CN117405466A - Sample preparation method for detecting and analyzing trace metal impurity elements in quartz stone - Google Patents

Sample preparation method for detecting and analyzing trace metal impurity elements in quartz stone Download PDF

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Publication number
CN117405466A
CN117405466A CN202210804376.2A CN202210804376A CN117405466A CN 117405466 A CN117405466 A CN 117405466A CN 202210804376 A CN202210804376 A CN 202210804376A CN 117405466 A CN117405466 A CN 117405466A
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China
Prior art keywords
quartz
quartz stone
self
grinding
stone
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Chinese (zh)
Inventor
李建德
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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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Priority to CN202210804376.2A priority Critical patent/CN117405466A/en
Publication of CN117405466A publication Critical patent/CN117405466A/en
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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
    • 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
    • G01N1/286Preparing 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
    • G01N2001/2866Grinding or homogeneising

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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)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention aims to provide a sample preparation method for detecting and analyzing trace metal impurity elements in quartz stone so as to improve the detection accuracy. The method comprises the following steps: 1. quartz stone is placed on a self-made tungsten-molybdenum alloy plate, and is knocked by a self-made tungsten-molybdenum alloy hammer to be broken; 2. clamping a pure quartz block with proper size and without external red skin by using a polytetrafluoroethylene clamp, putting the pure quartz block into a self-made tungsten-molybdenum grinding bowl, knocking the quartz block to proper size by using a grinding rod, and grinding the quartz block into particles; 3. the sample of particles was weighed using a tetrafluoroethylene spoon.

Description

Sample preparation method for detecting and analyzing trace metal impurity elements in quartz stone
Technical Field
The invention relates to a sample preparation method for detecting and analyzing trace metal impurity elements in quartz, which is suitable for preparing samples for detecting and analyzing trace elements in quartz.
Background
The existing sampling method for analyzing metal impurity elements in quartz stone by using a real detection unit mainly comprises the steps of wrapping quartz stone with common A4 printing white paper, breaking the quartz stone by using an iron hammer, then screening the broken quartz sand on A4 paper by putting the broken quartz sand on a screen with a certain mesh number, putting the quartz sand on A4 paper below the screen into an evaporation dish, flushing the quartz sand with deionized water for many times, putting the quartz sand into an oven, drying the quartz sand for 4 hours, and then performing detection analysis on trace elements. Since the detection limit of metal impurity elements in quartz stone reaches the mg/Kg level, the quartz stone is extremely easy to be polluted by the outside and the result is distorted, the method has the following defects:
1. because the hardness of the quartz stone is 7, the texture is hard, and the hardness of the common hammer is lower than 7, and the texture is soft, the surface of the quartz sand is inevitably occupied by scrap iron when the hammer is used for knocking, and the scrap iron adhered to the quartz sand is difficult to be simply washed by water;
2. if the common printing paper is used for wrapping the broken quartz sand, broken paper scraps can still remain in the broken quartz sand, and the broken quartz sand cannot be washed cleanly by deionized water;
3. and the screen is woven by metal wires, the screen is not cleaned, and the residue of the previous sample can pollute the sample being analyzed.
In summary, the conventional sampling method for testing can affect the authenticity of the metal impurity result in the quartz stone, and serious economic loss can be brought to quartz sand production enterprises by the fact that the unrealistic detection result is serious.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a sample preparation method for detecting and analyzing trace metal impurity elements in quartz stone so as to improve the detection accuracy.
The technical scheme adopted for solving the technical problems is as follows: a sample preparation method for detecting and analyzing trace metal impurity elements in quartz stone comprises the following steps:
1. quartz stone is placed on a self-made tungsten-molybdenum alloy plate, and is knocked by a self-made tungsten-molybdenum alloy hammer to be broken;
2. clamping a pure quartz block with proper size and without external red skin by using a polytetrafluoroethylene clamp, putting the pure quartz block into a self-made tungsten-molybdenum grinding bowl, knocking the quartz block to proper size by using a grinding rod, and grinding the quartz block into particles;
3. the sample of particles was weighed using a tetrafluoroethylene spoon.
Compared with the technology, the invention has the following obvious advantages:
1. the invention fully carries out the statistics of the conventional analysis types of the metal impurity elements of the quartz stone by the clients, and finds that the analysis of two elements of tungsten and molybdenum is almost free from the requirement, so that the pollution of tungsten and molybdenum to the sample in the sampling process is not considered excessively;
2. the hardness of quartz is about 7, the texture is brittle, the hardness of tungsten-molybdenum alloy is up to more than 20, the texture is hard, the quartz stone is easy to break by using the tungsten-molybdenum alloy, tungsten-molybdenum fragments are not adhered to the surface of quartz crushed stone, and therefore the influence of the tungsten-molybdenum alloy on a test result in the sample preparation process is not considered;
3. the invention does not need to screen by a screen, so that the pollution of the residue of other samples on the screen to the sample is avoided;
4. the method does not need to use deionized water for washing or baking in an oven, so that the sample preparation time is shortened, the time of the whole test flow is shortened, and the detection efficiency is improved.
Detailed description of the preferred embodiments
The present invention will be described in further detail with reference to examples.
Example 1
Example (one):
taking quartz stone No. 1, wherein the traditional method is to coat the quartz stone with an iron hammer, knock out the quartz stone with the iron hammer, then clamp and take a piece of quartz stone with a polytetrafluoroethylene clamp, wrap the quartz stone with common A4 printing paper, put the quartz stone on an iron plate, knock the quartz stone into pieces with the iron hammer, pour the quartz stone into a screen, screen the quartz stone, leave the quartz stone on the A4 paper, pour the quartz stone into an evaporation dish, wash the quartz stone with deionized water, put the quartz stone into an oven for drying, and obtain a sample, and test results 1: 15.88mg/kg of aluminum (Al), 4.35 mg/kg of calcium (Ca), 3.16 mg/kg of iron (Fe), 2.38 mg/kg of potassium (K) and 3.77mg/kg of sodium (Na); the method comprises the steps of putting quartz stones on a self-made tungsten-molybdenum alloy plate, knocking out the quartz stones by a self-made tungsten-molybdenum hammer, then clamping the other knocked quartz stones and the self-made tungsten-molybdenum grinding bowl by a polytetrafluoroethylene clamp, continuously knocking out quartz stones by a grinding rod, grinding particles with proper sizes, obtaining a sample, and testing to obtain a result 2: 15.76mg/kg of aluminum (Al), 4.24mg/kg of calcium (Ca), 1.25mg/kg of iron (Fe), 2.07/mg/kg of potassium (K) and 1.95mg/kg of sodium (Na).
Example (ii):
taking quartz stone No. 2, wherein the traditional method is to coat the quartz stone with an iron hammer, knock out the quartz stone with the iron hammer, then clamp and take a piece of quartz stone with a polytetrafluoroethylene clamp, wrap the quartz stone with common A4 printing paper, put the quartz stone on an iron plate, knock the quartz stone into pieces with the iron hammer, pour the quartz stone into a screen, screen the quartz stone, leave the quartz stone on the A4 paper, pour the quartz stone into an evaporation dish, wash the quartz stone with deionized water, put the quartz stone into an oven for drying, and obtain a sample, and test results 1: 26.87mg/kg of aluminum (Al), 9.35 mg/kg of calcium (Ca), 8.22 mg/kg of iron (Fe), 4.59 mg/kg of potassium (K) and 11.36 mg/kg of sodium (Na); the method comprises the steps of putting quartz stones on a self-made tungsten-molybdenum alloy plate, knocking out the quartz stones by a self-made tungsten-molybdenum hammer, then clamping the other knocked quartz stones and the self-made tungsten-molybdenum grinding bowl by a polytetrafluoroethylene clamp, continuously knocking out quartz stones by a grinding rod, grinding particles with proper sizes, obtaining a sample, and testing to obtain a result 2: 26.46mg/kg of aluminum (Al), 9.13/mg kg of calcium (Ca), 5.53mg/kg of iron (Fe), 3.64/mg/kg of potassium (K) and 6.45mg/kg of sodium (Na).
Example (iii):
taking quartz stone No. 3, wherein the traditional method is to coat the quartz stone with an iron hammer, knocking out the quartz stone with the iron hammer, then clamping a piece of quartz stone with a polytetrafluoroethylene clamp, wrapping the quartz stone with common A4 printing paper, putting the quartz stone on an iron plate, knocking the quartz stone into pieces with the iron hammer, pouring the pieces into a screen, sieving the pieces, leaving the sieved quartz sand on the A4 paper, pouring the pieces into an evaporation dish, washing the evaporation dish with deionized water, putting the evaporation dish into an oven, and drying the evaporation dish to obtain a sample, and testing to obtain a result 1: 55.68mg/kg of aluminum (Al), 20.32/mg/kg of calcium (Ca), 11.95/mg/kg of iron (Fe), 6.74/mg/kg of potassium (K) and 10.33/mg/kg of sodium (Na); the method comprises the steps of putting quartz stones on a self-made tungsten-molybdenum alloy plate, knocking out the quartz stones by a self-made tungsten-molybdenum hammer, then clamping the other knocked quartz stones and the self-made tungsten-molybdenum grinding bowl by a polytetrafluoroethylene clamp, continuously knocking out quartz stones by a grinding rod, grinding particles with proper sizes, obtaining a sample, and testing to obtain a result 2: 54.45mg/kg of aluminum (Al), 20.29mg/kg of calcium (Ca), 7.61mg/kg of iron (Fe), 5.72 mg/kg of potassium (K) and 6.98mg/kg of sodium (Na).
Through test data analysis in three embodiments, the detection result of the sample prepared by the method is obviously smaller than the value of each element of the detection result of the sample prepared by the traditional method, and is characterized in that the result data obtained by the method is closer to the true value of the element in the quartz stone due to iron (Fe), potassium (K) and sodium (Na) which are greatly influenced by the outside.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the embodiments, it should be understood by those skilled in the art that modifications and equivalent substitutions can be made thereto without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered by the scope of the claims of the present invention.

Claims (1)

1. A sample preparation method for detecting and analyzing trace metal impurity elements in quartz stone is characterized by comprising the following steps:
(1) Putting quartz stone on an alloy plate, and knocking by using an alloy hammer to crush the quartz stone;
(2) Clamping pure quartz blocks with proper sizes and without external red skin, putting the pure quartz blocks into a self-made tungsten-molybdenum grinding pot, knocking the quartz blocks to proper sizes by using a grinding rod, and grinding the quartz blocks into particles;
(3) Weighing a particle sample by using a spoon;
the alloy plate in the step (1) is a self-made tungsten-molybdenum alloy plate, and the alloy hammer is a self-made tungsten-molybdenum alloy hammer;
in the step (2), the clamp is a polytetrafluoroethylene clamp, the grinding bowl is a self-made tungsten-molybdenum alloy grinding bowl, and the grinding rod is a self-made tungsten-molybdenum alloy grinding rod;
the spoon in the step (3) is a polytetrafluoroethylene spoon.
CN202210804376.2A 2022-07-09 2022-07-09 Sample preparation method for detecting and analyzing trace metal impurity elements in quartz stone Pending CN117405466A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210804376.2A CN117405466A (en) 2022-07-09 2022-07-09 Sample preparation method for detecting and analyzing trace metal impurity elements in quartz stone

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210804376.2A CN117405466A (en) 2022-07-09 2022-07-09 Sample preparation method for detecting and analyzing trace metal impurity elements in quartz stone

Publications (1)

Publication Number Publication Date
CN117405466A true CN117405466A (en) 2024-01-16

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CN202210804376.2A Pending CN117405466A (en) 2022-07-09 2022-07-09 Sample preparation method for detecting and analyzing trace metal impurity elements in quartz stone

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