CN114659865A - Method for measuring chemical components of microcrystalline boron glass - Google Patents
Method for measuring chemical components of microcrystalline boron glass Download PDFInfo
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- 239000011521 glass Substances 0.000 title claims abstract description 117
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 105
- 238000000034 method Methods 0.000 title claims abstract description 56
- 239000000126 substance Substances 0.000 title claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims abstract description 45
- 229930195725 Mannitol Natural products 0.000 claims abstract description 45
- 239000000594 mannitol Substances 0.000 claims abstract description 45
- 235000010355 mannitol Nutrition 0.000 claims abstract description 45
- 239000000843 powder Substances 0.000 claims abstract description 43
- 239000000243 solution Substances 0.000 claims abstract description 39
- 238000012360 testing method Methods 0.000 claims abstract description 25
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 44
- 239000000203 mixture Substances 0.000 claims description 38
- 238000004458 analytical method Methods 0.000 claims description 25
- 239000012086 standard solution Substances 0.000 claims description 24
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 20
- 229910017604 nitric acid Inorganic materials 0.000 claims description 20
- 238000000227 grinding Methods 0.000 claims description 19
- 238000001704 evaporation Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 239000000523 sample Substances 0.000 abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 15
- 239000012488 sample solution Substances 0.000 abstract description 9
- 230000029087 digestion Effects 0.000 abstract description 6
- 238000005259 measurement Methods 0.000 abstract description 6
- 239000000377 silicon dioxide Substances 0.000 abstract description 5
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- YWCYJWYNSHTONE-UHFFFAOYSA-O oxido(oxonio)boron Chemical compound [OH2+][B][O-] YWCYJWYNSHTONE-UHFFFAOYSA-O 0.000 abstract description 2
- 239000012085 test solution Substances 0.000 abstract description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 14
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 12
- 239000002253 acid Substances 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 229910052697 platinum Inorganic materials 0.000 description 7
- 229910052810 boron oxide Inorganic materials 0.000 description 5
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 4
- 239000004576 sand Substances 0.000 description 4
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- 238000002479 acid--base titration Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 238000010668 complexation reaction Methods 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 229910004014 SiF4 Inorganic materials 0.000 description 1
- 229910020439 SiO2+4HF Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000002133 sample digestion Methods 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
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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
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The invention discloses a method for measuring chemical components of microcrystalline boron glass, belongs to the technical field of chemical measurement of microcrystalline boron glass, and solves the technical problem that the boron content in a measured glass sample test solution is far lower than the actual boron content in glass when the components of the traditional microcrystalline boron glass are accurately measured. According to the method for determining the chemical components of the microcrystalline boron glass, mannitol is added in the initial digestion process of microcrystalline boron glass powder, so that boron and mannitol in a solution form a hydroxyl complex, volatilization of the boron is inhibited, and then digestion is carried out under the condition of water bath low temperature. When the chemical components of the microcrystalline boron glass are tested, a sample solution for testing the boron dioxide in the microcrystalline boron glass does not need to be prepared separately except for the main content of non-silicon dioxide.
Description
Technical Field
The invention belongs to the technical field of chemical determination of microcrystalline boron glass, and particularly relates to a method for determining chemical components of microcrystalline boron glass.
Background
The microcrystalline boron glass consists of a glass phase and a crystal phase, the glass properties of the crystal phase and the crystal grain have different sizes, the microcrystalline glass containing boron has excellent physical properties and better water resistance and acid and alkali resistance, and is widely applied to a plurality of fields of food, medicine, electronic display and the like. With the information technology approaching the 6G era, glass and ceramic gradually replace metal and plastic due to the fact that the glass and ceramic meet the electromagnetic performance requirements of 6G signals, are attractive and have good texture, and become the first-choice protective cover plate of the mobile terminal. The microcrystalline boron glass has the advantages of both microcrystalline glass and boron glass, has excellent mechanical, thermal and photoelectric properties, and represents the development direction of cover plate glass in the 6G era. Due to the rapid development of the mobile terminal cover plate material, the formula of the microcrystalline glass is diversified, and the precision and the speed of the chemical component test are higher in the research, development and inspection test processes.
When the conventional microcrystalline boron glass composition is precisely measured (solution method), the preparation of a measurement sample solution used and the measurement analysis generally require the following steps:
step 1: milling glass powder; step 2: preparing mixed acid of hydrofluoric acid and perchloric acid, and repeatedly dissolving and evaporating to dryness by combining a high-temperature sand bath; and step 3: dissolving with nitric acid; and 4, step 4: the volumetric flask has constant volume to be measured; and 5: and testing the result. The principle of the traditional method in the process of digesting the glass powder in the test process is as follows:
SiO2+4HF＝2H2O+SiF4↑；
the silicon dioxide reacts with hydrofluoric acid to produce colorless gas silicon tetrafluoride which is then volatilized at high temperature during which time B2O3Boric acid is formed and volatilized at high temperature of the sand bath, so that B in the microcrystalline boron glass is generated2O3The test content is low or none; in addition, in addition to the test process, the content of boron trioxide in the microcrystalline boron glass needs to be tested by adopting high-temperature alkali fusion → acid pickling dissolution → mannitol complexation → acid-base titration independently; multiple operation steps, inaccurate measurement result and inapplicability to boron-containing microcrystalline glassAnd (4) accurately measuring.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a method for determining chemical components of microcrystalline boron glass, which is used for solving the technical problems that a sample solution needs to be prepared and determined for many times, the component result is not accurate in comparison and the like when the component of microcrystalline boron glass is determined by the traditional method.
The method is used for solving the technical problem that the boron content in the measured glass sample test solution is far lower than the actual boron content in the glass when the components of the traditional microcrystalline boron glass are accurately measured.
The traditional measurement method is not used for obtaining data by one-time measurement, and is used for obtaining the content of other elements except the main content (SiO2) of the glass component by times. The invention solves the defects of the test and can obtain the contents of all elements except the main content (SiO2) of the glass at one time.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention discloses a method for measuring chemical components of microcrystalline boron glass, which comprises the following steps:
step 1: firstly, uniformly mixing microcrystalline boron glass powder and mannitol to obtain a mixture; adding water to the mixture until the mixture is completely soaked; then adding hydrofluoric acid, performing water bath treatment, and repeatedly evaporating until the microcrystalline boron glass powder is completely dissolved and the hydrofluoric acid is completely evaporated; finally, adding nitric acid and water, carrying out water bath constant-temperature solution and constant volume to obtain a solution to be detected;
and 2, step: and testing the components in the standard solution by using an analyzer, drawing a working curve, analyzing the solution to be tested by using the analyzer in the same method for drawing the working curve to obtain analysis data, and comparing and calculating the analysis data and the working curve to obtain the specific content of the components in the solution to be tested.
Further, in the step 1, the dosage ratio of the microcrystalline boron glass powder to the mannitol is (1: 0.5): (1:2).
Further, in the step 1, the temperature of the water bath treatment is 80-100 ℃.
Further, in step 1, the amount ratio of the nitric acid to the water is (1: 0.5) to (1: 5).
Further, in step 2, the standard solution includes mannitol, and the concentration of mannitol in the standard solution is consistent with that of mannitol in the solution to be tested.
Further, the concentration of the solution to be detected is consistent with that of mannitol in the standard solution.
Further, in the step 1, the microcrystalline boron glass powder is prepared by grinding massive microcrystalline boron glass by a grinding machine, wherein the grinding time is 10-30 min.
Further, the analytical instrument comprises an atomic absorption spectrometer and a plasma spectrometer.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a method for determining chemical components of microcrystalline boron glass, which is characterized in that mannitol is added in the initial digestion process of microcrystalline boron glass powder, so that boron and mannitol in a solution form a hydroxyl complex, the volatilization of the boron is inhibited, and the digestion is carried out in a water bath at a low temperature of 80-100 ℃, the temperature control is simple and accurate during the preparation of a sample solution, and the defect that the boron in the traditional method for rapidly and accurately determining the components of the microcrystalline boron glass volatilizes at a high temperature of a sand bath is avoided; meanwhile, only two kinds of acid are needed in the process of preparing the sample solution, and the using amount of the acid is greatly reduced, so that non-sample impurities introduced in the preparation process are also greatly reduced, and the quality of sample solution preparation is improved; moreover, the sample solution is prepared without adopting two different methods, so that the sample solution can be prepared at one time by measuring the chemical components of the boron-containing microcrystalline glass; the method has higher test accuracy and higher test speed than the traditional test method. When the chemical components of the microcrystalline boron glass are tested, a sample solution for testing the boron dioxide in the microcrystalline boron glass does not need to be prepared separately except for the main content of non-silicon dioxide. Therefore, the method for measuring the chemical components of the microcrystalline boron glass can measure the content of all elements except the main content (silicon oxide) at one time, has the advantages of rapid sample digestion process, simplicity, easy control, low temperature and minimum reagent variety, and is suitable for the chemical component analysis of the microcrystalline glass containing boron (which is easily volatilized by heating).
Drawings
FIG. 1 is a schematic diagram of a calibration curve prepared according to the present invention.
Detailed Description
To make the features and effects of the invention comprehensible to those skilled in the art, general description and definitions shall be provided below with respect to terms and words mentioned in the specification and claims. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
The theory or mechanism described and disclosed herein, whether correct or incorrect, should not limit the scope of the present invention in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features defined herein as numerical ranges or percentage ranges, such as values, amounts, levels and concentrations, are provided for brevity and convenience only. Accordingly, the description of numerical ranges or percentage ranges should be considered to cover and specifically disclose all possible subranges and individual numerical values (including integers and fractions) within the range.
Unless otherwise specified herein, "comprising," including, "" containing, "" having, "or the like, means" consisting of … … "and" consisting essentially of … …, "e.g.," a comprises a "means" a comprises a and the other, "and" a comprises a only.
In the present context, for the sake of brevity, all possible combinations of various features in various embodiments or examples are not described. Therefore, the respective features in the respective embodiments or examples may be arbitrarily combined as long as there is no contradiction between the combinations of the features, and all the possible combinations should be considered as the scope of the present specification.
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The following examples use instrumentation conventional in the art. Experimental procedures without specific conditions noted in the following examples, generally according to conventional conditions, or according to conditions recommended by the manufacturer. The various starting materials used in the examples which follow, unless otherwise indicated, are conventional commercial products having specifications which are conventional in the art. In the description of the present invention and the following examples, "%" represents weight percent, "parts" represents parts by weight, and proportions represent weight ratios, unless otherwise specified.
The invention discloses a method for measuring chemical components of microcrystalline boron glass, which comprises the steps of firstly, uniformly mixing microcrystalline boron glass powder and mannitol to obtain a mixture; adding water to the mixture until the mixture is completely soaked; then adding hydrofluoric acid, performing water bath treatment, and repeatedly evaporating until the microcrystalline boron glass powder is completely dissolved and the hydrofluoric acid is completely evaporated; finally, adding nitric acid and water, carrying out water bath constant-temperature clearing, and then fixing the volume to obtain a solution to be detected;
the standard solution was then tested for composition by analytical instrumentation and a working curve was plotted:
prepared by using national standard substance (meeting GBW (E)080242)100 mu m/mL: such as: glass sample composition removal (SiO)2About 60%) and approximately, 20% Al2O3，9％B2O3，9％Na2When the balance of O is 2 percent of other impurities, preparing a working curve series:
as shown in fig. 1:
working curve 1 point: 18% Al2O3+8％B2O3+8％Na2O + other + mannitol;
working curve 2 point: 20% Al2O3+9％B2O3+9％Na2O + other + mannitol;
working curve 3 point: 22% Al2O3+10％B2O3+10％Na2O + other + mannitol;
and analyzing the solution to be detected by adopting an analyzer by the same method of drawing a working curve to obtain analysis data, and comparing and calculating the analysis data and the working curve to obtain the specific content of the component of the solution to be detected.
Compared with the traditional analysis method, the method has the following same points and different points:
for example, in both methods, the analytical equipment Shimadzu ICPE-9000, a high-temperature furnace, a pH meter and the like are used, and the liquid standard substance is a substance meeting the national standard substance GBW (E) 080242; the solid reagent is (GR) reagent. After the glassware was verified by measurement, an ICP analysis process was used:
1) the process of pulverizing the glass sample into fine powder is the same.
2) The digestion process of the sample by the traditional method comprises the following steps: repeatedly dissolving the sample, HF acid and perchloric acid in sand bath, and then (1: 1) adding nitric acid and water to a constant volume to a volumetric flask for testing;
the digestion process of the sample comprises the following steps: repeatedly dissolving the sample, mannitol and HF acid in a water bath, and then (1: 1) adding nitric acid and water to a constant volume to test in a volumetric flask.
3) The ICP test procedure is the same, with the following differences:
preparing a traditional working curve: preparing a nitric acid standard liquid, 3% nitric acid and water;
the working curve preparation of the invention: preparing nitric acid standard liquid, 3% nitric acid, water and mannitol;
therefore, the finally obtained test result does not contain the content of boron element in the test result obtained by the traditional method, and the content of diboron trioxide in the microcrystalline boron glass is tested by independently adopting high-temperature alkali fusion → acid pickling dissolution → mannitol complexation → acid-base titration, so that the operation process is complex;
the test result obtained by the method of the invention can obtain the content of the boron element at one time.
4) Acquiring boron element content data in a traditional analysis method:
melting glass powder, sodium hydroxide and sodium carbonate in a high-temperature furnace, dissolving the glass powder, nitric acid and water in a water bath, and then titrating by using a PH meter, an indicator and a manual method to obtain data;
the traditional test method obtains the same element data as the method;
the traditional method needs long time, particularly manual titration data (the time is 4-6 h; within 30min of ICP), the data acquisition environment is different from other data acquisition environments, and comparative analysis cannot be directly carried out.
Example 1
A method for measuring chemical components of microcrystalline boron glass comprises the following steps:
step 1: grinding the massive microcrystalline boron glass by a grinder, setting the grinding time for 30min to obtain microcrystalline boron glass powder, and uniformly mixing 500mg of microcrystalline boron glass powder and 500mg of high-purity mannitol in a platinum pot to obtain a mixture; adding water to the mixture until the mixture is completely infiltrated; then adding hydrofluoric acid, carrying out water bath treatment at 100 ℃, and repeatedly evaporating until the microcrystalline boron glass powder is completely dissolved and the hydrofluoric acid is completely evaporated; finally, 5ml of nitric acid (1: 1) is added into every 100ml of solution, water is added, water bath is carried out for dissolving, then the volume is determined, and the solution to be measured is obtained after cooling to the room temperature;
step 2: testing components in the standard solution by using a plasma spectrometer (ICP) to obtain a 500mg sample, adjusting the standard solution to a mannitol curve with the same concentration according to glass components, namely adding 500mg mannitol to prepare, and drawing a working curve; and obtaining the analysis data of the sample, and comparing and calculating the analysis data to obtain the specific content of the components of the solution to be detected.
In the sample HW208 in the microcrystalline boron glass powder obtained by the embodiment, the content of boron oxide is 0.11%.
Example 2
A method for measuring chemical components of microcrystalline boron glass comprises the following steps:
step 1: grinding the massive microcrystalline boron glass by a grinder, setting the grinding time for 20min to obtain microcrystalline boron glass powder, and uniformly mixing 400mg of microcrystalline boron glass powder and 400mg of high-purity mannitol in a platinum pot to obtain a mixture; adding water to the mixture until the mixture is completely infiltrated; then adding hydrofluoric acid, carrying out water bath treatment at 95 ℃ and repeatedly evaporating until the microcrystalline boron glass powder is completely dissolved and the hydrofluoric acid is completely evaporated, finally adding (1: 1) 5ml of nitric acid into every 100ml of solution, adding water, carrying out water bath to dissolve, then fixing the volume, and cooling to room temperature to obtain a solution to be measured;
step 2: testing components in the standard solution by using a plasma spectrometer (ICP), wherein the sample is 400mg, the standard solution is adjusted to be a mannitol curve with the same concentration according to the components of the glass, namely, the standard solution is prepared by adding 400mg of mannitol, and a working curve is drawn; and obtaining the analysis data of the sample, and comparing and calculating the analysis data to obtain the specific content of the components of the solution to be detected.
The boron oxide content of the microcrystalline boron glass powder CG21-22-224 obtained in the embodiment is 2.43%.
Example 3
A method for measuring chemical components of microcrystalline boron glass comprises the following steps:
step 1: grinding the bulk microcrystalline boron glass by a grinder, setting the grinding time for 10min to obtain microcrystalline boron glass powder, and uniformly mixing 300mg of microcrystalline boron glass powder and 300mg of high-purity mannitol in a platinum pot to obtain a mixture; adding water to the mixture until the mixture is completely wetted; then adding hydrofluoric acid, carrying out water bath treatment at 90 ℃, and repeatedly evaporating until the microcrystalline boron glass powder is completely dissolved and the hydrofluoric acid is completely evaporated; finally, 5ml of nitric acid (1: 1) is added into every 100ml of solution, water bath is carried out for dissolving, then the volume is determined, and the solution to be measured is obtained after cooling to the room temperature;
step 2: and testing the components in the standard solution by using an Atomic Absorption Spectrometer (AAS) to obtain a 300mg sample, adjusting the standard solution to a mannitol curve with the same concentration according to the glass components, namely adding 300mg mannitol to prepare, drawing a working curve to obtain sample analysis data, and comparing and calculating the analysis data to obtain the specific content of the components in the solution to be tested.
The content of boron oxide in the microcrystalline boron glass powder of the CG31-22-214 sample obtained in the embodiment is 1.57%.
Example 4
A method for measuring chemical components of microcrystalline boron glass comprises the following steps:
step 1: grinding the bulk microcrystalline boron glass by a grinder, setting the grinding time for 10min to obtain microcrystalline boron glass powder, and uniformly mixing 200mg of microcrystalline boron glass powder and 200mg of high-purity mannitol in a platinum pot to obtain a mixture; adding water to the mixture until the mixture is completely infiltrated; then adding hydrofluoric acid, carrying out water bath treatment at 85 ℃, and repeatedly evaporating until the microcrystalline boron glass powder is completely dissolved and the hydrofluoric acid is completely evaporated; finally, 5ml of nitric acid (1: 1) is added into every 100ml of solution, water bath is carried out for dissolving, then the volume is determined, and the solution to be measured is obtained after cooling to the room temperature;
step 2: testing the components in the standard solution by using a plasma spectrometer (ICP), wherein the sample is 200mg, the standard solution is adjusted to be a mannitol curve with the same concentration according to the components of the glass, namely, 200mg of mannitol is added for preparation, and a working curve is drawn; and obtaining the analysis data of the sample, and comparing and calculating the analysis data to obtain the specific content of the components of the solution to be detected.
The content of boron oxide in the sample of the microcrystalline boron glass powder HW70 obtained in the embodiment is 4.03%.
Example 5
A method for measuring chemical components of microcrystalline boron glass comprises the following steps:
step 1: grinding the large-block microcrystalline boron glass by a grinder, setting the grinding time for 10min to obtain microcrystalline boron glass powder, and uniformly mixing 100mg of microcrystalline boron glass powder and 100mg of high-purity mannitol in a platinum pot to obtain a mixture; adding water to the mixture until the mixture is completely infiltrated; then adding hydrofluoric acid, carrying out water bath treatment at 80 ℃, and repeatedly evaporating until the microcrystalline boron glass powder is completely dissolved and the hydrofluoric acid is completely evaporated; finally, 5ml of nitric acid (1: 1) is added into every 100ml of solution, water bath is carried out for dissolving, then the volume is determined, and the solution to be measured is obtained after cooling to the room temperature;
step 2: testing the components in the standard solution by using a plasma spectrometer (ICP), wherein the sample is 100mg, the standard solution is adjusted to be a mannitol curve with the same concentration according to the components of the glass, namely, 100mg of mannitol is added for preparation, and a working curve is drawn; and obtaining the analysis data of the sample, and comparing and calculating the analysis data to obtain the specific content of the components of the solution to be detected.
The content of boron oxide in the microcrystalline boron glass powder CG707 obtained in the embodiment is 4.70%.
Example 6
A method for measuring the chemical components of microcrystalline boron glass comprises the following steps:
step 1: grinding the massive microcrystalline boron glass by a grinder, setting the grinding time for 20min to obtain microcrystalline boron glass powder, and uniformly mixing 100mg of microcrystalline boron glass powder and 50mg of high-purity mannitol in a platinum pot to obtain a mixture; adding water to the mixture until the mixture is completely infiltrated; then adding hydrofluoric acid, carrying out water bath treatment at 100 ℃, and repeatedly evaporating until the microcrystalline boron glass powder is completely dissolved and the hydrofluoric acid is completely evaporated; finally, 5ml of nitric acid (1: 1) is added into every 100ml of solution, water bath is carried out for dissolving, then the volume is determined, and the solution to be measured is obtained after cooling to the room temperature;
step 2: testing components in the standard solution by adopting a plasma spectrometer (ICP) to obtain a 100mg sample, adjusting the standard solution to a mannitol curve with the same concentration according to glass components, namely adding 50mg mannitol to prepare, and drawing a working curve; and obtaining the analysis data of the sample, and comparing and calculating the analysis data to obtain the specific content of the components of the solution to be detected.
Example 7
A method for measuring chemical components of microcrystalline boron glass comprises the following steps:
step 1: grinding the massive microcrystalline boron glass by a grinder, setting the grinding time for 30min to obtain microcrystalline boron glass powder, and uniformly mixing 100mg of microcrystalline boron glass powder and 400mg of high-purity mannitol in a platinum pot to obtain a mixture; adding water to the mixture until the mixture is completely wetted; then adding hydrofluoric acid, carrying out water bath treatment at 90 ℃, and repeatedly evaporating until the microcrystalline boron glass powder is completely dissolved and the hydrofluoric acid is completely evaporated; finally, 5ml of nitric acid (1: 1) is added into every 100ml of solution, water bath is carried out for dissolving, then the volume is determined, and the solution to be measured is obtained after cooling to the room temperature;
step 2: testing the components in the standard solution by using a plasma spectrometer (ICP), wherein the sample is 100mg, the standard solution is adjusted to be a mannitol curve with the same concentration according to the components of the glass, namely, 400mg of mannitol is added for preparation, and a working curve is drawn; and obtaining the analysis data of the sample, and comparing and calculating the analysis data to obtain the specific content of the components of the solution to be detected.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (8)
1. The method for measuring the chemical components of the microcrystalline boron glass is characterized by comprising the following steps of:
step 1: firstly, uniformly mixing microcrystalline boron glass powder and mannitol to obtain a mixture; adding water to the mixture until the mixture is completely wetted; then adding hydrofluoric acid, performing water bath treatment, and repeatedly evaporating until the microcrystalline boron glass powder is completely dissolved and the hydrofluoric acid is completely evaporated; finally, adding nitric acid and water, carrying out water bath constant-temperature solution and constant volume to obtain a solution to be detected;
step 2: and testing the components in the standard solution by using an analyzer, drawing a working curve, analyzing the solution to be tested by using the analyzer in the same method for drawing the working curve to obtain analysis data, and comparing and calculating the analysis data and the working curve to obtain the specific content of the components in the solution to be tested.
2. The method for measuring chemical components of microcrystalline boron glass according to claim 1, wherein in step 1, the dosage ratio of the microcrystalline boron glass powder to mannitol is (1: 0.5): (1:2).
3. The method for measuring the chemical composition of the microcrystalline boron glass according to claim 1, wherein the temperature of the water bath treatment in step 1 is 80 ℃ to 100 ℃.
4. The method for measuring chemical composition of microcrystalline boron glass according to claim 1, wherein in step 1, the ratio of the amount of nitric acid to the amount of water is (1: 0.5) to (1: 5).
5. The method for measuring the chemical composition of the microcrystalline boron glass according to claim 1, wherein in the step 2, the standard solution comprises mannitol, and the concentration of the mannitol in the standard solution is consistent with that of the mannitol in the solution to be measured.
6. The method for measuring the chemical composition of the microcrystalline boron glass according to claim 5, wherein in the step 2, the concentration of the solution to be measured is consistent with the concentration of mannitol in the standard solution.
7. The method for measuring the chemical components of the microcrystalline boron glass according to claim 1, wherein in the step 1, the microcrystalline boron glass powder is prepared by grinding bulk microcrystalline boron glass by a grinder, and the grinding time is 10-30 min.
8. The method for determining the chemical composition of the microcrystalline boron glass according to claim 1, wherein in the step 2, the analytical instrument comprises an atomic absorption spectrometer and a plasma spectrometer.
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| CN104535557A (en) * | 2014-11-25 | 2015-04-22 | 内蒙古包钢钢联股份有限公司 | Dissolving method for boron in mold powder and determination method for boron content |
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| CN104535557A (en) * | 2014-11-25 | 2015-04-22 | 内蒙古包钢钢联股份有限公司 | Dissolving method for boron in mold powder and determination method for boron content |
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| 王虹;沙德仁;周亚红;: "电感耦合等离子体原子发射光谱法测定玻璃中硼", 理化检验(化学分册), no. 12, 18 December 2010 (2010-12-18), pages 1386 - 1388 * |
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| CN115856198A (en) * | 2022-11-22 | 2023-03-28 | 甘肃旭盛显示科技有限公司 | Method for detecting boron oxide in OLED glass carrier plate |
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