CN116609143A - Sample preparation method for analyzing hydroxyl content in quartz ore - Google Patents

Sample preparation method for analyzing hydroxyl content in quartz ore Download PDF

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Publication number
CN116609143A
CN116609143A CN202210120450.9A CN202210120450A CN116609143A CN 116609143 A CN116609143 A CN 116609143A CN 202210120450 A CN202210120450 A CN 202210120450A CN 116609143 A CN116609143 A CN 116609143A
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China
Prior art keywords
quartz
equal
polishing
plate
plates
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Pending
Application number
CN202210120450.9A
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Chinese (zh)
Inventor
李建德
徐艳艳
赵秀芳
张鹏
蒋丽微
丰丹丹
高丽荣
舒敏娣
张誉文
许帆
胡静
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East China Sea Research Institute National Silicon Materials Deep Processing Product Quality Supervision And Inspection Center
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East China Sea Research Institute National Silicon Materials Deep Processing Product Quality Supervision And Inspection Center
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Application filed by East China Sea Research Institute National Silicon Materials Deep Processing Product Quality Supervision And Inspection Center filed Critical East China Sea Research Institute National Silicon Materials Deep Processing Product Quality Supervision And Inspection Center
Priority to CN202210120450.9A priority Critical patent/CN116609143A/en
Publication of CN116609143A publication Critical patent/CN116609143A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32Polishing; Etching
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
    • G01N2021/3572Preparation of samples, e.g. salt matrices
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N2021/3595Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/50Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57Improving the yield, e-g- reduction of reject rates

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Engineering & Computer Science (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

The invention discloses a sample preparation method for analyzing the hydroxyl content in quartz ore, which comprises the steps of selecting quartz blocks with good crystallization and less impurities from quartz ore, and cutting quartz plates from the selected quartz blocks by a cutting machine; polishing two sides of the cut quartz plate on a polishing machine by sand paper, keeping the two sides of the quartz plate parallel in the polishing process, and putting the polished quartz plate into a vibration cylinder for vibration; and taking out and cleaning the vibrated quartz plate, polishing the glass plate on a brush rotating at a high speed, cleaning the polished quartz plate, drying in a drying oven, and detecting by using a Fourier transform infrared spectrometer.

Description

Sample preparation method for analyzing hydroxyl content in quartz ore
Technical Field
The invention belongs to the field of physical detection and analysis, and particularly relates to a sample preparation method for analyzing the hydroxyl content in quartz ores.
Background
Crystal ore is a natural high purity silica mineral and is also a traditional mineral raw material for quartz glass. As the crystal is a rare mineral seed, is always used as a strategic resource in China in the middle of 20 th century, through long-term development and use, the crystal resource in China is nearly exhausted, the usage amount of quartz glass is enlarged, and the research of new mineral raw material sources is promoted. For the last twenty years, efforts have been made to develop widely distributed gangue on the crust as raw materials for quartz glass to thoroughly solve the shortage of crystal resources. In seventies, the united states starts to use gangue quartz to replace quartz glass in middle, high and low grades in production, compared with developed countries, the processing technology of quartz glass raw materials in China is behind, the quality of raw materials can only meet the requirements of preparing resistant glass, the hydroxyl content in the quartz glass is unstable, and the technical difficulties of high-purity and low-hydroxyl quartz glass raw materials are not overcome. Along with the development of science and technology, the demand of the high-tech field for high-performance quartz glass is continuously increased, but the technical level of raw materials lacks a rapid and efficient method for detecting the hydroxyl content in the raw materials, and restricts the development of quartz glass in China.
Disclosure of Invention
The invention aims to provide a sample preparation method for analyzing the hydroxyl content in quartz ores, which can conveniently and quickly observe, analyze and analyze the hydroxyl content in quartz ores.
In order to solve the problems, the invention adopts the following technical scheme: a sample preparation method for analyzing the hydroxyl content in quartz ore comprises the following steps:
and selecting quartz blocks with good crystallization and few impurities from the quartz ore, wherein the diameter of the quartz blocks is more than or equal to 5cm.
Further, quartz plates with two parallel sides are cut from the selected quartz blocks by a cutting machine, the diameter of the quartz plates is more than or equal to 5cm, the thickness of the quartz plates is more than or equal to 10mm, and the number of the quartz plates is more than or equal to 2.
Further, the two sides of the cut quartz plate are polished on a polishing machine by 400-mesh sand paper, and the two sides of the quartz plate are kept parallel in the polishing process, and the polishing time is more than or equal to 30min.
Further, the polished quartz plate is put into a vibration cylinder for vibration, fused quartz glass fragments are put into the vibration cylinder, the quartz glass fragments account for about three fourths of the volume of the vibration cylinder, a proper amount of 600-mesh silicon carbide is put into the vibration cylinder, and the vibration time is more than or equal to 24 hours.
Further, the polished quartz plate is taken out and washed, a proper amount of cerium oxide is put on a round brush fixed on a motor, and then the glass plate is polished on a brush rotating at a high speed, and the steps are repeated for more than 10 times.
Further, the polished quartz plate is cleaned, and is placed in an oven for more than or equal to 4 hours, and the temperature of the oven is controlled to be more than or equal to 100 ℃.
Further, detecting the dried quartz plate in a Fourier transform infrared spectrometer, and recording the absorbance value of the wavelength at the position of 2.73 mu m, wherein the calculation formula of the hydroxyl content is as follows:
wherein:
a-absorbance;
b-transmittance;
k-is well-established and is related to the nature of the absorbing material and the wavelength λ of the incident light;
d-sample thickness in non-millimeters (mm);
c-the hydroxyl content of the sample in units of micrograms per gram (. Mu.g/g).
The invention has the following effects:
the quartz plates with two parallel sides are cut from the selected quartz blocks by a cutting machine, so that the thickness uniformity of the quartz plates can be ensured, the calculation of the hydroxyl content is not influenced, the diameter of the quartz plates is more than or equal to 5cm, the thickness of the quartz plates is more than or equal to 10mm, the polishing of the quartz plates can be facilitated, and a certain thickness of the quartz plates can be ensured after polishing.
Polishing two sides of the cut quartz plate on a polishing machine by using 400-mesh sand paper, so that sand holes on two sides of the quartz plate can be polished; the polished quartz plate is put into a vibration cylinder for vibration, a proper amount of 600-mesh silicon carbide is put into the vibration cylinder, the vibration time is more than or equal to 24 hours, the vibration cylinder principle can be fully utilized, sand holes on two sides of the quartz plate are ensured to be completely polished, and the two sides of the quartz plate are ensured to be smooth as much as possible.
Taking out and cleaning the polished quartz plate, placing a proper amount of cerium oxide on a round brush fixed on a motor, and polishing the glass plate on the brush rotating at a high speed, thereby ensuring that both sides of the quartz plate are in a mirror surface state, ensuring the transmittance of infrared light, and ensuring that the cerium oxide is nontoxic and odorless.

Claims (2)

1. A sample preparation method for analyzing the hydroxyl content of quartz ore, which is characterized by comprising the following steps:
selecting quartz blocks with good crystallization and few impurities from quartz ores, and cutting quartz plates from the selected quartz blocks by using a cutting machine; polishing two sides of the cut quartz plate on a polishing machine by sand paper, keeping the two sides of the quartz plate parallel in the polishing process, and putting the polished quartz plate into a vibration cylinder for vibration; and taking out and cleaning the vibrated quartz plate, polishing the glass plate on a brush rotating at a high speed, cleaning the polished quartz plate, and drying in an oven.
2. The method according to claim 1, wherein: the diameter of the quartz block is more than or equal to 5cm, the two sides of the cut quartz plates are parallel, the diameter of the quartz plates is more than or equal to 5cm, the thickness of the cut quartz plates is more than or equal to 10mm, the number of the quartz plates is more than or equal to 2, sand paper used on a polishing machine is 400 meshes, the polishing time is more than or equal to 30min, fused quartz glass fragments are placed in a vibration cylinder, the quartz glass fragments account for about three quarters of the volume of the vibration cylinder, a proper amount of 600 meshes of silicon carbide is placed in the vibration cylinder, the vibration time is more than or equal to 24h, a proper amount of cerium oxide is placed on a circular brush fixed on a motor, the cleaned quartz plates are placed in an oven for more than or equal to 4h, and the temperature of the oven is controlled to be more than or equal to 100 ℃.
CN202210120450.9A 2022-02-09 2022-02-09 Sample preparation method for analyzing hydroxyl content in quartz ore Pending CN116609143A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210120450.9A CN116609143A (en) 2022-02-09 2022-02-09 Sample preparation method for analyzing hydroxyl content in quartz ore

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210120450.9A CN116609143A (en) 2022-02-09 2022-02-09 Sample preparation method for analyzing hydroxyl content in quartz ore

Publications (1)

Publication Number Publication Date
CN116609143A true CN116609143A (en) 2023-08-18

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Country Status (1)

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CN (1) CN116609143A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116930115A (en) * 2023-09-15 2023-10-24 久智光电子材料科技有限公司 Quartz glass hydroxyl detection method and detection device

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116930115A (en) * 2023-09-15 2023-10-24 久智光电子材料科技有限公司 Quartz glass hydroxyl detection method and detection device
CN116930115B (en) * 2023-09-15 2023-12-12 久智光电子材料科技有限公司 Quartz glass hydroxyl detection method and detection device

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