CN110864949A - Preparation method of tungsten block sample for glow discharge mass spectrometry detection - Google Patents
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/286—Preparing 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
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- 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
- G01N1/286—Preparing 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
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Abstract
The invention relates to a preparation method of a tungsten block sample for glow discharge mass spectrometry detection, which comprises the following steps: cutting the tungsten bar column, polishing, cleaning the tungsten bar column by an organic reagent, embedding the tungsten bar column, roughly grinding the tungsten block, finely grinding the tungsten bar column, soaking and washing by acid liquor, washing by deionized water, cleaning by the organic reagent and drying by blowing. The invention solves the problem that the size of the slender tungsten bar is not suitable for glow discharge mass spectrometry detection and analysis, and the common metallographic mosaic powder replaces the conductive metallographic mosaic powder with relatively higher price, thereby reducing the detection cost.
Description
Technical Field
The invention relates to a preparation method of a tungsten block sample for glow discharge mass spectrometry detection, and belongs to the technical field of metal element analysis and test.
Background
Tungsten is a rare metal and an important strategic resource, and is widely applied to the fields of steel industry, tungsten carbide-based hard alloy, heat-intensity and wear-resistant alloy, electric vacuum lighting materials and the like. The tungsten strip is the most common industrial raw material form of tungsten, and is prepared by processing tungsten ore through multiple processes such as excavation, grinding, water reselection, refining and the like to prepare tungsten powder with the purity of over 95 percent, and then performing pressing, sintering and hammer melting production. The prospect of tungsten is wide, and detection and analysis of tungsten are crucial in China as the first tungsten-producing big country in the world.
There are many documents on methods for measuring impurity elements in tungsten, such as national standard methods GB/T4324 and GB/T26496. The method is single element analysis, has long detection and analysis period, is complicated and time-consuming in a sample treatment process, and needs strong acid, an oxidation-reduction agent, a color-developing agent, a complexing agent and the like.
Glow Discharge Mass Spectrometry (GDMS), a direct analysis technique of solid samples, has a very low limit of element detection, and can analyze more than 70 elements in a short time. The method is widely applied to the analysis of trace and ultra-trace impurity elements of materials such as high-purity metals, semiconductors and the like, but has a plurality of difficulties in analyzing small-size and irregular-shape material samples. U.S. Thermo Fisher Scientific, Element GD rapid entry manual, mentions that smaller samples can be pressed into In blocks for analysis, but this method is abandoned given that In is an expensive, dilute metal and is used very infrequently In most laboratories. According to the regulations of GB/T3459-2006, the tungsten bars are divided into tungsten square bars and tungsten round bars according to different shapes, the width of the tungsten square bars is 10-16 mm, and the height of the tungsten round bars is 10-16 mm; the latter has a diameter of 16 to 30 mm. The glow discharge mass spectrometer of Thermo Fisher Scientific, usa, has a sample holder with a pore size of 18mm and an excitation range of 10mm in diameter. When the size of the tungsten bar is smaller than the aperture of the sample clamp, the sample cannot be fixed and cannot be analyzed. Therefore, sample preparation methods suitable for detecting different samples need to be developed to meet the requirements of glow discharge mass spectrometry.
In the traditional observation of metallographic phase, some materials are limited by the shape and size of the materials, and the samples cannot be directly prepared. At the moment, a hot-pressing embedding method is adopted, and the material is embedded by a metallographic phase sample embedding machine to obtain a sample block with a proper size, so that the sample is conveniently prepared, and the aim of observing the metallographic phase is fulfilled. Sample preparation referenced to GDMS is hereby incorporated by reference. The mosaic powder used for embedding samples in the market is various in variety, including non-conductive type and conductive type. The price of the conductive metallographic mosaic powder is about 5 times that of the non-conductive metallographic mosaic powder, and in consideration of sample preparation cost, if a simple method which can prepare a sample suitable for GDMS analysis by using the non-conductive metallographic mosaic powder can be developed, the method has important significance for laboratories.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the preparation method of the tungsten block sample for glow discharge mass spectrometry detection, which has the advantages of few steps, convenience in operation and capability of reducing the detection cost.
According to the technical scheme provided by the invention, the preparation method of the tungsten block sample for glow discharge mass spectrometry detection comprises the following steps:
firstly, selecting a tungsten bar, fixing the tungsten bar on a cutting machine, and cutting to obtain the tungsten bar with the upper end surface and the lower end surface both being planes;
secondly, respectively polishing the upper end surface and the lower end surface of the tungsten bar column in the same direction through sample grinding abrasive paper in a sample grinding machine until the upper end surface and the lower end surface of the tungsten bar column are both smooth in surface and consistent in grain direction;
thirdly, cleaning the tungsten bar column by using an organic reagent to remove oil stains on the surface of the tungsten bar column;
fourthly, vertically placing the tungsten bar column at the central position in the metallographic sample embedding machine, enabling the upper end face of the tungsten bar column to be upward, enabling the lower end face of the tungsten bar column to be downward and to be attached to the sample embedding block, pouring metallographic embedding powder into the metallographic sample embedding machine and plugging, setting the heating temperature of the metallographic sample embedding machine to be 125-165 ℃, keeping the temperature for 10-20 min, embedding the sample to obtain a tungsten block, and covering the upper end face of the tungsten bar column with the solidified metallographic embedding powder;
fifthly, roughly grinding the tungsten block corresponding to the upper end surface of the tungsten bar through grinding abrasive paper in the sample grinding machine, and removing metallographic phase embedding powder until the upper end surface of the tungsten bar is exposed;
sixthly, accurately grinding the upper end surface of the tungsten bar by using a metallographic grinding and polishing machine, and removing coarse grinding marks and impurities left by grinding of a sample grinding machine;
and seventhly, soaking and washing the tungsten block with an acid solution, washing the tungsten block with deionized water, and finally washing the upper end face of the tungsten bar column with an organic reagent and drying the tungsten bar column for later use.
Preferably, the diameter of the tungsten bar selected in the first step is 10-18 mm, and the height of the tungsten bar is 5-60 mm.
Preferably, the sample abrasive paper of the second step is 40-80 mesh silicon carbide abrasive paper.
Preferably, the organic reagent in the third step is one of absolute ethyl alcohol, diethyl ether, acetone and carbon tetrachloride.
Preferably, the metallographic mosaic powder produced in the fourth step is one of HY601-H black bakelite powder 500 g/bottle, HY601-B white jade powder 500 g/bottle and HY603-T transparent plastic powder 1000 g/bottle, which are produced by Wuyi Hengyu instruments ltd.
Preferably, the sanding sandpaper in the fifth step is 80-200 meshes of zirconia sandpaper or alumina sandpaper.
Preferably, the acid solution in the seventh step is a nitric acid solution with a mass concentration of 5-20 wt%.
Preferably, the organic reagent in step seven is one of absolute ethyl alcohol, diethyl ether, acetone and carbon tetrachloride.
The invention solves the problem that the size of the slender tungsten bar is not suitable for glow discharge mass spectrometry detection and analysis, and the common metallographic mosaic powder replaces the conductive metallographic mosaic powder with relatively higher price, thereby reducing the detection cost.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
A preparation method of a tungsten block sample for glow discharge mass spectrometry detection comprises the following steps:
firstly, selecting a tungsten bar with the diameter of 14mm, fixing the tungsten bar on a cutting machine for water-cooling cutting to prevent overheating, and obtaining the tungsten bar with the upper end surface and the lower end surface both being planes and the height of 20 mm;
secondly, respectively polishing the upper end surface and the lower end surface of the tungsten bar in the same direction through 80-mesh silicon carbide abrasive paper in a sample grinding machine, wherein the rotating speed of the sample grinding machine is controlled at 2800r/min until the upper end surface and the lower end surface of the tungsten bar are both smooth in surface and consistent in grain direction;
thirdly, cleaning the tungsten bar column by using absolute ethyl alcohol, and removing oil stains on the surface of the tungsten bar column;
fourthly, vertically placing the tungsten bar column at the central position in the metallographic sample embedding machine, enabling the upper end face of the tungsten bar column to be upward, enabling the lower end face of the tungsten bar column to be downward and attaching a sample embedding block, pouring HY601-H black bakelite powder produced by Wujiang Wuyi Hengyu instruments ltd into the metallographic sample embedding machine, plugging, setting the heating temperature of the metallographic sample embedding machine to be 135 ℃ and the heat preservation time to be 18min, carrying out sample embedding to obtain a tungsten block with the diameter of 30mm, and enabling the black bakelite powder to just cover the upper end face of the tungsten bar column;
fifthly, roughly grinding the tungsten block corresponding to the upper end face of the tungsten bar through 80-mesh silicon carbide abrasive paper in a sample grinding machine, controlling the rotating speed of the sample grinding machine at 2800r/min, and removing the black bakelite powder until the upper end face of the tungsten bar is exposed;
sixthly, accurately grinding the upper end surface of the tungsten bar column on a metallographic grinding and polishing machine by using 120-mesh zirconium oxide abrasive paper, controlling the rotating speed of the metallographic grinding and polishing machine at 1200r/min, and removing coarse grinding marks and impurities left after grinding of a sample grinder;
and seventhly, dipping and washing the tungsten block by using 5 wt% nitric acid solution, washing the tungsten block by using deionized water after dipping and washing, and finally washing the upper end surface of the tungsten bar column by using absolute ethyl alcohol and drying the tungsten bar column for later use.
Feasibility test: the tungsten block sample prepared in example 1 was placed on a GDMS sample stage, and pre-sputtering was performed for 15min, and the main elements P, Fe, Al, Si, Mg, Ni, Ca, and Mo were examined, and data collection was started when the mass concentration was substantially stable, to obtain the content of each element, and compared with the measurement result by ICP-MS, to evaluate the feasibility of the present invention, and the results are shown in table 1.
TABLE 1
Example 2
A preparation method of a tungsten block sample for glow discharge mass spectrometry detection comprises the following steps:
firstly, selecting a tungsten bar with the diameter of 12mm, fixing the tungsten bar on a cutting machine for water-cooling cutting to prevent overheating, and obtaining the tungsten bar with the upper end surface and the lower end surface both being flat and the height of 26 mm;
secondly, respectively polishing the upper end surface and the lower end surface of the tungsten bar in the same direction through 60-mesh silicon carbide abrasive paper in a sample grinding machine, and controlling the rotating speed of the sample grinding machine at 2800r/min until the upper end surface and the lower end surface of the tungsten bar are both smooth in surface and consistent in grain direction;
thirdly, cleaning the tungsten bar column by using acetone to remove oil stains on the surface of the tungsten bar column;
fourthly, vertically placing the tungsten bar column at the central position in the metallographic sample embedding machine, enabling the upper end face of the tungsten bar column to be upward, enabling the lower end face of the tungsten bar column to be downward and be attached to the sample embedding block, pouring HY601-B white jade powder produced by Wujiang Wuyi Hengyu instruments ltd into the metallographic sample embedding machine, plugging, setting the heating temperature of the metallographic sample embedding machine to be 130 ℃ and the heat preservation time to be 15min, carrying out sample embedding to obtain a tungsten block with the diameter of 30mm, and enabling the white jade powder to just cover the upper end face of the tungsten bar column;
fifthly, roughly grinding the tungsten block corresponding to the upper end face of the tungsten bar through 60-mesh silicon carbide abrasive paper in a sample grinding machine, controlling the rotating speed of the sample grinding machine at 2800r/min, and removing the white corundum powder until the upper end face of the tungsten bar is exposed;
sixthly, accurately grinding the upper end surface of the tungsten bar column on a metallographic grinding and polishing machine by using 120-mesh alumina abrasive paper, controlling the rotating speed of the metallographic grinding and polishing machine at 1200r/min, and removing coarse grinding marks and impurities left after grinding by a sample grinder;
and seventhly, dipping and washing the tungsten block by using 10 wt% nitric acid solution, washing the tungsten block by using deionized water, and finally washing the upper end surface of the tungsten bar column by using acetone and drying the tungsten bar column for later use.
Feasibility test: the tungsten block sample prepared in example 2 was placed on a GDMS sample stage, and pre-sputtering was performed for 15min, and the main elements P, Fe, Al, Si, Mg, Ni, Ca, and Mo were examined, and data collection was started when the mass concentration was substantially stable, to obtain the content of each element, and compared with the measurement result by ICP-MS, to evaluate the feasibility of the present invention, and the results are shown in table 2.
TABLE 2
Example 3
A preparation method of a tungsten block sample for glow discharge mass spectrometry detection comprises the following steps:
firstly, selecting a tungsten bar with the diameter of 16mm, fixing the tungsten bar on a cutting machine for water-cooling cutting to prevent overheating, and obtaining the tungsten bar with the upper end surface and the lower end surface both being flat and the height of 15 mm;
secondly, respectively polishing the upper end surface and the lower end surface of the tungsten bar in the same direction through 40-mesh silicon carbide abrasive paper in a sample grinding machine, and controlling the rotating speed of the sample grinding machine at 2800r/min until the upper end surface and the lower end surface of the tungsten bar are both smooth in surface and consistent in grain direction;
thirdly, cleaning the tungsten bar column by using carbon tetrachloride to remove oil stains on the surface of the tungsten bar column;
fourthly, vertically placing the tungsten bar column at the central position in the metallographic sample embedding machine, enabling the upper end face of the tungsten bar column to be upward, enabling the lower end face of the tungsten bar column to be downward and attaching the sample embedding block, pouring HY603-T transparent plastic powder produced by Wujiang Wuyi Hengyu instruments ltd into the metallographic sample embedding machine, plugging, setting the heating temperature of the metallographic sample embedding machine to be 125 ℃ and the heat preservation time to be 12min, carrying out sample embedding to obtain a tungsten block with the diameter of 30mm, and enabling the transparent plastic powder to just cover the upper end face of the tungsten bar column;
fifthly, roughly grinding the tungsten block corresponding to the upper end face of the tungsten bar through 40-mesh silicon carbide abrasive paper in a sample grinding machine, controlling the rotating speed of the sample grinding machine at 2800r/min, and removing transparent plastic powder until the upper end face of the tungsten bar is exposed;
sixthly, performing fine grinding on the upper end surface of the tungsten bar column on a metallographic grinding and polishing machine by using 200-mesh alumina abrasive paper, controlling the rotating speed of the metallographic grinding and polishing machine at 1200r/min, and removing coarse grinding marks and impurities left after grinding by a sample grinder;
and seventhly, soaking and washing the tungsten block by using a 5 wt% nitric acid solution, washing the tungsten block by using deionized water, and finally washing the upper end surface of the tungsten bar column by using carbon tetrachloride and drying the tungsten bar column for later use.
Feasibility test: the tungsten block sample prepared in example 3 was placed on a GDMS sample stage, and pre-sputtering was performed for 15min, and the main elements P, Fe, Al, Si, Mg, Ni, Ca, and Mo were examined, and data collection was started when the mass concentration was substantially stable, to obtain the content of each element, and compared with the measurement result by ICP-MS, to thereby evaluate the feasibility of the present invention, and the results are shown in table 3.
TABLE 3
The test results of GDMS (glow discharge mass spectrometry) are used for verifying the sample preparation method, and the data results in tables 1, 2 and 3 show that the measured value of the glow mass spectrometer is basically consistent with the test result of the inductively coupled plasma mass spectrometer, and the metallographic mosaic powder is used for not influencing the sample, thereby being beneficial to popularization and application.
The above-described embodiments are merely illustrative of specific embodiments of the present invention, and therefore should not be construed as limiting the scope of the invention. Any modifications of the present invention which would occur to those skilled in the art and which are within the spirit of the invention are considered to be within the scope of the present invention.
Claims (8)
1. A preparation method of a tungsten block sample for glow discharge mass spectrometry detection is characterized by comprising the following steps:
firstly, selecting a tungsten bar, fixing the tungsten bar on a cutting machine, and cutting to obtain the tungsten bar with the upper end surface and the lower end surface both being planes;
secondly, respectively polishing the upper end surface and the lower end surface of the tungsten bar column in the same direction through sample grinding abrasive paper in a sample grinding machine until the upper end surface and the lower end surface of the tungsten bar column are both smooth in surface and consistent in grain direction;
thirdly, cleaning the tungsten bar column by using an organic reagent to remove oil stains on the surface of the tungsten bar column;
fourthly, vertically placing the tungsten bar column at the central position in the metallographic sample embedding machine, enabling the upper end face of the tungsten bar column to be upward, enabling the lower end face of the tungsten bar column to be downward and to be attached to the sample embedding block, pouring metallographic embedding powder into the metallographic sample embedding machine and plugging, setting the heating temperature of the metallographic sample embedding machine to be 125-165 ℃, keeping the temperature for 10-20 min, embedding the sample to obtain a tungsten block, and covering the upper end face of the tungsten bar column with the solidified metallographic embedding powder;
fifthly, roughly grinding the tungsten block corresponding to the upper end surface of the tungsten bar through grinding abrasive paper in the sample grinding machine, and removing metallographic phase embedding powder until the upper end surface of the tungsten bar is exposed;
sixthly, accurately grinding the upper end surface of the tungsten bar by using a metallographic grinding and polishing machine, and removing coarse grinding marks and impurities left by grinding of a sample grinding machine;
and seventhly, soaking and washing the tungsten block with an acid solution, washing the tungsten block with deionized water, and finally washing the upper end face of the tungsten bar column with an organic reagent and drying the tungsten bar column for later use.
2. The method of claim 1, wherein the tungsten sample is prepared by a method comprising the following steps: the diameter of the tungsten bar selected in the first step is 10-18 mm, and the height after cutting is 5-60 mm.
3. The method of claim 1, wherein the tungsten sample is prepared by a method comprising the following steps: and the sample abrasive paper of the second step is 40-80-mesh silicon carbide abrasive paper.
4. The method of claim 1, wherein the tungsten sample is prepared by a method comprising the following steps: and the organic reagent in the third step is one of absolute ethyl alcohol, ether, acetone and carbon tetrachloride.
5. The method of claim 1, wherein the tungsten sample is prepared by a method comprising the following steps: and step four, the metallographic phase embedding powder is one of black bakelite powder, white jade powder and transparent plastic powder.
6. The method of claim 1, wherein the tungsten sample is prepared by a method comprising the following steps: and fifthly, the polishing abrasive paper is 80-200 meshes of zirconia abrasive paper or alumina abrasive paper.
7. The method of claim 1, wherein the tungsten sample is prepared by a method comprising the following steps: and the acid solution in the seventh step is a nitric acid solution with the mass concentration of 5-20 wt%.
8. The method of claim 1, wherein the tungsten sample is prepared by a method comprising the following steps: and the organic reagent in the step seven is one of absolute ethyl alcohol, diethyl ether, acetone and carbon tetrachloride.
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Application publication date: 20200306 |