CN116577318A - Method for detecting tungsten element of coating in ternary material - Google Patents
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- 239000000463 material Substances 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 43
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 28
- 239000010937 tungsten Substances 0.000 title claims abstract description 28
- 239000011248 coating agent Substances 0.000 title claims abstract description 16
- 238000000576 coating method Methods 0.000 title claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 76
- 239000002253 acid Substances 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 238000012360 testing method Methods 0.000 claims abstract description 21
- 239000012086 standard solution Substances 0.000 claims abstract description 16
- 238000001514 detection method Methods 0.000 claims abstract description 14
- 239000011159 matrix material Substances 0.000 claims abstract description 13
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 13
- 239000012498 ultrapure water Substances 0.000 claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 11
- 239000010439 graphite Substances 0.000 claims abstract description 11
- 238000005303 weighing Methods 0.000 claims abstract description 9
- 238000002133 sample digestion Methods 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000007865 diluting Methods 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 42
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 32
- -1 polytetrafluoroethylene Polymers 0.000 claims description 24
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 24
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 24
- 230000029087 digestion Effects 0.000 claims description 22
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 claims description 5
- 238000011010 flushing procedure Methods 0.000 claims description 4
- 238000009616 inductively coupled plasma Methods 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000012898 sample dilution Substances 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 238000007781 pre-processing Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 6
- 238000000120 microwave digestion Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- 239000004033 plastic Substances 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 7
- 238000011084 recovery Methods 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000010668 complexation reaction Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 150000007524 organic acids Chemical class 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000011975 tartaric acid Substances 0.000 description 2
- 235000002906 tartaric acid Nutrition 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- HFCVPDYCRZVZDF-UHFFFAOYSA-N [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O Chemical compound [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O HFCVPDYCRZVZDF-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical class 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
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 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
- 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
-
- 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
- G01N1/38—Diluting, dispersing or mixing samples
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Plasma & Fusion (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Engineering & Computer Science (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a method for detecting tungsten element of a coating in a ternary material, which comprises the following steps: step 1: preparing a standard solution: preparing a plurality of plastic volumetric flasks, adding a mixed acid solution, and then adding tungsten standard solution and matrix solution with different volumes; step 2: sample pretreatment: weighing a ternary material sample to be measured in a beaker; transferring the mixed acid solution A into a beaker; step 3: sample digestion: and placing the sample in a graphite heating plate to be digested for a certain time until the solution in the beaker is in a clear state. Step 4: diluting and fixing the volume of a sample: adding ultrapure water into the beaker, and fixing the volume to obtain a solution to be measured; step 5: and (3) detection: and cleaning by using a mixed acid solution, and testing the solution to be tested, so that the content of the doped W element in the ternary material sample to be tested is obtained. The invention has the advantages that: according to the method, the material is digested by using the co-mixed acid system, so that the microwave digestion effect can be achieved, and the impurity elements introduced in the testing process can be reduced.
Description
Technical Field
The invention relates to a method for detecting tungsten element of a coating in a ternary material.
Background
The amount ratio of substances of nickel, cobalt and manganese in the nickel cobalt lithium manganate ternary positive electrode material has great influence on the crystal structure of the material and the capacity of the battery. As the nickel content increases, the corresponding material capacity can also increase, but the structure of the material becomes unstable. In the prior art, the method of doping and coating other elements (such as aluminum, zirconium, boron and the like) is often adopted to ensure the stability of the material structure. In the latest technology, tungsten (W) is added in the doped elements, tungsten precipitates are easy to generate in a conventional acid (hydrochloric acid and nitric acid) system, W in a free state changes, and the test fluctuation is large, so that the tungsten content in the ternary material is necessary to be detected. Wherein, patent CN201711287834.5 is a method for measuring the content of silicon, manganese, iron and tungsten in cobalt-based alloy, which is limited by the purchase unit price of microwave digestion equipment reaching about 40 ten thousand, and has higher detection cost; secondly, adding boric acid solution tends to introduce B element into the sample, which is unfavorable for detecting the B content existing in the sample. In the scheme of a tungsten-analysis laboratory for measuring tungsten ores by an ICP-AES method, in the year of 2008, volume 27, naOH is required to be introduced as a medium, but in the digestion process of ternary materials, an acid medium is adopted, so that certain reaction can occur, meanwhile, a precipitation phenomenon can occur when a NaOH solution is added into a ternary material solution after digestion by acid, and the method is not suitable for use of ternary materials. Document "method for determining tungsten in tungsten catalyst by tartaric acid complexation method and citric acid complexation method" compares, gansu technology, 11 months in 2020, 36 th volume, 22 nd phase ", and organic acid is added into sample to be tested for complexation. Because the ternary material is used for the production of automobile batteries, the requirement on impurity control is very high, and an organic acid solution is added into a sample to be measured, so that the accurate measurement of the impurity content of the sample is not facilitated. Meanwhile, the W element in the material is usually a complex anion [ WO 4 ] 2- Is present in the form of (c). During digestion of the sample, a large amount of hydrochloric acid is added so that [ WO 4 ] 2- With H in hydrochloric acid + H is produced by the reaction 2 WO 4 Precipitation, so that the solution sample is uneven, and the detection result fluctuates greatly; if inThe organic acid is difficult to solve in the process of sample digestion due to high temperature digestion and volatilization of hydrochloric acid 4 ] 2- Complexing.
Disclosure of Invention
The invention aims to provide a method for detecting tungsten element of a coating in a ternary material, which utilizes a co-mixed acid system to digest materials, so that the effect of microwave digestion can be achieved, and impurity elements introduced in the testing process can be reduced.
The aim of the invention is realized by the following technical scheme: a method for detecting tungsten element of coating in ternary material comprises the following steps:
step 1: preparing standard solution
Preparing a plurality of plastic volumetric flasks, adding about 11% of mixed acid solution into each volumetric flask, and then adding tungsten standard solution and matrix solution with different volumes into each volumetric flask respectively; fixed volume for standby;
step 2: sample pretreatment
Weighing a ternary material sample to be measured in a polytetrafluoroethylene beaker; the mixed acid solution A is moved into a polytetrafluoroethylene beaker, and is gently shaken, so that materials in the polytetrafluoroethylene beaker are completely dissolved;
step 3: sample digestion
Setting heating temperature and heating time by using a graphite heating plate, and placing a sample in the graphite heating plate to digest for a certain time until the solution in the polytetrafluoroethylene beaker is in a clear state; at the moment, ultrapure water is used for flushing the inner wall of the beaker, so that the phenomenon that materials are not digested is prevented.
Step 4: sample dilution constant volume
After digestion in the step 3 is completed, adding ultra-pure water into a polytetrafluoroethylene beaker to accelerate the temperature reduction of the solution, transferring the solution to a plastic volumetric flask after the solution is cooled to room temperature, and uniformly shaking to obtain a solution to be measured;
step 5: detection of
And cleaning a sample injection system of an inductively coupled plasma emission spectrometer (ICP-OES) by using a 1% mixed acid solution, testing a standard solution after cleaning, and testing a solution to be tested after testing, thereby obtaining the content of the doped W element in the ternary material sample to be tested.
Preferably, the specific method for preparing the standard solution in the step 1 is as follows: 4 volumetric flasks of 100mL were prepared, and 10mL of hydrochloric acid (hydrochloric acid concentration 36% -38%) and 1mL of hydrofluoric acid (hydrofluoric acid concentration > 40%) were added to the volumetric flasks. Then respectively adding 0mL, 0.4mL, 1.2mL and 2.0mL of tungsten standard solution with the concentration of 1000 mug/mL into each volumetric flask; and then 10mL of ternary sample matrix solution is respectively added into each volumetric flask, and the volumetric flask is fixed for later use. (by introducing the matrix solution, the recovery rate of the sample is improved)
Preferably, the preparation method of the ternary sample matrix solution comprises the following steps: accurately weighing 4+/-0.004 g of ternary sample (without W element) in a polytetrafluoroethylene beaker, adding 20-45mL of concentrated hydrochloric acid and 1-3mL of hydrofluoric acid, digesting for 1-2 hours at 200-280 ℃, transferring the solution after the digestion is completed, and fixing the volume to 100mL for later use. As a matrix solution.
Preferably, the specific method for preprocessing the sample in the step 2 is as follows: weighing 0.4+/-0.004 g of ternary material sample to be measured in a 150mL polytetrafluoroethylene beaker, then using a bottleneck liquid distributor to move about 10-20mL of mixed acid solution A into the polytetrafluoroethylene beaker, slightly shaking, dissolving the material stuck on the inner wall of the beaker into the solution, and completely dissolving the material in the polytetrafluoroethylene beaker.
Preferably, the mixed acid solution A is a mixture of concentrated hydrochloric acid, hydrofluoric acid and water; the concentrated hydrochloric acid is of AR grade, and the hydrofluoric acid is of MOS grade;
the preparation method of the mixed acid solution A comprises the following steps: 3-3.5L of concentrated hydrochloric acid (AR grade) and 300-400mL of hydrofluoric acid (MOS grade) are added into a 5L PP container, and then ultrapure water is added into the container to prepare 5L of solution.
Preferably, the specific operation method of the digestion of the sample in the step 3 is as follows: and (3) using a graphite heating plate, setting the heating temperature to be 225-235 ℃ and the heating time to be 1h, putting the sample in the graphite heating plate for digestion, and after 20-30 minutes of digestion, flushing the inner wall of the beaker by using ultrapure water at the moment to prevent the non-digestion phenomenon of the materials.
Preferably, the specific operation method of diluting the sample to a constant volume in the step 4 is as follows: after digestion in the step 3 is completed, adding ultra-pure water into a polytetrafluoroethylene beaker, accelerating the temperature reduction of the solution, transferring the solution to a 100mL volumetric flask after the solution is cooled to room temperature, fixing the volume, and shaking uniformly to obtain the solution to be measured.
Compared with the prior art, the invention has the advantages that: according to the method for detecting the tungsten element of the coating in the ternary material, disclosed by the invention, the material is digested by using the mixed acid system, so that the effect of microwave digestion can be achieved, and the impurity elements introduced in the testing process can be reduced. In addition, the detection method of the invention is used for repeatedly testing the same sample (ternary material), and the tested data show that the repeatability level is within 0.5%, the solution state is stable, and no obvious change exists between different days, so that the detection method of the invention is stable and reliable. Through verification of the recovery rate, the recovery rate reaches 95-105%. The detection method maintains a ternary common inorganic acid system without introducing a NaOH alkali system; no microwave digestion equipment is required to be introduced, and meanwhile, B element is not required to be introduced, so that the interference on a sample is prevented; the tartaric acid solution is not required to be introduced into the sample to be detected, and the risk of introducing impurity elements is increased, so that the authenticity of the sample detection is affected.
Detailed Description
The following describes the present invention in detail with reference to examples:
example 1:
a method for detecting tungsten element of coating in ternary material comprises the following steps:
step 1: preparing standard solution
The specific method for preparing the standard solution in the step 1 is as follows: 4 volumetric flasks of 100mL were prepared, and 10mL of hydrochloric acid (hydrochloric acid concentration 36% -38%) and 1mL of hydrofluoric acid (hydrofluoric acid concentration > 40%) were added to the volumetric flasks. Then respectively adding 0mL, 0.4mL, 1.2mL and 2.0mL of tungsten standard solution with the concentration of 1000 mug/mL into each volumetric flask; and then 10mL of ternary sample matrix solution is respectively added into each volumetric flask, and the volumetric flask is fixed for later use. (by introducing the matrix solution, the recovery rate of the sample is improved)
The preparation method of the ternary sample matrix solution comprises the following steps: accurately weighing 4+/-0.004 g ternary sample without W element in a 150mL quartz beaker, adding 45mL concentrated hydrochloric acid, digesting for 1-2 hours at 200-280 ℃, transferring the solution after the digestion is completed, and fixing the volume to 100mL for later use.
Step 2: sample pretreatment
Weighing 0.4+/-0.004 g of ternary material sample to be measured in a 150mL polytetrafluoroethylene beaker, then using a bottleneck liquid distributor to move about 10-20mL of mixed acid solution A into the polytetrafluoroethylene beaker, slightly shaking, dissolving the material stuck on the inner wall of the beaker into the solution, and completely dissolving the material in the polytetrafluoroethylene beaker.
The mixed acid solution A is a mixture of concentrated hydrochloric acid, hydrofluoric acid and water; the concentrated hydrochloric acid is of AR grade, and the hydrofluoric acid is of MOS grade;
the preparation method of the mixed acid solution A comprises the following steps: 3-3.5L of concentrated hydrochloric acid (AR grade) and 300-400mL of hydrofluoric acid (MOS grade) are added into a 5L PP container, and then ultrapure water is added into the container to prepare 5L of solution.
Step 3: sample digestion
And (3) using a graphite heating plate, setting the heating temperature to be 225-235 ℃ and the heating time to be 1h, putting the sample in the graphite heating plate for digestion, and after 20-30 minutes of digestion, flushing the inner wall of the beaker by using ultrapure water at the moment to prevent the non-digestion phenomenon of the materials.
Step 4: sample dilution constant volume
After digestion in the step 3 is completed, adding ultra-pure water into a polytetrafluoroethylene beaker, accelerating the temperature reduction of the solution, transferring the solution to a 100mL volumetric flask after the solution is cooled to room temperature, fixing the volume, and shaking uniformly to obtain the solution to be measured.
Step 5: detection of
And testing the standard solution by using an inductively coupled plasma emission spectrometer (ICP-OES), and testing the solution to be tested after testing, thereby obtaining the content of the doped W element in the ternary material sample to be tested.
The same sample (ternary material) was subjected to repeated tests based on the above detection method, and the data of the tests are shown in table 1. As can be seen from the data shown in the table below, the repeatability level RSD of the detection method of the invention can reach 0.09%, which shows that the detection method of the invention is stable and reliable.
TABLE 1 repeated test results for the same sample
From the above data, the repeated test results of the same bottle of solution are stable, the relative standard deviation is less than 0.5%, and the detection data are stable. At the same time, the samples were left to stand overnight for testing without significant deviation in data.
Embodiment two: comparison of recovery data
It should be noted that the foregoing description is only a preferred embodiment of the present invention, and although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood that modifications, equivalents, improvements and modifications to the technical solution described in the foregoing embodiments may occur to those skilled in the art, and all modifications, equivalents, and improvements are intended to be included within the spirit and principle of the present invention.
Claims (7)
1. A method for detecting tungsten element of coating in ternary material is characterized in that: it comprises the following steps:
step 1: preparing standard solution
Preparing a plurality of volumetric flasks, adding a certain amount of hydrochloric acid and hydrofluoric acid into each volumetric flask, and then respectively adding tungsten standard solutions with different volumes into each volumetric flask; then adding an equal amount of ternary sample matrix solution into each volumetric flask respectively, and fixing the volume for later use;
step 2: sample pretreatment
Weighing a ternary material sample to be measured in a polytetrafluoroethylene beaker; the mixed acid solution A is moved into a polytetrafluoroethylene beaker, and is gently shaken, so that materials in the polytetrafluoroethylene beaker are completely dissolved;
step 3: sample digestion
Setting heating temperature and heating time by using a graphite heating plate, and placing a sample in the graphite heating plate to digest until the solution in the polytetrafluoroethylene beaker is in a clear state;
step 4: sample dilution constant volume
After digestion in the step 3 is completed, adding ultra-pure water into a polytetrafluoroethylene beaker to accelerate the cooling of the solution, transferring the solution into a volumetric flask after the solution is cooled to room temperature, and uniformly shaking to obtain a solution to be measured;
step 5: detection of
Testing a standard solution by using an inductively coupled plasma emission spectrometer ICP-OES, and cleaning and testing a sample injection system of the inductively coupled plasma emission spectrometer ICP-OES by using a 1% mixed acid solution before testing; and then testing the solution to be tested, so as to obtain the content of the doped W element in the ternary material sample to be tested.
2. The method for detecting tungsten element in coating in ternary material according to claim 1, wherein the method comprises the following steps:
the specific method for preparing the standard solution in the step 1 is as follows: preparing 4 volumetric flasks of 100mL, adding 10mL of hydrochloric acid and 1mL of hydrofluoric acid into the volumetric flasks, wherein the concentration of the hydrochloric acid is 36% -38%, and the concentration of the hydrofluoric acid is more than 40%; then respectively adding 0mL, 0.4mL, 1.2mL and 2.0mL of tungsten standard solution with the concentration of 1000 mug/mL into each volumetric flask; and then 10mL of ternary sample matrix solution is respectively added into each volumetric flask, and the volumetric flask is fixed for later use.
3. The method for detecting tungsten element in a coating in a ternary material according to claim 1 or 2, wherein the method comprises the following steps: the preparation method of the ternary sample matrix solution comprises the following steps:
accurately weighing 4+/-0.004 g of ternary sample (without W element) in a polytetrafluoroethylene beaker, adding 20-45mL of concentrated hydrochloric acid and 1-3mL of hydrofluoric acid, digesting for 1-2 hours at 200-280 ℃, transferring the solution after digestion, and fixing the volume to 100mL for later use, and taking the solution as a matrix solution.
4. The method for detecting tungsten element in coating in ternary material according to claim 1, wherein the method comprises the following steps:
the specific method for preprocessing the sample in the step 2 is as follows: weighing 0.4+/-0.004 g of ternary material sample to be measured in a 150mL polytetrafluoroethylene beaker, then using a bottleneck liquid separator to remove 10-20mL of mixed acid solution A into the polytetrafluoroethylene beaker, slightly shaking, dissolving the material adhered to the inner wall of the beaker into the solution, and completely dissolving the material in the polytetrafluoroethylene beaker.
5. The method for detecting tungsten element in coating in ternary material according to claim 1 or 4, wherein the method comprises the following steps: the preparation method of the mixed acid solution A specifically comprises the following steps: 3-3.5L of concentrated hydrochloric acid and 300-400mL of hydrofluoric acid are added into a PP container made of 5L of PP material, and then ultrapure water is added into the mixture to prepare 5L of solution.
6. The method for detecting tungsten element in coating in ternary material according to claim 1, wherein the method comprises the following steps:
the specific operation method for digesting the sample in the step 3 is as follows: and (3) using a graphite heating plate, setting the heating temperature to be 225-235 ℃ and the heating time to be 1h, putting the sample in the graphite heating plate for digestion, and after 20-30 minutes of digestion, flushing the inner wall of the beaker by using ultrapure water at the moment to prevent the non-digestion phenomenon of the materials.
7. The method for detecting tungsten element in coating in ternary material according to claim 1, wherein the method comprises the following steps:
the specific operation method of diluting and fixing the volume of the sample in the step 4 is as follows: after digestion in the step 3 is completed, adding ultra-pure water into a polytetrafluoroethylene beaker, accelerating the temperature reduction of the solution, transferring the solution to a 100mL volumetric flask after the solution is cooled to room temperature, fixing the volume, and shaking uniformly to obtain the solution to be measured.
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