CN113109121A - Sample preparation method and test method of trititanium pentoxide crystal particles in glow discharge mass spectrum - Google Patents
Sample preparation method and test method of trititanium pentoxide crystal particles in glow discharge mass spectrum Download PDFInfo
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- CN113109121A CN113109121A CN202110436847.4A CN202110436847A CN113109121A CN 113109121 A CN113109121 A CN 113109121A CN 202110436847 A CN202110436847 A CN 202110436847A CN 113109121 A CN113109121 A CN 113109121A
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- 239000013078 crystal Substances 0.000 title claims abstract description 72
- 238000005464 sample preparation method Methods 0.000 title claims abstract description 30
- 238000010998 test method Methods 0.000 title claims abstract description 9
- 238000001819 mass spectrum Methods 0.000 title description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 96
- 238000005406 washing Methods 0.000 claims abstract description 72
- 238000012360 testing method Methods 0.000 claims abstract description 58
- 229910052738 indium Inorganic materials 0.000 claims abstract description 43
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 43
- AZCUJQOIQYJWQJ-UHFFFAOYSA-N oxygen(2-) titanium(4+) trihydrate Chemical compound [O-2].[O-2].[Ti+4].O.O.O AZCUJQOIQYJWQJ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000001036 glow-discharge mass spectrometry Methods 0.000 claims abstract description 28
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- 238000001035 drying Methods 0.000 claims abstract description 18
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- 238000000034 method Methods 0.000 claims description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
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- 229920001343 polytetrafluoroethylene Polymers 0.000 description 11
- 239000004810 polytetrafluoroethylene Substances 0.000 description 11
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 5
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- HIZCIEIDIFGZSS-UHFFFAOYSA-L trithiocarbonate Chemical compound [S-]C([S-])=S HIZCIEIDIFGZSS-UHFFFAOYSA-L 0.000 description 4
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Classifications
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- 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
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/68—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using electric discharge to ionise a gas
Abstract
The invention provides a sample preparation method and a test method of trititanium pentoxide crystal particles in glow discharge mass spectrometry, wherein the sample preparation method comprises the following steps: (1) carrying out acid washing, first water washing, first ethanol washing and first drying on the indium sheet in sequence to obtain a processed indium sheet; (2) sequentially carrying out second ethanol washing, second water washing, third ethanol washing and second drying on the titanium pentoxide crystal particles to obtain treated titanium pentoxide crystal particles; (3) placing the titanium pentoxide crystal particles on the surface of an indium sheet, and tabletting to obtain a sample to be detected; the step (1) and the step (2) are not in sequence; the sample preparation method avoids the introduction of impurities as much as possible, thereby shortening the analysis time and ensuring the accuracy of data; the test method can obtain stronger signals through specific test parameters and has high sensitivity.
Description
Technical Field
The invention relates to the technical field of testing, in particular to the technical field of glow discharge mass spectrometry, and particularly relates to a sample preparation method of trititanium pentoxide crystal particles in glow discharge mass spectrometry.
Background
The glow discharge mass spectrometry is an analysis method for performing mass spectrometry by using a glow discharge source as an ion source and connecting the glow discharge source with a mass spectrometry instrument, and is mainly used for detecting the content of trace elements in a material, and the corresponding analysis instrument is called as a glow discharge mass spectrometer. One of the core components of the glow discharge mass spectrometer is a glow discharge chamber, which is used for glow discharge of a sample to be detected and ionization into ion beams after neutral particles are sputtered. Aiming at the shape and size of a sample to be detected, the glow discharge chamber is divided into a sheet-shaped glow discharge chamber and a needle-shaped glow discharge chamber, wherein the size requirement of the sheet-shaped glow discharge chamber on the sheet-shaped sample to be detected is generally 20mm multiplied by 2mm, and the size requirement of the needle-shaped glow discharge chamber on the needle-shaped sample to be detected is generally 20mm multiplied by 2 mm. However, in the actual production, processing and use processes, the sample to be tested has various forms, including irregular block, powder, granule, chip, needle and the like, and cannot be effectively fixed by the sample clamp in the glow discharge chamber, which seriously hinders the GDMS analysis.
Aiming at the problem that a fine sample to be detected cannot be effectively fixed by a sample clamp in a glow discharge mass spectrometer, the prior art discloses a plurality of novel sample loading parts to be detected. For example, CN210923569U discloses a sample stage for testing small-sized samples by a glow discharge mass spectrometer with model number ELEMENTGD, which is composed of a high-purity copper sample stage body and soldering tin, wherein a groove is formed on the high-purity copper sample stage body, and the soldering tin is arranged in the groove; the diameter of the surface of the high-purity copper sample table body is 25 mm-50 mm, and the height is 5 mm-20 mm; the groove is a cylindrical groove, the diameter is more than 20mm, and the depth is more than or equal to 3 mm. The sample platform is provided with the groove through the high-purity copper body, and the proper amount of soldering tin is placed in the groove, so that a small-size sample can be fixed on the high-purity copper sample, the soldering tin can not expose the lower surface of the sample, and the influence of the soldering tin on the sample during testing is avoided.
CN212542352U discloses an indium carrier for glow discharge mass spectrometer to measure needle-like samples, wherein the indium carrier for glow discharge mass spectrometer to measure needle-like samples is rod-like, a hole is provided on an end face of one end, a groove is provided on a side face of the indium carrier corresponding to the hole, and a base is provided at the other end of the indium carrier. In the actual sample preparation process, the indium carrier is firstly erected on a table top through the base, then a fine needle-shaped sample is inserted into the hole, then the needle-shaped sample is fixed by applying pressure through the positioning of the groove, and then the whole body is fixed through a sample clamp in the glow discharge mass spectrometer and is measured.
CN212848303U discloses a sample holder for glow discharge mass spectrometry, which comprises a sample holder main body; the sample clamp main body is provided with an article placing groove; a clamping piece is arranged in the article placing groove, and a fastening piece matched with the clamping piece is arranged on the inner wall of the article placing groove; the clamping piece moves in the horizontal direction under the action of the fastening piece.
Although there have been improvements in equipment for glow discharge mass spectrometry, it is still difficult to adapt existing sample holders or carriers for testing particulate samples.
The titanium pentoxide particles are suitable for antireflection films; a beam splitter; a cold light film; a filter; high-reflection film; coating a film on the glasses; reflective films, etc., are materials for vacuum coating, and the purity of the material has an important influence on the performance of the material.
However, since impurities are easily mixed in the conventional pressing method, it is necessary to develop a method for preparing a granular sample for a specific substance.
Disclosure of Invention
In view of the problems in the prior art, the invention provides a sample preparation method and a test method of titanium pentoxide crystal particles in glow discharge mass spectrometry, wherein the sample preparation method avoids the introduction of impurities as much as possible through the combination of a series of washing steps, thereby shortening the analysis time and ensuring the accuracy of data; the test method can obtain stronger signals by selecting specific test parameters, and has high sensitivity.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a sample preparation method of titanium pentoxide crystal particles in glow discharge mass spectrometry, which comprises the following steps:
(1) carrying out acid washing, first water washing, first ethanol washing and first drying on the indium sheet in sequence to obtain a processed indium sheet;
(2) sequentially carrying out second ethanol washing, second water washing, third ethanol washing and second drying on the titanium pentoxide crystal particles to obtain treated titanium pentoxide crystal particles;
(3) placing the titanium pentoxide crystal particles on the surface of an indium sheet, and tabletting to obtain a sample to be detected;
the step (1) and the step (2) have no sequence.
According to the invention, different washing procedures are adopted according to different characteristics of the indium sheet and the titanium pentoxide particles, so that the situation that impurities are introduced into the indium sheet and the titanium pentoxide particles can be avoided at the same time, wherein the indium sheet is subjected to acid washing to remove other metal impurities on the surface of the indium sheet, then first water washing is carried out to remove impurities such as residual acid and dust, and first ethanol washing is carried out to reduce the moisture on the surface and shorten the first drying time, so that not only are the impurities removed, but also the possibility of introducing the impurities is greatly reduced; and the titanium pentoxide crystal particles are washed by ethanol and then by water, so that impurities on the surfaces of the titanium pentoxide crystal particles can be removed better.
Preferably, the acid washing, the first water washing and the first ethanol washing in the step (1) are respectively and independently carried out in a cup made of polytetrafluoroethylene.
Preferably, the indium sheet in step (1) is a high purity indium sheet.
Preferably, the high purity indium sheet has a purity of 99.999 wt% or more, such as 99.999 wt%, 99.9991 wt%, 99.9992 wt%, 99.9993 wt%, 99.9994 wt%, 99.9995 wt%, 99.9996 wt%, 99.9997 wt%, 99.9998 wt%, or 99.9999 wt%, etc., but is not limited to the recited values, and other values not recited in this range are also applicable.
Preferably, the acid used in step (1) is nitric acid.
The invention preferably adopts nitric acid, which can effectively avoid chlorine element or sulfur element introduced by hydrochloric acid or sulfuric acid, thereby reducing the accuracy of the test.
Preferably, the nitric acid has a concentration of 10 to 25 wt%, and may be, for example, 10 wt%, 12 wt%, 14 wt%, 15 wt%, 17 wt%, 19 wt%, 20 wt%, 22 wt%, 24 wt%, or 25 wt%, etc., but is not limited to the recited values, and other values not recited in this range are also applicable.
According to the invention, the concentration of the nitric acid is preferably controlled to be 10-25 wt%, so that impurities on the surface of the indium sheet can be better removed.
Preferably, the time for the acid washing is 2 to 5min, for example, 2min, 2.4min, 2.7min, 3min, 3.4min, 3.7min, 4min, 4.4min, 4.7min or 5min, etc., but is not limited to the recited values, and other values not recited in the range are also applicable.
Preferably, the number of times of the first water washing in step (1) is at least three, and for example, may be 3, 4, 5 or 6 times, etc., but is not limited to the recited values, and other values not recited in the range are also applicable.
Preferably, the number of first ethanol washes is at least one, and may be, for example, 1, 2, 3, 4, 5, or 6, etc., but is not limited to the recited values, and other values not recited within this range are equally applicable.
Preferably, the first drying comprises blow drying.
Preferably, the average particle diameter of the crystal particles of the trititanium pentoxide in the step (2) is 1 to 3mm, and may be, for example, 1mm, 1.3mm, 1.5mm, 1.7mm, 1.9mm, 2.2mm, 2.4mm, 2.6mm, 2.8mm, or 3mm, but is not limited to the values listed, and other values not listed in this range are also applicable.
The size of the trithiocarbonate crystal particles is 1-3 mm, the trithiocarbonate crystal particles are different from a flaky sample or a needle-shaped sample of glow discharge mass spectrometry due to the fact that the trithiocarbonate crystal particles are granular, testing is difficult, and the trithiocarbonate crystal particles have the characteristic of low melting point.
Preferably, the vaporization temperature of the trititanium pentoxide crystal particles is 1500 to 2000 ℃, and may be, for example, 1500 ℃, 1556 ℃, 1612 ℃, 1667 ℃, 1723 ℃, 1778 ℃, 1834 ℃, 1889 ℃, 1945 ℃ or 2000 ℃, etc., but not limited to the enumerated values, and other values not enumerated within this range are also applicable.
The evaporation temperature is suitable for manufacturing materials such as titanium pentoxide coating.
Preferably, the density of the titanium pentoxide crystal particles is 3-6 g/cm3For example, it may be 3g/cm3、3.4g/cm3、3.7g/cm3、4g/cm3、4.4g/cm3、4.7g/cm3、4.89g/cm3、5g/cm3、5.4g/cm3、5.7g/cm3Or 6g/cm3Etc., but are not limited to the enumerated values, and other values not enumerated within the range are equally applicable, and preferably 4.89g/cm3。
Preferably, the second ethanol wash in step (2) is performed under ultrasonic conditions.
The cleaning of the titanium pentoxide particles is carried out under the conditions of ethanol and ultrasound, so that the titanium pentoxide particles can be cleaned more cleanly.
Preferably, the time of the second ethanol washing is 2 to 5min, for example, 2min, 2.4min, 2.7min, 3min, 3.4min, 3.7min, 4min, 4.4min, 4.7min or 5min, etc., but is not limited to the values listed, and other values not listed in the range are also applicable.
Preferably, the number of times of the second water washing is at least three, and for example, may be 3 times, 4 times, 5 times, 6 times, 8 times, or the like.
Preferably, the second drying includes drying.
Preferably, the titanium pentoxide crystal particles are clamped by tweezers and placed on the surface of the indium sheet.
Preferably, the forceps are made of polytetrafluoroethylene.
Preferably, the pressure of the tablet in step (3) is 2 to 8MPa, and may be, for example, 2MPa, 2.7MPa, 3.4MPa, 4MPa, 4.7MPa, 5.4MPa, 6MPa, 6.7MPa, 7.4MPa or 8MPa, but is not limited to the above-mentioned values, and other values not mentioned in the above range are also applicable.
Preferably, the tabletting time is 1.5 to 3 seconds, for example, 1.5s, 1.7s, 1.9s, 2s, 2.2s, 2.4s, 2.5s, 2.7s, 2.9s or 3s, but not limited to the recited values, and other values not recited in this range are also applicable.
As a preferable technical scheme of the invention, the sample preparation method comprises the following steps:
(1) sequentially carrying out acid washing on indium sheets with the purity of more than or equal to 99.999 wt% for 2-5 min by using nitric acid with the purity of more than or equal to 25 wt%, at least three times of first water washing, at least one time of first ethanol washing and first drying to obtain processed indium sheets;
(2) sequentially carrying out second ethanol washing, at least three times of second water washing, third ethanol washing and second drying on the titanium pentoxide crystal particles with the particle size of 1-3 mm and the evaporation temperature of 1500-2000 ℃ for 2-5 min to obtain treated titanium pentoxide crystal particles;
(3) placing the titanium pentoxide crystal particles on the surface of an indium sheet, and tabletting, wherein the pressure of tabletting is 2-8 MPa, and the time of tabletting is 1.5-3 s to obtain a sample to be detected;
the step (1) and the step (2) have no sequence.
In order to avoid introducing pollution, the sample preparation process of the present invention may be further preferably performed in a fume hood, and the water is preferably deionized water or pure water.
In a second aspect, the invention provides a method for testing the trititanium pentoxide crystal particles in the glow discharge mass spectrum, wherein the method for testing the trititanium pentoxide crystal particles in the glow discharge mass spectrum adopts the method for preparing the sample of the trititanium pentoxide crystal particles in the glow discharge mass spectrum.
Preferably, the test method comprises: and placing a sample to be tested in a sample chamber, vacuumizing, cooling, and then carrying out sputtering test to obtain impurity data in the titanium pentoxide crystal particles.
Preferably, the cooling time is 8 to 12min, for example, 8min, 8.5min, 8.9min, 9.4min, 9.8min, 10.3min, 10.7min, 11.2min, 11.6min or 12min, but not limited to the values listed, and other values not listed in this range are also applicable.
Preferably, the voltage of the sputtering test is 1.0 to 2.0kV, and may be, for example, 1.0kV, 1.2kV, 1.3kV, 1.4kV, 1.5kV, 1.6kV, 1.7kV, 1.8kV, 1.9kV, or 2.0kV, but is not limited to the values listed, and other values not listed in the range are also applicable, and preferably 1.5 kV.
Preferably, the current of the sputtering test is 1.0 to 3.0mA, and may be, for example, 1.0mA, 1.3mA, 1.5mA, 1.7mA, 1.9mA, 2.0mA, 2.2mA, 2.4mA, 2.6mA, 2.8mA, or 3.0mA, but is not limited to the values listed, and other values not listed in the range are also applicable, and preferably 2.0 mA.
Preferably, the resolution of the sputtering test is 3400 to 4000, and may be 3400, 3460, 3530, 3600, 3660, 37340, 3800, 3860, 3930 or 4000, for example, but is not limited to the values listed, and other values not listed in the range are also applicable.
The invention preferably selects the parameters of the test, and has better test accuracy for the titanium pentoxide sample.
The type of the glow discharge mass spectrometer is not particularly limited, and any instrument which can be used for glow discharge mass spectrometry detection and is well known to those skilled in the art can be adopted, such as NuAstrum, ElementGD or VG9000, and the like, wherein NuAstrum and VG9000 are preferred, and the minimum temperature of the NuAstrum and the VG9000 can reach-180 ℃ through liquid nitrogen refrigeration, and are more suitable for the trititanium pentoxide crystal particles of the application.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) the sample preparation method of the titanium pentoxide crystal particles in the glow discharge mass spectrum can ensure that pollution is not introduced as much as possible in the sample preparation process, so that the analysis of impurity elements of the titanium pentoxide crystal particles is successfully carried out, the analysis time is within 75min, the accuracy of data is ensured, and the maximum relative error after the sample preparation method is repeated for five times is within 5.6%;
(2) according to the sample preparation method of the trititanium pentoxide crystal particles in the glow discharge mass spectrum, different washing methods are adopted for the indium sheet and the trititanium pentoxide particles, and a better washing effect is achieved for the characteristics of the indium sheet and the trititanium pentoxide particles;
(3) the method for testing the trititanium pentoxide crystal particles in the glow discharge mass spectrum has better test accuracy by selecting specific process parameters.
Drawings
FIG. 1 is a graph of test data for samples made in example 1 of the present invention.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
First, an embodiment
Example 1
The embodiment provides a sample preparation method of trititanium pentoxide crystal particles in glow discharge mass spectrometry, which comprises the following steps:
(1) putting a round indium sheet with the purity of 99.9995 wt% into a polytetrafluoroethylene cup, pickling for 3min by nitric acid with the purity of 15 wt%, washing for three times by first water, wherein the first water is rinsing, adding absolute ethyl alcohol for first ethanol washing, the first ethanol washing is alcohol rinsing, and then drying for the first time by blow drying to obtain a processed indium sheet;
(2) placing titanium pentoxide crystal particles with the particle size of 1-3 mm and the evaporation temperature of 1650 ℃ into a polytetrafluoroethylene cup, adding an absolute ethyl alcohol solution, performing ultrasonic treatment for 3min, performing third washing with water, rinsing with water, pouring absolute ethyl alcohol for third alcohol washing, rinsing with alcohol, placing the titanium pentoxide crystal particles on filter paper, and drying with a baking lamp to obtain treated titanium pentoxide crystal particles;
(3) clamping the titanium pentoxide crystal particles obtained in the step (2) on the surface of an indium sheet by using a pair of tweezers, then placing the indium sheet in a polytetrafluoroethylene grinding tool, and tabletting by using a press machine, wherein the pressure of tabletting is 5MPa, and the tabletting time is 2s, so as to obtain a sample to be detected;
the step (1) and the step (2) have no sequence.
The embodiment also provides a method for testing the trititanium pentoxide crystal particles in glow discharge mass spectrometry, which comprises the following steps: fixing a sample to be tested by using a sample clamp, placing the sample in a sample chamber, vacuumizing and pushing the sample into a discharge chamber, after refrigerating for 10min, setting the voltage to be 1.5kV and the current to be 2.0mA, properly adjusting the resolution of the instrument to be about 3500, carrying out sputtering test, and measuring the impurity data in the titanium pentoxide crystal particles.
The data chart of the test of this embodiment is shown in fig. 1, and it can be seen from fig. 1 that the instrument is completely stable at about 60min, and the data of the analysis test can be obtained, and the maximum relative error is 3.2% after five times of repetition.
Example 2
The embodiment provides a sample preparation method of trititanium pentoxide crystal particles in glow discharge mass spectrometry, which comprises the following steps:
(1) putting a round indium sheet with the purity of 99.999 wt% into a polytetrafluoroethylene cup, carrying out acid washing for 5min by using 10 wt% nitric acid, carrying out first washing for four times, wherein the first washing is rinsing, adding absolute ethyl alcohol for first ethyl alcohol washing, carrying out first ethyl alcohol washing by using alcohol rinsing, and carrying out blow-drying for first drying to obtain a processed indium sheet;
(2) putting the trititanium pentoxide crystal particles with the particle size of 1-2 mm and the evaporation temperature of 1500 ℃ into a polytetrafluoroethylene cup, adding an absolute ethyl alcohol solution, performing ultrasonic treatment for 2min, performing third washing with water for the second time, wherein the second washing is rinsing, then pouring absolute ethyl alcohol for the third alcohol washing, wherein the third alcohol washing is alcohol rinsing, and then putting the trititanium pentoxide crystal particles on filter paper and drying by using a baking lamp to obtain the treated trititanium pentoxide crystal particles;
(3) clamping the titanium pentoxide crystal particles obtained in the step (2) on the surface of an indium sheet by using a pair of tweezers, then placing the indium sheet in a polytetrafluoroethylene grinding tool, and tabletting by using a press machine, wherein the pressure of tabletting is 8MPa, and the tabletting time is 3s, so as to obtain a sample to be detected;
the step (1) and the step (2) have no sequence.
The embodiment also provides a method for testing the trititanium pentoxide crystal particles in glow discharge mass spectrometry, which comprises the following steps: fixing a sample to be tested by using a sample clamp, placing the sample in a sample chamber, vacuumizing and pushing the sample into a discharge chamber, setting the voltage to be 2.0kV and the current to be 1.0mA after refrigerating for 12min, properly adjusting the resolution of the instrument to be about 3400, carrying out sputtering test, and measuring the impurity data in the titanium pentoxide crystal particles.
The analysis time of the test of the embodiment is about 61min, the instrument is completely stable, the data of the analysis test can be obtained, and the maximum relative error after five times of repetition is 2.8%.
Example 3
The embodiment provides a sample preparation method of trititanium pentoxide crystal particles in glow discharge mass spectrometry, which comprises the following steps:
(1) putting a round indium sheet with the purity of 99.9998 wt% into a polytetrafluoroethylene cup, pickling with nitric acid with the purity of 25 wt% for 2min, and carrying out first washing with water for three times, wherein the first washing is rinsing, then adding absolute ethyl alcohol for first ethyl alcohol washing, the first ethyl alcohol washing is alcohol rinsing, and then carrying out blow-drying for first drying to obtain a processed indium sheet;
(2) placing the titanium pentoxide crystal particles with the particle size of 1.5-3 mm and the evaporation temperature of 2000 ℃ into a polytetrafluoroethylene cup, adding an absolute ethyl alcohol solution, performing ultrasonic treatment for 5min, then performing secondary washing for 5 times, wherein the secondary washing is rinsing, then pouring absolute ethyl alcohol for performing tertiary alcohol washing, wherein the tertiary alcohol washing is alcohol rinsing, and then placing the titanium pentoxide crystal particles on filter paper and drying by using a baking lamp to obtain treated titanium pentoxide crystal particles;
(3) clamping the titanium pentoxide crystal particles obtained in the step (2) on the surface of an indium sheet by using a pair of tweezers, then placing the indium sheet in a polytetrafluoroethylene grinding tool, and tabletting by using a press machine, wherein the pressure of tabletting is 2MPa, and the tabletting time is 1.5s, so as to obtain a sample to be detected;
the step (1) and the step (2) have no sequence.
The embodiment also provides a method for testing the trititanium pentoxide crystal particles in glow discharge mass spectrometry, which comprises the following steps: fixing a sample to be tested by using a sample clamp, placing the sample in a sample chamber, vacuumizing and pushing the sample into a discharge chamber, setting the voltage to be 1.0kV and the current to be 3.0mA after refrigerating for 8min, properly adjusting the resolution of the instrument to be about 3900, and carrying out sputtering test to obtain impurity data in the titanium pentoxide crystal particles.
The analysis time of the test of the embodiment is about 55min, the instrument is completely stable, the data of the analysis test can be obtained, and the maximum relative error after five times of repetition is 4.0%.
Example 4
This example provides a sample preparation method of trititanium pentoxide crystal particles in glow discharge mass spectrometry, which is the same as in example 1 except that the concentration of nitric acid in step (1) is 2 wt%.
The analysis time of the test of the embodiment is about 70min, the instrument is completely stable, the data of the analysis test can be obtained, and the maximum relative error after five times of repetition is 5.4%.
Example 5
This example provides a sample preparation method of trititanium pentoxide crystal particles in glow discharge mass spectrometry, which is the same as in example 1 except that the concentration of nitric acid in step (1) is 30 wt%.
The analysis time of the test of the embodiment is about 55min, the instrument is completely stable, the data of the analysis test can be obtained, and the maximum relative error after five times of repetition is 3.4%.
Example 6
This example provides a method for testing trititanium pentoxide crystal particles in glow discharge mass spectrometry, which is the same as in example 1 except that the refrigeration time is 5 min.
The analysis time of the test of the embodiment is about 75min, the instrument is completely stable, the data of the analysis test can be obtained, and the maximum relative error after five times of repetition is 5.6%.
Example 7
This example provides a method for testing the crystal particles of trititanium pentoxide in glow discharge mass spectrometry, which is the same as in example 1 except that the refrigeration time is 16 min.
The analysis time of the test of the embodiment is about 68min, the instrument is completely stable, the data of the analysis test can be obtained, and the maximum relative error after five times of repetition is 4.9%.
Second, comparative example
Comparative example 1
The comparative example provides a sample preparation method of trititanium pentoxide crystal particles in glow discharge mass spectrometry, which is the same as in example 1 except that the step (1) is not subjected to acid washing.
The analysis time of the comparative example test is about 120min, the instrument is completely stable, the data of the analysis test can be obtained, and the maximum relative error after five times of repetition is 12.3%.
Comparative example 2
The comparative example provides a sample preparation method of trititanium pentoxide crystal particles in glow discharge mass spectrometry, which is the same as in example 1 except that the step (1) replaces acid washing with absolute ethyl alcohol washing.
The analysis time of the comparative example test is about 110min, the instrument is completely stable, the data of the analysis test can be obtained, and the maximum relative error after five times of repetition is 13.5%.
Comparative example 3
This comparative example provides a sample preparation method of trititanium pentoxide crystal particles in glow discharge mass spectrometry, which is the same as in example 1 except that the second ethanol washing is not performed in step (2).
The analysis time of the comparative example test is about 125min, the instrument is completely stable, the data of the analysis test can be obtained, and the maximum relative error after five times of repetition is 14.8%.
Comparative example 4
This comparative example provides a sample preparation method for trititanium pentoxide crystal particles in glow discharge mass spectrometry, which is the same as in example 1 except that in step (2), the second ethanol washing is replaced with the same acid washing as in step (1).
The analysis time of the comparative example test is about 109min, the instrument is completely stable, the data of the analysis test can be obtained, and the maximum relative error after five times of repetition is 16.4%.
In conclusion, the sample preparation method provided by the invention avoids the introduction of impurities as much as possible, so that the analysis time is shortened, the analysis time is within 75min, the accuracy of data is ensured, and the maximum relative error after five times of repetition is within 5.6%; the test method can obtain stronger signals through specific test parameters and has high sensitivity.
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A sample preparation method of trititanium pentoxide crystal particles in glow discharge mass spectrometry is characterized by comprising the following steps:
(1) carrying out acid washing, first water washing, first ethanol washing and first drying on the indium sheet in sequence to obtain a processed indium sheet;
(2) sequentially carrying out second ethanol washing, second water washing, third ethanol washing and second drying on the titanium pentoxide crystal particles to obtain treated titanium pentoxide crystal particles;
(3) placing the titanium pentoxide crystal particles on the surface of an indium sheet, and tabletting to obtain a sample to be detected;
the step (1) and the step (2) have no sequence.
2. A sample preparation method as claimed in claim 1, wherein in step (1) said indium flakes are high purity indium flakes;
preferably, the purity of the high-purity indium sheet is more than or equal to 99.999 wt%.
3. The sample preparation method according to claim 1 or 2, wherein the acid to be pickled in step (1) is nitric acid;
preferably, the concentration of the nitric acid is 10-25 wt%;
preferably, the acid washing time in the step (1) is 2-5 min.
4. The sample preparation method according to any one of claims 1 to 3, wherein the number of times of the first water washing in step (1) is at least three;
preferably, the number of the first ethanol washing is at least one.
5. A sample preparation method as claimed in any one of claims 1 to 4, wherein the average particle diameter of the crystal particles of the trititanium pentoxide in step (2) is 1 to 3 mm;
preferably, the evaporation temperature of the titanium pentoxide crystal particles is 1500-2000 ℃.
6. The sample preparation method according to any one of claims 1 to 5, wherein the second ethanol washing in step (2) is performed under ultrasonic conditions;
preferably, the time of the second ethanol washing is 2-5 min;
preferably, the number of times of the second water washing is at least three.
7. The sample preparation method according to any one of claims 1 to 6, wherein the pressure of the pellet in the step (3) is 2 to 8 MPa;
preferably, the tabletting time is 1.5-3 s.
8. A method for testing the trititanium pentoxide crystal particles in glow discharge mass spectrometry is characterized in that the method for testing the trititanium pentoxide crystal particles in glow discharge mass spectrometry is used for sample preparation according to any one of claims 1-7.
9. The testing method of claim 8, wherein the testing method comprises: and placing a sample to be tested in a sample chamber, vacuumizing, cooling, and then carrying out sputtering test to obtain impurity data in the titanium pentoxide crystal particles.
10. The test method according to claim 8 or 9, wherein the refrigeration time is 8-12 min;
preferably, the voltage of the sputtering test is 1.0-2.0 kV;
preferably, the current of the sputtering test is 1.0-3.0 mA;
preferably, the resolution of the sputtering test is 3400-4000.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102175754A (en) * | 2010-12-27 | 2011-09-07 | 中国科学院上海硅酸盐研究所 | New method for analyzing non-conductor material by utilizing glow discharge mass spectrum |
| US20170269004A1 (en) * | 2016-03-18 | 2017-09-21 | Hemlock Semiconductor Corporation | Low impurity detection method for characterizing metals within a surface and sub-surface of polycrystalline silicon |
| CN108918226A (en) * | 2018-07-23 | 2018-11-30 | 江苏隆达超合金航材有限公司 | A kind of preparation method of the titanium sponge detected for GDMS and titanium grain specimens |
| CN109239179A (en) * | 2018-08-27 | 2019-01-18 | 新疆众和股份有限公司 | The measuring method of trace impurity in a kind of high purity aluminium oxide polycrystal material |
| CN109502639A (en) * | 2018-12-13 | 2019-03-22 | 宁波新福钛白粉有限公司 | A method of preparing the compound mixed crystal powder of titanium dioxide and titanium pentoxide |
| CN111537320A (en) * | 2020-05-15 | 2020-08-14 | 宁波锦越新材料有限公司 | Sample preparation method for GDMS detection and sample |
| CN111896665A (en) * | 2020-07-30 | 2020-11-06 | 宁波创润新材料有限公司 | Preparation method of high-purity electrolytic manganese sample for GDMS detection and impurity analysis method of high-purity electrolytic manganese sample |
-
2021
- 2021-04-22 CN CN202110436847.4A patent/CN113109121A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102175754A (en) * | 2010-12-27 | 2011-09-07 | 中国科学院上海硅酸盐研究所 | New method for analyzing non-conductor material by utilizing glow discharge mass spectrum |
| US20170269004A1 (en) * | 2016-03-18 | 2017-09-21 | Hemlock Semiconductor Corporation | Low impurity detection method for characterizing metals within a surface and sub-surface of polycrystalline silicon |
| CN108918226A (en) * | 2018-07-23 | 2018-11-30 | 江苏隆达超合金航材有限公司 | A kind of preparation method of the titanium sponge detected for GDMS and titanium grain specimens |
| CN109239179A (en) * | 2018-08-27 | 2019-01-18 | 新疆众和股份有限公司 | The measuring method of trace impurity in a kind of high purity aluminium oxide polycrystal material |
| CN109502639A (en) * | 2018-12-13 | 2019-03-22 | 宁波新福钛白粉有限公司 | A method of preparing the compound mixed crystal powder of titanium dioxide and titanium pentoxide |
| CN111537320A (en) * | 2020-05-15 | 2020-08-14 | 宁波锦越新材料有限公司 | Sample preparation method for GDMS detection and sample |
| CN111896665A (en) * | 2020-07-30 | 2020-11-06 | 宁波创润新材料有限公司 | Preparation method of high-purity electrolytic manganese sample for GDMS detection and impurity analysis method of high-purity electrolytic manganese sample |
Non-Patent Citations (2)
| Title |
|---|
| 侯艳霞等: "辉光放电质谱法测定纯锡中２４种杂质元素和锡记忆效应的消除", 《理化检验-化学分册》 * |
| 侯艳霞等: "辉光放电质谱法测定纯锡中２４种杂质元素和锡记忆效应的消除", 《理化检验-化学分册》, 31 December 2020 (2020-12-31), pages 315 - 319 * |
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