CN116699057A - Chemical analysis method for strontium oxide content - Google Patents
Chemical analysis method for strontium oxide content Download PDFInfo
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- CN116699057A CN116699057A CN202310717852.1A CN202310717852A CN116699057A CN 116699057 A CN116699057 A CN 116699057A CN 202310717852 A CN202310717852 A CN 202310717852A CN 116699057 A CN116699057 A CN 116699057A
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- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000009614 chemical analysis method Methods 0.000 title claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 34
- 239000011521 glass Substances 0.000 claims abstract description 32
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 30
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 27
- 239000012086 standard solution Substances 0.000 claims abstract description 23
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 22
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 22
- 239000007853 buffer solution Substances 0.000 claims abstract description 19
- AMMWFYKTZVIRFN-UHFFFAOYSA-N sodium 3-hydroxy-4-[(1-hydroxynaphthalen-2-yl)diazenyl]-7-nitronaphthalene-1-sulfonic acid Chemical compound [Na+].C1=CC=CC2=C(O)C(N=NC3=C4C=CC(=CC4=C(C=C3O)S(O)(=O)=O)[N+]([O-])=O)=CC=C21 AMMWFYKTZVIRFN-UHFFFAOYSA-N 0.000 claims abstract description 19
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 17
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 12
- 238000004458 analytical method Methods 0.000 claims abstract description 11
- CEQFOVLGLXCDCX-WUKNDPDISA-N methyl red Chemical compound C1=CC(N(C)C)=CC=C1\N=N\C1=CC=CC=C1C(O)=O CEQFOVLGLXCDCX-WUKNDPDISA-N 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001704 evaporation Methods 0.000 claims abstract description 4
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 4
- 239000000779 smoke Substances 0.000 claims abstract description 4
- SGHZXLIDFTYFHQ-UHFFFAOYSA-L Brilliant Blue Chemical compound [Na+].[Na+].C=1C=C(C(=C2C=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=2C(=CC=CC=2)S([O-])(=O)=O)C=CC=1N(CC)CC1=CC=CC(S([O-])(=O)=O)=C1 SGHZXLIDFTYFHQ-UHFFFAOYSA-L 0.000 claims abstract description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 16
- 235000019270 ammonium chloride Nutrition 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 4
- 238000007865 diluting Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 2
- 239000000523 sample Substances 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 12
- 238000002474 experimental method Methods 0.000 abstract description 3
- 238000004448 titration Methods 0.000 description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 9
- 229910000018 strontium carbonate Inorganic materials 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000005388 borosilicate glass Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229910001427 strontium ion Inorganic materials 0.000 description 3
- IPWGBWXYYLCOLW-UHFFFAOYSA-N 3-(2-methylphenyl)-3h-2-benzofuran-1-one Chemical compound CC1=CC=CC=C1C1C2=CC=CC=C2C(=O)O1 IPWGBWXYYLCOLW-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 238000003926 complexometric titration Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000010561 standard procedure Methods 0.000 description 2
- 239000012085 test solution Substances 0.000 description 2
- 238000004876 x-ray fluorescence Methods 0.000 description 2
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 1
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
-
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a chemical analysis method for strontium oxide content, which belongs to the technical field of detection and analysis and comprises the following steps: s1, adding a glass sample into a platinum crucible, adding hydrofluoric acid, heating until the mixture is nearly evaporated to dryness, adding the hydrofluoric acid and perchloric acid, continuously evaporating until no white smoke is generated, adding a nitric acid solution, heating until residues are completely dissolved, and adding water to dilute the mixture to obtain a sample to be tested; s2, adding a sample to be tested into a container, dropwise adding methyl red, adding an ammonia water solution to neutralize to yellow, then adding water, a magnesium chloride solution, a pH=10 buffer solution and a chrome black T indicator, titrating to a brilliant blue by using an EDTA standard solution as an end point, and recording a consumption volume V1; and S3, mixing a magnesium chloride solution, water, a pH=10 buffer solution and a chrome black T indicator, titrating to a light blue color by using an EDTA standard solution as an end point, and recording the consumption volume V0. The method has the advantages of simple experiment, strong operability and high repeated stability.
Description
Technical Field
The invention belongs to the technical field of detection and analysis, and particularly relates to a chemical analysis method for strontium oxide content.
Background
The development of new glass is more and more remarkable for the glass industry, and SrO is a constituent component of most new glass, and the important significance of SrO is attracting attention. The alkaline earth metal oxide SrO can improve the strain point and Young's modulus of glass, reduce the thermal expansion coefficient, and effectively reduce the high-temperature viscosity of glass so as to improve the meltability and formability of the glass, but when the content is too high, secondary bubbles appear in clarification, and the density of the glass is increased. Therefore, how to rapidly and accurately detect the strontium oxide content in the glass is an important link in the current detection technical field. Since strontium oxide is used as a novel raw material in glass production, no widely used method for detecting strontium oxide in glass is currently available, which has an influence on the control and adjustment of glass components.
In order to solve the problems, the invention designs a chemical analysis method for the strontium oxide content, which is simple and has strong operability, can rapidly analyze the strontium oxide content in glass, and is greatly helpful for replacing the glass material or adjusting the components.
Disclosure of Invention
The invention aims to provide a chemical analysis method for strontium oxide content, which aims to solve the problem that the method for detecting strontium oxide in glass is not widely applied.
The aim of the invention can be achieved by the following technical scheme:
a method for chemical analysis of strontium oxide content comprising the steps of:
s1, adding a glass sample into a platinum crucible, adding hydrofluoric acid, setting the temperature to be 250-280 ℃, adding hydrofluoric acid and perchloric acid when the temperature is close to dryness by evaporation, continuing to evaporate until no white smoke is generated, adding a nitric acid solution, heating until residues are completely dissolved, and adding water to dilute the mixture to obtain a sample to be tested;
s2, adding a sample to be tested into a container, dropwise adding methyl red, adding an ammonia water solution to neutralize to yellow, then adding water, a magnesium chloride solution, a pH=10 buffer solution and a chrome black T indicator, titrating to a brilliant blue by using an EDTA standard solution as an end point, and recording a consumption volume V1;
and S3, mixing a magnesium chloride solution, water, a pH=10 buffer solution and a chrome black T indicator, titrating to a light blue color by using an EDTA standard solution as an end point, and recording the consumption volume V0.
According to the formulaAnd calculating the strontium oxide content. Wherein, the concentration of the C-EDTA standard solution in the formula; v1-consume the volume of EDTA standard solution, mL during titration; v0-blank consumes the volume, mL, of EDTA standard solution; m-weight of sample, g; molar mass of M-strontium oxide, g/mol,103.62g/mol.
Further, the ph=10 buffer solution was prepared by the following steps:
weighing ammonium chloride, dissolving in water, adding an ammonia water solution, and diluting with water to obtain a pH=10 buffer solution, wherein the dosage ratio of the ammonium chloride, the water and the ammonia water solution is 67.5g:570mL:1000mL, the ammonia solution is formed by mixing concentrated ammonia water with mass fraction of 25.0% -28.0% with pure water in equal volume.
Further, the ratio of the amounts of the glass sample, hydrofluoric acid, perchloric acid and nitric acid solution in S1 was 0.4000g:30mL:1mL:10mL; the volume ratio of hydrofluoric acid added in batches is 2:1.
further, 250mL of a test sample was prepared per 0.4g of glass sample.
Further, the mass fraction of hydrofluoric acid in S1 is 40%; the mass fraction of perchloric acid is 70.0-72.0%; the nitric acid solution is prepared by mixing concentrated nitric acid with the mass fraction of 65.0-68.0% and pure water with the same volume.
Further, the dosage ratio of the sample to be tested in S2, methyl red, water, magnesium chloride solution, ph=10 buffer solution, and chrome black T indicator is 25mL:1 drop: 30mL:10mL:10mL:1 drop; in S3, the dosage ratio of the magnesium chloride solution, water, ph=10 buffer solution and chrome black T indicator is 10mL:30mL:10mL:1 drop; wherein the ammonia water solution is formed by mixing concentrated ammonia water with the mass fraction of 25.0% -28.0% with pure water in equal volume.
Further, the concentration of methyl red was 1g/L, the concentration of magnesium chloride solution was 0.025mol/L, and the mass fraction of the chrome black T indicator was 1%.
The invention has the beneficial effects that:
the invention solves the problem that the prior detection standard lacks a chemical analysis method for the strontium oxide content in glass. The chemical analysis method of the strontium oxide content designed by the invention is used for preprocessing a sample to be detected by using a detection method, and rapidly analyzing the strontium oxide content and the high-purity strontium carbonate main content in glass by using the method, thereby being greatly helpful for replacing the glass material or adjusting the components. Meanwhile, the method is simple in experiment, high in operability and high in repeated stability.
According to the chemical analysis method of strontium oxide, disclosed by the invention, based on the principle of EDTA complexometric titration, namely, under the condition of pH=10, an EDTA solution is used for complexometric titration of strontium ions, and firstly, the strontium ions in the solution to be detected and chrome black T are used as an indicator to generate purple or purple complex, and the stability of the complex is inferior to that of the complex formed by the complex and the EDTA solution, so that when the EDTA solution is used for dripping, the strontium ions are separated from the complex of the indicator and then combined with EDTA, the solution changes from reddish wine to blue, and finally, the end point is reached. The magnesium salt is added in the titration process, so that the color reaction of the indicator is more obvious; the invention has obvious color judgment and color change transition at the titration end point, and can not cause excessive titration. The titration process of the invention can not influence the strontium content due to other elements, and the titration result is accurate. The method of the invention can be used for titration of the strontium oxide content in glass and titration of the main content in high-purity strontium carbonate.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Preparation of chemical reagents:
hydrochloric acid solution: mixing 36.0-38.0% of concentrated hydrochloric acid and the equal volume of pure water.
Aqueous ammonia solution: mixing 25.0% -28.0% of concentrated ammonia water and the equal volume of pure water.
Methyl red: 0.10g of methyl red is weighed and dissolved in ethanol, and then the volume is fixed to 100mL.
0.025mol/L magnesium chloride solution: 2.3802g of the mixture is weighed, added with pure water for dissolution, and the mixture is put into a 1000mL volumetric flask for constant volume and shaking for later use.
Chrome black T indicator: 0.50g of chrome black T and 4.5g of hydroxylamine chloride were weighed, dissolved in ethanol, diluted to 100mL with ethanol and stored in a brown bottle.
ph=10 buffer solution: 67.5g of ammonium chloride was weighed and dissolved in a proper amount of water, 570mL of aqueous ammonia solution was added, and the mixture was diluted with water to 1000mL.
The nitric acid solution is prepared by mixing concentrated nitric acid with the mass fraction of 65.0-68.0% and pure water with the same volume.
The mass fraction of hydrofluoric acid is 40%, and the mass fraction of perchloric acid is 70.0-72.0%.
Example 1
The main component selected in this embodiment is SiO 2 % of 82.50%, al 2 O 3 % is 3.70%, srO% is 3.40%, B 2 O 3 10.40% borosilicate glass. The specific operation steps and detection data are as follows:
(1) Accurately weighing 0.4007g of glass sample in a platinum crucible, adding 20mL of hydrofluoric acid, heating on an electric furnace, setting the temperature to 250 ℃, adding 10mL of hydrofluoric acid and 1mL of perchloric acid before approaching to dryness, and evaporating until white smoke is exhausted. Adding 10mL of nitric acid solution, and heating until the residue is completely dissolved;
(2) Cooling, transferring into a 250mL volumetric flask, fixing the volume, and shaking uniformly for later use;
(3) Accurately transferring 25mL into an conical flask, adding 1 drop of methyl red, neutralizing to yellow by using an ammonia solution, adding 30mL of water, 10mL of magnesium chloride solution, 10mL of pH=10 buffer solution and 1 drop of chrome black T indicator, titrating to light blue by using an EDTA standard solution with known concentration of 0.01509mol/L purchased in the market as an end point, and recording the consumption volume V1;
(4) Blank experiment: taking 10mL of 0.025mol/L magnesium chloride solution in a 250mL triangular flask, adding 30mL of water, adding 10mL of pH=10 buffer solution and 1 drop of chrome black T indicator, titrating to light blue with EDTA standard solution with known concentration of 0.01516mol/L as an end point, and recording consumption volume V0;
wherein the concentration of the C-EDTA standard solution and the mol/L are the same; v1-consume the volume of EDTA standard solution, mL during titration; v0-blank consumes the volume, mL, of EDTA standard solution; m-weight of sample, g; molar mass of M-strontium oxide, g/mol,103.62g/mol:
by adopting the calculation method of the invention, the results of six titrations are counted, and the obtained results are shown in the following table 1:
TABLE 1
As shown in the test results, the titration results by the method of the invention show that the average value and the standard value are 3.40 percent, the error is 0.04 percent, the relative standard deviation is 0.0087, and each group of data is more stable.
Comparative example 1
The accuracy of the method of the present invention was verified by comparing the results of quantitative analysis of strontium oxide content in glass with the borosilicate glass samples used in the examples.
(1) And according to the operation rules of the X-ray fluorescence spectrum analyzer and based on borosilicate glass components, the range of each component is widened up and down, namely, glass sample wafers with different components are fused to establish a standard curve. The various standard ingredients are shown in table 2 below:
TABLE 2
The composition of the various standard samples and the composition of the borosilicate glass to be measured can be known, the glass to be measured has the composition within the curve interval range, and the linear correlation degree R of each element is approximately 0.99999, so that the measurement accuracy can be ensured.
(2) Sample preparation: and cutting the sample into glass samples with square sizes of 4cm and 4cm, and placing the glass samples in a sample box to be tested to perform curve component scanning. To verify its stability and accuracy, the number of scans was set to 6 and 2 sets of parallel swatches were separately cut and tested, with the following statistics:
TABLE 3 Table 3
TABLE 4 Table 4
As can be seen from the above tables 3 and 4, comparing the X-ray fluorescence spectrum analysis detection data with the detection data of the method of the present invention, it is easy to find that the detection data of the method of the present invention has relatively high accuracy, and can be used for detecting the strontium oxide content in glass.
Example 2
In this example, high-purity strontium carbonate with purity of 99.7% is selected for verification of example 1 and comparative example 1, and titration analysis is performed on the content of the high-purity strontium carbonate by adopting the method of the invention, and the specific implementation steps are as follows:
(1) Weighing 0.04g (0.0002 g) of sample (dried at 105-110deg.C) into a conical flask, adding small amount of distilled water, covering a surface dish, dripping 0.4mL of hydrochloric acid solution to dissolve sample until it is clear, adding water to 30mL, heating to boil, removingCO 2 Taking down the cooling (if there is sediment, filtering);
(2) Adding 1 drop of methyl red, neutralizing to yellow by using an ammonia solution, adding 30mL of water, 10mL of magnesium chloride solution, 10mL of pH=10 buffer solution and 1 drop of chrome black T indicator, titrating to light blue by using an EDTA standard solution with the concentration of 0.01516mol/L as an end point, and recording the consumption volume V1;
(3) Sample blank test: taking 10mL of magnesium chloride solution in a 250mL triangular flask, adding 30mL of water, adding 10mL of pH=10 buffer solution and 1 drop of chrome black T indicator, titrating to a light blue color by using an EDTA standard solution with the concentration of 0.01516mol/L as an end point, and recording the consumption volume V0;
(4) Calculating results, wherein: concentration of C-EDTA standard solution, mol/L; v1-consume the volume of EDTA standard solution, mL during titration; v0-blank consumes the volume, mL, of EDTA standard solution; m-weight of sample, g;
statistical six-titration data are described in table 5 below:
TABLE 5
The titration result by adopting the method provided by the invention shows that the average value and the standard value are 99.70%, the error is 0.01%, the relative standard deviation is 0.0001, and each group of data is relatively stable.
Comparative example 2
The titration analysis of the high-purity strontium carbonate content is carried out by adopting the method of the national standard HG/T4508-2013 high-purity strontium carbonate, and the titration analysis is compared with the method to verify the accuracy of the titration analysis result of the high-purity strontium carbonate content.
(1) Weighing about 0.8012g of a dried (105 ℃ +/-2 ℃) sample with constant mass, accurately measuring to 0.0002g, placing in a 100mL beaker, adding about 30mL of water, covering a surface dish, dropwise adding 3mL of hydrochloric acid solution until the sample is completely dissolved, heating and boiling to remove carbon dioxide, cooling, transferring all to a 250mL volumetric flask, diluting to a scale with pure water, and shaking uniformly for later use;
(2) Transferring 25mL of the solution by using a pipette, placing the solution in a 250mL conical flask, titrating about 20mL by using 0.01516mol/L EDTA standard solution, adding 15mL of ammonia water solution and 20mL of 95% ethanol, adding a proper amount of o-tolylphthalide complexing indicator-naphthol green B mixed indicator, titrating by using the EDTA standard solution until the solution is bright green as a terminal point, and recording the volume V1;
(3) 25mL of pure water is taken and placed in a 250mL conical flask, about 20mL of EDTA standard solution with the concentration of 0.01516mol/L is titrated, 15mL of ammonia water solution and 20mL of 95% ethanol are added, a proper amount of o-tolylphthalide complexing indicator-naphthol green B mixed indicator is added, 0.01516mol/L of EDTA standard solution is titrated until the solution is bright green, and the consumption volume V0 is recorded;
(4) Calculating the result, namely calculating the numerical value, mL, of the volume of the EDTA standard titration solution consumed by the V0-titration blank test solution; v1-titration of the numerical value of the volume of the disodium ethylenediamine tetraacetate standard titration solution consumed by the test solution, mL; accurate value of C-EDTA standard titration solution concentration, mol/L; m-sample mass, g; m-molar mass of strontium carbonate, g/mol, i.e. 147.62g/mol.
(5) The six titration data were counted as follows:
titration results using standard methods showed an average value of 99.70% from standard value, an error of 0.07% and a relative standard deviation of 0.0003. By comparing the detection result of the method with the detection result of the national standard, the detection method can be easily found to accurately detect the content of the high-purity strontium carbonate, and has advantages compared with the national standard method.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A method for chemical analysis of strontium oxide content, comprising the steps of:
s1, adding a glass sample into a platinum crucible, adding hydrofluoric acid, setting the temperature to be 250-280 ℃, adding hydrofluoric acid and perchloric acid when the temperature is close to dryness by evaporation, continuing to evaporate until no white smoke is generated, adding a nitric acid solution, heating until residues are completely dissolved, and adding water to dilute the mixture to obtain a sample to be tested;
s2, adding a sample to be tested into a container, dropwise adding methyl red, adding an ammonia water solution to neutralize to yellow, then adding water, a magnesium chloride solution, a pH=10 buffer solution and a chrome black T indicator, titrating to a brilliant blue by using an EDTA standard solution as an end point, and recording a consumption volume V1;
and S3, mixing a magnesium chloride solution, water, a pH=10 buffer solution and a chrome black T indicator, titrating to a light blue color by using an EDTA standard solution as an end point, and recording the consumption volume V0.
2. A method of chemical analysis of strontium oxide content according to claim 1, wherein the ph=10 buffer solution is prepared by:
weighing ammonium chloride, dissolving in water, adding an ammonia water solution, and diluting with water to obtain a pH=10 buffer solution, wherein the dosage ratio of the ammonium chloride, the water and the ammonia water solution is 67.5g:570mL:1000mL, the ammonia solution is formed by mixing concentrated ammonia water with mass fraction of 25.0% -28.0% with pure water in equal volume.
3. The method according to claim 1, wherein the ratio of the amounts of the glass sample, hydrofluoric acid, perchloric acid and nitric acid solution in S1 is 0.4000g:30mL:1mL:10mL; the volume ratio of hydrofluoric acid added in batches is 2:1.
4. a method of chemical analysis of strontium oxide content according to claim 1, wherein 250mL of test sample is prepared per 0.4g of glass sample.
5. The chemical analysis method of strontium oxide content according to claim 1, wherein the mass fraction of hydrofluoric acid in S1 is 40%; the mass fraction of perchloric acid is 70.0-72.0%; the nitric acid solution is prepared by mixing concentrated nitric acid with the mass fraction of 65.0-68.0% and pure water with the same volume.
6. The method for chemical analysis of strontium oxide content according to claim 1, wherein the ratio of the amount of the sample to be tested, methyl red, water, magnesium chloride solution, ph=10 buffer solution, chrome black T indicator in S2 is 25mL:1 drop: 30mL:10mL:10mL:1 drop; in S3, the dosage ratio of the magnesium chloride solution, water, ph=10 buffer solution and chrome black T indicator is 10mL:30mL:10mL:1 drop; wherein the ammonia water solution is formed by mixing concentrated ammonia water with the mass fraction of 25.0% -28.0% with pure water in equal volume.
7. A chemical analysis method for strontium oxide content according to claim 6, wherein the concentration of methyl red is 1g/L and the mass fraction of the chrome black T indicator is 1%.
8. A chemical analysis method for strontium oxide content according to claim 6, wherein the concentration of the magnesium chloride solution is 0.025mol/L.
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