, dissolving strong acid I first level, S4, dissolving strong acid II second level, S5, cooling and fixing volume, and S6, respectively testing and analyzing standard series working solution, sample solution and blank solution on ICPMS. However, the acid dissolution method for digesting quartz sand often has the problems of incomplete digestion and inaccurate trace element measurement, in particular to measurement of zirconium (Zr) element in the quartz sand. In zircon-containing minerals, zircon is very chemically stable and only a few acids such as hydrofluoric acid can react with zircon, however, zircon is difficult to digest completely because of the very slow rate of direct reaction of zircon with hydrofluoric acid and the like (zircon forms a zirconium-rich layer on the surface of zircon when dissolved in acid, limiting the digestion rate of zircon, for example, 50 mg zircon is digested with 2 mL hydrofluoric acid at 120 ℃ in a sealed tank over 72 h ℃). Disclosure of Invention Aiming at the technical problems and the defects existing in the field, the invention provides a method for detecting the content of zirconium element in high-purity quartz sand, and the accuracy of measuring the content of zirconium (Zr) in the quartz sand is greatly improved by optimizing the digestion process. The specific technical scheme is as follows: A method for detecting the content of zirconium element in high-purity quartz sand comprises the following steps: Heating and digesting high-purity quartz sand by using an acid digestion solution in a closed environment, and evaporating a solvent after digestion is completed to obtain a residue; Transferring the residue into a heat-resistant container by using nitric acid, evaporating the solvent, adding strong alkali, and heating to perform alkali dissolution reaction, wherein the alkali dissolution reaction comprises heating to 200-300 ℃ for a period of time, and heating to 550-950 ℃ for a period of time (such as 650-900 ℃ and the like, preferably 650-900 ℃); cooling after the alkali dissolution reaction is finished, dissolving a