CN-121978086-A - Method for measuring silicon dioxide in quartz glass based on high-temperature fusion reaction-inductively coupled plasma atomic emission spectrometer

Abstract

The invention relates to a method for measuring silicon dioxide in quartz glass based on a high-temperature melting reaction-inductively coupled plasma atomic emission spectrometer. The method comprises the steps of crushing and grinding a sample to be powder, adding a strong alkali flux into the obtained powder sample, uniformly mixing to obtain a mixture, melting the mixture at high temperature, leaching reactants with hot water and fixing the volume, drawing a standard curve of silicon element concentration-spectral line emission intensity, testing the silicon content in a sample solution, and calculating the silicon dioxide content according to the content of the determined silicon. According to the invention, after a strong alkali flux is added into a powdery sample obtained by grinding the sample for high-temperature melting reaction, heating water is used for dissolving reactants, and an inductively coupled plasma atomic emission spectrometer is used for measuring the silicon content in the solution, so that the silicon dioxide content in a quartz glass sample is calculated.

Inventors

• YANG XIAOHUI
• YANG XUEDONG
• WANG LEI
• LIU HUANMIN
• DU DAYAN
• CAI SUYAN
• LI XINYI

Assignees

• 中国国检测试控股集团股份有限公司

Dates

Publication Date

20260505

Application Date

20260213

Claims (10)

1. 1. A method for determining silica in quartz glass based on a high temperature fusion reaction-inductively coupled plasma atomic emission spectrometer, comprising the steps of: Step one, crushing and grinding a sample into powder; adding a strong alkali flux into the powdery sample obtained in the first step, and uniformly mixing to obtain a mixture; step three, leaching reactants by hot water and fixing the volume; Drawing a standard curve of silicon element concentration-spectral line emission intensity; Step five, testing the silicon content in the sample solution; And step six, calculating the content of silicon dioxide according to the content of the measured silicon.
2. 2. The method for measuring silica in silica glass based on high temperature fusion reaction-inductively coupled plasma atomic emission spectrometer according to claim 1, wherein in step one, the sample is at least one selected from the group consisting of silica glass and products, silica glass fibers and products, natural silica glass raw materials, and synthetic silica sand.
3. 3. The method for measuring silica in silica glass based on high-temperature fusion reaction-inductively coupled plasma atomic emission spectrometer according to claim 2, wherein in the first step, the natural silica glass raw material is at least one selected from the group consisting of silica ore, silica sand, quartz ore and quartz powder.
4. 4. The method for measuring silica in quartz glass based on high temperature melting reaction-inductively coupled plasma atomic emission spectrometry according to claim 1, wherein in the second step, the strong alkali flux includes at least one of alkali carbonate and alkali hydroxide.
5. 5. The method for measuring silica in quartz glass based on high temperature melting reaction-inductively coupled plasma atomic emission spectrometry of claim 4 wherein in step two, said strong base flux comprises at least one of anhydrous sodium carbonate, anhydrous potassium carbonate, sodium hydroxide, potassium hydroxide.
6. 6. The method for measuring silicon dioxide in quartz glass based on high-temperature melting reaction-inductively coupled plasma atomic emission spectrometry according to claim 1, wherein in the second step, the mass ratio of the sample to the strong alkali flux is 1:2-1:20, and the high-temperature melting temperature is 500-1150 ℃.
7. 7. The method for measuring silica in quartz glass based on high temperature melting reaction-inductively coupled plasma atomic emission spectrometry according to claim 1, wherein in the third step, the hot water is silicon-free ultrapure water.
8. 8. The method for measuring silica in quartz glass based on high temperature melting reaction-inductively coupled plasma atomic emission spectrometry according to claim 1, wherein in the fourth step, the drawing of the standard curve of silicon element concentration-spectral line emission intensity specifically comprises preparing a series of standard solutions of silicon element using standard solutions of silicon element having national standard sample certificates, measuring the standard solutions of silicon element, and drawing the standard curve of silicon element concentration-spectral line emission intensity.
9. 9. The method for measuring silica in quartz glass based on high temperature melting reaction-inductively coupled plasma atomic emission spectrometry according to claim 1, wherein in the fifth step, the mass fraction ω si of the silicon element content in the sample solution is calculated according to formula (1): .................................(1) wherein: omega si -mass percent of silicon element in the sample; C si -concentration of elemental silicon in the sample solution in micrograms per milliliter (μg/mL); c 0 -concentration of silicon element in blank solution in micrograms per milliliter (μg/mL); v-volume of sample solution in milliliters (mL); f-the multiple by which the sample solution is diluted; m-mass of sample in grams (g).
10. 10. The method for measuring silica in quartz glass based on high temperature melting reaction-inductively coupled plasma atomic emission spectrometry according to claim 1, wherein in the sixth step, the mass fraction ω siO2 of the silica content is calculated according to formula (3): .....................(2) .....................(3) wherein: Omega siO2 -mass percent of silica in the sample,%; omega si -mass percent of silicon element in the sample; 28.0855-the relative atomic mass of silicon; 15.9994-relative atomic mass of oxygen; m-mass of sample in grams (g).

Description

Method for measuring silicon dioxide in quartz glass based on high-temperature fusion reaction-inductively coupled plasma atomic emission spectrometer Technical Field The invention belongs to the technical field of high-purity quartz glass detection, and particularly relates to a method for measuring silicon dioxide in quartz glass based on a high-temperature melting reaction-inductively coupled plasma atomic emission spectrometer. Background Quartz glass is a special industrial technical glass containing only a single component of silicon dioxide, and the main component is high-purity silicon dioxide (SiO 2), wherein the purity is generally more than 99.9%, and the quartz glass contains no or very small (ppm or even ppb) of other element impurities and gas-liquid inclusion. The quartz glass has a series of excellent performances such as high temperature resistance, chemical erosion resistance (hydrofluoric acid and hot phosphoric acid removal), irradiation resistance, heat shock resistance, low expansion coefficient, good electrical insulation performance, high full spectrum optical transmission and the like by virtue of a unique compact arrangement of a silicon oxygen tetrahedral covalent bond structure, is widely applied to high-end technical fields such as semiconductors, optical fibers, communication, optical instruments, national defense safety, aerospace, electronic information, new energy sources and the like, plays an important role all the time in modern industry and technological development, and is an indispensable key basic material in the technical field of modern science. The purity of silica in quartz glass is a key technical indicator determining its performance and application area. The silicon dioxide content is generally in the range of 99.9% -99.99%, along with the technical development of high-end application fields such as semiconductors, optical fiber communication, 5G communication, artificial intelligence, quantum computation and the like, the requirements of the fields on the purity of quartz glass are gradually improved from the traditional 99.99% to more than 99.99%, 99.999% or higher, the requirements on the purity of silicon dioxide are extremely high, the content of impurity elements is extremely low (ppb level), gas-liquid inclusion and inclusion are extremely few, and the severe quality requirement promotes the high-purity quartz glass detection technology to become a key link for guaranteeing the quality and safety of industrial chains. Currently, the method for measuring the content of silicon dioxide in quartz glass comprises the following basic principles of grinding a quartz glass sample, burning the quartz glass sample to constant at high temperature (960 ℃ plus or minus 5 ℃) until the constant, reducing the mass fraction to loss due to ignition, then digesting all silicon dioxide into silicon tetrafluoride to remove the silicon tetrafluoride, burning the silicon dioxide to constant, and calculating and measuring the content of silicon dioxide by adopting a weight loss and residue (impurity element) after acid treatment by adopting a weight loss subtracting method in the ferrous metallurgy industry YB/T4225-2010 of the method. As a traditional chemical analysis method, the high-temperature burning hydrofluoric acid digestion differential method needs to accurately control the weighing amount of a sample (accurate to 0.0001g or more), strictly control the burning temperature, the operation time and the laboratory environment conditions, has higher requirements on experimental technology, complicated experimental steps, long time consumption and high energy consumption caused by repeated high-temperature burning, and has great limitation and difficulty in measuring the ultra-pure quartz glass sample with the silicon dioxide content of more than 99.99 percent by a gravimetric method based on the factors. The method for measuring and representing the content of silicon dioxide in high-purity quartz is newly formulated (project plan number: 20250579-T-609), which defines the difference of the content of silicon dioxide by subtracting the total content of 15 trace elements from 100%, namely the content of silicon dioxide, namely the purity of silicon dioxide. The main reasons why the calculation method cannot objectively reflect the content of the actual silicon dioxide in the quartz glass are that 1, except 15 impurity elements listed in the standard solicitation opinion manuscript, the quartz glass possibly contains other metal impurity elements such as barium, zirconium, germanium, cobalt, rubidium, cesium and the like and non-metal elements such as fluorine, chlorine, carbon, hydrogen and the like, the impurity elements influence the chemical purity of the quartz glass, and the method only subtracts the total content of 15 impurity elements and lacks the rigor theoretically. 2. The existence of the inclusion can affect the chemical purity of the quartz glass because the