WO2023128941A1 - An analysis method - Google Patents

An analysis method Download PDF

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Publication number
WO2023128941A1
WO2023128941A1 PCT/TR2022/050557 TR2022050557W WO2023128941A1 WO 2023128941 A1 WO2023128941 A1 WO 2023128941A1 TR 2022050557 W TR2022050557 W TR 2022050557W WO 2023128941 A1 WO2023128941 A1 WO 2023128941A1
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WO
WIPO (PCT)
Prior art keywords
sample
analysis method
analysis
quartz
acid
Prior art date
Application number
PCT/TR2022/050557
Other languages
French (fr)
Inventor
Ali İhsan TURAN
Original Assignee
Esan Eczacibaşi Endüstri̇yel Hammaddeler Sanayi̇ Ve Ti̇caret Anoni̇m Şi̇rketi̇
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from TR2021/021044 external-priority patent/TR2021021044A2/en
Application filed by Esan Eczacibaşi Endüstri̇yel Hammaddeler Sanayi̇ Ve Ti̇caret Anoni̇m Şi̇rketi̇ filed Critical Esan Eczacibaşi Endüstri̇yel Hammaddeler Sanayi̇ Ve Ti̇caret Anoni̇m Şi̇rketi̇
Publication of WO2023128941A1 publication Critical patent/WO2023128941A1/en

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/04—Devices for withdrawing samples in the solid state, e.g. by cutting
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44—Sample treatment involving radiation, e.g. heat

Definitions

  • the invention relates to an analysis method, which enables the quartz analysis to be performed in a short time and with high precision, enables the sodium content in the quartz to be measured, enables the risks in terms of occupational health and safety to be reduced, and eliminates high maintenance and operational costs.
  • the quartz refers to the silicon dioxide (SiOz) crystals quite commonly found in the earth and extracted from the open pit mines and contains in its pure form 46.5% by weight silicon (Si) and 53.3% by weight oxygen (O2). Iron (Fe), sodium (Na), aluminum (Al), titanium (Ti) and magnesium (Mg) are among the elements frequently encountered in the extracted quartz.
  • quartz Being a material frequently used in many industries worldwide, quartz is subjected to various processes before being used, according to the substances it contains and the proportions of these substances. Quartz is subjected to an analysis method in order to determine its contents. Since quartz is a mineral that is soluble only in hydrofluoric acid (HF), it is mixed with HF in a platinum crucible according to the state of the art. The other processes may be performed after enabling the evaporation of the added acid by the heat. Said dissolution process is only a preparatory step and takes about 2.5 days to be complete. This leads to the inability to efficiently use the time, material and human resources.
  • HF hydrofluoric acid
  • the platinum crucible containing the quartz is kept for 1 hour in an oven.
  • the mineral which is dissolved in hydrochloric acid (HCI) after the oven drying process, finally liquefies and is thus made ready for being introduced to the analysis device.
  • HCI hydrochloric acid
  • ICP-OES Inductively Coupled Plasma-Optical Emission Spectroscopy
  • the minimum measurement value of said device is 5 ppm and sodium and other elements present in small amounts below 5 ppm in quartz may not be detected with this device.
  • the operational and maintenance costs are quite high for the platinum crucible used in said technique that wears off as a result of oven drying and heat treatment.
  • the platinum crucibles rapidly wear off and require frequent maintenance and/or replacement.
  • the dissolution and evaporation steps performed in the platinum crucibles are the processes requiring monitoring, they are implemented in open systems. This both poses great risk in terms of occupational health and safety, considering the strong acids used, and exposes the quartz, the analysis of which is intended to be performed in a precise manner, to the contaminations possible to originate from the external sources.
  • an analysis method which enables the quartz analysis to be performed in a short time and with high precision, enables the sodium content in the quartz to be measured, enables the risks in terms of occupational health and safety to be reduced, and eliminates high maintenance and operational costs, has been provided.
  • An object of the invention is to develop an analysis method via which the contents of the quartz mineral may be determined in a short time.
  • Another object of the invention is to develop an analysis method, which protects the quartz mineral from the contaminations likely to originate from external sources as well as minimizing the risk in terms of occupational health and safety, since the acid dissolution process is to take place in a closed system.
  • Another object of the invention is to develop an analysis method, in which the monitoring for the sample is not necessary during the dissolution and in which the human resources may be used efficiently.
  • the invention relates to an analysis method, which enables the quartz analysis to be performed in a short time and with high precision, enables the sodium content in the quartz to be measured, enables the risks in terms of occupational health and safety to be reduced, and eliminates high maintenance and operational costs.
  • the analysis method according to the invention comprises, in its most basic form, the following process steps:
  • the above-mentioned sample is taken from the quartz mineral, and in a preferred embodiment of the invention, 0.1 - 0.3 grams of sample is weighed and prepared for analysis.
  • the sample is transferred into a container manufactured from a material that is preferably, but not limited to, Teflon material.
  • Teflon material preferably, but not limited to Teflon material.
  • hydrofluoric acid is added to the sample along with at least one type of acid different from hydrofluoric acid with a view to reduce the acid use, slow down the wear rates of the materials used and carry out the analysis in an environment safe from the perspective of occupational health and safety.
  • the acid mixture used as the solvent within the scope of invention preferably comprises, along with hydrofluoric acid, an acid that is preferably, but not limited to, nitric acid.
  • the acid mixture used in the analysis method developed within the scope of invention preferably comprises 9 - 11 ml hydrofluoric acid and/or 2 - 4 ml nitric acid.
  • the acid mixture comprises 9 - 11 ml hydrofluoric acid and 2 - 4 ml nitric acid together.
  • a reaction takes place. It takes about 10 - 20 minutes for the reaction to become complete and after allowing said duration to elapse, the cap of the teflon container is placed and the container is placed into the digestion device.
  • the digestion device preferred within the scope of invention dissolves the quartz by 100% preferably by means of the microwave rays.
  • the dissolution process according to the state of the art which takes about 2 - 3 days and which is performed by heating a platinum container, takes place in 70 - 80 minutes in the method according to the invention. Additionally, since the quartz is enabled to be dissolved completely, the sodium element, the measurement of which is not possible in the state of the art, is rendered possible to measure with the method according to the invention. This accordingly makes the analysis more precise and more accurate as compared to the state of the art.
  • a CEM MARS - 6 microwave device is used as the digestion device within the scope of invention, the options are not limited to said device.
  • said device is set to 1750 - 2000 W and 190 - 210 °C before the digestion process is started.
  • the sample After the digestion process that takes 70 - 80 minutes is completed in the digestion device, the sample becomes completely liquid.
  • the sample, which has been liquefied, is transferred into the single-use containers.
  • the single-use containers that are used are manufactured from plastic material.
  • the single-use containers have an interior volume of 45 - 55 ml.
  • the quartz solution introduced to the single-use containers is subjected to detailed measurements in an analysis device.
  • an Inductively Coupled Plasma-Mass Spectrometer (ICP-MS) device is used as the analysis device within the scope of invention, the options are not limited to said device.
  • an Agilent 7800 ICP-MS device is used as the analysis device.
  • the minimum measurement point is 5 ppm in the ICP-OES devices used for analysis according to the state of the art
  • the minimum measurement value is 0.01 ppm for ICP-MS device preferred within the scope of the invention. In this way, it is ensured that the measurement even for the elements that are present in very small quantities in quartz may be performed accurately.
  • the method according to the invention unlike the state of the art, does not involve the use of a platinum container, an oven and high quantities of acid, enables the method to be more advantageous from the financial perspective as well as from the perspective of occupational health and safety. Additionally, that the dissolution process is performed in 70 - 80 minutes instead of 2 - 3 days and within a closed digestion device, more generally in a closed system, instead of by way of heating in an oven, enables the sample to be subjected to analysis to be protected from the contaminations likely to originate from the external sources and enables the analysis to be performed in a rapid and safe manner without the need being left for the monitoring of the sample.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention relates to an analysis method, which enables the analysis of pure quartz to be performed in a short time and with high precision, enables the sodium content in the quartz to be measured, enables the risks in terms of occupational health and safety to be reduced. More specifically, the invention relates to an analysis method whereby the measurement of the substances in the quartz may be performed in a short time and with high precision, wherein the method comprises the process steps of taking a sample from quartz, weighing the sample, combining the sample with at least one or more than one acid, liquefying the sample by means of the digestion device, transferring the sample in liquid state into the single-use containers, and determining the contents of the sample, which has been transferred into the single-use containers, by means of the analysis device.

Description

AN ANALYSIS METHOD
Subject of the Invention
The invention relates to an analysis method, which enables the quartz analysis to be performed in a short time and with high precision, enables the sodium content in the quartz to be measured, enables the risks in terms of occupational health and safety to be reduced, and eliminates high maintenance and operational costs.
State of the Art
The quartz refers to the silicon dioxide (SiOz) crystals quite commonly found in the earth and extracted from the open pit mines and contains in its pure form 46.5% by weight silicon (Si) and 53.3% by weight oxygen (O2). Iron (Fe), sodium (Na), aluminum (Al), titanium (Ti) and magnesium (Mg) are among the elements frequently encountered in the extracted quartz.
Being a material frequently used in many industries worldwide, quartz is subjected to various processes before being used, according to the substances it contains and the proportions of these substances. Quartz is subjected to an analysis method in order to determine its contents. Since quartz is a mineral that is soluble only in hydrofluoric acid (HF), it is mixed with HF in a platinum crucible according to the state of the art. The other processes may be performed after enabling the evaporation of the added acid by the heat. Said dissolution process is only a preparatory step and takes about 2.5 days to be complete. This leads to the inability to efficiently use the time, material and human resources.
After the evaporation of hydrofluoric acid, the platinum crucible containing the quartz is kept for 1 hour in an oven. The mineral, which is dissolved in hydrochloric acid (HCI) after the oven drying process, finally liquefies and is thus made ready for being introduced to the analysis device. According to the state of the art, Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) device is preferred as the analysis device. The minimum measurement value of said device is 5 ppm and sodium and other elements present in small amounts below 5 ppm in quartz may not be detected with this device.
In addition to the above-mentioned disadvantages, the operational and maintenance costs are quite high for the platinum crucible used in said technique that wears off as a result of oven drying and heat treatment. As a result of the preparation and analysis processes requiring long time and taking a total time of about 3 days and of the work being performed at elevated temperatures, the platinum crucibles rapidly wear off and require frequent maintenance and/or replacement. Further, since the dissolution and evaporation steps performed in the platinum crucibles are the processes requiring monitoring, they are implemented in open systems. This both poses great risk in terms of occupational health and safety, considering the strong acids used, and exposes the quartz, the analysis of which is intended to be performed in a precise manner, to the contaminations possible to originate from the external sources.
The need has arisen to carry out an innovation in the related art in order to solve the problems mentioned above. With the invention, an analysis method, which enables the quartz analysis to be performed in a short time and with high precision, enables the sodium content in the quartz to be measured, enables the risks in terms of occupational health and safety to be reduced, and eliminates high maintenance and operational costs, has been provided.
Object of the Invention
An object of the invention is to develop an analysis method via which the contents of the quartz mineral may be determined in a short time.
Another object of the invention is to develop an analysis method, which has high measurement precision and which enables even the measurement of the other elements such as sodium that are present in very small quantities in quartz. Another object of the invention is to develop an analysis method via which high maintenance and operational costs are eliminated.
Another object of the invention is to develop an analysis method, which protects the quartz mineral from the contaminations likely to originate from external sources as well as minimizing the risk in terms of occupational health and safety, since the acid dissolution process is to take place in a closed system.
Another object of the invention is to develop an analysis method, in which the monitoring for the sample is not necessary during the dissolution and in which the human resources may be used efficiently.
The structural and characteristic features and all the advantages of the invention will be more clearly understood owing to the detailed description provided below. Accordingly, the evaluation should be made taking this detailed description into consideration.
Detailed Description of the Invention
The invention relates to an analysis method, which enables the quartz analysis to be performed in a short time and with high precision, enables the sodium content in the quartz to be measured, enables the risks in terms of occupational health and safety to be reduced, and eliminates high maintenance and operational costs.
In this detailed description, the preferred alternatives of the analysis method according to the invention are explained in a way only enabling a better understanding of the subject matter and not leading to any limiting effect.
By said method, it is aimed to perform the analysis for the sample obtained from the quartz mineral in a rapid and precise manner. The analysis process that takes about 3 days including the duration needed for preparation according to the state of the art is completed within about 2 hours by the method according to the invention and it is also possible to determine the quantities of the components like sodium and other elements, the quantities of which are unable to be determined by the existing methods.
The analysis method according to the invention comprises, in its most basic form, the following process steps:
• Taking a sample from quartz,
• weighing the sample,
• combining the sample with at least one or more than one acid,
• liquefying the sample by means of the digestion device,
• transferring the sample in liquid state into the single-use containers, and
• determining the contents of the sample, which has been transferred into the single-use containers, by means of the analysis device.
The above-mentioned sample is taken from the quartz mineral, and in a preferred embodiment of the invention, 0.1 - 0.3 grams of sample is weighed and prepared for analysis. The sample is transferred into a container manufactured from a material that is preferably, but not limited to, Teflon material. According to the state of the art, only hydrofluoric acid is used for liquefying the sample by way of dissolution of the same. However, within the scope of the invention, hydrofluoric acid is added to the sample along with at least one type of acid different from hydrofluoric acid with a view to reduce the acid use, slow down the wear rates of the materials used and carry out the analysis in an environment safe from the perspective of occupational health and safety.
The acid mixture used as the solvent within the scope of invention preferably comprises, along with hydrofluoric acid, an acid that is preferably, but not limited to, nitric acid. The acid mixture used in the analysis method developed within the scope of invention preferably comprises 9 - 11 ml hydrofluoric acid and/or 2 - 4 ml nitric acid. In a preferred embodiment of the invention, the acid mixture comprises 9 - 11 ml hydrofluoric acid and 2 - 4 ml nitric acid together.
After the combination of the sample with the acid mixture, a reaction takes place. It takes about 10 - 20 minutes for the reaction to become complete and after allowing said duration to elapse, the cap of the teflon container is placed and the container is placed into the digestion device. The digestion device preferred within the scope of invention dissolves the quartz by 100% preferably by means of the microwave rays. The dissolution process according to the state of the art, which takes about 2 - 3 days and which is performed by heating a platinum container, takes place in 70 - 80 minutes in the method according to the invention. Additionally, since the quartz is enabled to be dissolved completely, the sodium element, the measurement of which is not possible in the state of the art, is rendered possible to measure with the method according to the invention. This accordingly makes the analysis more precise and more accurate as compared to the state of the art.
Although a CEM MARS - 6 microwave device is used as the digestion device within the scope of invention, the options are not limited to said device. In a preferred embodiment of the invention, said device is set to 1750 - 2000 W and 190 - 210 °C before the digestion process is started.
After the digestion process that takes 70 - 80 minutes is completed in the digestion device, the sample becomes completely liquid. The sample, which has been liquefied, is transferred into the single-use containers. In a preferred embodiment of the invention, the single-use containers that are used are manufactured from plastic material. Further, in a preferred embodiment of the invention, the single-use containers have an interior volume of 45 - 55 ml. As a result of sealing the solution and transferring the same into the single-use containers, it ensured that the sample is protected from all kinds of contaminants likely to originate from the external sources, and thus, a more accurate analysis is performed.
The quartz solution introduced to the single-use containers is subjected to detailed measurements in an analysis device. Although an Inductively Coupled Plasma-Mass Spectrometer (ICP-MS) device is used as the analysis device within the scope of invention, the options are not limited to said device. In a preferred embodiment of the invention, an Agilent 7800 ICP-MS device is used as the analysis device. Whereas the minimum measurement point is 5 ppm in the ICP-OES devices used for analysis according to the state of the art, the minimum measurement value is 0.01 ppm for ICP-MS device preferred within the scope of the invention. In this way, it is ensured that the measurement even for the elements that are present in very small quantities in quartz may be performed accurately. As a result, it becomes possible to perform the precise measurement of sodium and the similar elements, which may not be measured by the device and/or dissolution method and/or digestion method employed under the normal conditions. Owing to the use of an ICP-MS device within the scope of the invention instead of an ICP-OES device, the measurement precision is increased by about 500 times. The analysis performed with said devices takes 25 - 35 minutes in a preferred embodiment of the invention.
That the method according to the invention, unlike the state of the art, does not involve the use of a platinum container, an oven and high quantities of acid, enables the method to be more advantageous from the financial perspective as well as from the perspective of occupational health and safety. Additionally, that the dissolution process is performed in 70 - 80 minutes instead of 2 - 3 days and within a closed digestion device, more generally in a closed system, instead of by way of heating in an oven, enables the sample to be subjected to analysis to be protected from the contaminations likely to originate from the external sources and enables the analysis to be performed in a rapid and safe manner without the need being left for the monitoring of the sample.
Owing to the analysis method developed within the scope of the invention, which enables the quartz analysis to be performed in a short time and with high precision, enables the sodium content in the quartz to be measured, enables the risks in terms of occupational health and safety to be reduced, and eliminates high maintenance and operational costs, the above-mentioned problems and drawbacks of the state of the art encountered by the users are enabled to be eliminated.

Claims

1. An analysis method whereby the measurement of the substances in the quartz may be performed in a short time and with high precision characterized in that the method comprises the process steps of
• taking a sample from quartz,
• weighing the sample,
• combining the sample with at least one or more than one acid,
• liquefying the sample by means of the digestion device,
• transferring the sample in liquid state into the single-use containers, and
• determining the contents of the sample, which has been transferred into the single-use containers, by means of the analysis device.
2. An analysis method according to Claim 1 characterized in that 0.1 - 0.3 grams of quartz sample is weighed and prepared for analysis.
3. An analysis method according to Claim 1 or Claim 2 characterized in that obtained sample is transferred into a container manufactured from teflon material.
4. An analysis method according to any one of the preceding claims characterized in that hydrofluoric acid is added to the sample in order to liquefy the sample by way of dissolution of the same.
5. An analysis method according to any one of the preceding claims characterized in that nitric acid is added to the sample in order to liquefy the sample by way of dissolution of the same.
6. An analysis method according to any one of Claims 1 - 3 characterized in that hydrofluoric acid and nitric acid are added to the sample in order to liquefy the sample by way of dissolution of the same.
7. An analysis method according to Claim 4 characterized in that 9 - 11 ml hydrofluoric acid is added to the sample.
7
8. An analysis method according to Claim 5 characterized in that 2 - 4 ml nitric acid is added to the sample.
9. An analysis method according to Claim 6 characterized in that 9 - 11 ml hydrofluoric acid and 2 - 4 ml nitric acid are added to the sample.
10. An analysis method according to any one of the preceding claims characterized in that a device that will enable the sample to dissolve by 100% in the acid or acid mixture is used as the digestion device.
11. An analysis method according to any one of the preceding claims characterized in that a CEM MARS - 6 microwave device is used as the digestion device.
12. An analysis method according to Claim 11 characterized in that the digestion device is set to 1750 - 2000 W before the digestion process is started.
13. An analysis method according to any one of Claims 10 - 12 characterized in that the digestion device is set to 190 - 210 °C before the digestion process is started.
14. An analysis method according to Claim 1 characterized in that the single-use containers that are used are manufactured from plastic material.
15. An analysis method according to Claim 1 characterized in that the single-use containers have an interior volume of 45 - 55 ml.
16. An analysis method according to any one of the preceding claims characterized in that an Inductively Coupled Plasma-Mass Spectrometer (ICP-MS) device is used as the analysis device.
17. An analysis method according to any one of the preceding claims characterized in that an Agilent 7800 ICP-MS device is used as the analysis device.
18. An analysis method according to any one of the preceding claims characterized in that the reaction taking place upon the addition of acid or acid mixture lasts 10 - 20 minutes.
8
19. An analysis method according to any one of the preceding claims characterized in that the process in the digestion device lasts 70 - 80 minutes.
20. An analysis method according to any one of the preceding claims characterized in that the process in the analysis device lasts 25 - 35 minutes.
21. An analysis method according to any one of the preceding claims characterized in that the quantity of sodium in the quartz may be determined as a result of the analysis.
9
PCT/TR2022/050557 2021-12-27 2022-06-09 An analysis method WO2023128941A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
TR2021021044 2021-12-27
TR2021/021044 TR2021021044A2 (en) 2021-12-27 A METHOD OF ANALYSIS

Publications (1)

Publication Number Publication Date
WO2023128941A1 true WO2023128941A1 (en) 2023-07-06

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5968259A (en) * 1997-08-27 1999-10-19 Shin-Etsu Quartz Products Co., Ltd. High-purity quartz glass and method for the preparation thereof
JP2015040789A (en) * 2013-08-22 2015-03-02 株式会社 東ソー分析センター Analytical method of zirconium in quartz

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5968259A (en) * 1997-08-27 1999-10-19 Shin-Etsu Quartz Products Co., Ltd. High-purity quartz glass and method for the preparation thereof
JP2015040789A (en) * 2013-08-22 2015-03-02 株式会社 東ソー分析センター Analytical method of zirconium in quartz

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
XUELIN DONG ET AL.: "Determination of trace elements in high-purity quartz samples by ICP-OES and ICP-MS: A normal-pressure digestion pretreatment method for eliminating unfavorable substrate Si", ANALYTICA CHIMICA ACTA, vol. 1110, 2020, pages 11 - 18, XP086125139, ISSN: 0003-2670, DOI: 10.1016/j.aca. 2020.03.00 6 *

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